WO2006106947A1

WO2006106947A1 - Abrasive base inhibited from reacting with fluorine compound and process for producing the same

Info

Publication number: WO2006106947A1
Application number: PCT/JP2006/306900
Authority: WO
Inventors: Kazuo Yasuzawa; Koichi Tokudome; Hiroshi Kobayashi
Original assignee: Tosoh Finechem Corporation
Priority date: 2005-04-04
Filing date: 2006-03-31
Publication date: 2006-10-12
Also published as: JP5443687B2; JPWO2006106947A1

Abstract

An abrasive base which is inhibited from reacting with NaF; and a process for producing the abrasive base. The process for abrasive base production comprises heating anhydrous calcium secondary phosphate in the presence of a magnesium compound and a polyphosphate. The amount of the magnesium compound to be present in terms of magnesium amount is in the range of 1,500-5,000 ppm of the anhydrous calcium secondary phosphate. The amount of the polyphosphate to be present is such that the molar ratio of the cation ingredient as a component of the polyphosphate to the magnesium in the magnesium compound is from 0.4/n to 12/n (wherein n is the valence of the cation ingredient). The heating is conducted at a temperature in the range of 100-300°C. The abrasive base contains magnesium and a polyphosphate and comprises, as the main component, anhydrous calcium secondary phosphate inhibited from reacting with a fluorine compound. The magnesium content is 1,500-5,000 ppm and the molar ratio of the cation ingredient contained as a component of the polyphosphate to the magnesium contained is from 0.4/n to 12/n.

Description

Specification

Polishing base with reduced reactivity with fluorine compound and method for producing the same

[0001] The present invention relates to a polishing base in which reactivity with a fluorine compound is suppressed and a method for producing the same.

Background art

[0002] Dicalcium phosphate (DCP) has been used for many years as a dentifrice polishing base. In Japanese Patent Publication No. 7-106970 (Patent Document 1), an average value force of crystallite size measured by X-ray diffractometry is obtained. Hydrocalcium hydrogen phosphate having crystallites of S200-3500 angstroms An abrasive substrate obtained by firing a Japanese product at a temperature of 70 ° C to 1200 ° C is disclosed. The invention described in this publication provides a polishing substrate that has a low polishing and high cleaning effect, is stable in a water suspension system, and prevents calcium ions from being eluted by water as much as possible. It is the purpose.

[0003] Further, in recent years, fluorinated agents are frequently used in toothpastes for preventing caries. Patent Document 1 describes a toothpaste containing an abrasive base material and Na monofluorophosphate (MFP) which is a fluorinating agent in Examples. However, dicalcium phosphate (DCP) reacts with F ions of fluorinating agent, especially Na fluoride (NaF), and impairs F's caries prevention effect. For this reason, dicalcium phosphate (DCP) is replaced by a silica agent with low reactivity with Na fluoride in toothpastes containing Na fluoride as a fluorinating agent.

[0004] Patent Document 1: Japanese Patent Publication No. 7-106970

Disclosure of the invention

Problems to be solved by the invention

[0005] Fluorinating agents for dentifrice mainly include Na monofluorophosphate (MFP) and Na fluoride (NaF), and NaF has a wide range of uses because of its rapid efficacy. On the other hand, as described above, toothpaste bases (such as DCP, calcium carbonate, and hydroxylated A1) other than siri force are highly reactive with NaF (reactive with F ions) and therefore contain NaF as a fluorine agent. The dentifrice was unusable. For this reason, when using a dentifrice base other than silica, an F ion gradual MFP is used. As described in Patent Document 1, calcium hydrogen phosphate 'anhydrate can be used only in combination with monofluorophosphate Na (MFP). However, since NaF is faster than MFP, in practice, toothpaste combining NaF and silica is the mainstream.

[0006] Under such circumstances, the development ability of dicalcium phosphate (DCP) capable of stably maintaining NaF for a long period of time when the reactivity with NaF, which is a fluorinating agent, is low. However, in spite of many years of efforts, no one has been known that has sufficient stability to be put to practical use.

[0007] Therefore, the present invention is to provide a polishing base that suppresses reactivity with NaF and a method for producing the same.

Means for solving the problem

[0008] The present invention for solving the above problems is as follows.

[1] A method for producing a polishing base, comprising heat-treating a dicalcium calcium phosphate anhydrate in the presence of a magnesium-containing compound and a condensed phosphate,

The abundance of the magnesium-containing compound is in the range of 1500 to 5000 ppm as a magnesium amount with respect to the dicalcium phosphate anhydrate,

The amount of condensed phosphate is such that the molar ratio of the cation component constituting the condensed phosphate to magnesium of the magnesium-containing compound is 0.4 Zn to 12 Zn (where n is the valence of the cation component) And)

The said manufacturing method whose heat processing conditions are the range of 100-300 degreeC.

