CN111944137B - Epoxidized polyester resin for weather-resistant high-impact-resistance powder coating and preparation method thereof - Google Patents
Epoxidized polyester resin for weather-resistant high-impact-resistance powder coating and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/914—Polymers modified by chemical after-treatment derived from polycarboxylic acids and polyhydroxy compounds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- 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
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Abstract
The invention belongs to the technical field of preparation of polyacid resins, and particularly relates to an epoxidized polyester resin for a weather-resistant high-impact-resistance powder coating and a preparation method thereof. The polyester resin of the present invention comprises the following main raw materials in terms of moles: 9-18 mol of ethylsuccinic acid; 7-15 mol of tridecanedioic acid; neopentyl glycol 8-16 mol; 4-9mol of trimethylolpropane; 10-20 mol of 2-ethyl-1, 3-hexanediol; 5-10 mol of adipic acid; 40-55 mol of epoxy chloropropane; 10-15 mol of strong base. According to the invention, linear dihydric alcohol and dibasic acid are used for preparing carboxyl-terminated polyester resin, and then the carboxyl-terminated polyester resin, epichlorohydrin and strong base are subjected to epoxidation reaction to obtain the epoxidized polyester resin. The epoxy polyester resin chain segment has a good linear structure, the water resistance and weather resistance of the raw material with the branched chain are ensured, the prepared powder coating does not need to additionally use a curing agent, and the powder coating can obtain a high-impact-resistance weather-resistant coating film with the powder coating after the powder coating is cured at low temperature with outdoor weather-resistant high-acid-value carboxyl polyester resin, and has the advantages of low cost and excellent performance.
Description
Technical Field
The invention belongs to the technical field of preparation of polyacid resins, and particularly relates to an epoxidized polyester resin for a weather-resistant high-impact-resistance powder coating and a preparation method thereof.
Background
The powder coating has good protective performance and decorative performance, so the powder coating is widely applied to the conventional coating industry at present, such as the coating of guardrails of expressways, outdoor units of air conditioners, indoor metal tables and chairs and the like. At present, polyester resin and TGIC or HAA are used for curing outdoor weather-resistant powder coating, and as the molecular weight of a curing agent is small, the functionality is high, the crosslinking degree of a cured coating film is high, the impact resistance is general, the coating film can only pass positive and negative impact of 50cm, and the coating film is often easy to collide and crack and is damaged when being used in areas which are easy to collide and scratch, such as forklifts, guardrails and the like.
The mixed powder coating prepared by using macromolecular epoxy resin and polyester resin is favorable for improving the shock resistance because the molecular weight of the epoxy resin and the polyester resin is larger. For example, the following patent documents are disclosed correspondingly:
CN 107163235B and CN 108503814B both use special epoxidized polyester resin to replace E-12 epoxy resin to be respectively used in 50/50 and 60/40 powder coatings, and satisfactory application effects are achieved. However, since CN 107163235B is epoxidized by using hydrogen peroxide, the epoxidation process is complicated and the epoxidation cannot be completely performed, so that partial unsaturated double bonds still exist in the chain segment, while CN 108503814B is epoxidized and terminated by using resorcinol diglycidyl ether which is high in cost and poor in weather resistance, so that the cost of the product of the above patent is still high, and meanwhile, the formulation is selected so that the product can only be used in indoor mixed powder coating and has relatively poor outdoor weather resistance.
Therefore, it is necessary to improve the above scheme, and invent a weather-resistant high impact powder coating epoxy polyester resin, so that it can be widely applied to the environmental conditions of guardrails of highways, air conditioners and outdoor units, and the coating of indoor metal tables and chairs.
Disclosure of Invention
In order to solve the technical problems, the invention provides an epoxidized polyester resin for a weather-resistant high-impact powder coating;
also provides a preparation method of the polyester resin.
The polyester resin provided by the invention is mainly obtained by taking ethylsuccinic acid, tridecanedioic acid, neopentyl glycol, 1, 4-butanediol, 2-ethyl-1, 3-hexanediol, adipic acid, epichlorohydrin, strong base and the like as raw materials and reacting the raw materials.
The invention provides an epoxidized polyester resin for weather-resistant high-impact powder coating, which comprises the following main raw materials in mole number:
9-18 mol of ethylsuccinic acid; 7-15 mol of tridecanedioic acid; neopentyl glycol 8-16 mol; 4-9mol of trimethylolpropane; 10-20 mol of 2-ethyl-1, 3-hexanediol; 5-10 mol of adipic acid; 40-55 mol of epoxy chloropropane; 10-15 mol of strong base, wherein the strong base is selected from sodium hydroxide or potassium hydroxide with the purity of more than 90%.
