CN101338006A - Acrylic resin with self-crosslinking characteristic and method for preparing same - Google Patents

Acrylic resin with self-crosslinking characteristic and method for preparing same Download PDF

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Publication number
CN101338006A
CN101338006A CNA2008100301041A CN200810030104A CN101338006A CN 101338006 A CN101338006 A CN 101338006A CN A2008100301041 A CNA2008100301041 A CN A2008100301041A CN 200810030104 A CN200810030104 A CN 200810030104A CN 101338006 A CN101338006 A CN 101338006A
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CN101338006B (en
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黄帼清
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JIANGMEN PAINT FACTORY CO Ltd
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JIANGMEN PAINT FACTORY CO Ltd
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Abstract

The invention discloses acrylic resin with the self-crosslinking characteristic and a preparation method thereof. The acrylic resin is made from the raw materials with the following weight percentage of 25 percent to 30 percent of normal butanol, 10 percent to 16 percent of dimethylbenzene, 2 percent to 5 percent of pom, 4 percent to 7 percent of acrylamide, 12 percent to 18 percent of butyl methacrylate, 15 percent to 20 percent of butyl acrylate, 2 percent to 5 percent of acrylic acid, 12 percent to 16 percent of styrene, 0.1 percent to 0.3 percent of U626 antioxidants, 0.6 percent to 1.5 percent of BOP and 4 percent to 8 percent of butyl acetate. The invention can self cross link to form indissoluble and non-fusible coatings under a certain roasting temperature without the addition of cross linking agents due to containing the self-crosslinking groups, also can coordinate with the resin containing epoxy groups, hydroxyl groups and carboxy groups to prepare the coatings with different performances, therefore, the invention has the excellent application characteristic, and has a wide application range.