[2] Magnesium-containing compound strength (1) Magnesium-containing compound contained in dicalcium phosphate anhydrate, (2) Magnesium-containing compound added to dicalcium phosphate anhydrate before heat treatment Or (3) a magnesium-containing compound contained in the anhydrous dibasic calcium phosphate and a magnesium-containing compound added to the anhydrous calcium phosphate before heat treatment [1 ] The manufacturing method of description.

[3] Anhydrous dicalcium phosphate dibasic acid The production method according to [1], obtained by dehydrating dicalcium phosphate dihydrate at 100 to 200 ° C.

[4] Anhydrous dibasic calcium phosphate strength The production method according to [1], obtained by dehydrating a slurry of dicalcium phosphate dihydrate at 80 to 110 ° C. [5] The magnesium-containing compound is at least one selected from the group consisting of magnesium hydroxide, primary magnesium phosphate, dibasic magnesium phosphate, tertiary magnesium phosphate, and magnesium pyrophosphate [1] ] To [4].

[6] The condensed phosphate is pyrophosphate, polyphosphate, metaphosphate or ultraphosphate, and the cationic component constituting the condensed phosphate is sodium, potassium, calcium, magnesium, aluminum, or The production method according to any one of [1] to [5], which is an amorphous.

[7] The condensed phosphate is a pyrophosphate, and is a pyrophosphate added to dicalcium phosphate prior to heat treatment with pyrophosphate, according to any one of [1] to [5] Production method.

[8] Pyrophosphate strength Sodium pyrophosphate, potassium pyrophosphate, calcium pyrophosphate, magnesium pyrophosphate and ammonium pyrophosphate group power is at least one selected from [6] or [7] Manufacturing method.

[9] The condensed phosphate according to any one of [1] to [5], wherein the condensed phosphate is a polyphosphate, and is a polyphosphate added to dicalcium phosphate before heat treatment for polyphosphate. The manufacturing method.

[10] Polyphosphate strength Sodium polyphosphate, potassium polyphosphate, calcium polyphosphate, ammonium polyphosphate, and at least one kind of group strength including magnesium polyphosphate strength is selected. [9] .

[11] A method for producing a polishing base, comprising mixing a magnesium-containing compound and a condensed phosphate in a dicalcium phosphate non-hydrate that has been heat-treated until no endothermic peak is observed near 130 ° C,

The amount of condensed phosphate is such that the molar ratio of the cation component constituting the condensed phosphate to magnesium of the magnesium-containing compound is 0.4 Zn to 12 Zn (where n is the valence of the cation component) The production method.

[12] The magnesium-containing compound is magnesium hydroxide, primary magnesium phosphate, secondary The production method according to [11], which is at least one selected from the group power of magnesium diphosphate, magnesium triphosphate, and magnesium pyrophosphate.

[13] The condensed phosphate is pyrophosphate, polyphosphate, metaphosphate or ultraphosphate, and the cationic component constituting the condensed phosphate is sodium, potassium, calcium, magnesium, aluminum, or The production method according to [11], which is an amorphous.

[14] The production method according to any one of [1] to [13], wherein the polishing base suppresses reactivity with a fluorine compound.

[15] A polishing base, which is obtained by the production method according to any one of [1] to [11] and has reduced reactivity with a fluorine compound.

[16] The above-mentioned polishing base comprising a dibasic calcium phosphate anhydrate as a main component and containing magnesium and condensed phosphate and suppressing reactivity with a fluorine compound.

[17] Magnesium content is in the range of 1500 to 5000 ppm, and abundance of condensed phosphate The molar ratio of the cation component constituting the condensed phosphate to magnesium is in the range of 0.4 Zn to 12 Zn (provided that , N is the valence of the cationic component). [16].

[18] The polishing base according to any one of [15] to [17], wherein the fluorine compound is sodium fluoride.

The invention's effect

[0009] According to the present invention, it is possible to provide a polishing base in which the reactivity to NaF that can withstand practical use is suppressed.

BEST MODE FOR CARRYING OUT THE INVENTION

[0010] The present invention provides a polishing base having an effect of suppressing reactivity with a fluorine compound, comprising heat-treating dicalcium phosphate anhydrate in the presence of a magnesium-containing compound and a condensed phosphate. The present invention relates to a method for producing an agent (first embodiment).

Furthermore, the present invention has an effect of suppressing reactivity with a fluorine compound, including mixing a magnesium-containing compound and a condensed phosphate, which are heat-treated until no endothermic peak is observed at around 130 ° C. The present invention relates to a method for producing a polishing base (second embodiment). [0011] Hereinafter, the first aspect will be described.

