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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- preparation
- add
- described step
- modification
- protective system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Paints Or Removers (AREA)
- Graft Or Block Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310672882.1A CN103740225B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of modification acrylate protective system |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310672882.1A CN103740225B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of modification acrylate protective system |
Publications (2)
Publication Number | Publication Date |
---|---|
CN103740225A CN103740225A (en) | 2014-04-23 |
CN103740225B true CN103740225B (en) | 2016-04-20 |
Family
ID=50497296
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201310672882.1A Active CN103740225B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of modification acrylate protective system |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN103740225B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104312361A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of self-crosslinked acrylate anticorrosive coating |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
-
2013
- 2013-12-12 CN CN201310672882.1A patent/CN103740225B/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN103740225A (en) | 2014-04-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104312361A (en) | Preparation method of self-crosslinked acrylate anticorrosive coating | |
EA201400861A1 (en) | APPLICATION OF POLYMERIC COMPOSITION | |
CN104945578B (en) | A kind of rubber graft copolymer and preparation method thereof of anti-dripping melt, thermoplastification | |
CN103044614A (en) | Preparation method for silane coupling agent modified acrylic ester | |
JP2012521456A5 (en) | ||
WO2015044335A3 (en) | Bicontinuous microemulsion polymerized coating for water treatment | |
CN103087255A (en) | Crosslinking fluorine modified acrylic ester nanometer polymer emulsion and preparation method thereof | |
Wang et al. | Preparation and reticulation of styrene acrylic/epoxy complex latex | |
CN103740225B (en) | A kind of preparation method of modification acrylate protective system | |
CN105037614B (en) | High-solid-content leather finishing agent prepared on basis of miniemulsion polymerization method and method thereof | |
CN111995708A (en) | Based on amphiphilic Janus SiO2Nano particle fluorine-containing polyacrylate finishing agent and preparation method thereof | |
JP2011168683A5 (en) | ||
JP2020526619A5 (en) | ||
CN104592438A (en) | Three-layer core-shell structure interpenetrating network emulsion having high adhesion force to metal substrate and synthesis method of emulsion | |
CN104031214A (en) | St/MAH-g-MMA (styrene/maleic anhydride-grafted-methyl methacrylate) graft copolymer, and preparation method and application thereof | |
CN103848634B (en) | A kind of polymer ceramic water reducer and preparation method thereof | |
CN102167772B (en) | Fluorine-containing easily processed acrylate rubber and preparation method thereof | |
CN105175654A (en) | Hexagonal boron nitride micro-constrained acrylate latex nanocomposite | |
CN105294927A (en) | Butyl acrylate/butadiene/styrene latex and preparation method thereof | |
CN102199258A (en) | Polyether modified silicon acrylic flexible resin and preparation method thereof | |
CN102504089B (en) | Preparation method of water-resistant acrylic ester core-shell emulsion | |
CN106749876A (en) | A kind of fluoroacrylic resin and preparation method thereof | |
FI3722341T3 (en) | Aqueous dispersion of copolymer particles of vinyl acetate and a cyclic ketene acetal monomer | |
CN103539880B (en) | Take fluorinated copolymer as seeded emulsion polymerization and its preparation method of assistant for emulsifying agent | |
CN108676114A (en) | A kind of synthetic method of acrylic resin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CP02 | Change in the address of a patent holder | ||
CP02 | Change in the address of a patent holder |
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. |