CN106632879A - Preparation method of dispersion resin - Google Patents
Preparation method of dispersion resin Download PDFInfo
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- CN106632879A CN106632879A CN201611170978.8A CN201611170978A CN106632879A CN 106632879 A CN106632879 A CN 106632879A CN 201611170978 A CN201611170978 A CN 201611170978A CN 106632879 A CN106632879 A CN 106632879A
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- parts
- dispersion
- resin
- epoxy resin
- dibenzoyl peroxide
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
- C08G18/673—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen containing two or more acrylate or alkylacrylate ester groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to dispersion resin and a preparation method thereof, and belongs to the technical field of resin. The dispersion resin is prepared from 20 to 30 parts of isophorone diisocyanate, 3 to 5 parts of hydroxymethyl acrylamide, 15 to 20 parts of trimethylolpropane triallyl ester, 20 to 30 parts of epoxy resin E51, 20 to 30 parts of polyether glycol, 5 to 10 parts of methyl pyrrolidone, 30 to 50 parts of methyl ethyl ketone, 3 to 5 parts of triethanolamine, 15 to 20 parts of ethyl methacrylate, 3 to 5 parts of dibutyl tin dilaurate and 1 to 3 parts of dibenzoyl peroxide. According to the dispersion resin disclosed by the invention, a polyurethane-epoxy resin-acrylate hybridized dispersion with more excellent performance is obtained by using two substances of the epoxy resin and the acrylate to modify a waterborne polyurethane dispersion, and the polyurethane-epoxy resin-acrylate hybridized dispersion integrates the advantages of polyurethane, the epoxy resin and the acrylate.
Description
Technical field
The present invention relates to a kind of resin and preparation method thereof, it is more particularly related to a kind of resin dispersion and
Its preparation method, belongs to resin technology field.
Background technology
With the gradually enhancing of increasingly strict and people's environmental consciousness of environmental regulation, solvent borne polyurethane is due to containing height
VOC, to environmentally undesirable, it is using being increasingly restricted.And the aqueous polyurethane with water as decentralized medium becomes environmental friendliness
The emphasis of polyurethane resin developmental research.But single aqueous pu dispersions mechanics performance of latex film is not good, chemical resistance
Bad with water-fast, solvent resistance, hardness is relatively low.To improve the film performance of aqueous pu dispersions, expanding aqueous polyurethane
Aqueous pu dispersions just must be modified by dispersion range of application.The modified report of relevant aqueous pu dispersions
Road is more, most modified to it only with a kind of component, causes its performance still can not meet many demands.Additionally, by
Have the advantages that high-modulus, high intensity and chemical resistance are good in epoxy resin, acrylate has preferable resistance to water, weather-proof
Property.
The content of the invention
Present invention seek to address that the performance issue of existing aqueous pu dispersions, there is provided a kind of resin dispersion, this point
Dispersion resin combines the advantage of polyurethane, epoxy resin and acrylate.
In order to realize foregoing invention purpose, its specific technical scheme is as follows:
A kind of resin dispersion, it is characterised in that:Including following raw materials by weight:
Isoflurane chalcone diisocyanate 20-30 parts
NMA 3-5 parts
Trimethylolpropane tris allyl ester 15-20 parts
Epoxy resin E51 20-30 parts
Polyether Glycols 20-30 parts
Methyl pyrrolidone 5-10 parts
MEK 30-50 parts
Triethanolamine 3-5 parts
EMA 15-20 parts
Dibutyl tin laurate 3-5 parts
Dibenzoyl peroxide 1-3 parts.
