CN102532401B - Elastic emulation and preparation method thereof - Google Patents
Elastic emulation and preparation method thereof Download PDFInfo
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- CN102532401B CN102532401B CN201110440798.8A CN201110440798A CN102532401B CN 102532401 B CN102532401 B CN 102532401B CN 201110440798 A CN201110440798 A CN 201110440798A CN 102532401 B CN102532401 B CN 102532401B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 12
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims description 46
- 238000006116 polymerization reaction Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000004945 emulsification Methods 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 8
- 239000004816 latex Substances 0.000 claims description 8
- 229920000126 latex Polymers 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- -1 organosilicon Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 5
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000002902 bimodal effect Effects 0.000 claims description 2
- GNEPOXWQWFSSOU-UHFFFAOYSA-N dichloro-methyl-phenylsilane Chemical compound C[Si](Cl)(Cl)C1=CC=CC=C1 GNEPOXWQWFSSOU-UHFFFAOYSA-N 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 2
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 7
- 238000011109 contamination Methods 0.000 abstract description 2
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000237502 Ostreidae Species 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
Landscapes
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to elastic emulation, which is formed by polymerizing hard monomers, soft monomers, functional monomers, composite emulsifiers, organic silicon, initiators, pH modifiers and deionized water. A preparation method of the elastic emulation is further provided. The elastic emulation has high elasticity, better anti-contamination performance, lower film-forming temperature and better waterproof performance and is capable of being widely used in the preparation processing of building coatings such as outer wall systems and waterproof coating systems, particularly application systems where emulation has elasticity and film-forming temperature is lower.
Description
Technical field
The present invention relates to the building coating emulsion, relate in particular to a kind of elastic emulsion and preparation method thereof.
Background technology
Along with improving constantly of scientific and technical development and building coating performance, emulsion is as a kind of requisite component, at much polymkeric substance breast coating, binding agent, flocculation agent, synthetic rubber, during the production of impact-resistant copolymerized thing etc. is synthetic, become a very important part.And give itself to have many good characteristics, make it in the historical progress of last 100 years, gradually changed into a foundation stone in chemical industry.And at this wherein, the cinnamic acrylic ester emulsion is various due to the monomeric species of its raw material, range of product mainly with and there is good integrated application performance, make its development in this field always rapider.
Self-evident, the application of cinnamic acrylic ester emulsion in building trade is also more and more important, and, along with the continuous enhancing of people's environmental consciousness, water milk type coating has become important developing direction of coatings industry.
How to improve the performance of Water-borne Coatings Emulsion, the defect such as one of them key factor is exactly the problem of emulsion, and traditional emulsion exists film-forming temperature higher, and water tolerance is bad, and greatly limited its application in water milk type coating.
Summary of the invention
Purpose of the present invention, provide a kind of elastic emulsion for the problems referred to above exactly, fundamentally overcome the defect of the Water-borne Coatings Emulsion aspect of performance caused due to the emulsion factor.
Another object of the present invention is to provide a kind of method for preparing elastic emulsion of the present invention.
The technical scheme that the present invention adopted in order to reach the goal is:
A kind of elastic emulsion of the present invention is formed by following polymerizable raw material:
Hard monomer, soft monomer, functional monomer, compound emulsifying agent, organosilicon, initiator, pH adjusting agent and deionized water;
Wherein, described hard monomer is at least one in vinylbenzene and methyl methacrylate;
Described soft monomer is at least one in butyl acrylate, ethyl propenoate and Isooctyl acrylate monomer;
Described functional monomer is at least one in vinylformic acid, methacrylic acid, Hydroxyethyl acrylate and hydroxyethyl methylacrylate;
Described compound emulsifying agent is that phenolic ether sulphate and alkylphenol polyoxyethylene were by weight 5.2: 0.8 composite making;
Described organosilicon is METHYL TRICHLORO SILANE and dichloromethyl phenylsilane 7.5: 3.5 composite making in mass ratio;
Described initiator is persulphate;
Described pH adjusting agent is the pH adjusting agent that hierarchy of control pH value is 5-9.
Above-mentioned a kind of elastic emulsion, wherein, described hard monomer is vinylbenzene and methyl methacrylate 3.2: 4.8 composite making in mass ratio.