The polyester resin also adopts the following auxiliary materials during preparation:
a first catalyst: monobutyl tin oxide, the dosage is 0.05-0.1% of the total mass of the main raw materials;
a second catalyst: benzyl trimethyl ammonium chloride, the consumption is 0.5-1.5% of the quality of epichlorohydrin;
the antioxidant is beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate, and the dosage of the antioxidant is 0.1 to 0.3 percent of the total mass of the main raw materials.
The preparation method of the polyester resin comprises the following steps:
A. adding neopentyl glycol and trimethylolpropane into a reaction kettle, heating to melt and stirring, then adding a first catalyst of monobutyl tin oxide, uniformly mixing, adding ethylsuccinic acid and tridecanedioic acid to perform esterification reaction, then heating, preserving heat and performing esterification dehydration reaction;
B. when the acid value of the polymer is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol, heating under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated out, wherein the acid value of the reactant is less than 35 mgKOH/g;
C. adding an antioxidant, reacting under vacuum to promote further chain extension reaction of the polyester resin, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g;
D. cooling, adding adipic acid with formula amount to perform carboxyl end capping reaction, heating to perform esterification end capping reaction, and stopping reaction when the acid value of the reactant is 20-30 mgKOH/g;
E. cooling, adding epoxy chloropropane and a second catalyst benzyl trimethyl ammonium chloride, stirring until the epoxy chloropropane and the second catalyst benzyl trimethyl ammonium chloride are dissolved, then carrying out heat preservation reaction, cooling when the acid value of the polymer is lower than 1mgKOH/g, adding strong base, and continuing the heat preservation reaction after the strong base is completely added;
F. sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 600g/mol and 500-.
Preferably, in the step A, neopentyl glycol and trimethylolpropane in the formula amount are added into a reaction kettle, the mixture is heated to 130-.
B. When the acid value of the polymer is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol with the formula amount, starting a nitrogen blowing system, gradually heating to 210-220 ℃ at the heating rate of 5-7 ℃/h under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated, wherein the acid value of the reactant is less than 35 mgKOH/g.
C. And adding an antioxidant with the formula amount, starting a vacuum system, keeping the vacuum degree of-0.098 to-0.095 Mpa, reacting for 1-3h, promoting the further chain extension reaction of the polyester resin, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g.
D. When the temperature is reduced to 200 ℃, adding adipic acid with the formula amount to carry out carboxyl end capping reaction, heating to 225-230 ℃ at the speed of 10 ℃/h to carry out esterification end capping reaction for 2-4h, and stopping the reaction when the acid value of the reactant is 20-30 mgKOH/g.
E. And then cooling to 100-105 ℃, adding the epoxy chloropropane and a second catalyst benzyltrimethylammonium chloride in a formula amount, stirring until the epoxy chloropropane and the benzyltrimethylammonium chloride are dissolved, carrying out heat preservation reaction for 2-4h, cooling to 30-35 ℃ when the acid value of the polymer is lower than 1mgKOH/g, equally dividing 4 batches, adding the strong base in a formula amount, wherein the interval of each batch is 15-20min, starting chilled water during alkali strengthening, always keeping the temperature in the reaction kettle at 30-35 ℃, and continuing the heat preservation reaction for 1-2h at 30-35 ℃ after the strong base is completely added.
F. Sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 600g/mol together with 500-; the sampling detection is to carry out detection after filtering salt and removing solvent of the sample.
Preferably, the preparation method of the epoxidized polyester resin for the weather-resistant high-impact powder coating comprises the following steps:
A. adding neopentyl glycol and trimethylolpropane with a formula amount into a reaction kettle, heating to 135 ℃ firstly, starting stirring after complete melting, then adding a first catalyst of monobutyl tin oxide with a formula amount, uniformly mixing, adding ethylsuccinic acid and tridecanedioic acid with a formula amount for esterification reaction, after the materials are added, gradually heating from 135 ℃ to 185 ℃ at a heating rate of 10-12 ℃/h, and carrying out heat preservation esterification dehydration reaction for 3-5 h;
B. when the acid value of the polymer is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol according to the formula amount, starting a nitrogen blowing system, gradually heating to 210-220 ℃ at the heating rate of 5-7 ℃/h under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated, wherein the acid value of the reactant is less than 35 mgKOH/g;
C. then adding the antioxidant with the formula amount, starting a vacuum system, keeping the vacuum degree of-0.098 to-0.095 Mpa, reacting for 1-3h, promoting the polyester resin to further carry out chain extension reaction, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g;
D. when the temperature is reduced to 200 ℃, adding adipic acid with the formula amount to carry out carboxyl end capping reaction, heating to 225-230 ℃ at the speed of 10 ℃/h to carry out esterification end capping reaction for 2-4h, and stopping the reaction when the acid value of the reactant is 20-30 mgKOH/g;
E. then cooling to 100-;
F. sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 600g/mol together with 500-; the sampling detection is to carry out detection after filtering salt and removing solvent of the sample.