A kind of preparation method of resin dispersion, it is characterised in that:Comprise the following steps that:
A, by methyl pyrrolidone, EMA, dibutyl tin laurate at 120 DEG C, vacuum decompression dehydration 1.5h,
It is standby;Under nitrogen protection, in equipped with agitator, thermometer, the four-hole bottle of condenser pipe, isoflurane chalcone diisocyanate is added
With the polyether Glycols of dehydration, stirring is started, be gradually warmed up to 80 DEG C, holding is reacted at this temperature;
B ,-the content of NCO group is measured by sampling in reactant, after setting is reached, adds crosslinking agent trimethylolpropane tris alkene
Propyl ester, keeps this thermotonus 2h;Judge reaction end with n-Butylamine titration method;Reach and add after terminal dissolved with methylol acryloyl
The solution and epoxy resin E51 of amine, insulation reaction 5h;Regarding the size addition acetone of viscosity in course of reaction so as to meet the requirements;
C, finally reaction system cooled to less than 45 DEG C;Triethanolamine is neutralized, and adds water emulsification to obtain under high speed shear
PU-Epoxy hydridization dispersion.
D, the dispersion of above-mentioned preparation is put into four-hole bottle, at 75 DEG C 0.5h is incubated;It is uniform in 3h at 75-80 DEG C
The acetone soln of dibenzoyl peroxide and dibenzoyl peroxide initiator is added dropwise, the poly- 2h of free radical emulsion is carried out;
E, the methyl ethyl ketone solution of rear dibenzoyl peroxide initiator is dripped off then at 85-90 DEG C of insulation 1.5h;Vacuum sloughs reaction
MEK and other fugitive constituents in system obtains resin dispersion.
The Advantageous Effects that the present invention brings:
Two kinds of materials of present invention epoxy resin and acrylate are modified to aqueous pu dispersions, obtain performance more excellent
PU-Epoxy-acrylate hybrid dispersion, the dispersion combines polyurethane, epoxy resin and acrylate
Advantage.
Specific embodiment
Embodiment 1
A kind of resin dispersion, it is characterised in that:Including following raw materials by weight:
20 parts of isoflurane chalcone diisocyanate
3 parts of NMA
15 parts of trimethylolpropane tris allyl ester
20 parts of epoxy resin E51
20 parts of polyether Glycols
5 parts of methyl pyrrolidone
30 parts of MEK
3 parts of triethanolamine
15 parts of EMA
3 parts of dibutyl tin laurate
1 part of dibenzoyl peroxide.
Embodiment 2
A kind of resin dispersion, it is characterised in that:Including following raw materials by weight:
30 parts of isoflurane chalcone diisocyanate
5 parts of NMA
20 parts of trimethylolpropane tris allyl ester
30 parts of epoxy resin E51
30 parts of polyether Glycols
10 parts of methyl pyrrolidone
50 parts of MEK
5 parts of triethanolamine
20 parts of EMA
5 parts of dibutyl tin laurate
3 parts of dibenzoyl peroxide.
Embodiment 3
A kind of resin dispersion, it is characterised in that:Including following raw materials by weight:
25 parts of isoflurane chalcone diisocyanate
4 parts of NMA
18 parts of trimethylolpropane tris allyl ester
25 parts of epoxy resin E51
25 parts of polyether Glycols
7 parts of methyl pyrrolidone
40 parts of MEK
4 parts of triethanolamine
18 parts of EMA
4 parts of dibutyl tin laurate
2 parts of dibenzoyl peroxide.
Embodiment 4
A kind of preparation method of resin dispersion, comprises the following steps that:
A, by methyl pyrrolidone, EMA, dibutyl tin laurate at 120 DEG C, vacuum decompression dehydration 1.5h,
It is standby;Under nitrogen protection, in equipped with agitator, thermometer, the four-hole bottle of condenser pipe, isoflurane chalcone diisocyanate is added
With the polyether Glycols of dehydration, stirring is started, be gradually warmed up to 80 DEG C, holding is reacted at this temperature;
B ,-the content of NCO group is measured by sampling in reactant, after setting is reached, adds crosslinking agent trimethylolpropane tris
Allyl ester, keeps this thermotonus 2h;Judge reaction end with n-Butylamine titration method;Reach and add after terminal dissolved with methylol third
The solution and epoxy resin E51 of acrylamide, insulation reaction 5h;Regarding the size addition acetone of viscosity in course of reaction so as to meet
Require;
C, finally reaction system cooled to less than 45 DEG C;Triethanolamine is neutralized, and adds water emulsification to obtain under high speed shear
PU-Epoxy hydridization dispersion.
