CN107216761A - The preparation method of the water soluble acrylic resin of high solid - Google Patents
The preparation method of the water soluble acrylic resin of high solid Download PDFInfo
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- CN107216761A CN107216761A CN201710580294.3A CN201710580294A CN107216761A CN 107216761 A CN107216761 A CN 107216761A CN 201710580294 A CN201710580294 A CN 201710580294A CN 107216761 A CN107216761 A CN 107216761A
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- water soluble
- soluble acrylic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
- C09D5/028—Pigments; Filters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses a kind of preparation method of the water soluble acrylic resin of high solid, it is reacted under initiator effect and obtained by the mix monomer of acrylic acid, styrene, butyl acrylate, methyl acrylate, methyl methacrylate and hydroxypropyl acrylate.The present invention synthesizes the water-based acrylic resin of large arch dam, high-hydrophilic using solvent method by the preferably synthetic technique of many experiments, and is configured to water soluble acrylic acid amido coatings with it, so as to can reach a large amount of purposes for reducing VOC in coating, the feature of environmental protection is strong.The water soluble acrylic acid amido coatings film prepared has excellent adhesive force, and glossiness is good, and with excellent hardness and impact resistance, achieves extraordinary technique effect.
Description
Technical field
The present invention relates to a kind of coating, and in particular to a kind of preparation of the water soluble acrylic resin of environmentally friendly high solid
Method, belongs to technical field of polymer materials.
Background technology
In recent years, with the continuous enhancing of people's environmental consciousness, many countries have issued control VOC
(VOC) volatility in environmental regulation, research and development environment-friendly coating and application techniques, reduction coating material production and construction
Organic compound (VOC), it has also become the center of domestic and international most of coating and resin design work, therefore high solid coating,
Water paint, powdery paints, radiation curable coating are more and more widely paid attention to.Wherein high solid coating can be saved because of it
Coating material production and solvent in, reduce pollution；Water paint using water and hydrophilic solvent because that, as diluent, can be subtracted
Control VOC (VOC) discharge less, thus important directions and study hotspot as paint development.
But there is presently no the coating with high solid coating and water paint two-fold advantage.The present invention uses solvent
Method synthesis large arch dam, the water-based acrylic resin of high-hydrophilic, and water soluble acrylic acid amido coatings are configured to it, so as to reach
A large amount of purposes for reducing VOC in coating.
The content of the invention
Goal of the invention：The purpose of the present invention is in view of the shortcomings of the prior art, component, the present invention to be screened by many experiments
The advantage of comprehensive high solid coating and water paint, the water soluble acrylic acid tree of large arch dam, high-hydrophilic is synthesized using solvent method
Fat, and water soluble acrylic acid amido coatings are configured to it, so as to reach a large amount of purposes for reducing VOC in coating.
Technical scheme, to realize object above, the technical solution adopted by the present invention is：
A kind of preparation method of the water soluble acrylic resin of high solid, it comprises the following steps：
(1) reaction dissolvent is added in the four-hole boiling flask equipped with agitator, condenser, thermometer and constant pressure funnel；
Acrylic acid, styrene, butyl acrylate, methyl acrylate, methyl methacrylate and hydroxypropyl acrylate are well mixed, obtained
Initiator, is then dissolved in mix monomer by mix monomer；
(2) reaction dissolvent in four-hole boiling flask is warming up to after backflow, the mix monomer for being dissolved with initiator is added dropwise, during dropwise addition
Between be 4~5 hours, maintain the reflux for temperature, continue to react 2~3 hours, then initiator was added every 1 hour, add after end,
50~70 DEG C are cooled to, dimethyl ethanol amine neutralizer is added, continues to stir 0.5~1.5 hour, water is then added, by resin
It is deployed into the solid water soluble acrylic resin containing for 60~80%.
