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CN102532402A - Lacquer emulsion and preparation method thereof - Google Patents

Lacquer emulsion and preparation method thereof Download PDF

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Publication number
CN102532402A
CN102532402A CN2011104409964A CN201110440996A CN102532402A CN 102532402 A CN102532402 A CN 102532402A CN 2011104409964 A CN2011104409964 A CN 2011104409964A CN 201110440996 A CN201110440996 A CN 201110440996A CN 102532402 A CN102532402 A CN 102532402A
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CN
China
Prior art keywords
emulsion
preparation
mineral varnish
monomer
true mineral
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CN2011104409964A
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Chinese (zh)
Inventor
陆超
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SHANGHAI MORFANT NEW MATERIAL TECHNOLOGY Co Ltd
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SHANGHAI MORFANT NEW MATERIAL TECHNOLOGY Co Ltd
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Priority to CN2011104409964A priority Critical patent/CN102532402A/en
Publication of CN102532402A publication Critical patent/CN102532402A/en
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Abstract

The invention relates to a lacquer emulsion which is prepared by polymerizing the following raw materials: a hard monomer, a soft monomer, a functional monomer, a composite emulsifying agent, organic silicon, an initiator, a pH regulating agent and deionized water. The invention also provides a preparation method of the lacquer emulsion. Compared with the prior art, the lacquer emulsion has the advantages of good water tolerance, high paint film hardness, low film-forming temperature and the like. The reasons are as follows: the emulsion prepared by using the method is higher in solid content, and the highest solid content can reach 56%; at least one reaction-type emulsifying agent is adopted, thus the stability of the emulsion is improved, and the water tolerance of a latex film is improved; and proper monomers and monomer proportion are selected, and the glass transition temperature and lowest film-forming temperature of the polymer are reduced, so that the formed paint film is higher in hardness and lower in film-forming temperature.