Specifically, the carboxyl-terminated polyester resin is prepared by using linear dihydric alcohol and dibasic acid, and then the carboxyl-terminated polyester resin is subjected to epoxidation reaction with epichlorohydrin and strong base to obtain the epoxidized polyester resin. The epoxidized polyester resin has good chain segment linear structure, low softening point and high activity of an epoxy group, can be fully cured at low temperature (160 ℃), ensures the water resistance and weather resistance of the raw material with a branched chain, does not need an additional curing agent for the prepared powder coating, can obtain a high-impact-resistance and weather-resistance coating film with the powder coating after the outdoor weather-resistance high-acid-value carboxyl polyester resin is cured at low temperature, and has the advantages of low cost and excellent performance.
Detailed Description
The present invention will now be further described with reference to specific embodiments in order to enable those skilled in the art to better understand the present invention.
The polyester resin raw materials in the invention are as follows:
9-18 mol of ethylsuccinic acid
7-15 mol of tridecanedioic acid
Neopentyl glycol 8 to 16mol
4-9mol of trimethylolpropane
10-20 mol of 2-ethyl-1, 3-hexanediol
5-10 mol of adipic acid
40-55 mol of epoxy chloropropane
10-15 mol of strong base,
The strong alkali refers to sodium hydroxide or potassium hydroxide, and the purity is over 90 percent.
The catalyst for polyester synthesis is monobutyl tin oxide, and the using amount of the catalyst is 0.05-0.1% of the total mass of the raw materials; (i.e., the first catalyst);
the antioxidant is an antioxidant 1076, namely n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, and the dosage of the antioxidant is 0.1 to 0.3 percent of the total mass of the main raw materials.
The catalyst for epoxidation is benzyltrimethylammonium chloride, and the dosage of the catalyst is 0.5 to 1.5 percent of the mass of epichlorohydrin; (i.e., a second catalyst);
wherein the strong base refers to sodium hydroxide or potassium hydroxide, and the purity is more than 90%.
Example 1
The preparation method of the epoxidized polyester resin for the weather-resistant high-impact powder coating comprises the following steps:
A. adding neopentyl glycol and trimethylolpropane with the formula amount into a reaction kettle, heating to 135 ℃ to be completely melted, starting stirring, adding a first catalyst namely monobutyl tin oxide with the formula amount, uniformly mixing, adding ethylsuccinic acid and tridecanedioic acid with the formula amount to perform an esterification reaction, after the materials are added, gradually heating from 135 ℃ to 185 ℃ at the heating rate of 12 ℃/h, and carrying out a heat preservation esterification dehydration reaction for about 4 h;
B. when the acid value of the polymer is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol according to the formula amount, starting a nitrogen blowing system, gradually heating to 215 ℃ at the heating rate of 5-7 ℃/h under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated, wherein the acid value of a reactant is less than 35 mgKOH/g;
C. then adding the antioxidant with the formula amount, starting a vacuum system, keeping the vacuum degree of-0.098 to-0.095 Mpa, reacting for 2 hours, promoting the polyester resin to further carry out chain extension reaction, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g;
D. when the temperature is reduced to 200 ℃, adding adipic acid with the formula amount to carry out carboxyl end capping reaction, heating to 225 ℃ at the speed of 10 ℃/h to carry out esterification end capping reaction for 3h, and stopping the reaction when the acid value of the reactant is 25 mgKOH/g;
E. then cooling to 100 ℃, adding epichlorohydrin and a second catalyst benzyltrimethylammonium chloride according to the formula amount, stirring until the materials are dissolved, carrying out heat preservation reaction for 3 hours, cooling to 30 ℃ when the acid value of the polymer is lower than 1mgKOH/g, uniformly dividing 4 batches, adding strong base according to the formula amount, wherein the interval of each batch is 15-20min, starting chilled water during alkali strengthening, always keeping the temperature in the reaction kettle at about 30 ℃ (certainly 35 ℃), and continuing heat preservation reaction for 1-2 hours at 30 ℃ after the strong base is completely added;
F. sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 600g/mol together with 500-; the sampling detection is to carry out detection after filtering salt and removing solvent on the taken sample (the expression of the temperature or the vacuum degree in the embodiment 1 only gives one of the most preferable values, and the method in the embodiments 2 to 4 can fluctuate within the range given by the invention content of the specification, and is the same as the method in the embodiment 1).