Preferably, the preparation method of the water soluble acrylic resin of above-described a kind of high solid, it is wrapped
Include following steps：
(1) ethylene glycol fourth is added in the four-hole boiling flask equipped with agitator, condenser, thermometer and constant pressure funnel
Ether；Acrylic acid, styrene, butyl acrylate, methyl acrylate, methyl methacrylate and hydroxypropyl acrylate are mixed equal
It is even, mix monomer is obtained, then initiator cumyl peroxide is dissolved in mix monomer；
(2) reaction dissolvent in four-hole boiling flask is warming up to after backflow, the mix monomer for being dissolved with initiator is added dropwise, during dropwise addition
Between be 4~5 hours, maintain the reflux for temperature, continue to react 2 hours, then initiator was added every 1 hour, secondary draw is added altogether
Agent is sent out, is added after end, 60 DEG C are cooled to, dimethyl ethanol amine neutralizer is added, continues to stir 0.5 hour, then adds water,
Resin is deployed into the solid water soluble acrylic resin containing for 70%.
Preferably, the preparation method of the water soluble acrylic resin of above-described high solid a kind of, second two
The weight percentage of alcohol butyl ether is that the weight percentage of 15~25%, acrylic acid is the weight percent of 5~10%, styrene
Content is that the weight percentage of 5~10%, butyl acrylate is that the weight percentage of 15~36%, methyl acrylate is 3
~10%, the weight percentage of methyl methacrylate be the weight percentage of 3~8%, hydroxypropyl acrylate be 20~
40%th, the weight percentage of cumyl peroxide is 1~10%.
A kind of water soluble acrylic acid amido coatings, it include water soluble acrylic resin, amino resins, dispersant, defoamer,
Wetting agent, pigment, levelling agent, butyl glycol ether；
Described water soluble acrylic resin is prepared by any one of claims 1 to 3 methods described.
Preferably, above-described a kind of water soluble acrylic acid amido coatings, it is by water soluble acrylic resin 60
~120 parts, 10~24 parts of amino resins, 0.5~1 part of dispersant, 0.2~0.4 part of defoamer, 0.2~0.4 part of wetting agent, face
25~40 parts of material, 0.2~0.4 part of levelling agent, 10~20 parts of 3~6 parts of butyl glycol ether and water are made.Described water soluble propene
Acid resin is prepared by any one of claims 1 to 3 methods described.
Beneficial effect：Compared to the prior art, the present invention has the following advantages：
The present invention obtains optimal raw material by many experiments screening and constitutes and match, the comprehensive high solid coating of the present invention
With the advantage of water paint, by the preferably synthetic technique of many experiments, using solvent method synthesize large arch dam, high-hydrophilic it is aqueous
Acrylic resin, and it is configured to it water soluble acrylic acid amido coatings, so that a large amount of purposes for reducing VOC in coating are can reach,
The feature of environmental protection is strong.And the water soluble acrylic acid amido coatings film prepared has excellent adhesive force, and glossiness is good, and has
Excellent hardness and impact resistance, achieve extraordinary technique effect.
Embodiment
Embodiment 1
1st, a kind of preparation method of the water soluble acrylic resin of high solid, it comprises the following steps：
(1) quantitative second two is added in the four-hole boiling flask equipped with agitator, condenser, thermometer and constant pressure funnel
23 parts of alcohol butyl ether；Again by 9.37 parts of acrylic acid, 9.55 parts of styrene, 3.54 parts of butyl acrylate, 8.73 parts of methyl acrylate, first
7 parts of base methyl acrylate, 25.6 parts of hydroxypropyl acrylate are well mixed, and obtain mix monomer；Then it is initiator peroxidating two is different
4.9 parts of propyl benzene (DCP) is dissolved in mix monomer.
(2) butyl glycol ether solvent in flask is warming up to after backflow, the mix monomer for being dissolved with initiator, about 4- is added dropwise
5h completion of dropping, maintains the reflux for temperature, continues to react 2h or so, then adds 2.4 parts of initiator every 1h, adds altogether 2 times, mends
Plus after terminating, slightly lurid transparent viscous liquid is made, 60 DEG C or so are cooled to, dimethyl ethanol amine neutralizer is added
11.6 parts, continue to stir 0.5h, by 77.7g water addition systems in the way of dropwise addition, resin is deployed into solid contain for 70%
Water-based acrylic resin.
