CN107118353B - Water-soluble polyester-imide resin and preparation method thereof - Google Patents
Water-soluble polyester-imide resin and preparation method thereof Download PDFInfo
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- CN107118353B CN107118353B CN201710353216.XA CN201710353216A CN107118353B CN 107118353 B CN107118353 B CN 107118353B CN 201710353216 A CN201710353216 A CN 201710353216A CN 107118353 B CN107118353 B CN 107118353B
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- 229920005989 resin Polymers 0.000 title claims abstract description 40
- 239000011347 resin Substances 0.000 title claims abstract description 40
- 229920003055 poly(ester-imide) Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002253 acid Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 14
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 14
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920003180 amino resin Polymers 0.000 claims description 12
- 229920000877 Melamine resin Polymers 0.000 claims description 11
- 239000004640 Melamine resin Substances 0.000 claims description 11
- BPXVHIRIPLPOPT-UHFFFAOYSA-N 1,3,5-tris(2-hydroxyethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound OCCN1C(=O)N(CCO)C(=O)N(CCO)C1=O BPXVHIRIPLPOPT-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000013557 residual solvent Substances 0.000 claims description 9
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 8
- 150000004985 diamines Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 230000003472 neutralizing effect Effects 0.000 claims description 8
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229960002887 deanol Drugs 0.000 claims description 7
- 239000012972 dimethylethanolamine Substances 0.000 claims description 7
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 6
- 150000007974 melamines Chemical class 0.000 claims description 6
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 5
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 229920001225 polyester resin Polymers 0.000 claims description 4
- 239000004645 polyester resin Substances 0.000 claims description 4
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 150000004072 triols Chemical class 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 4
- 150000001412 amines Chemical class 0.000 abstract description 2
- 150000007942 carboxylates Chemical class 0.000 abstract 1
- 150000007519 polyprotic acids Polymers 0.000 abstract 1
- 150000005846 sugar alcohols Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 239000007787 solid Substances 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- DAXZJJHDDZHZPA-UHFFFAOYSA-N 1-butoxybutane;1,3,5-triazine-2,4,6-triamine Chemical compound CCCCOCCCC.NC1=NC(N)=NC(N)=N1 DAXZJJHDDZHZPA-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
-
- 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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- 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
- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention relates to a water-soluble polyester-imide resin and a preparation method thereof, wherein the polyester-imide resin with carboxyl end groups is prepared from polyalcohol and polybasic acid, and then neutralized and salified by amine to obtain the water-soluble carboxylate modified polyester-imide resin.
Description
Technical Field
The invention belongs to the field of organic chemical engineering high polymer materials, and particularly relates to a water-soluble polyester-imide resin and a preparation method thereof.
Background
In recent years, with the rapid development of the domestic motor and electrical appliance industry, in the era of advocating environmental protection and emission reduction, the solvent-based insulating paint contains a large amount of toxic and harmful benzene organic solvents, and most of the organic solvents are directly discharged into the atmosphere when coils are subjected to dipping treatment, drying and curing, so that serious environmental pollution is caused; and has great potential safety hazard in the using process, does not meet the requirements of environmental protection regulations and is limited in application, so that the development of the water-soluble insulating resin taking water as a solvent is necessary.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide environment-friendly water-soluble polyester-imide which uses water to replace an organic solvent in the traditional insulating paint and a preparation method thereof.
The polyester-imide resin is a high-temperature-resistant resin with excellent comprehensive performance, a certain amount of carboxyl groups are reserved in the synthetic process of the polyester-imide resin and used as hydrophilic groups, organic amine is used for neutralization and salt formation, the polyester-imide resin with good water solubility can be obtained, a large amount of hydroxyl groups and carboxyl groups are contained in the molecular chain of the polyester-imide and can be subjected to condensation reaction with amino resin, and a polyester-imide cured product has good mechanical property, solvent resistance and electrical insulation property.
In order to achieve the purpose, the invention adopts the following technical scheme:
the water-soluble polyester-imide resin comprises the following raw materials: trimellitic anhydride, dibasic acids, diols, triols and diamines.
The raw materials comprise the following components in parts by weight: 80-100 parts of trimellitic anhydride, 50-80 parts of dibasic acid, 80-120 parts of dihydric alcohol, 20-50 parts of trihydric alcohol and 25-50 parts of diamine.
Optionally, the dibasic acid is one or a mixture of isophthalic acid and terephthalic acid.
Optionally, the dihydric alcohol is one or more than two of neopentyl glycol, ethylene glycol, propylene glycol and butanediol; the trihydric alcohol is a heat-resistant monomer tris (2-hydroxyethyl) isocyanurate.
Optionally, the diamine is one of diaminodiphenylmethane and diaminodiphenyl ether.