The raw material amounts of examples 1 to 4 are shown in table 1 below:
TABLE 1 raw material amounts of examples 1 to 4
Note: the dosage of the first catalyst, namely the monobutyl tin oxide, is the percentage of the total mass of the raw materials; the dosage of the second catalyst benzyltrimethylammonium chloride is the mass percentage of the epichlorohydrin; the antioxidant is beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, and the dosage of the antioxidant is the percentage of the total mass of the main raw materials.
TABLE 2 acid number and softening point of the products of examples 1-4
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Epoxy equivalent (g/mol) | 554 | 589 | 532 | 513 |
| Softening Point (. degree. C.) | 87 | 89 | 86 | 84 |
Example 5
The formula of the epoxy polyester resin curing system powder coating is generally as follows in parts by weight:
wherein the weather-resistant polyester resin is purchased from New Material Ltd of Anhui Shenjia, model SJ4H, and acid value is 51 mgKOH/g.
Preparing a coating layer: and uniformly mixing the materials according to the formula requirement of the epoxidized polyester resin curing system powder coating, extruding, tabletting and crushing the materials by using a double-screw extruder, and then crushing and sieving the tablets to prepare the powder coating. The powder coating is sprayed on the galvanized iron substrate after surface treatment by an electrostatic spray gun, the film thickness is 80-90 mu m, and then the powder coating is baked and cured at 160 ℃/15min to obtain the coating.
The detection of the coating index is based on GB/T21776 2008 'Standard guide for powder coating and coating detection'; the impact resistance test is carried out according to GB/T1732-1993 'paint film impact resistance determination', wherein the maximum impact height of a paint film impactor is 100 cm; the adhesion rating is in accordance with GB/T9286 1998 test of marking test of paint films of colored paint and varnish; weather resistance test the artificial weathering test was carried out continuously for 500h according to the procedures of the specified steps A in Table 3 of GB/T1865 + 2009 xenon arc radiation for artificial weathering and artificial radiation exposure filtration of colored paint and varnish.
The following comparative examples 1 to 4 are comparative control cases of the product of the present invention, and are specifically as follows:
comparative example 1: the commercial common TGIC curing system finished product powder coating has the film thickness of 80-90 mu m and the curing conditions: 200 ℃/10 min.
Comparative example 2: the film thickness of the commercial common HAA curing system finished product powder coating is 80-90 mu m, and the curing conditions are as follows: 200 ℃/10 min.
Comparative example 3: CN 107163235B coating film prepared in example 1 (preparation method and curing conditions were in accordance with CN 107163235B, film thickness 80-90 μm)
Comparative example 4: CN 108503814B coating film prepared in example 1 (preparation method and curing conditions were in accordance with CN 108503814B, film thickness 80-90 μm)
TABLE 3 basic Properties of the examples and comparative examples
As can be seen from the comparison of the performance of the coating after the product is applied in the table, after the product is cured at the low temperature of 160 ℃, the appearance of the coated product is smooth, the glossiness is good, the impact resistance is excellent, and the impact resistance can reach 70 cm; the weather resistance of 500h is inspected to be unchanged or not obviously changed, and the weather resistance requirement of outdoor weather-resistant polyester powder coating is completely met (comparative example 1 and comparative example 2);
the outdoor weather-resistant polyester powder coating products (comparative example 1 and comparative example 2) sold in the market have smooth appearance, equal gloss and weather resistance to the products of the invention or are slightly inferior to the products of the invention, but are seriously inferior to the products of the invention in the aspect of impact resistance; the epoxy resin adopted in the comparative examples 3 and 4 is suitable for indoor powder coating, the weather resistance is poor, and the phenomena of serious light loss, slight coating falling or bubbling are generated after the artificial aging test is carried out for 500 h.
