CN102746759B - Method for preparing polyacrylate amino water-based baking varnish - Google Patents
Method for preparing polyacrylate amino water-based baking varnish Download PDFInfo
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- CN102746759B CN102746759B CN201110101672.8A CN201110101672A CN102746759B CN 102746759 B CN102746759 B CN 102746759B CN 201110101672 A CN201110101672 A CN 201110101672A CN 102746759 B CN102746759 B CN 102746759B
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- emulsion
- monomer
- deionized water
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229920000058 polyacrylate Polymers 0.000 title claims abstract description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 3
- 239000002966 varnish Substances 0.000 title abstract 2
- 239000003999 initiator Substances 0.000 claims abstract description 36
- 239000000839 emulsion Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000000178 monomer Substances 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000003995 emulsifying agent Substances 0.000 claims description 18
- 210000000160 tapetum lucidum Anatomy 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 238000009413 insulation Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 229920000877 Melamine resin Polymers 0.000 claims description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 8
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000004945 emulsification Methods 0.000 claims description 8
- 238000009775 high-speed stirring Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 3
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical group [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000007921 spray Substances 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000004383 yellowing Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 10
- 239000004342 Benzoyl peroxide Substances 0.000 description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 description 6
- 229920002125 Sokalan® Polymers 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000004446 light reflex Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention relates to a method for preparing a polyacrylate amino water-based baking varnish, which comprises the steps of a pre-emulsion preparation, an initiator aqueous solution preparation, cross-linking reaction and the like. The polyacrylate resin possessing a linear molecular structure is changed to the polyacrylate resin possessing a netted molecular structure, the compactness of a film and the protective effect as well as the adhesion on a substrate can be improved; the undesirable phenomena of reflective film blackening, mouldiness and the like due to no water resistance performance, no salt spray resistance performance, no aging resistance performance and easy yellowing of a focus layer can be completely changed.
Description
Technical field
The present invention relates to a kind of modification of focus layer polyacrylic acid resinoid of tapetum lucidum, particularly the preparation method of the amino water-based stoving paint of polyacrylic ester for a kind of tapetum lucidum.
Background technology
Tapetum lucidum is to utilize optical principle, light reflex reflection can be got back to the PVC film of a kind of special construction at light source place.By the good thin film layer of weather resistance, tiny glass beads layer, focus layer, reflecting layer, adhesive-layer and peel ply form.Tapetum lucidum is mainly used in guide plate, the direction board of various road and rails, airport, mine safety board, scenery, trade mark, place name sign, car plate etc.
The focus layer of existing tapetum lucidum is polyacrylic acid resinoid, it passes through high degree of accuracy coating machine using soot layer as base material, be coated with, make focus layer be wrapped in glass microballon surface, directly contact with reflecting layer, due to its hydrophilic characteristic, easily cause that tapetum lucidum is not water-fast, not salt spray resistance, blackout, mouldy, the retro-reflecting coefficient that reduced tapetum lucidum, this series of problems not yet has good solution at present.
Summary of the invention
The object of the invention is to solve above-mentioned deficiency, the preparation method of the amino water-based stoving paint of a kind of tapetum lucidum polyacrylic ester is provided.
The technical scheme that realizes the object of the invention is: a kind of tapetum lucidum by preparation method's concrete technology step of the amino water-based stoving paint of polyacrylic ester is:
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass percentage ratio is: methyl methacrylate 20-40%, butyl acrylate 30-60%, vinylformic acid 10-20%, each monomer total amount is 100%, deionized water quality is 10% of monomer total amount, add emulsifying agent, emulsifying agent quality is the 3-6% of monomer total mass, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water and initiator, its quality is respectively 10% and 0.3-1% of monomer total mass in step (1), is stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion and each 1/3 amount of initiator solution adds in reactor, stir, be warming up to 60-90 DEG C, insulation reaction 1h at this temperature;
(4), then in 2-3h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 10-15% of total mass in reactor, stir, filter discharging.
The preparation method of polyacrylate dispersion for above-mentioned tapetum lucidum, described emulsifying agent is allyloxy Nonyl pheno (10) ether.
The preparation method of polyacrylate dispersion for above-mentioned tapetum lucidum, described initiator is superoxide.
The preparation method of polyacrylate dispersion for above-mentioned tapetum lucidum, is warming up to 80 DEG C in described step (3).Reaction mechanism of the present invention is acrylic acid ester emulsion type free radicals copolymerization reaction, under the effect through the acrylate monomer of Over emulsfication at peroxide initiator, through chain several radical polymerization stages of initiation → chainpropagation → chain termination, finally completes reaction.
The present invention has positive effect: due to the employing of technique scheme, compared with prior art, tool of the present invention has the following advantages:
(1), become network molecular structure by the polyacrylate resin of former linearity molecular structure, the compactness of raising paint film and provide protection and the sticking power to ground;
(2), thoroughly changed not water-fast due to focus layer, not salt spray resistance, not ageing-resistant and easy xanthochromia and the tapetum lucidum blackout that causes, the bad phenomenon such as mouldy.
Embodiment
(embodiment 1)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 30kg, butyl acrylate 60kg, vinylformic acid 10kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 3kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 0.3kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 37.7kg and initiator solution 3.43kg adds in reactor, stir, be warming up to 60 DEG C, insulation reaction 1h at this temperature;
(4), then in 2h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 12.3kg of total mass in reactor, stir, filter discharging.