A preparation method of water-soluble polyester imide resin takes a raw material formula of the water-soluble polyester imide resin as a reference, and comprises the following steps:
the method comprises the following steps: adding a catalyst into a mixture of dibasic acid, dihydric alcohol and trihydric alcohol according to a formula, and putting the mixture into a reaction bottle for mixing and melting;
step two: adding dimethylbenzene into the mixed molten liquid, heating and refluxing;
step three: continuing heating until the acid value is 7-10 mgKOH/g, cooling, adding diamine and trimellitic anhydride, heating until the acid value reaches 40-70 mgKOH/g, reducing pressure, and removing residual solvent to obtain polyester resin;
step four: and (3) adding a cosolvent to dilute the polyester resin obtained in the fourth step, adding a water-based amino resin after the resin is cooled, and adjusting the pH value by using a neutralizing agent to obtain the water-soluble polyesterimide.
Specifically, the catalyst is n-butyl titanate.
Optionally, the cosolvent is one or more of ethylene glycol butyl ether, propylene glycol methyl ether, butanol, ethylene glycol methyl ether and propylene glycol butyl ether.
Optionally, the neutralizing agent is one or a mixture of more than two of ethanolamine, ammonia water and dimethylethanolamine.
Optionally, the aqueous amino resin is one of methylated melamine resin and butylated melamine resin.
Compared with the prior art, the invention has the beneficial technical effects that:
the water-soluble polyester-imide resin has the characteristics of high temperature resistance, energy conservation and environmental protection, and the preparation method has the advantages of simple process, convenience in operation, easiness in industrialization and better practical value.
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
adding 90g of neopentyl glycol, 21g of propylene glycol, 27g of tris (2-hydroxyethyl) isocyanurate, 60g of isophthalic acid and 0.5g of butyl orthotitanate into a reaction bottle, starting to heat until the materials are melted, and starting to stir; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 80g of trimellitic anhydride and 30g of diaminodiphenylmethane, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 125g of ethylene glycol monobutyl ether is added, 28g of waterborne amino resin methylated melamine resin is added when the temperature of the resin is reduced to below 60 ℃, 25g of neutralizer ethanolamine is used for regulating the pH value to be 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Example 2:
adding 50g of neopentyl glycol, 45g of propylene glycol, 35g of tris (2-hydroxyethyl) isocyanurate, 60g of terephthalic acid and 0.5g of butyl orthotitanate into a reaction bottle, starting heating until the materials are molten, and starting stirring; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 100g of trimellitic anhydride and 40g of diaminodiphenylmethane, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 140g of butyl cellosolve is added, 33g of waterborne amino resin methylated melamine resin is added when the temperature is reduced to below 60 ℃, 25g of neutralizer dimethylethanolamine is used for regulating the pH value to 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Example 3:
adding 50g of neopentyl glycol, 45g of ethylene glycol, 35g of tris (2-hydroxyethyl) isocyanurate, 30g of terephthalic acid, 30g of isophthalic acid and 0.5g of butyl orthotitanate into a reaction bottle, starting heating until the materials are molten, and starting stirring; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 100g of trimellitic anhydride and 40g of diaminodiphenylmethane, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 70g of butyl cellosolve and 70g of ethylene glycol monomethyl ether are added, 29.5g of waterborne amino resin butyl ether melamine resin is added when the temperature is reduced to below 60 ℃, 25g of neutralizer dimethylethanolamine is used for regulating the pH value to 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Example 4:
adding 50g of neopentyl glycol, 45g of butanediol, 45g of tris (2-hydroxyethyl) isocyanurate, 30g of terephthalic acid, 30g of isophthalic acid and 0.5g of butyl orthotitanate into a reaction bottle, starting to heat until the materials are molten, and starting to stir; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 80g of trimellitic anhydride and 30g of diaminodiphenylmethane, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 140g of ethylene glycol monobutyl ether is added, 26.5g of waterborne amino resin butyl etherified melamine resin is added when the temperature is reduced to below 60 ℃, 25g of neutralizer ammonia water is used for regulating the pH value to 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Example 5:
adding 50g of neopentyl glycol, 45g of ethylene glycol, 35g of tris (2-hydroxyethyl) isocyanurate, 40g of terephthalic acid, 30g of isophthalic acid and 0.5g of butyl orthotitanate into a reaction bottle, starting heating until the materials are molten, and starting stirring; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 100g of trimellitic anhydride and 40g of diaminodiphenyl ether, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 100g of propylene glycol butyl ether and 45g of butanol are added, 30.5g of waterborne amino resin butyl etherified melamine resin is added when the temperature is reduced to below 60 ℃, 25g of dimethyl ethanolamine serving as a neutralizing agent is used for regulating the pH value to be 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Example 6:
adding 70g of propylene glycol, 45g of ethylene glycol, 50g of tris (2-hydroxyethyl) isocyanurate, 40g of terephthalic acid, 30g of isophthalic acid and 0.5g of n-butyl titanate into a reaction bottle, starting heating until the materials are melted, and starting stirring; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, adding 90g of trimellitic anhydride and 35g of diaminodiphenyl ether, continuously heating to 200 ℃, keeping the temperature for reaction until the acid value is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 100g of ethylene glycol monobutyl ether and 55g of ethylene glycol monomethyl ether are added, 31.0g of waterborne amino resin butyl ether melamine resin is added when the temperature is reduced to below 60 ℃, 25g of neutralizing agent dimethylethanolamine is used for regulating the pH value to 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Comparative example:
adding 70g of propylene glycol, 45g of ethylene glycol, 50g of tris (2-hydroxyethyl) isocyanurate, 70g of phthalic anhydride and 0.5g of n-butyl titanate into a reaction bottle, starting heating until the materials are melted, and starting stirring; continuously heating to 200 ℃, and keeping the temperature for reaction until the material system becomes clear and the acid value is less than 10mgKOH/g, and then cooling; when the temperature is reduced to 160 ℃, 90g of trimellitic anhydride and 35g of diaminodiphenyl ether are added, the temperature is continuously increased to 200 ℃, and the reaction is carried out under the temperature until the acid value is
When the concentration of KOH is 60mgKOH/g, vacuumizing, decompressing, extracting residual solvent, and cooling; when the temperature is reduced to 150 ℃, 100g of ethylene glycol monobutyl ether and 55g of ethylene glycol monomethyl ether are added, 31.0g of waterborne amino resin butyl ether melamine resin is added when the temperature is reduced to below 60 ℃, 25g of neutralizing agent dimethylethanolamine is used for regulating the pH value to 7.0-9.0, and the water-soluble polyester-imide resin is obtained. The water-soluble resin is viscous transparent liquid with solid content of about 70 percent.
Deionized water was added to the above examples to dilute to 30% solids for performance testing. The results are given in table 1 below:
TABLE 1
As can be seen from Table 1, the solution obtained by neutralizing and salifying the polyesterimide resin prepared by the present invention with more carboxyl functional groups has good water solubility, and the polyesterimide impregnated resin prepared by the method can improve the operation conditions of factories and is beneficial to environmental protection. It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and although the embodiments have been described in detail for the present invention, those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. A preparation method of water-soluble polyester-imide resin is characterized by comprising the following steps: the water-soluble polyester-imide resin comprises the following raw materials: trimellitic anhydride, dibasic acids, diols, triols and diamines; the raw materials comprise the following components in parts by weight: 80-100 parts of trimellitic anhydride, 50-80 parts of dibasic acid, 80-120 parts of dihydric alcohol, 20-50 parts of trihydric alcohol and 25-50 parts of diamine;
the preparation method of the water-soluble polyester-imide resin comprises the following steps:
the method comprises the following steps: adding a catalyst into a mixture of dibasic acid, dihydric alcohol and trihydric alcohol according to a formula, and putting the mixture into a reaction bottle for mixing and melting;
the dibasic acid is one or a mixture of isophthalic acid and terephthalic acid;
the dihydric alcohol is one or more than two of neopentyl glycol, ethylene glycol, propylene glycol and butanediol;
the trihydric alcohol is a heat-resistant monomer tris (2-hydroxyethyl) isocyanurate;
step two: adding dimethylbenzene into the mixed molten liquid, heating and refluxing;
step three: continuing heating until the acid value is 7-10 mgKOH/g, cooling, adding diamine and trimellitic anhydride, heating until the acid value reaches 40-70 mgKOH/g, reducing pressure, and removing residual solvent to obtain polyester resin;
the diamine is one of diaminodiphenylmethane and diaminodiphenyl ether;
step four: adding a cosolvent to dilute the polyester resin obtained in the fourth step, adding a water-based amino resin after the resin is cooled, and adjusting the pH value by using a neutralizing agent to obtain water-soluble polyesterimide;
the aqueous amino resin is one of methylated melamine resin and butylated melamine resin.
2. The method for preparing a water-soluble polyesterimide resin as claimed in claim 1, wherein: the catalyst is tetrabutyl titanate.
3. The method for preparing a water-soluble polyesterimide resin as claimed in claim 1, wherein: the cosolvent is one or more than two of ethylene glycol butyl ether, propylene glycol methyl ether, butanol, ethylene glycol methyl ether and propylene glycol butyl ether.
4. The method for preparing a water-soluble polyesterimide resin as claimed in claim 1, wherein: the neutralizing agent is one or a mixture of more than two of ethanolamine, ammonia water and dimethylethanolamine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710025207 | 2017-01-13 | ||
| CN2017100252078 | 2017-01-13 |
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| CN107118353B true CN107118353B (en) | 2020-10-02 |
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| CN108102367B (en) * | 2018-01-15 | 2020-07-28 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity environment-friendly polyesterimide dip resin and preparation method and application thereof |
| CN109385204B (en) * | 2018-10-12 | 2021-04-23 | 湖北长海新能源科技有限公司 | Water-soluble polyester imide insulating paint and preparation method thereof |
| CN112760009A (en) * | 2021-01-20 | 2021-05-07 | 徐松波 | Flame-retardant epoxy coating and preparation method thereof |
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