D, the dispersion of above-mentioned preparation is put into four-hole bottle, at 75 DEG C 0.5h is incubated;Uniformly drip in 3h at 75 DEG C
Plus the acetone soln of dibenzoyl peroxide and dibenzoyl peroxide initiator, carry out the poly- 2h of free radical emulsion;
E, the methyl ethyl ketone solution of rear dibenzoyl peroxide initiator is dripped off then at 85 DEG C of insulation 1.5h;Vacuum sloughs reaction system
In MEK and other fugitive constituents obtain resin dispersion.
Embodiment 5
A kind of preparation method of resin dispersion, comprises the following steps that:
A, by methyl pyrrolidone, EMA, dibutyl tin laurate at 120 DEG C, vacuum decompression dehydration 1.5h,
It is standby;Under nitrogen protection, in equipped with agitator, thermometer, the four-hole bottle of condenser pipe, isoflurane chalcone diisocyanate is added
With the polyether Glycols of dehydration, stirring is started, be gradually warmed up to 80 DEG C, holding is reacted at this temperature;
B ,-the content of NCO group is measured by sampling in reactant, after setting is reached, adds crosslinking agent trimethylolpropane tris
Allyl ester, keeps this thermotonus 2h;Judge reaction end with n-Butylamine titration method;Reach and add after terminal dissolved with methylol third
The solution and epoxy resin E51 of acrylamide, insulation reaction 5h;Regarding the size addition acetone of viscosity in course of reaction so as to meet
Require;
C, finally reaction system cooled to less than 45 DEG C;Triethanolamine is neutralized, and adds water emulsification to obtain under high speed shear
PU-Epoxy hydridization dispersion.
D, the dispersion of above-mentioned preparation is put into four-hole bottle, at 75 DEG C 0.5h is incubated;Uniformly drip in 3h at 80 DEG C
Plus the acetone soln of dibenzoyl peroxide and dibenzoyl peroxide initiator, carry out the poly- 2h of free radical emulsion;
E, the methyl ethyl ketone solution of rear dibenzoyl peroxide initiator is dripped off then at 90 DEG C of insulation 1.5h;Vacuum sloughs reaction system
In MEK and other fugitive constituents obtain resin dispersion.
Embodiment 6
A kind of preparation method of resin dispersion, comprises the following steps that:
A, by methyl pyrrolidone, EMA, dibutyl tin laurate at 120 DEG C, vacuum decompression dehydration 1.5h,
It is standby;Under nitrogen protection, in equipped with agitator, thermometer, the four-hole bottle of condenser pipe, isoflurane chalcone diisocyanate is added
With the polyether Glycols of dehydration, stirring is started, be gradually warmed up to 80 DEG C, holding is reacted at this temperature;
B ,-the content of NCO group is measured by sampling in reactant, after setting is reached, adds crosslinking agent trimethylolpropane tris
Allyl ester, keeps this thermotonus 2h;Judge reaction end with n-Butylamine titration method;Reach and add after terminal dissolved with methylol third
The solution and epoxy resin E51 of acrylamide, insulation reaction 5h;Regarding the size addition acetone of viscosity in course of reaction so as to meet
Require;
C, finally reaction system cooled to less than 45 DEG C;Triethanolamine is neutralized, and adds water emulsification to obtain under high speed shear
PU-Epoxy hydridization dispersion.
D, the dispersion of above-mentioned preparation is put into four-hole bottle, at 75 DEG C 0.5h is incubated;Uniformly drip in 3h at 78 DEG C
Plus the acetone soln of dibenzoyl peroxide and dibenzoyl peroxide initiator, carry out the poly- 2h of free radical emulsion;
E, the methyl ethyl ketone solution of rear dibenzoyl peroxide initiator is dripped off then at 88 DEG C of insulation 1.5h;Vacuum sloughs reaction system
In MEK and other fugitive constituents obtain resin dispersion.