(embodiment 2)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 25kg, butyl acrylate 60kg, vinylformic acid 15kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 4kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 0.5kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 38kg and initiator solution 3.5kg adds in reactor, stir, be warming up to 80 DEG C, insulation reaction 1h at this temperature;
(4), then in 2.5h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 14.94kg of total mass in reactor, stir, filter discharging.
(embodiment 3)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 25kg, butyl acrylate 63kg, vinylformic acid 12kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 6kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 1kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 38.7kg and initiator solution 3.67kg adds in reactor, stir, be warming up to 90 DEG C, insulation reaction 1h at this temperature;
(4), then in 3h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 19.05kg of total mass in reactor, stir, filter discharging.
(embodiment 4)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 30kg, butyl acrylate 50kg, vinylformic acid 20kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 3kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 0.3kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 37.7kg and initiator solution 3.43kg adds in reactor, stir, be warming up to 60 DEG C, insulation reaction 1h at this temperature;
(4), then in 2h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 12.3kg of total mass in reactor, stir, filter discharging.
(embodiment 5)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 20kg, butyl acrylate 60kg, vinylformic acid 20kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 4kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 0.5kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 38kg and initiator solution 3.5kg adds in reactor, stir, be warming up to 80 DEG C, insulation reaction 1h at this temperature;
(4), then in 2.5h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 14.94kg of total mass in reactor, stir, filter discharging.
(embodiment 6)
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass is: methyl methacrylate 50kg, butyl acrylate 30kg, vinylformic acid 20kg, deionized water 10kg, add emulsifying agent, emulsifying agent allyloxy Nonyl pheno (10) ether quality is 6kg, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water 10kg and initiator benzoyl peroxide 1kg, be stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion 38.7kg and initiator solution 3.67kg adds in reactor, stir, be warming up to 90 DEG C, insulation reaction 1h at this temperature;
(4), then in 3h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 19.05kg of total mass in reactor, stir, filter discharging.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. a preparation method for the amino water-based stoving paint of polyacrylic ester for tapetum lucidum, concrete technology step is:
(1), prepare pre-emulsion, taking monomer and deionized water mixes, each monomer mass percentage ratio is: methyl methacrylate 20-40%, butyl acrylate 30-60%, vinylformic acid 10-20%, each monomer total amount is 100%, deionized water quality is 10% of monomer total amount, add emulsifying agent, emulsifying agent quality is the 3-6% of monomer total mass, high-speed stirring emulsification;
(2), prepare initiator solution, take deionized water and initiator, its quality is respectively 10% and 0.3-1% of monomer total mass in step (1), is stirred to abundant dissolving;
(3), get above-mentioned pre-emulsion and each 1/3 amount of initiator solution adds in reactor, stir, be warming up to 60-90 DEG C, insulation reaction 1h at this temperature;
(4), then in 2-3h, drip remaining pre-emulsion and initiator solution, dropwise rear insulation reaction 2h, cooling;
(5), add melamineformaldehyde resin, quality is the 10-15% of total mass in reactor, stir, filter discharging.
2. the preparation method of polyacrylate dispersion for tapetum lucidum according to claim 1, is characterized in that: described emulsifying agent is allyloxy Nonyl pheno (10) ether.
3. the preparation method of polyacrylate dispersion for tapetum lucidum according to claim 1, is characterized in that: described initiator is superoxide.
4. the preparation method of polyacrylate dispersion for tapetum lucidum according to claim 1, is characterized in that: in described step (3), be warming up to 80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110101672.8A CN102746759B (en) | 2011-04-22 | 2011-04-22 | Method for preparing polyacrylate amino water-based baking varnish |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110101672.8A CN102746759B (en) | 2011-04-22 | 2011-04-22 | Method for preparing polyacrylate amino water-based baking varnish |
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| Publication Number | Publication Date |
|---|---|
| CN102746759A CN102746759A (en) | 2012-10-24 |
| CN102746759B true CN102746759B (en) | 2014-09-10 |
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| CN201110101672.8A Expired - Fee Related CN102746759B (en) | 2011-04-22 | 2011-04-22 | Method for preparing polyacrylate amino water-based baking varnish |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1333299A (en) * | 2000-07-10 | 2002-01-30 | 成都亚恩科技实业有限公司 | Process for preparing acrylic ester elastic emulsion |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1333299A (en) * | 2000-07-10 | 2002-01-30 | 成都亚恩科技实业有限公司 | Process for preparing acrylic ester elastic emulsion |
Non-Patent Citations (2)
| Title |
|---|
| 水性丙烯酸树脂的合成及其氨基烘漆研制;闫福安;《武汉化工学院学报》;20031231;第25卷(第2期);第8页 * |
| 闫福安.水性丙烯酸树脂的合成及其氨基烘漆研制.《武汉化工学院学报》.2003,第25卷(第2期),8. |
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| CN102746759A (en) | 2012-10-24 |
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Application publication date: 20121024 Assignee: JIANGSU QUNYUE NEW MATERIALS CO., LTD. Assignor: Changzhou Huawei Advanced Material Co., Ltd Contract record no.: 2015320000192 Denomination of invention: Method for preparing polyacrylate amino water-based baking varnish Granted publication date: 20140910 License type: Exclusive License Record date: 20150415 |
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