Description

A kind of true mineral varnish emulsion and preparation method thereof
Technical field
The present invention relates to trade sales coating, relate in particular to a kind of true mineral varnish emulsion and preparation method thereof.
Background technology
True mineral varnish is claimed anti-mineral varnish again, mainly adopts versicolor natural stone-powder and polymer emulsion mixed preparing to form.It is sprayed on the exterior wall of buildings, and decorative effect exactly likes marble, and grouan is a kind of ideal material that replaces the lithotome decorative cover.
But the existing true mineral varnish that uses, the shortcoming that the ubiquity water tolerance is bad, coating all can be turned white after each raining, and becomes loose.This is that the prescription reason mainly is that the benzene emulsion of selecting for use need add emulsifying agent when synthetic because coating absorbs moisture institute heroic spirit.These not polymerisable emulsifying agents show formation one deck emulsion layer of bonding non-chemically at paint film; In case meet water or make moist and to cause the paint film water absorption and swelling; Cause " frosting "; " whiting ", its result has not only influenced the sense organ of building appearance, and greatly reduces the physicals of the true mineral varnish that is sprayed on building appearance.
Summary of the invention
The object of the invention provides a kind of true mineral varnish emulsion to the problems referred to above exactly, and this emulsion water resistance is good, and pencil hardness is hard, and is firm with the natural stone-powder bonding.
Another object of the present invention is to provide a kind of method of the Ben Fazhen of preparation mineral varnish emulsion.
The technical scheme that the present invention is adopted in order to reach the goal is:
A kind of true mineral varnish emulsion of the present invention is formed by following polymerizable raw material:
Hard monomer, soft monomer, functional monomer, compound emulsifying agent, organosilicon, initiator, pH regulator agent and deionized water;
Wherein, said hard monomer is at least a in vinylbenzene and the TEB 3K;
Said soft monomer is at least a in Bing Xisuandingzhi, ethyl propenoate and the Isooctyl acrylate monomer;
Said functional monomer is at least a in vinylformic acid, methylacrylic acid, Hydroxyethyl acrylate and the Rocryl 400;
Said compound emulsifying agent be nonyl phenol ether sulphate and TX10 by weight 1.5: 5.5 composite making;
Said organosilicon is that METHYL TRICHLORO SILANE and dichloromethyl phenylsilane are by 4.5: 2.5 composite making of mass ratio;
Said initiator is a persulphate;
Said pH regulator agent is the pH regulator agent of hierarchy of control pH value for 5-9.
Above-mentioned a kind of true mineral varnish emulsion, wherein, said hard monomer for for vinylbenzene and TEB 3K by 5.8: 2.2 composite making of mass ratio.
Above-mentioned a kind of true mineral varnish emulsion, wherein, said raw materials in part by weight is following:
Above-mentioned raw materials is the commercially available prod.
The present invention also provides a kind of preparation method of above-mentioned true mineral varnish emulsion, may further comprise the steps:
A. earlier with quantitative compound emulsifying agent, deionized water joins in the polymerization reaction kettle, stirs and intensification;
B. with quantitative deionized water, compound emulsifying agent, hard monomer add in the preparatory emulsification still, under the constant speed condition, stir and obtain pre-emulsion after 80 minutes, wherein 10% subsequent use as rebasing seed reaction solution of weighing;
C. the temperature with the polymerization reaction kettle of steps A is raised to 75-80 ℃; Drop into the rebasing seed reaction solution among the step B, added again rebasing initiator for reaction 80-100 minute, continue to add deionized water toward polymerization reaction kettle; Slowly cool the temperature to 60 ℃, and the control controlled temperature is at 55-60 ℃;
D. polymerization reaction kettle was vacuumized 2 hours, be warming up to 85 ℃ of remaining 90% pre-emulsions again, drop in the polymerization reaction kettle, drip initiator with second constant speed simultaneously with first constant speed with step B preparation;
When E. question response drops to 2.5 hours, suspend dropping pre-emulsion and initiator, in preparatory emulsification still, add quantitative soft monomer; Add organosilicon simultaneously; Stir and prepare mixed reaction solution after 35 minutes,, drip mixed reaction solution and initiator toward polymerization reaction kettle simultaneously with the 3rd constant speed;