Claims (2)
1. a kind of resin dispersion, it is characterised in that:Including following raw materials by weight:
Isoflurane chalcone diisocyanate 20-30 parts
NMA 3-5 parts
Trimethylolpropane tris allyl ester 15-20 parts
Epoxy resin E51 20-30 parts
Polyether Glycols 20-30 parts
Methyl pyrrolidone 5-10 parts
MEK 30-50 parts
Triethanolamine 3-5 parts
EMA 15-20 parts
Dibutyl tin laurate 3-5 parts
Dibenzoyl peroxide 1-3 parts.
2. the preparation method of a kind of resin dispersion according to claim 1, it is characterised in that:Including following technique step
Suddenly:
A, by methyl pyrrolidone, EMA, dibutyl tin laurate at 120 DEG C, vacuum decompression dehydration 1.5h,
It is standby;Under nitrogen protection, in equipped with agitator, thermometer, the four-hole bottle of condenser pipe, isoflurane chalcone diisocyanate is added
With the polyether Glycols of dehydration, stirring is started, be gradually warmed up to 80 DEG C, holding is reacted at this temperature;
B ,-the content of NCO group is measured by sampling in reactant, after setting is reached, adds crosslinking agent trimethylolpropane tris
Allyl ester, keeps this thermotonus 2h;Judge reaction end with n-Butylamine titration method;Reach and add after terminal dissolved with methylol third
The solution and epoxy resin E51 of acrylamide, insulation reaction 5h;Regarding the size addition acetone of viscosity in course of reaction so as to meet
Require;
C, finally reaction system cooled to less than 45 DEG C;Triethanolamine is neutralized, and adds water emulsification to obtain under high speed shear
PU-Epoxy hydridization dispersion;
D, the dispersion of above-mentioned preparation is put into four-hole bottle, at 75 DEG C 0.5h is incubated;Uniformly it is added dropwise in 3h at 75-80 DEG C
The acetone soln of dibenzoyl peroxide and dibenzoyl peroxide initiator, carries out the poly- 2h of free radical emulsion;
E, the methyl ethyl ketone solution of rear dibenzoyl peroxide initiator is dripped off then at 85-90 DEG C of insulation 1.5h;Vacuum sloughs reaction
MEK and other fugitive constituents in system obtains resin dispersion.
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CN201611170978.8A CN106632879A (en) | 2016-12-16 | 2016-12-16 | Preparation method of dispersion resin |
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CN201611170978.8A CN106632879A (en) | 2016-12-16 | 2016-12-16 | Preparation method of dispersion resin |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101235148A (en) * | 2007-12-29 | 2008-08-06 | 华南理工大学 | Multiple crosslinking ultraviolet light solidifying water polyurethane dispersoid and its preparation method and application |
CN101519480A (en) * | 2009-01-22 | 2009-09-02 | 广东天银化工实业有限公司 | Method for preparing self-cross linking type water-based acrylic resin and polyurethane hybrid |
CN104530374A (en) * | 2014-10-25 | 2015-04-22 | 重庆市旭星化工有限公司 | Synthetizing method of epoxy modifying aqueous polyurethane |
CN105732909A (en) * | 2016-04-15 | 2016-07-06 | 武汉赫斯特涂层材料股份有限公司 | Preparation method of acrylic acid polysiloxane waterborne emulsion |
-
2016
- 2016-12-16 CN CN201611170978.8A patent/CN106632879A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101235148A (en) * | 2007-12-29 | 2008-08-06 | 华南理工大学 | Multiple crosslinking ultraviolet light solidifying water polyurethane dispersoid and its preparation method and application |
CN101519480A (en) * | 2009-01-22 | 2009-09-02 | 广东天银化工实业有限公司 | Method for preparing self-cross linking type water-based acrylic resin and polyurethane hybrid |
CN104530374A (en) * | 2014-10-25 | 2015-04-22 | 重庆市旭星化工有限公司 | Synthetizing method of epoxy modifying aqueous polyurethane |
CN105732909A (en) * | 2016-04-15 | 2016-07-06 | 武汉赫斯特涂层材料股份有限公司 | Preparation method of acrylic acid polysiloxane waterborne emulsion |
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Application publication date: 20170510 |