Above-mentioned a kind of elastic emulsion, wherein, the latex micella particle diameter of described elastic emulsion is 80～140 nanometers, and latex particle size presents bimodal distribution in the size distribution analysis, wherein, latex micella particle diameter be 100 nanometers account for total amount 5-15%, and present normal distribution between the 80-120 nanosection; Latex micella particle diameter be 130 nanometers account for total amount 70-75%, and present normal distribution between the 120-140 nanosection.
Above-mentioned a kind of elastic emulsion, wherein, the parts by weight of described raw material are as follows:
Above-mentioned raw materials is commercially available prod.
The present invention also provides a kind of preparation method of elastic emulsion, comprises the following steps:
A. first by quantitative compound emulsifying agent and deionized water, join in polymerization reaction kettle, stir and heat up;
B. in the pre-emulsification still quantitative deionized water, compound emulsifying agent, hard monomer added, stir after 30 minutes and obtain pre-emulsion, weighing 16% weight ratio wherein is standby as rebasing seed reaction solution;
C. the temperature of polymerization reaction kettle is raised to 85-90 ℃, drop into the rebasing seed reaction solution prepared in step B, then add rebasing initiator for reaction 30-45 minute, toward polymerization reaction kettle, continue to add deionized water, slowly cool the temperature to 65 ℃, and control temperature at 65-70 ℃;
D. polymerization reaction kettle is vacuumized to 4 hours, then be warming up to 75 ℃ of residue pre-emulsions that step B is prepared, drop in polymerization reaction kettle with the first constant speed from the pre-emulsification still, drip initiator with the second constant speed simultaneously;
When E. question response drops to 1.5 hours, suspend and drip pre-emulsion and initiator, add quantitative soft monomer and functional monomer in the pre-emulsification still, add organosilicon simultaneously, stir and obtain mixed reaction solution after 55 minutes, with the 3rd constant speed, toward polymerization reaction kettle, drip mixed reaction solution and initiator simultaneously;
F., after dripping end, polymerization reaction kettle, at 85-90 ℃ of insulation 0.5-1 hour, is cooled to 40 ℃,, regulate the pH value at 5-9 by pH adjusting agent, regulate solid content at 25%-60% with deionized water, filter discharging with 100 order filter bags.
The preparation method of above-mentioned a kind of elastic emulsion, wherein, pre-emulsification still described in step B is for opening curved blade type, the number of blade is 5 leaves, its diameter and pre-emulsification still diameter ratio are 0.66, its blade diameter is 4.2 with the ratio of depth of blade, and the mixing speed of pre-emulsification still is controlled at 850-880 rev/min.
The preparation method of above-mentioned a kind of elastic emulsion, wherein, the deionized water specific conductivity described in steps A, B, C is controlled at 0.1 μ s/cm-1 μ s/cm.
The preparation method of above-mentioned a kind of elastic emulsion, wherein, the vacuum keep vacuumized described in rapid D is at the 280-300 mmhg, and described the first constant speed is 50～80 milliliters of per minutes, and described the second constant speed is 3～5 milliliters of per minutes.
The preparation method of above-mentioned a kind of elastic emulsion, wherein, described the 3rd constant speed of step e is 250～300 milliliters of per minutes.
The preparation method of above-mentioned a kind of elastic emulsion, wherein, in step F, pH adjusting agent is ammoniacal liquor, wherein NH
3content be controlled at 5-8%, described deionized water specific conductivity is controlled at 350 μ s/cm～380 μ s/cm.
Formulation selection of the present invention the proportioning of suitable soft, hard monomer, having applied negatively charged ion and nonionic emulsifying agent mixes, and pass through hud polymerization, the gradient dropwise reaction makes, thereby guaranteed that cinnamic acrylic ester emulsion of the present invention has higher elasticity, contamination resistance preferably, lower film-forming temperature, and water tolerance preferably, can be widely used in the preparation process of building coating, such as external wall system, the waterproof paint system, especially need emulsion to have in elasticity and the lower application system of film-forming temperature.
Embodiment
Below by specific embodiment, the present invention is carried out to a step elaboration, but should not limit by any way the present invention.