F. after dripping end,, be cooled to 40 ℃, regulate the pH value behind 5-9, regulate solid content at 45%-56%, filter discharging with 100 order filter bags with deionized water with the pH regulator agent 85-90 ℃ of insulation 5.5-6 hour.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, the preparatory emulsification still described in the step B is for opening curved blade type, and the number of blade is 5 leaves, and its diameter is 0.77 with preparatory emulsification still diameter ratio, and its blade diameter is 4.7 with the ratio of depth of blade.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, the condition of constant speed described in the step B is that mixing speed is controlled at 650-750 rev/min.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, deionized water specific conductivity described in steps A, B, the C is controlled at 0.1 μ s/cm-1 μ s/cm.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, the vacuum tightness that vacuumizes described in the step D remains on the 180-200 mmhg, and said first constant speed is 150~300 milliliters of PMs, and said second constant speed is 50~80 milliliters of PMs.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, said the 3rd constant speed of step e is 100~150 milliliters of PMs.
The preparation method of above-mentioned a kind of true mineral varnish emulsion, wherein, the pH regulator agent is ammoniacal liquor, wherein NH in the step F 3Content be controlled at 2-5%, said deionized water specific conductivity is controlled at 250 μ s/cm~280 μ s/cm.
Advantages such as the present invention compared with prior art has water-tolerant, and hardness of paint film height and film-forming temperature are low, its reason have following some:
1. the emulsion that makes of the present invention has higher solid content, and high solids content can reach 56%;
2. the present invention adopts at least a reactive emulsifier, thereby has improved the stability and the water tolerance of improving latex film of emulsion;
3. select suitable monomers and monomer ratio, second-order transition temperature and minimum film-forming temperature reduction with polymkeric substance make the paint film of formation have higher hardness and lower film-forming temperature.
Embodiment
Below through specific embodiment the present invention is carried out a step and sets forth, but should not limit the present invention by any way.
Embodiment:
A. earlier with the compound emulsifying agent of 0.2 weight part, the deionized water of 12 weight parts joins in the polymerization reaction kettle, stirs and intensification;
B. with the deionized water of 35 weight parts; 1.8 weight part compound emulsifying agent; 18 weight part hard monomers (TEB 3K of the vinylbenzene of 15 weight parts and 3 weight parts is composite) add in the preparatory emulsification still; Under the constant speed condition (720 rev/mins), stir and obtain pre-emulsion after 80 minutes, weighing 5.48 weight parts wherein are subsequent use as rebasing seed reaction solution;
C. the temperature with the polymerization reaction kettle of steps A is raised to 75-80 ℃; Drop into the rebasing seed reaction solution of 5.48 weight parts among the step B; Add rebasing initiator for reaction 80-100 minute of 0.2 weight part again; Past polymerization reaction kettle continues to add the deionized water of 8 weight parts, slowly cools the temperature to 60 ℃, and the control controlled temperature is at 55-60 ℃;
D. polymerization reaction kettle was vacuumized 2 hours; Be warming up to 85 ℃ of remaining 49.32 weight part pre-emulsions again with step B preparation; Drop in the polymerization reaction kettle with first constant speed (180 milliliters of PMs), drip the initiator of 0.8 weight part simultaneously with second constant speed (55 milliliters of PMs);
When E. question response drops to 2.5 hours; Suspend and drip pre-emulsion and initiator; The soft monomer (different monooctyl ester of 28 parts by weight of acrylic and 25 parts by weight of acrylic butyl esters are composite) that in preparatory emulsification still, adds 53 weight parts; The organosilicon (METHYL TRICHLORO SILANE and dichloromethyl phenylsilane press mass ratio 4.5: 2.5 composite) that adds 1 weight part simultaneously; Stir and make mixed reaction solution after 35 minutes,, drip the initiator of mixed reaction solution and 1 weight part toward polymerization reaction kettle simultaneously with the 3rd constant speed (120 milliliters of PMs);
F. treat in the preparatory emulsification still that it is after mixed reaction solution all drips the back that material all dropwises, and 85-90 ℃ of insulation 5.5-6 hour, is cooled to 40 ℃; As required; With in the ammoniacal liquor of 2 weight parts and behind the pH, regulate solid content 54% with deionized water, filter discharging with 100 order filter bags.
Above-mentioned rebasing initiator and initiator are persulphate.
The true mineral varnish emulsion that this embodiment prepares, its each item performance is following: the oyster white aqueous dispersion, not stratified, there is not deposition, no skinning is uniform state after the stirring; Viscosity: 240 ± 10mpa.s; PH value: 7 ± 1; Solid content: 54%.
Above embodiment only supplies to explain the present invention's usefulness; But not limitation of the present invention; The technician in relevant technologies field under the situation that does not break away from the spirit and scope of the present invention, can also make various conversion or modification; Therefore all technical schemes that are equal to also should belong to category of the present invention, should be limited each claim.

