CN103740225B - A kind of preparation method of modification acrylate protective system - Google Patents
A kind of preparation method of modification acrylate protective system Download PDFInfo
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- CN103740225B CN103740225B CN201310672882.1A CN201310672882A CN103740225B CN 103740225 B CN103740225 B CN 103740225B CN 201310672882 A CN201310672882 A CN 201310672882A CN 103740225 B CN103740225 B CN 103740225B
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Abstract
A kind of preparation method of modification acrylate protective system, comprise the preparation of polyimide solution, the preparation of acrylic ester emulsion, preparation three processes of modification acrylate protective system, through modified acrylic ester polymer, there are excellent water tolerance and preservative property.
Description
Technical field
The present invention relates to a kind of preparation method of modification acrylate protective system, belong to chemical field.
Technical background
Acrylic ester emulsion has good sticking power, weathering resistance, is widely used because of its excellent performance, is applied to multiple fields such as coating, sizing agent and floor polisher.Current acrylate is mainly solvent type, big for environment pollution, and the water tolerance of water-and acrylate and less stable, therefore, the study on the modification of acrylate is become highly significant, this patent adopts fluorine-bearing modifier to acrylatcs systems modification, and obtained fluorinated acrylate has excellent water tolerance and oxidation-resistance.
Summary of the invention
The object of this invention is to provide a kind of preparation method of modification acrylate protective system, the acrylate obtained has excellent water tolerance and preservative property.
For realizing above object, the preparation method of a kind of modification acrylate protective system of the present invention, its step is specially:
(1) preparation of polyimide solution: 4,4'-dioctyl diphenylamine (ODA) is at N, fully dissolve in N-N,N-DIMETHYLACETAMIDE, add trimellitic acid 1,2-anhydride (TMA), be stirred to homogeneous phase, add toluene, reflux divides water, continue heating and separate toluene, the solid of separating out after cooling carries out suction filtration oven dry, obtains polyimide powder;
(2) preparation of acrylic ester emulsion: distilled water, emulsifier sodium lauryl sulfate (SDS) are stirred 20min and obtain mixing solutions; Temperature is risen to 82 DEG C, add initiator ammonium persulfate (APS); Performed polymer is prepared for raw material, reaction 2h with methyl methacrylate (MMA), methyl acrylate (MA), vinyl cyanide (AN);
(3) preparation of modification acrylate protective system: rise to 90 DEG C, adds dodecafluoroheptyl methacrylate (FA), polyimide powder, carries out modification to acrylatcs systems, stirring reaction 2h in above-mentioned performed polymer; Add PH conditioning agent sodium bicarbonate adjustment system pH to 7, reaction 10min, obtained modified acrylate emulsion.
In described step (1), the mass ratio of TMA and ODA is 1:0.6-1.
In described step (2), mixing speed is 550r/min.
In described step (2), the mass ratio of MMA, MA and AN is 15:10:1.
In described step (3), the mass ratio of FA, polyimide powder, performed polymer is 1-10:1-10:100.
In described step (3), mixing speed is 1000r/min.
The beneficial effect that the present invention produces is, the present invention adopts fluorine-bearing modifier to acrylatcs systems modification, the fluorinated acrylate made has excellent water tolerance and oxidation-resistance, and polyimide molecule chain contains the larger phenyl ring of rigidity and imide ring, and cause the reactive force of polyimide molecule interchain stronger by the existence of imido grpup isopolarity group, cause the molecular chain of polyimide tightly packed, therefore polyimide modified acrylate has outstanding high-low temperature resistant and antiseptic property.
Embodiment
Embodiment 1:
A preparation method for modification acrylate protective system, its step is specially: be weight part below
(1) preparation of polyimide solution: by 0.6 part 4,4'-dioctyl diphenylamine (ODA) is at N, fully dissolve in N-N,N-DIMETHYLACETAMIDE, add 1 part of trimellitic acid 1,2-anhydride (TMA), be stirred to homogeneous phase, add toluene, reflux divides water, continue heating and separate toluene, the solid of separating out after cooling carries out suction filtration oven dry, obtains polyimide powder;
(2) preparation of acrylic ester emulsion: 30 parts of distilled water, 4 parts of emulsifier sodium lauryl sulfates (SDS) are stirred 20min and obtained mixing solutions, and mixing speed is 550r/min; Temperature is risen to 82 DEG C, add 0.3 part of initiator ammonium persulfate (APS); Performed polymer is prepared, reaction 2h for raw material with 30 parts of methyl methacrylates (MMA), 20 parts of methyl acrylates (MA), 2 parts of vinyl cyanide (AN);
(3) preparation of modification acrylate protective system: rise to 90 DEG C, 1 part of dodecafluoroheptyl methacrylate (FA), 10 parts of polyimide powders are added in 100 parts of performed polymers, carry out modification to acrylatcs systems, stirring reaction 2h, mixing speed is 1000r/min; Add PH conditioning agent sodium bicarbonate adjustment system pH to 7, reaction 10min, obtained modified acrylate emulsion.