Embodiment:
A. first by the deionized water of the compound emulsifying agent of 1.5 weight parts and 15 weight parts, join in polymerization reaction kettle, stir and heat up;
B. by the deionized water of 25 weight parts, 0.5 the compound emulsifying agent of weight part, the hard monomer of 37 weight parts (vinylbenzene that comprises 22 weight parts and 15 parts by weight of methylmethacrylate) adds in the pre-emulsification still, stir and obtain pre-emulsion after 30 minutes, weighing 10 weight parts wherein are standby as rebasing seed reaction solution;
C. the temperature of steps A polymerization reaction kettle is raised to 85-90 ℃, drop into the rebasing seed reaction solution of 10 weight part prepared in step B, add again the rebasing initiator of 1 weight part (persulphate) reaction 30-45 minute, continue to add 5 parts by weight of deionized water toward polymerization reaction kettle, slowly cool the temperature to 65 ℃, and control temperature at 65-70 ℃;
D. polymerization reaction kettle is vacuumized to 4 hours, be warming up to again 75 ℃ of residues that step B is obtained, 52.5 weight part pre-emulsions, the first constant speed from the pre-emulsification still (60 milliliters of per minutes) drops in polymerization reaction kettle, drips the initiator (persulphate) of 2 weight parts with the second constant speed (60 milliliters of per minutes) simultaneously;
When E. question response drops to 1.5 hours, suspend and drip pre-emulsion and initiator, add the butyl acrylate of 38 weight parts and the vinylformic acid of 20 weight parts in the pre-emulsification still, the organosilicon that simultaneously adds 1 weight part, stir and prepare mixed reaction solution after 55 minutes, with the 3rd constant speed (250 milliliters of per minutes), continue to drip the initiator (persulphate) of mixed reaction solution and 1 weight part simultaneously;
F. after in the pre-emulsification still, mixed reaction solution all dropwises, stop dripping, polymerization reaction kettle is incubated to 0.5-1 hour at 85-90 ℃, be cooled to 40 ℃, as required, after ammonia neutralization pH with 2 weight parts, with deionized water, regulate solid content at 25%-60%, with 100 order filter bags, filter discharging.
The elastic emulsion that this embodiment prepares, its properties is as follows: the oyster white aqueous dispersion, not stratified, without precipitation, without skinning, be uniform state after stirring; Viscosity: 200 ± 50mpa.s; PH value: 7 ± 1; Solid content: 45%.
Above embodiment is used for illustrative purposes only, but not limitation of the present invention, person skilled in the relevant technique, without departing 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 by each claim.
Claims (9)
1. an elastic 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 adjusting agent and deionized water;
Wherein, described hard monomer is at least one in vinylbenzene and methyl methacrylate;
Described soft monomer is at least one in butyl acrylate, ethyl propenoate and Isooctyl acrylate monomer;
Described functional monomer is at least one in vinylformic acid, methacrylic acid, Hydroxyethyl acrylate and hydroxyethyl methylacrylate;
Described compound emulsifying agent is that phenolic ether sulphate and alkylphenol polyoxyethylene make by weight 5.2:0.8 is composite;
Described organosilicon is that 7.5:3.5 is composite in mass ratio makes for METHYL TRICHLORO SILANE and dichloromethyl phenylsilane;
Described initiator is persulphate;
Described pH adjusting agent is the pH adjusting agent that hierarchy of control pH value is 5-9,
The latex micella particle diameter of described elastic emulsion is 80～140 nanometers, and latex particle size presents bimodal distribution in the size distribution analysis, wherein, latex micella particle diameter be 100 nanometers account for total amount 5-15%, and present normal distribution between the 80-120 nanosection; Latex micella particle diameter be 130 nanometers account for total amount 70-75%, and present normal distribution between the 120-140 nanosection.
2. a kind of elastic emulsion as claimed in claim 1, is characterized in that, described hard monomer is that 3.2:4.8 is composite in mass ratio makes for vinylbenzene and methyl methacrylate.