The anhydrous dibasic calcium phosphate used in the method for producing a polishing base of the present invention is not particularly limited as long as it is an anhydrous dibasic calcium phosphate. For example, (1) a reaction between calcium hydroxide and phosphoric acid at a temperature at which dibasic calcium phosphate anhydrate is formed, for example, at about 80 ° C, and the resulting dicalcium phosphate anhydrate is separated and dried. (2) Reacting calcium hydroxide and phosphoric acid at about 40 ° C, the temperature at which dicalcium phosphate dihydrate is generated, Examples include dicalcium phosphate anhydrous obtained by separating and drying the Japanese product and then dehydrating it. The dehydration of dicalcium phosphate dihydrate can be performed, for example, at 100 to 200 ° C, and particularly preferably in the range of 150 to 170 ° C. Further, as the dibasic calcium phosphate anhydrate used in the manufacturing method of the polishing base of the present invention, (3) the dicalcium phosphate dihydrate produced in the above (2) is heated to 80 ° C. or more in the form of a slurry. An anhydrous dicalcium phosphate obtained by dehydration can also be mentioned. This heating is preferably performed at 110 ° C. or lower.

In the heat treatment of the method of the present invention, the magnesium-containing compound present together with the dicalcium phosphate anhydrate is contained in (1) the anhydrous calcium phosphate anhydrate containing the magnesium-containing compound. (2) Magnesium-containing compound added to dicalcium phosphate anhydrate before heat treatment, or (3) Magnesium-containing compound contained in dicalcium phosphate anhydrate This compound is a magnesium-containing compound added to a dicalcium phosphate anhydrous before heat treatment. In general, dibasic calcium phosphate anhydrate contains magnesium as an impurity as an impurity. The magnesium-containing compound contained in (1) dicalcium phosphate non-hydrate is a magnesium compound contained as an impurity derived from the raw material. Furthermore, the magnesium-containing compound in the present invention is a magnesium-containing compound newly added to the dicalcium phosphate anhydrous other than the magnesium compound derived from impurities. This is the magnesium-containing compound added to the dicalcium phosphate phosphate before the heat treatment of (2). In addition, the magnesium-containing compound in the present invention is both the magnesium-containing compound and the magnesium-containing compound contained in the anhydrous dibasic calcium phosphate of (3) and before the heat treatment. It can also be a magnesium-containing compound added to anhydrous calcium diphosphate. The “magnesium-containing compound contained in the dicalcium phosphate anhydrous” in (1) and (3) may be any compound. However, such a magnesium-containing compound is generally magnesium phosphate. However, it may be a magnesium-containing compound other than magnesium phosphate.

[0013] When a magnesium-containing compound is newly added to dicalcium phosphate anhydrate, the magnesium-containing compound may be, for example, a solid (powder or granular). it can. In this case, the magnesium-containing compound is, for example, hydroxyammonium, magnesium chloride, primary magnesium phosphate, secondary magnesium phosphate, tertiary magnesium phosphate, magnesium sulfate, acidic magnesium, nitric acid. Magnesium, magnesium carbonate, magnesium acetate, magnesium benzoate, magnesium lactate, magnesium oleate, magnesium oxalate, magnesium stearate, magnesium pyrophosphate or magnesium succinate, or a mixture of these. it can . However, the magnesium-containing compound is preferably magnesium hydroxide, primary magnesium phosphate, secondary magnesium phosphate, tertiary magnesium phosphate, or magnesium pyrophosphate. Or it is especially preferable that it is tribasic magnesium phosphate.

[0014] The condensed phosphate used in the production method of the present invention can be, for example, pyrophosphate, polyphosphate, metaphosphate or ultraphosphate. Further, the cationic component constituting the condensed phosphate can be, for example, sodium, potassium, calcium, magnesium, aluminum, or ammonium.

[0015] The condensed phosphate may preferably be a pyrophosphate, which is, for example, sodium pyrophosphate, potassium pyrophosphate, calcium pyrophosphate, sodium hydrogen pyrophosphate, potassium hydrogen pyrophosphate, pyrophosphoric acid It can be aluminum, aluminum hydrogen pyrophosphate, magnesium pyrophosphate, ammonium pyrophosphate, or a mixture thereof. However, the pyrophosphate is particularly preferably sodium pyrophosphate, preferably sodium pyrophosphate, potassium pyrophosphate, calcium pyrophosphate, magnesium pyrophosphate or ammonium pyrophosphate. [0016] Further, the condensed phosphate may preferably be a polyphosphate, and examples of the polyphosphate include sodium polyphosphate, potassium polyphosphate, aluminum polyphosphate, magnesium polyphosphate, and ammonium polyphosphate. Can be mentioned. Examples of the metaphosphate include sodium metaphosphate, potassium metaphosphate, aluminum metaphosphate, magnesium metaphosphate, and ammonium metaphosphate. Examples of the ultraphosphate include sodium ultraphosphate, potassium ultraphosphate, aluminum ultraphosphate, magnesium ultraphosphate, and ammonium ultraphosphate.

[0017] The magnesium-containing compound and the condensed phosphate are, for example, a solid (powder or granular form) mixed with dicalcium phosphate anhydrous and then heat-treated. Alternatively, an aqueous solution or suspension containing the magnesium-containing compound and the condensed phosphate may be mixed with or sprayed with the dibasic calcium phosphate anhydrate, followed by heat treatment.