Claims (10)

1. a true mineral varnish emulsion is characterized in that, is to be formed by following polymerizable raw material:
Hard monomer, soft monomer, functional monomer, compound emulsifying agent, organosilicon, initiator, pH regulator agent and deionized water;
Wherein, said hard monomer is at least a in vinylbenzene and the TEB 3K;
Said soft monomer is at least a in Bing Xisuandingzhi, ethyl propenoate and the Isooctyl acrylate monomer;
Said functional monomer is at least a in vinylformic acid, methylacrylic acid, Hydroxyethyl acrylate and the Rocryl 400;
Said compound emulsifying agent be nonyl phenol ether sulphate and TX10 by weight 1.5: 5.5 composite making;
Said organosilicon is that METHYL TRICHLORO SILANE and dichloromethyl phenylsilane are by 4.5: 2.5 composite making of mass ratio;
Said initiator is a persulphate;
Said pH regulator agent is the pH regulator agent of hierarchy of control pH value for 5-9.
2. a kind of true mineral varnish emulsion as claimed in claim 1 is characterized in that, said hard monomer for for vinylbenzene and TEB 3K by 5.8: 2.2 composite making of mass ratio.
3. according to claim 1 or claim 2 a kind of true mineral varnish emulsion is characterized in that said raw materials in part by weight is following:
4. the preparation method of a true mineral varnish emulsion as claimed in claim 1 is characterized in that, may further comprise the steps:
A. earlier with quantitative compound emulsifying agent, deionized water joins in the polymerization reaction kettle, stirs and intensification;
B. with quantitative deionized water, compound emulsifying agent, hard monomer add in the preparatory emulsification still, under the constant speed condition, stir and obtain pre-emulsion after 80 minutes, wherein 10% subsequent use as rebasing seed reaction solution of weighing;
C. the temperature with the polymerization reaction kettle of steps A is raised to 75-80 ℃; Drop into the rebasing seed reaction solution among the step B, added again rebasing initiator for reaction 80-100 minute, continue to add deionized water toward polymerization reaction kettle; Slowly cool the temperature to 60 ℃, and the control controlled temperature is at 55-60 ℃;
D. polymerization reaction kettle was vacuumized 2 hours, be warming up to 85 ℃ of remaining 90% pre-emulsions again, drop in the polymerization reaction kettle, drip initiator with second constant speed simultaneously with first constant speed with step B preparation;
When E. question response drops to 2.5 hours, suspend dropping pre-emulsion and initiator, in preparatory emulsification still, add quantitative soft monomer; Add organosilicon simultaneously; Stir and prepare mixed reaction solution after 35 minutes,, drip mixed reaction solution and initiator toward polymerization reaction kettle simultaneously with the 3rd constant speed;
F. after dripping end,, be cooled to 40 ℃, regulate the pH value behind 5-9, regulate solid content at 45%-56%, filter discharging with 100 order filter bags with deionized water with the pH regulator agent 85-90 ℃ of insulation 5.5-6 hour.
5. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4; It is characterized in that the preparatory emulsification still described in the step B is for opening curved blade type, the number of blade is 5 leaves; Its diameter is 0.77 with preparatory emulsification still diameter ratio, and its blade diameter is 4.7 with the ratio of depth of blade.
6. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4 is characterized in that, the condition of constant speed described in the step B is that mixing speed is controlled at 650-750 rev/min.
7. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4 is characterized in that, deionized water specific conductivity described in steps A, B, the C is controlled at 0.1 μ s/cm-1 μ s/cm.
8. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4; It is characterized in that; The vacuum tightness that vacuumizes described in the step D remains on the 180-200 mmhg, and said first constant speed is 150~300 milliliters of PMs, and said second constant speed is 50~80 milliliters of PMs.
9. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4 is characterized in that, said the 3rd constant speed of step e is 100~150 milliliters of PMs.
10. the preparation method of a kind of true mineral varnish emulsion as claimed in claim 4 is characterized in that, the pH regulator agent is ammoniacal liquor, wherein NH in the step F 3Content be controlled at 2-5%, said deionized water specific conductivity is controlled at 250 μ s/cm~280 μ s/cm.
CN2011104409964A 2011-12-23 2011-12-23 Lacquer emulsion and preparation method thereof Pending CN102532402A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977257A (en) * 2012-12-25 2013-03-20 上海三瑞高分子材料有限公司 Water-whitening proof maishi paint emulsion of core-shell structure and method for preparing same
CN104356287A (en) * 2014-11-03 2015-02-18 上海三瑞高分子材料有限公司 Internal and external cross-linking real stone paint pure acrylic emulsion with high water whitening resistance and preparation method
CN105884962A (en) * 2014-12-31 2016-08-24 衡水新光化工有限责任公司 Emulsion for stonelike paint and stonelike paint with emusion as film forming matter
CN106634372A (en) * 2016-12-29 2017-05-10 成都巴德富科技有限公司 Low-water-absorptivity stone-like coating emulsion and preparation method thereof
CN108264805A (en) * 2017-12-31 2018-07-10 成都巴德富科技有限公司 A kind of quick-drying porcelain tendre lacquer and preparation method thereof
CN108383937A (en) * 2018-02-28 2018-08-10 中山市巴德富化工科技有限公司 A kind of water-fast acrylic acid ester emulsion of hydrophobic high rigidity and preparation method thereof
CN109207012A (en) * 2018-08-21 2019-01-15 安徽省鸣新材料科技有限公司 A kind of compound foamed aluminum plate of parian and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6005042A (en) * 1996-03-11 1999-12-21 Clariant Gmbh Aqueous polymer dispersions as binders for elastic, nonblocking and scratch-resistant coatings
CN101921360A (en) * 2010-01-27 2010-12-22 陕西科技大学 A kind of preparation method of nano-scale silicon-acrylic core-shell type composite emulsion for latex paint
CN101982477A (en) * 2010-09-25 2011-03-02 西北工业大学 Acrylic emulsion capable of simultaneously modifying two silane coupling agents and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6005042A (en) * 1996-03-11 1999-12-21 Clariant Gmbh Aqueous polymer dispersions as binders for elastic, nonblocking and scratch-resistant coatings
CN101921360A (en) * 2010-01-27 2010-12-22 陕西科技大学 A kind of preparation method of nano-scale silicon-acrylic core-shell type composite emulsion for latex paint
CN101982477A (en) * 2010-09-25 2011-03-02 西北工业大学 Acrylic emulsion capable of simultaneously modifying two silane coupling agents and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977257A (en) * 2012-12-25 2013-03-20 上海三瑞高分子材料有限公司 Water-whitening proof maishi paint emulsion of core-shell structure and method for preparing same
CN104356287A (en) * 2014-11-03 2015-02-18 上海三瑞高分子材料有限公司 Internal and external cross-linking real stone paint pure acrylic emulsion with high water whitening resistance and preparation method
CN105884962A (en) * 2014-12-31 2016-08-24 衡水新光化工有限责任公司 Emulsion for stonelike paint and stonelike paint with emusion as film forming matter
CN105884962B (en) * 2014-12-31 2018-08-31 衡水新光新材料科技有限公司 A kind of lacquer lotion and using the lotion as the lacquer of film forming matter
CN106634372A (en) * 2016-12-29 2017-05-10 成都巴德富科技有限公司 Low-water-absorptivity stone-like coating emulsion and preparation method thereof
CN108264805A (en) * 2017-12-31 2018-07-10 成都巴德富科技有限公司 A kind of quick-drying porcelain tendre lacquer and preparation method thereof
CN108264805B (en) * 2017-12-31 2019-12-24 成都巴德富科技有限公司 Quick-drying soft porcelain stone-like paint and preparation method thereof
CN108383937A (en) * 2018-02-28 2018-08-10 中山市巴德富化工科技有限公司 A kind of water-fast acrylic acid ester emulsion of hydrophobic high rigidity and preparation method thereof
CN109207012A (en) * 2018-08-21 2019-01-15 安徽省鸣新材料科技有限公司 A kind of compound foamed aluminum plate of parian and preparation method thereof

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