Description

A kind of acrylic resin and preparation method thereof with self-crosslinking characteristic
Technical field
The present invention relates to a kind of synthetic resins, specifically a kind of synthetic resins with self-crosslinking group the invention still further relates to a kind of processing method for preparing this synthetic resins.
Background technology
At present baking vanish need cooperate aminoresin could toast after fixing with acrylic resin becomes and has filming of desired properties, therefore, should use very inconveniently, and often deficiencies such as gloss, hardness, appearance effect is bad may occur because supporting aminoresin and the possible uncompatibility problem of acrylic resin make to film.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of self-crosslinkable, also can cooperate the acrylic resin that contains epoxy group(ing), hydroxyl, carboxy resin copolymerization.
Another object of the present invention is that a kind of method of producing the aforesaid propylene acid resin will be provided.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of acrylic resin with self-crosslinking characteristic, its starting material by following weight per-cent are made: propyl carbinol 25~30%, dimethylbenzene 10~16%, polyoxymethylene 2~5%, acrylamide 4~7%, butyl methacrylate 12~18%, butyl acrylate 15~20%, vinylformic acid 2~5%, vinylbenzene 12~16%, U626 oxidation inhibitor 0.1~0.3%, BOP0.6~1.5% and N-BUTYL ACETATE 4~8%;
A kind of method of producing acrylic resin, its step is as follows:
1): take by weighing various raw materials in proportion;
2): in first material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid, 50%U626,50% acrylamide and 20% propyl carbinol and stir temperature requirement in jar≤35 ℃; Can add water coolant according to actual needs lowers the temperature;
3): in second material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid and 50%U626 and stir temperature requirement in jar≤35 ℃; Can add water coolant according to actual needs lowers the temperature;
4): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 3rd material-compound tank;
5): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 4th material-compound tank;
6): in reactor, drop into (account for and take by weighing raw material weight) 80% propyl carbinol, whole toluene, whole polyoxymethylene and 50% acrylamide and fully stir;
7): in first material-compound tank, drop into (account for and take by weighing raw material weight) 40%BPO and stir into even phase transparent liquid, and adopt the strainer of 1 μ m to filter;
8): after step 7) is finished 20 minutes, the material in the reactor is heated to 117~122 ℃, and liquid average rate in 75~85min that step 7) makes is splashed in the reactor, keeping reactor in the dropping process is reflux state;
9): when step 8) was finished preceding 20 minutes, will (account for and take by weighing raw material weight) 40%BPO and join to mix in second material-compound tank and become to spare the phase transparent liquid;
10): after step 8) is finished, be about to the liquid that step 9) makes and in 75~85min average rate, splash in the reactor, be incubated 30min finishing after and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
11): after insulation was finished, liquid average rate in 15~20min that step 4) is made splashed in the reactor, is incubated 30min after finishing and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
12): after insulation was finished, the liquid that step 5) is made splashed in the reactor in 15~20min, and is incubated 3h under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
13): after insulation is finished, the formation resin of lowering the temperature, and resin viscosity is controlled at: .25 ℃ of 8~25 seconds/lattice; The water displacement that we can write down reactor after forming resin comes the reaction effect of testing product;
14): resin is controlled at 80 ℃ temperature bottom discharge, and adopts 10 μ m or following strainer to filter, detect the outward appearance of resin and acid value simultaneously and pack after qualified.
The invention has the beneficial effects as follows: the present invention is owing to contain the group of self-crosslinkable, thereby need not add linking agent self-crosslinking under certain storing temperature in addition and form insoluble, infusible filming, also can cooperate the resin that contains epoxide group, oh group, carboxylic group to prepare filming of different performance, thereby having very excellent service performance, Application Areas is very extensive.
Embodiment
A kind of acrylic resin with self-crosslinking characteristic, its starting material by following weight per-cent are made: propyl carbinol 25~30%, dimethylbenzene 10~16%, polyoxymethylene 2~5%, acrylamide 4~7%, butyl methacrylate 12~18%, butyl acrylate 15~20%, vinylformic acid 2~5%, vinylbenzene 12~16%, U626 oxidation inhibitor 0.1~0.3%, BOP0.6~1.5% and N-BUTYL ACETATE 4~8%.
The polyoxymethylene that the present invention adopts is German imported raw material, BPO requires to produce for French atropic Filler company, in addition, described propyl carbinol water content≤0.1%, purity 〉=99.5%, described basic butyl acrylate, butyl acrylate, vinylformic acid and cinnamic purity 〉=99%.
A kind of optimum weight per-cent: propyl carbinol 27%, dimethylbenzene 12%, polyoxymethylene 3%, acrylamide 5%, butyl methacrylate 14%, butyl acrylate 16%, vinylformic acid 3%, vinylbenzene 14%, U626 oxidation inhibitor 0.2%, BOP0.8% and N-BUTYL ACETATE 5% with acrylic resin of self-crosslinking characteristic.
A kind of method of producing acrylic resin, its step is as follows:
1): take by weighing various raw materials in proportion;
2): in first material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid, 50%U626,50% acrylamide and 20% propyl carbinol and stir temperature requirement in jar≤35 ℃;
3): in second material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid and 50%U626 and stir temperature requirement in jar≤35 ℃;
4): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 3rd material-compound tank;
5): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 4th material-compound tank;
6): in reactor, drop into (account for and take by weighing raw material weight) 80% propyl carbinol, whole toluene, whole polyoxymethylene and 50% acrylamide and fully stir;
7): in first material-compound tank, drop into (account for and take by weighing raw material weight) 40%BPO and stir into even phase transparent liquid, and adopt the strainer of 1 μ m to filter;
8): after step 7) is finished 20 minutes, the material in the reactor is heated to 117~122 ℃, and liquid average rate in 75~85min that step 7) makes is splashed in the reactor, keeping reactor in the dropping process is reflux state;
9): when step 8) was finished preceding 20 minutes, will (account for and take by weighing raw material weight) 40%BPO and join to mix in second material-compound tank and become to spare the phase transparent liquid;
10): after step 8) is finished, be about to the liquid that step 9) makes and in 75~85min average rate, splash in the reactor, be incubated 30min finishing after and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
11): after insulation was finished, liquid average rate in 15~20min that step 4) is made splashed in the reactor, is incubated 30min after finishing and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
12): after insulation was finished, the liquid that step 5) is made splashed in the reactor in 15~20min, and is incubated 3h under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
13): after insulation is finished, the formation resin of lowering the temperature, and resin viscosity is controlled at: 25 ℃ of 8~25 seconds/lattice;
14): resin is controlled at 80 ℃ temperature bottom discharge, and adopts 10 μ m or following strainer to filter.
This tree has the structure expression of fat to be:
Figure A20081003010400101
The present invention is owing to contain the group of self-crosslinkable, thereby need not add linking agent self-crosslinking under certain storing temperature in addition and form insoluble, infusible filming, also can cooperate the resin that contains epoxide group, oh group, carboxylic group to prepare filming of different performance, thereby having very excellent service performance, Application Areas is very extensive.