3. a kind of elastic emulsion as claimed in claim 1, is characterized in that, the parts by weight of described raw material are as follows:
4. the preparation method of an elastic emulsion as claimed in claim 1, is characterized in that, comprises the following steps:
A. first by quantitative compound emulsifying agent and deionized water, join in polymerization reaction kettle, stir and heat up;
B. quantitative deionized water, compound emulsifying agent, hard monomer are joined in the pre-emulsification still, stir after 30 minutes and obtain pre-emulsion, weighing 16% weight ratio wherein is standby as rebasing seed reaction solution;
C. the temperature of polymerization reaction kettle is raised to 85-90 ℃, drops into the rebasing seed reaction solution prepared in step B, then add rebasing initiator for reaction 30-45 minute, toward polymerization reaction kettle, continue to add deionized water, slowly cool the temperature to 65 ℃, and control temperature at 65-70 ℃;
D. polymerization reaction kettle is vacuumized to 4 hours, then be warming up to 75 ℃ of residue pre-emulsions that step B is prepared, drop in polymerization reaction kettle with the first constant speed from the pre-emulsification still, drip initiator with the second constant speed simultaneously;
When E. question response drops to 1.5 hours, suspend and drip pre-emulsion and initiator, add quantitative soft monomer and functional monomer in the pre-emulsification still, add organosilicon simultaneously, stir and obtain mixed reaction solution after 55 minutes, with the 3rd constant speed, toward polymerization reaction kettle, drip mixed reaction solution and initiator simultaneously;
F. after dripping end, polymerization reaction kettle, at 85-90 ℃ of insulation 0.5-1 hour, is cooled to 40 ℃, by pH adjusting agent, regulates the pH value at 5-9, with deionized water, regulate solid content at 25%-60%, with 100 order filter bags, filter discharging.
5. the preparation method of a kind of elastic emulsion as claimed in claim 4, it is characterized in that, pre-emulsification still described in step B is for opening curved blade type, the number of blade is 5 leaves, its diameter and pre-emulsification still diameter ratio are 0.66, its blade diameter is 4.2 with the ratio of depth of blade, and the mixing speed of pre-emulsification still is controlled at 850-880 rev/min.
6. the preparation method of a kind of elastic emulsion as claimed in claim 4, is characterized in that, the deionized water specific conductivity described in steps A, B, C is controlled at 0.1 μ s/cm-1 μ s/cm.
7. the preparation method of a kind of elastic emulsion as claimed in claim 4, it is characterized in that, the vacuum keep vacuumized described in step D is at the 280-300 mmhg, and described the first constant speed is 50～80 milliliters of per minutes, and described the second constant speed is 3～5 milliliters of per minutes.
8. the preparation method of a kind of elastic emulsion as claimed in claim 4, is characterized in that, described the 3rd constant speed of step e is 250～300 milliliters of per minutes.
9. the preparation method of a kind of elastic emulsion as claimed in claim 4, is characterized in that, in step F, pH adjusting agent is ammoniacal liquor, wherein NH
3content be controlled at 5-8%, described deionized water specific conductivity is controlled at 350 μ s/cm～380 μ s/cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110440798.8A CN102532401B (en) | 2011-12-23 | 2011-12-23 | Elastic emulation and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110440798.8A CN102532401B (en) | 2011-12-23 | 2011-12-23 | Elastic emulation and preparation method thereof |
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| CN102532401A CN102532401A (en) | 2012-07-04 |
| CN102532401B true CN102532401B (en) | 2014-01-08 |
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| CN103483893A (en) * | 2013-08-23 | 2014-01-01 | 无锡市金盛助剂厂 | Waterproof paint and preparation method thereof |
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| CN106590293A (en) * | 2016-12-17 | 2017-04-26 | 吴德炳 | Preparation method of weather-resistant external wall coating |
| CN106905810B (en) * | 2017-03-23 | 2019-04-16 | 北京东方雨虹防水技术股份有限公司 | A kind of preparation method of water-based elastic paint lotion, water-based elastic paint lotion and coating |
| CN107987654A (en) * | 2017-11-02 | 2018-05-04 | 佛山市顺德区巴德富实业有限公司 | A kind of lotion for elastic exterior coating material and preparation method thereof |
| CN109970901A (en) * | 2019-04-04 | 2019-07-05 | 北京西尔玛道路养护工程有限公司 | A kind of polymeric latex resin and its preparation method and application |
| CN111648133B (en) * | 2020-06-02 | 2021-06-25 | 北京建筑材料科学研究总院有限公司 | A kind of ultra-low energy consumption building alkali-resistant flame-retardant waterproof breathable agent, film and preparation method thereof |
| CN114057948B (en) * | 2021-11-15 | 2023-07-21 | 湖北省纬庆高分子科技有限公司 | Water-based acrylic acid modified resin and preparation method thereof |
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2011
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| CN102532401A (en) | 2012-07-04 |
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