Embodiment 2:
A preparation method for modification acrylate protective system, its step is specially: be weight part below
(1) preparation of polyimide solution: by 0.8 part 4,4'-dioctyl diphenylamine (ODA) is at N, fully dissolve in N-N,N-DIMETHYLACETAMIDE, add 1 part of trimellitic acid 1,2-anhydride (TMA), be stirred to homogeneous phase, add toluene, reflux divides water, continue heating and separate toluene, the solid of separating out after cooling carries out suction filtration oven dry, obtains polyimide powder;
(2) preparation of acrylic ester emulsion: 30 parts of distilled water, 4 parts of emulsifier sodium lauryl sulfates (SDS) are stirred 20min and obtained mixing solutions, and mixing speed is 550r/min; Temperature is risen to 82 DEG C, add 0.3 part of initiator ammonium persulfate (APS); Performed polymer is prepared, reaction 2h for raw material with 30 parts of methyl methacrylates (MMA), 20 parts of methyl acrylates (MA), 2 parts of vinyl cyanide (AN);
(3) preparation of modification acrylate protective system: rise to 90 DEG C, 5 parts of dodecafluoroheptyl methacrylates (FA), 5 parts of polyimide powders are added in 100 parts of performed polymers, carry out modification to acrylatcs systems, stirring reaction 2h, mixing speed is 1000r/min; Add PH conditioning agent sodium bicarbonate adjustment system pH to 7, reaction 10min, obtained modified acrylate emulsion.
Embodiment 3:
A preparation method for modification acrylate protective system, its step is specially: be weight part below
(1) preparation of polyimide solution: by 1 part 4,4'-dioctyl diphenylamine (ODA) is at N, fully dissolve in N-N,N-DIMETHYLACETAMIDE, add 1 part of trimellitic acid 1,2-anhydride (TMA), be stirred to homogeneous phase, add toluene, reflux divides water, continue heating and separate toluene, the solid of separating out after cooling carries out suction filtration oven dry, obtains polyimide powder;
(2) preparation of acrylic ester emulsion: 30 parts of distilled water, 4 parts of emulsifier sodium lauryl sulfates (SDS) are stirred 20min and obtained mixing solutions, and mixing speed is 550r/min; Temperature is risen to 82 DEG C, add 0.3 part of initiator ammonium persulfate (APS); Performed polymer is prepared, reaction 2h for raw material with 30 parts of methyl methacrylates (MMA), 20 parts of methyl acrylates (MA), 2 parts of vinyl cyanide (AN);
(3) preparation of modification acrylate protective system: rise to 90 DEG C, 10 parts of dodecafluoroheptyl methacrylates (FA), 1 part of polyimide powder is added in 100 parts of performed polymers, carry out modification to acrylatcs systems, stirring reaction 2h, mixing speed is 1000r/min; Add PH conditioning agent sodium bicarbonate adjustment system pH to 7, reaction 10min, obtained modified acrylate emulsion.
Claims (1)
1. a preparation method for modification acrylate protective system, is characterized in that: step is as follows:
(1) preparation of polyimide powder: 4,4'-dioctyl diphenylamine (ODA) is at N, fully dissolve in N-N,N-DIMETHYLACETAMIDE, add trimellitic acid 1,2-anhydride (TMA), be stirred to homogeneous phase, add toluene, reflux divides water, continue heating and separate toluene, the solid of separating out after cooling carries out suction filtration oven dry, obtains polyimide powder;
(2) preparation of acrylic ester emulsion: distilled water, emulsifier sodium lauryl sulfate (SDS) are stirred 20min and obtain mixing solutions; Temperature is risen to 82 DEG C, add initiator ammonium persulfate (APS); Performed polymer is prepared for raw material, reaction 2h with methyl methacrylate (MMA), methyl acrylate (MA), vinyl cyanide (AN);
(3) preparation of modification acrylate protective system: rise to 90 DEG C, adds dodecafluoroheptyl methacrylate (FA), polyimide powder, carries out modification to acrylatcs systems, stirring reaction 2h in above-mentioned performed polymer; Add pH adjusting agent sodium bicarbonate adjustment system pH to 7, reaction 10min, obtained modified acrylate emulsion;
In described step (1), the mass ratio of TMA and ODA is 1:0.6-1;
In described step (2), mixing speed is 550r/min;
In described step (2), the mass ratio of MMA, MA and AN is 15:10:1;
In described step (3), the mass ratio of FA, polyimide powder, performed polymer is 1-10:1-10:100;
In described step (3), mixing speed is 1000r/min.
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| CN201310672882.1A CN103740225B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of modification acrylate protective system |
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| CN103740225B true CN103740225B (en) | 2016-04-20 |
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| KR100963376B1 (en) * | 2007-02-09 | 2010-06-14 | 주식회사 엘지화학 | Method for preparing polyimide and polyimide prepared by the same method |
| CN102220085B (en) * | 2011-05-09 | 2013-04-17 | 东华大学 | Polyimide coating with high-temperature resistance and preparation method thereof |
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Address after: 266000 Qingdao science and technology, Huangdao District, Shandong, No. two road, No. 167 Patentee after: Qingdao Advanced Marine Material Technology Co., Ltd. Address before: 266101, Qingdao Road, Zhuzhou District, Shandong, Laoshan, 143 Patentee before: Qingdao Advanced Marine Material Technology Co., Ltd. |