[0018] The abundance of the magnesium-containing compound is in the range of 1500 to 5000 ppm as a magnesium amount with respect to the dicalcium phosphate phosphate. “As the amount of magnesium” means the total amount of magnesium derived from the magnesium-containing compound and the magnesium-containing compound contained in the anhydrous dibasic calcium phosphate. The amount of magnesium derived from magnesium compounds contained as impurities in dibasic calcium phosphate anhydrate is also included. The abundance of the magnesium-containing compound is preferably in the range of 1700 to 4000 ppm, more preferably in the range of 2000 to 3000 ppm as the amount of magnesium relative to the dicalcium phosphate phosphate. Additive strength of magnesium-containing compounds If the amount of magnesium is less than 1500 ppm, the resulting F stability will not be sufficient. In other words, long-term F stability, which has a low level of F stability in the short term, is significantly reduced. Addition capacity of magnesium-containing compounds If the magnesium content exceeds 5000 ppm, the magnesium-containing compound reacts with F ions, and as a result, the stability tends to be lost.

[0019] The amount of the condensed phosphate is such that the molar ratio of the cation component constituting the condensed phosphate to magnesium of the magnesium-containing compound is in the range of 0.4 Zn to 12 Zn (where n is the cation component described above) Valence). This molar ratio is preferably in the range of 0.6 Zn to: LOZn, more preferably in the range of 0.7 / n to 8 / n. n is a cation component In the case of monovalent compounds such as potassium, potassium and ammonia, it is 1, and the molar ratio is in the range of 0.4-12. N is 2 when the cation component is divalent, such as magnesimu, and the molar ratio is in the range of 0.2-6. Furthermore, n is 3 when the cation component is trivalent such as aluminum, and the molar ratio is in the range of 0.4Z3-4.

[0020] The amount of the condensed phosphate added is either short-term or long-term when the molar ratio of the cation component constituting the condensed phosphate to magnesium derived from the magnesium-containing compound is less than 0.4 Zn. F stability is also poor. If this molar specific force exceeds 12Zn, short-term stability is good, but long-term stability tends to decrease.

[0021] In the production method of the present invention, the heat treatment conditions of the dicalcium phosphate anhydrous to which the magnesium-containing compound and the condensed phosphate are added are such that the temperature is in the range of 100 to 300 ° C. The heating temperature is preferably in the range of 150 to 250 ° C. It is appropriate that the heat treatment is performed at least until the crystal water of the added condensed phosphate hydrate is removed from the heat treatment. In consideration of this point, the heat treatment time is, for example, in the range of 1 to 10 hours. However, it is not limited to this range.

[0022] The second aspect will be described below.

The second aspect of the present invention includes mixing a magnesium-containing compound and a condensed phosphate with a dicalcium phosphate anhydrous heat-treated until no endothermic peak is observed at around 130 ° C.

[0023] The dicalcium phosphate anhydrate used in the method for producing the polishing base is a dicalcium phosphate anhydrate that has been heat-treated until no endothermic peak is observed at around 130 ° C. Such an anhydrous dicalcium phosphate is the same as the anhydrous calcium phosphate (1) to (3) described in the first embodiment of the present invention at 100 to 300 ° C, preferably 150 to 250 ° C. Examples thereof include those heated with C for 1 to 10 hours. The conditions for the heat treatment can be appropriately determined so as to obtain a dicalcium phosphate anhydrous that does not show an endothermic peak near 130 ° C as a result of thermal analysis by TG DAT.

[0024] As the magnesium-containing compound to be added to and mixed with the dicalcium phosphate anhydrous, for example, a solid (powder or granular) can be used. Examples of the magnesium-containing compound in this case are the same as in the first embodiment. Condensed phosphoric acid used in the second embodiment Examples of the salt are the same as in the first embodiment.

[0025] The magnesium-containing compound and the condensed phosphate are mixed with, for example, a solid (powder or granule) heat-treated dicalcium phosphate anhydrous. Mixing can be performed using, for example, a commercially available powder mixing apparatus (for example, a ribbon mixer or a V-type mixer). However, the mixing method is not limited to the above method. In addition, mixing should be carried out so that the mixture of dibasic phosphate strength succinic anhydride and magnesium-containing compound and condensed phosphate strength is almost evenly mixed. In addition, it can be determined appropriately in consideration of the particle size, mixing ratio, etc. of the dicalcium phosphate anhydrous, the magnesium-containing compound and the condensed phosphate.

[0026] An aqueous solution or suspension containing the magnesium-containing compound and the condensed phosphate may be mixed or sprayed with the heat-treated dicalcium phosphate anhydrous. In this case, after mixing or mixing after spraying, the mixture is dried.