Embodiment 2
1st, the water-based acrylic resin and the ratio input preparing tank of various filler accordings to the form below 1 prepared embodiment 1
In, stirred in sand mill, fineness is up to after 20 μm, and paste resin is made in filtering, adds the preparation such as quantitative amino resins, water
Into water soluble acrylic acid amido coatings.
The water soluble acrylic acid amido coatings formula of table 1 is constituted
| Material name | Weight (g) |
| The water soluble acrylic resin of embodiment 1 | 60 |
| Dispersant | 0.5 |
| Defoamer | 0.2 |
| R902 rutile type titanium whites | 25 |
| Wetting agent | 0.2 |
| Levelling agent | 0.2 |
| Butyl glycol ether | 3 |
| Water | 10.7 |
| SM5747 amino resins | 12 |
2nd, the performance of detection water soluble acrylic acid amido coatings is as shown in table 2 below：
The performance test results of the water soluble acrylic acid amido coatings of table 2
More than test result indicates that, the water soluble acrylic acid amido coatings that prepare of the present invention have good environmental protection
Property, and there is excellent adhesive force, glossiness and excellent hardness and impact resistance, and good environmental protection, achieve
Extraordinary technological progress.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the water soluble acrylic resin of high solid, it is characterised in that it comprises the following steps：
(1) reaction dissolvent is added in the four-hole boiling flask equipped with agitator, condenser, thermometer and constant pressure funnel；By third
Olefin(e) acid, styrene, butyl acrylate, methyl acrylate, methyl methacrylate and hydroxypropyl acrylate are well mixed, must mix
Initiator, is then dissolved in mix monomer by monomer；
(2) reaction dissolvent in four-hole boiling flask is warming up to after backflow, the mix monomer for being dissolved with initiator is added dropwise, time for adding is
4~5 hours, temperature is maintained the reflux for, continues to react 2~3 hours, then initiator was added every 1 hour, adds after end, cools
To 50~70 DEG C, dimethyl ethanol amine neutralizer is added, continues to stir 0.5~1.5 hour, then adds water, resin is allocated
Cheng Gu contains the water soluble acrylic resin for 60~80%.
2. the preparation method of the water soluble acrylic resin of high solid according to claim 1 a kind of, it is characterised in that
It comprises the following steps：
(1) butyl glycol ether is added in the four-hole boiling flask equipped with agitator, condenser, thermometer and constant pressure funnel；Will
Acrylic acid, styrene, butyl acrylate, methyl acrylate, methyl methacrylate and hydroxypropyl acrylate are well mixed, obtain mixed
Monomer is closed, then initiator cumyl peroxide is dissolved in mix monomer；
(2) reaction dissolvent in four-hole boiling flask is warming up to after backflow, the mix monomer for being dissolved with initiator is added dropwise, time for adding is
4~5 hours, temperature is maintained the reflux for, continues to react 2 hours, then initiator was added every 1 hour, secondary initiator is added altogether,
Add after end, be cooled to 60 DEG C, add dimethyl ethanol amine neutralizer, continue to stir 0.5 hour, then add water, will set
Fat is deployed into the solid water soluble acrylic resin containing for 70%.
3. the preparation method of the water soluble acrylic resin of high solid according to claim 2 a kind of, it is characterised in that
The weight percentage of butyl glycol ether is that the weight percentage of 15~25%, acrylic acid is the weight of 5~10%, styrene
Percentage composition is that the weight percentage of 5~10%, butyl acrylate is the weight percentage of 15~36%, methyl acrylate
It is that the weight percentage of 3~8%, hydroxypropyl acrylate is 20 for the weight percentage of 3~10%, methyl methacrylate
~40%, the weight percentage of cumyl peroxide is 1~10%.
4. a kind of water soluble acrylic acid amido coatings, it is characterised in that it includes water soluble acrylic resin, amino resins disperses
Agent, defoamer, wetting agent, pigment, levelling agent, butyl glycol ether；
Described water soluble acrylic resin is prepared by any one of claims 1 to 3 methods described.