Claims (4)

1. acrylic resin with self-crosslinking characteristic, it is characterized in that: the starting material by following weight per-cent are made: propyl carbinol 25~30%, dimethylbenzene 10~16%, polyoxymethylene 2~5%, acrylamide 4~7%, butyl methacrylate 12~18%, butyl acrylate 15~20%, vinylformic acid 2~5%, vinylbenzene 12~16%, U626 oxidation inhibitor 0.1~0.3%, BOP0.6~1.5% and N-BUTYL ACETATE 4~8%.
2. a kind of acrylic resin with self-crosslinking characteristic according to claim 1 is characterized in that: described propyl carbinol water content≤0.1%, purity 〉=99.5%.
3. a kind of acrylic resin with self-crosslinking characteristic according to claim 1 is characterized in that: described basic butyl acrylate, butyl acrylate, vinylformic acid and cinnamic purity 〉=99%.
4. method of producing the described acrylic resin of claim 1, it is characterized in that: this method comprises the steps:
1): take by weighing various raw materials in proportion;
2): in first material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid, 50%U626,50% acrylamide and 20% propyl carbinol and stir temperature requirement in jar≤35 ℃;
3): in second material-compound tank, add (account for and take by weighing raw material weight) 50% butyl methacrylate, 50% butyl acrylate, 50% vinylbenzene, 50% vinylformic acid and 50%U626 and stir temperature requirement in jar≤35 ℃;
4): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 3rd material-compound tank;
5): adding (account for and take by weighing raw material weight) 10%BPO and 50% N-BUTYL ACETATE stir in the 4th material-compound tank;
6): in reactor, drop into (account for and take by weighing raw material weight) 80% propyl carbinol, whole toluene, whole polyoxymethylene and 50% acrylamide and fully stir;
7): in first material-compound tank, drop into (account for and take by weighing raw material weight) 40%BPO and stir into even phase transparent liquid, and adopt the strainer of 1 μ m to filter;
8): after step 7) is finished 20 minutes, the material in the reactor is heated to 117~122 ℃, and liquid average rate in 75~85min that step 7) makes is splashed in the reactor, keeping reactor in the dropping process is reflux state;
9): when step 8) was finished preceding 20 minutes, will (account for and take by weighing raw material weight) 40%BPO and join to mix in second material-compound tank and become to spare the phase transparent liquid;
10): after step 8) is finished, be about to the liquid that step 9) makes and in 75~85min average rate, splash in the reactor, be incubated 30min finishing after and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
11): after insulation was finished, liquid average rate in 15~20min that step 4) is made splashed in the reactor, is incubated 30min after finishing and under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
12): after insulation was finished, the liquid that step 5) is made splashed in the reactor in 15~20min, and is incubated 3h under 120~122 ℃ of temperature, and the maintenance reactor is a reflux state;
13): after insulation is finished, the formation resin of lowering the temperature, and resin viscosity is controlled at: .25 ℃ of 8~25 seconds/lattice;
14): resin is controlled at 80 ℃ temperature bottom discharge, and adopts 10 μ m or following strainer to filter.
CN2008100301041A 2008-08-11 2008-08-11 Acrylic resin with self-crosslinking characteristic and method for preparing same Expired - Fee Related CN101338006B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732120A (en) * 2012-07-20 2012-10-17 深圳市亿铖达工业有限公司 Environment-friendly three-proofing paint
CN103469242A (en) * 2013-05-07 2013-12-25 西北师范大学 Butyl methacrylate-butyl acrylate-styrene terpolymer resin, and synthetic method and application thereof
CN104910690A (en) * 2014-03-13 2015-09-16 株式会社理光 Ink, inkjet recording method, and recorded matter

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100396707C (en) * 2005-08-16 2008-06-25 广东鸿昌化工有限公司 Microemulsion of fluorin containing crylic acid of self-crosslink in normal temperature and its production method
CN101050260A (en) * 2007-04-14 2007-10-10 广西民族大学 High polymer with self-crosslinked functional radicle and preparation method
CN101220563B (en) * 2007-11-22 2010-12-15 复旦大学 Environment protection type pigment resin printing adhesive agent capable of self crosslinking at low-temperature, and preparation thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732120A (en) * 2012-07-20 2012-10-17 深圳市亿铖达工业有限公司 Environment-friendly three-proofing paint
CN103469242A (en) * 2013-05-07 2013-12-25 西北师范大学 Butyl methacrylate-butyl acrylate-styrene terpolymer resin, and synthetic method and application thereof
CN104910690A (en) * 2014-03-13 2015-09-16 株式会社理光 Ink, inkjet recording method, and recorded matter
CN107513308A (en) * 2014-03-13 2017-12-26 株式会社理光 Aqueous ink for inkjet recording, ink jet recording method, ink mist recording thing

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