[0027] The abundance of the magnesium-containing compound is in the range of 1500 to 5000 ppm as a magnesium amount with respect to the dicalcium phosphate phosphate. “As the amount of magnesium” means the total amount of magnesium derived from the magnesium-containing compound and the magnesium-containing compound contained in the anhydrous dibasic calcium phosphate. The amount of magnesium derived from the magnesium compound contained as an impurity in the heat-treated calcium phosphate anhydrous is also included. The abundance of the magnesium-containing compound is preferably in the range of 1700 to 4000 ppm, more preferably in the range of 2000 to 3000 ppm as the amount of magnesium relative to the dicalcium phosphate anhydrous. Calorific power of magnesium-containing compounds If the magnesium content is less than 1500 ppm, the F stability obtained will be insufficient. In other words, long-term F stability with a low level of F stability in a short period of time is significantly reduced. Additive strength of magnesium-containing compounds When the magnesium content exceeds 5000 ppm, the magnesium-containing compound reacts with F ions, and as a result, the stability tends to be lost.

[0028] The amount of the condensed phosphate is such that the molar ratio of the cation component constituting the condensed phosphate to magnesium of the magnesium-containing compound is in the range of 0.4 Zn to 12 Zn (where n is the cation component described above) Valence). This molar ratio is preferably in the range of 0.6 Zn to: LOZn, more preferably in the range of 0.7 / n to 8 / n. n is a cation component In the case of monovalent compounds such as potassium, potassium and ammonia, it is 1, and the molar ratio is in the range of 0.4-12. N is 2 when the cation component is divalent, such as magnesimu, and the molar ratio is in the range of 0.2-6. Furthermore, n is 3 when the cation component is trivalent such as aluminum, and the molar ratio is in the range of 0.4Z3-4.

[0029] The amount of the condensed phosphate added is either short-term or long-term when the molar ratio of the cation component constituting the condensed phosphate to magnesium derived from the magnesium-containing compound is less than 0.4 Zn. F stability is also poor. If this molar specific force exceeds 12Zn, short-term stability is good, but long-term stability tends to decrease.

[0030] According to the present invention, there is provided an abrasive base comprising dibasic calcium phosphate anhydrate as a main component and containing magnesium and a condensed phosphate. This polishing base has a suppressed reactivity with a fluorine compound, particularly sodium fluoride. The condensed phosphate is the same as that described in the above production method.

[0031] The polishing base of the present invention has a magnesium content in the range of 1500 to 5000 ppm, and the content of the cation component constituting the condensed phosphate is as a molar ratio to the magnesium content of 0.4 Zn to It is in the range of 12Zn.

[0032] The magnesium content is preferably in the range of 1700 to 4000 ppm, more preferably in the range of 2000 to 3000 ppm. The magnesium content of the polishing base of the present invention includes the magnesium amount derived from the magnesium-containing compound newly added in the preparation of the polishing base and the magnesium compound contained as an impurity in the dicalcium phosphate anhydrous. This is the total amount of magnesium derived from the product. The amount of magnesium derived from the magnesium compound contained as an impurity in dibasic calcium phosphate anhydrate depends on the type of CaO (origin) that is the raw material of the dibasic calcium phosphate anhydrate and the production of dibasic calcium phosphate anhydrate. Force varying with method and conditions Generally in the range of 500-1500 ppm. The magnesium content is 1500ρρπ! Outside the range of ~ 5000ppm, the F stability obtained is not sufficient. In other words, long-term F stability with a low level of F stability in the short term is also significantly reduced.

[0033] The content of the cation component constituting the condensed phosphate is the content of magnesium (magnesium derived from a magnesium-containing compound newly added in the preparation of the polishing base. And a molar ratio to the total amount of magnesium derived from the magnesium compound contained as an impurity in the dicalcium phosphate anhydrate) is in the range of 0.4 Zn to 12 Zn, preferably in the range of 0.6 Zn to LOZn. More preferably, it is in the range of 0.7 Zn to 8 Zn. Reactivity with fluorine compounds, especially sodium fluoride, is suppressed for a long time because the content of the cation component constituting the condensed phosphate is in the range of 0.4 Zn to 12 Zn as a molar ratio to the magnesium content. In addition, short-term and long-term F stability is also improved.

[0034] The polishing base of the present invention has a stability with a residual F concentration of 700 ppm or more at 50 ° C. for 30 days in the test method described later in the presence of lOOOppm sodium fluoride. That is, in the present invention, “in which the reactivity with sodium fluoride is suppressed” means that the residual F concentration shows 700 ppm or more in the test under the above conditions.

Example

Hereinafter, the present invention will be described in more detail with reference to examples.

[0036] Example 1

[Preparation of anhydrous dibasic calcium phosphate]

1200 g of water was placed in a 3 L stainless steel container and heated to 40 ° C while stirring. After heating at 40 ° C, 75% phosphoric acid and 120g-CaO / L lime milk were added simultaneously. At this time, the pH of the reaction solution was adjusted to be constant around 4.0. When the specified amount of phosphoric acid had been added, the slurry pH was adjusted to around 6. After adjusting the pH, the slurry was heated to 93 ° C and aged for 1 hour for dehydration. After dehydration, the slurry was filtered with G4 filter paper, the cake was separated, and dried overnight at 70 ° C. to obtain a 300 g sample of anhydrous dicalcium phosphate. The amount of Mg in the dibasic calcium phosphate non-hydrate sample was 1250 ppm.