5. a kind of water soluble acrylic acid amido coatings according to claim 4, it is characterised in that it is by water-soluble acrylic tree
60~120 parts of fat, 10~24 parts of amino resins, 0.5~1 part of dispersant, 0.2~0.4 part of defoamer, wetting agent 0.2~0.4
Part, 25~40 parts of pigment, 0.2~0.4 part of levelling agent, 10~20 parts of 3~6 parts of butyl glycol ether and water are made.
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| CN201710580294.3A CN107216761A (en) | 2017-07-17 | 2017-07-17 | The preparation method of the water soluble acrylic resin of high solid |
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| CN201710580294.3A CN107216761A (en) | 2017-07-17 | 2017-07-17 | The preparation method of the water soluble acrylic resin of high solid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864359A (en) * | 2018-08-06 | 2018-11-23 | 江西省科学院应用化学研究所 | A kind of preparation method of high performance water-soluble high solid low viscosity acrylic resin |
| CN109053952A (en) * | 2018-07-24 | 2018-12-21 | 黄河三角洲京博化工研究院有限公司 | A kind of water-based acrylic resin and its application |
| CN109485783A (en) * | 2018-10-23 | 2019-03-19 | 杭州方周科技有限公司 | A kind of high gloss gloss oil is with water soluble acrylic resin and preparation method thereof |
| CN109912823A (en) * | 2017-12-12 | 2019-06-21 | 朱文杰 | A kind of preparation method of vehicle glass impact resistance rupture pressure disc |
| CN111217955A (en) * | 2018-11-26 | 2020-06-02 | 阜阳师范学院 | Water-based acrylic resin and preparation method thereof |
| CN111793160A (en) * | 2020-07-31 | 2020-10-20 | 江苏三木化工股份有限公司 | Water-based acrylic resin for industrial baking varnish and preparation method thereof |
| CN112694794A (en) * | 2020-11-09 | 2021-04-23 | 上海澍瑞化工科技有限公司 | Low-temperature cured water-based acrylic baking varnish resin |
| CN116694175A (en) * | 2023-02-14 | 2023-09-05 | 深圳市深赛尔股份有限公司 | Water-based self-cleaning scratch-resistant automobile coating and preparation method thereof |
| CN117511314A (en) * | 2023-10-26 | 2024-02-06 | 广州福诚美化工有限公司 | High-glossiness water-based paint and preparation process thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912823A (en) * | 2017-12-12 | 2019-06-21 | 朱文杰 | A kind of preparation method of vehicle glass impact resistance rupture pressure disc |
| CN109053952A (en) * | 2018-07-24 | 2018-12-21 | 黄河三角洲京博化工研究院有限公司 | A kind of water-based acrylic resin and its application |
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| CN108864359A (en) * | 2018-08-06 | 2018-11-23 | 江西省科学院应用化学研究所 | A kind of preparation method of high performance water-soluble high solid low viscosity acrylic resin |
| CN109485783A (en) * | 2018-10-23 | 2019-03-19 | 杭州方周科技有限公司 | A kind of high gloss gloss oil is with water soluble acrylic resin and preparation method thereof |
| CN111217955A (en) * | 2018-11-26 | 2020-06-02 | 阜阳师范学院 | Water-based acrylic resin and preparation method thereof |
| CN111793160A (en) * | 2020-07-31 | 2020-10-20 | 江苏三木化工股份有限公司 | Water-based acrylic resin for industrial baking varnish and preparation method thereof |
| CN112694794A (en) * | 2020-11-09 | 2021-04-23 | 上海澍瑞化工科技有限公司 | Low-temperature cured water-based acrylic baking varnish resin |
| CN116694175A (en) * | 2023-02-14 | 2023-09-05 | 深圳市深赛尔股份有限公司 | Water-based self-cleaning scratch-resistant automobile coating and preparation method thereof |
| CN117511314A (en) * | 2023-10-26 | 2024-02-06 | 广州福诚美化工有限公司 | High-glossiness water-based paint and preparation process thereof |
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