[0037] [Addition of magnesium-containing compound and sodium pyrophosphate]

Mg (OH) 0.72 wt to 100 g sample of dibasic calcium phosphate anhydrate

2

% And Na P 0-10H 0 with 2. 75wt% and screw cap type plastic container (1

4 2 7 2

L) and mixed by shaking for about 5 minutes by hand. The amount of Mg (OH) added is 3000 mg of magnesium.

2

It was equivalent to ppm. The mixed sample was heat-treated in an oven at 200 ° C. for 2 hours to obtain an abrasive base sample 1 of the present invention. [0038] As a result of ICP (inductively coupled radio frequency plasma spectroscopy) analysis, the existing amount of the magnesium-containing compound in the polishing base sample 1 obtained by the heat treatment was 3600 ppm as the amount of magnesium with respect to the dicalcium phosphate phosphate non-hydrate. there were. The amount of sodium present was 4000 ppm as a result of ICP (inductively coupled radio frequency plasma spectroscopy) analysis as described above. The molar ratio of sodium to magnesium was 1.17.

[0039] 0.24wt% magnesium hydroxide and 2.75wt% Na P O · 10Η per 30g sample of the above dibasic calcium phosphate anhydrate, and screw cap type plastic

4 2 7 2

Place in a container (0.3 L), shake by hand for about 5 minutes to mix, heat the sample after mixing in an oven at 230 ° C for 1 hour, Got. The abundance of magnesium and sodium in the abrasive base sample 2 obtained by the heat treatment was determined by ICP analysis in the same manner as described above.

[0040] With respect to 30 g of the above dibasic calcium phosphate anhydrate sample, Mg (PO) · 8Η 0 0.5

3 4 2 2

Add 6wt% and Na P O · 10% O 3.1wt%, screw cap type plastic container

4 2 7 2

(0.3L), shake for about 5 minutes by hand, and mix the sample after heat treatment in an oven at 230 ° C for 1 hour in an open system. Obtained. The abundances of magnesium and sodium in the polishing base sample 3 obtained by the heat treatment were determined by ICP analysis in the same manner as described above.

[0041] For comparison, a 30 g sample of the dibasic calcium phosphate anhydrate

Four

Add only 75〇 · 10Η〇 to 2.75wt% and screw cap type plastic container (0.3

2 7 2

The sample was mixed by shaking for about 5 minutes by hand, and the mixed sample was heat-treated in an open system for 1 hour in a 230 ° C drier to prepare a comparative sample. The abundance of magnesium and sodium in the comparative sample obtained by heat treatment was determined by ICP analysis in the same manner as described above.

[0042] [F stability evaluation method]

Add 4.89 g of evaluation sample, 45 g of 42% glycerin solution, 0.1 lg of sodium fluoride to a 100 ml polyethylene cap with a screw cap, stir in a shaker for 5 minutes, and then place in a thermostat set to the specified temperature . The sample is filtered, separated into solid and liquid after a predetermined time (days), and the F concentration in the filtrate is measured using an F ion electrode. By this method, F stability evaluation of the above polishing base samples 1, 2, 3 and the comparative sample was performed. [0043] [Table 1]

[0044] According to the present invention, the magnesium content power is 3600 ppm, which is in the range of 500 to 5000 ppm, and the sodium content is 1.17 in a molar ratio with respect to the magnesium content of 0.5 to 9. Polishing base 1 based on dicalcium phosphate phosphate as the main component has excellent stability against fluoride fluoride that can be put to practical use with a residual F concentration of 700 ppm or more at 50 ° C for 30 days. It was a thing.

[0045] The present invention, wherein the magnesium content is 2310ppm, which is in the range of 1500 to 5000ppm, and the sodium content is 2.42 in terms of a molar ratio to the magnesium content of 0.5-9. Abrasive base 2 based on dicalcium phosphate dibasic acid as a main component has excellent residual F concentration with a residual F concentration of 700 ppm or more at 50 ° C for 30 days. I had it.

[0046] Magnesium content power of 2150 ppm, which is in the range of 500 to 5000 ppm, and sodium content is 2.93 in a molar ratio with respect to magnesium content of 0.5-9. Abrasive base 3 based on dibasic calcium phosphate anhydrate is excellent in practical use for sodium fluoride with a residual F concentration of 700 ppm or more at 50 ° C for 30 days. It was a thing.

[0047] In the comparative sample, the sodium content is in the range of 0.5 to 9 as a molar ratio to the magnesium content of 3.95, but the magnesium content is outside the range of 1500 to 5000 ppm. 1340ppm. As a result, the residual F concentration at 50 ° C. for 30 days was 16 ppm, and the inhibitory effect on the reactivity with the fluorine compound was strong.

[0048] Comparative Example 1

The F stability evaluation of the abrasive I described in Examples of Patent Document 1 was performed.

TFC (Tosohichi's Finechem Co., Ltd.) product DCP—C 100g, Mg (PO) · 8Η 0 (No. 3 Magnesium phosphate) 1. Add 12 wt% to a screw cap plastic container (1 L), mix in the same manner as in Example 1, and heat-treat in a 150 ° C dryer for 2 hours. An abrasive sample was obtained. Magnesium and sodium abundances were determined by ICP analysis as described above. The F stability evaluation and composition analysis of this sample were performed in the same manner as described above. The results are shown in Table 2.

[0049] [Table 2]

[0050] From the above results, it can be seen from Patent Document 1 that the polishing agent I described in the Examples is much more stable against sodium fluoride than the polishing base of the present invention. It can be seen that there is no stability against low and practical levels of fluorinated agents. In the examples of Patent Document 1, sodium monofluorophosphate is used as a fluorine agent, and its stability against sodium fluoride has been tested.

[0051] Comparative Example 2

In the preparation of abrasive I described in the example of Patent Document 1, the heating conditions were 150 ° C. and 2 hours. When this condition is changed to 230 ° C, which is slightly higher than the processing temperature of Example 1 above, and when the amount of applied force of Z or Mg (PO) · 8 Η 0 (tertiary magnesium phosphate) is increased.

3 4 2 2

In addition, tests were also conducted to see what effect F evaluation results have. The results are shown in Table 3.

[0052] [Table 3] Addition amount Heat treatment F stability (residual F-ppm) Weight part Temperature (° c) Time (hr) 50 C x 7 days 50. C x 30 days

1 1 .12 1 50 2 1 93 15

2 2. 24 1 50 2 298 1 35

3 4. 7 1 50 2 1 88 1 28

4 1. 12 230 2 484 370

5 2. 24 230 2 474 357

6 4. 7 230 2 444 1 82 [0053] From the above results, in Patent Document 1, the polishing agent I described in the Examples is still stable against sodium fluoride even when the temperature of the heat treatment and the amount of tribasic magnesium phosphate are changed. It can be seen that even if these polishing agents I are further modified compared to the polishing base of the present invention, the polishing agents I are further modified so that they do not have a practical level of stability to fluorine agents.

[0054] Example 2

TFC product DCP-C (Mg concentration: 1630ppm) per 100g of sodium pyrophosphate 4.21wt% calorie, put in screw cap type plastic container (0.3L), mix in the same way as in Example 1, then 230 ° C In the dryer, heat treatment was performed for 1 hour to obtain an abrasive sample. Evaluation of F stability of this sample was performed in the same manner as in Example 1 above. Magnesium and sodium abundances were determined by ICP analysis as described above. The results are shown in Table 4.

[0055] [Table 4]

[0056] Example 3

TFC product DCP-A (Mg concentration: 1710 ppm) 30 g of sodium pyrophosphate is added to a screw cap type plastic container (0.3 L) and mixed in the same manner as in Example 1, then 230 ° C. In the dryer, heat treatment was performed for 1 hour to obtain an abrasive sample. Evaluation of F stability of this sample was performed in the same manner as in Example 1 above. Magnesium and sodium abundances were determined by ICP analysis as described above. The results are shown in Table 5.

[0057] [Table 5]

Example 4

[Preparation of anhydrous dibasic calcium phosphate]

Dibasic calcium phosphate anhydrate was synthesized in the same manner as in Example 1. Second synthesized The Mg concentration of the anhydrous calcium phosphate was 1850 ppm.

[0059] [Preparation of F stability evaluation sample]

Change the amount of 0.24 wt% sodium tripolyphosphate (Na P 0) addition of magnesium hydroxide to 30 g of the above dibasic calcium phosphate anhydride as shown in the table below.

5 3 10

After placing in a plastic container (0.3 L) and mixing in the same manner as in Example 1, heat treatment was performed in a 200 ° C drier for 2 hours to obtain an abrasive sample. The F stability evaluation of this sample was performed as described above. The results are shown in Table 6.

[0060] [Table 6]

* Mg, Na analysis; P (inductively coupled plasma spectroscopy) analysis

[0061] Example 5

[Heat treatment of anhydrous dibasic calcium phosphate]

1500 g of dibasic calcium phosphate anhydrate (Mg concentration, 1850 ppm) synthesized in Example 4 was placed in a stainless steel vat and heat-treated in an open system for 1 hour in a 230 ° C drier, and then heat treated dicalcium phosphate. An hydrate was obtained. Figure 1 shows the thermal analysis (TG DTA) results of the dicalcium phosphate anhydrate after heat treatment, and Fig. 1 shows the thermal analysis (TG-DTA) results of the dicalcium phosphate anhydrate before heat treatment. Shown in 2. As shown in Figs. 1 and 2, the dicalcium phosphate anhydrate before heat treatment has an endothermic peak around 130 ° C, whereas the dicalcium phosphate anhydrate after heat treatment has an endothermic peak. This endothermic peak was powerful.

[0062] [Adjustment of F stabilization evaluation sample]

For 30g of the above heat-treated dicalcium phosphate anhydrate, Mg (PO) 8Η 0 0.56

3 4 2 2 wt% and Na PO10Η O 3.1 wt% 3L) and mixed by shaking for about 5 minutes by hand to obtain an abrasive sample. The F stability evaluation of this sample was performed by the same method as the F stability evaluation method shown in Example 1. The abundance of magnesium and sodium was determined by ICP analysis as described above. The results are shown in Table 7.

[0063] [Table 7]

Industrial applicability

[0064] The polishing base of the present invention can be used as a polishing base for brushing teeth.

Brief Description of Drawings

[0065] [FIG. 1] Thermal analysis of anhydrous dibasic calcium phosphate after heat treatment in Example 5 (TG

DTA) results.

FIG. 2 shows the result of thermal analysis (TG DTA) of dicalcium phosphate phosphate before heat treatment in Example 5.

Claims

The scope of the claims

[1] A method for producing a polishing base, comprising heat-treating dicalcium phosphate anhydrous in the presence of a magnesium-containing compound and a condensed phosphate,

[2] Magnesium-containing compound strength (1) Magnesium-containing compound contained in dicalcium phosphate anhydrate, (2) Magnesium contained in dicalcium phosphate anhydrate before heat treatment Or (3) the magnesium-containing compound contained in the anhydrous calcium phosphate and the magnesium-containing compound added to the anhydrous calcium phosphate before the heat treatment. 1. The production method according to 1.

[3] The method according to claim 1, wherein the dicalcium phosphate dihydrate is obtained by dehydrating dicalcium phosphate dihydrate at 100 to 200 ° C.

[4] The method according to claim 1, wherein the anhydrous calcium phosphate dihydrate is obtained by dehydrating a slurry of dicalcium phosphate dihydrate at 80 to 110 ° C.

[5] Magnesium-containing composite strength is at least one selected from the group consisting of magnesium hydroxide, primary magnesium phosphate, secondary magnesium phosphate, tertiary magnesium phosphate, and magnesium pyrophosphate. 5. The production method according to any one of 4 above.

[6] The condensed phosphate is pyrophosphate, polyphosphate, metaphosphate or ultraphosphate, and the cationic component constituting the condensed phosphate is sodium, potassium, calcium, magnesium, aluminum, or The manufacturing method according to claim 1, which is ammonia.

[7] The condensed phosphate according to any one of claims 1 to 5, wherein the condensed phosphate is pyrophosphate, and is pyrophosphate added to calcium diphosphate before heat treatment. The manufacturing method of description.

[8] The pyrophosphoric acid strength Sodium pyrophosphate, potassium pyrophosphate, calcium pyrophosphate, magnesium pyrophosphate and ammonium pyrophosphate group power are at least one selected from the production method according to claim 6 or 7. .

[9] The condensed phosphate according to any one of claims 1 to 5, wherein the condensed phosphate is a polyphosphate and is a polyphosphate added to dicalcium phosphate prior to heat treatment of polyphosphate. The manufacturing method of description.

[10] The production method according to claim 9, wherein the polyphosphate strength is at least one selected from the group strength including sodium polyphosphate, potassium polyphosphate, calcium polyphosphate, ammonium polyphosphate, and magnesium polyphosphate strength.

[11] A method for producing a polishing base, comprising mixing a magnesium-containing compound and a condensed phosphate with a dicalcium phosphate phosphate that has been heat-treated until no endothermic peak is exhibited in the vicinity of 130 ° C.

[12] The magnesium-containing composite strength is at least one selected from the group consisting of magnesium hydroxide, primary magnesium phosphate, secondary magnesium phosphate, tertiary magnesium phosphate, and magnesium pyrophosphate. The manufacturing method as described.

[13] the condensed phosphate is pyrophosphate, polyphosphate, metaphosphate or ultraphosphate

12. The production method according to claim 11, wherein the cation component constituting the condensed phosphate is sodium, potassium, calcium, magnesium, aluminum, or ammonium.

[14] The polishing base according to any one of claims 1 to 13, wherein the polishing base has a suppressed reactivity with a fluorine compound.

The manufacturing method according to 1.

[15] A polishing base, which is obtained by the production method according to any one of claims 1 to 14 and suppresses reactivity with a fluorine compound.

[16] A polishing base mainly composed of dibasic calcium phosphate anhydrate, comprising magnesium and The polishing base comprising a condensed phosphate and having reduced reactivity with a fluorine compound

[17] Magnesium content is in the range of 1500 to 5000 ppm, and the presence of condensed phosphate is such that the molar ratio of the cation component constituting the condensed phosphate to magnesium is in the range of 0.4 / n to 12Zn ( The polishing base according to claim 16, wherein n is a valence of the cationic component.

[18] The polishing base according to any one of claims 15 to 17, wherein the fluorine compound is sodium fluoride.