Claims (8)
1. The epoxidized polyester resin for the weather-resistant high-impact powder coating is characterized by comprising the following main raw materials in mole number:
9-18 mol of ethylsuccinic acid; 7-15 mol of tridecanedioic acid; neopentyl glycol 8-16 mol; 4-9mol of trimethylolpropane; 10-20 mol of 2-ethyl-1, 3-hexanediol; 5-10 mol of adipic acid; 40-55 mol of epoxy chloropropane; 10-15 mol of strong base, wherein the strong base is selected from sodium hydroxide or potassium hydroxide with the purity of more than 90%;
the polyester resin also adopts the following auxiliary materials during preparation:
a first catalyst: the dosage of the monobutyl tin oxide is 0.05 to 0.1 percent of the total mass of the main raw materials;
a second catalyst: benzyl trimethyl ammonium chloride, the consumption is 0.5-1.5% of the quality of epichlorohydrin;
the antioxidant is beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate, and the dosage of the antioxidant is 0.1 to 0.3 percent of the total mass of the main raw materials;
the preparation method of the polyester resin comprises the following steps:
A. adding neopentyl glycol and trimethylolpropane into a reaction kettle, heating to melt and stirring, then adding a first catalyst of monobutyl tin oxide, uniformly mixing, adding ethylsuccinic acid and tridecanedioic acid to perform esterification reaction, then heating, preserving heat and performing esterification dehydration reaction;
B. when the acid value of the polymer obtained in the step A is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol, heating under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated, wherein the acid value of a reactant is less than 35 mgKOH/g;
C. adding an antioxidant, reacting under vacuum to promote further chain extension reaction of the polyester resin, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g;
D. cooling, adding adipic acid with formula amount to perform carboxyl end capping reaction, heating to perform esterification end capping reaction, and stopping reaction when the acid value of the reactant is 20-30 mgKOH/g;
E. cooling, adding epoxy chloropropane and a second catalyst benzyl trimethyl ammonium chloride, stirring until the epoxy chloropropane and the second catalyst benzyl trimethyl ammonium chloride are dissolved, then carrying out heat preservation reaction, cooling when the acid value of the polymer is lower than 1mgKOH/g, adding strong base, and continuing the heat preservation reaction after the strong base is completely added;
F. sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 500-600g/mol, filtering the salt and washing the material to delaminate and remove the water phase, removing the solvent from the organic phase to obtain the molten epoxidized polyester resin, cooling the polyester resin, and then crushing and granulating to obtain the polyester resin.
2. The epoxidized polyester resin for weather-resistant high impact powder coatings as claimed in claim 1, wherein A, neopentyl glycol and trimethylolpropane in formula amount are added into a reaction kettle, firstly heated to 130-.
3. The epoxidized polyester resin for weather-resistant high-impact powder coatings according to claim 1, wherein B, when the acid value of the polymer is less than 90mgKOH/g, 2-ethyl-1, 3-hexanediol with the formula amount is added, then a nitrogen bubbling system is started, the temperature is gradually increased to 210-220 ℃ at the temperature increase rate of 5-7 ℃/h under the protection of nitrogen, the reaction is carried out under the condition of heat preservation until no obvious distillate is evaporated, and the acid value of the reactant is less than 35 mgKOH/g.
4. The epoxidized polyester resin for weather-resistant high impact powder coating according to claim 1, wherein C is added with a formula amount of antioxidant, a vacuum system is started and kept at a vacuum degree of-0.098 MPa to-0.095 MPa for reaction for 1-3h to promote further chain extension reaction of the polyester resin, and vacuumizing is stopped when the acid value is reduced to below 12 mgKOH/g.
5. The epoxidized polyester resin for weather-resistant high-impact powder coatings according to claim 1, wherein D, when the temperature is reduced to 200 ℃, adipic acid with the formula amount is added for carboxyl end-capping reaction, the temperature is raised to 225-230 ℃ at a rate of 10 ℃/h for esterification end-capping reaction for 2-4h, and the reaction is stopped when the acid value of the reactant is 20-30 mgKOH/g.
6. The epoxidized polyester resin for weather-resistant high-impact powder coating as claimed in claim 1, wherein E.
7. The epoxidized polyester resin for weather-resistant high-impact powder coating as claimed in claim 1, wherein, F, sampling and detecting, when the epoxy equivalent of the polymer in the reaction kettle is 500-600g/mol, the reaction is stopped, the material is subjected to salt filtration and water washing to remove the water phase in a layering manner, the water phase contains residual salt and catalyst, the organic phase is subjected to high temperature of 105-110 ℃ and reduced pressure distillation under vacuum of-0.098 MPa to remove the solvent to obtain the molten epoxidized polyester resin, the polyester resin is cooled by a steel belt with condensed water, and then the polyester resin is crushed and granulated to obtain the polyester resin; the sampling detection is to carry out detection after filtering salt and removing solvent of the sample.
8. The epoxidized polyester resin for weather-resistant high impact powder coating according to claim 1, which is prepared by a process comprising the steps of:
A. adding neopentyl glycol and trimethylolpropane with a formula amount into a reaction kettle, heating to 135 ℃ firstly, starting stirring after complete melting, then adding a first catalyst of monobutyl tin oxide with a formula amount, uniformly mixing, adding ethylsuccinic acid and tridecanedioic acid with a formula amount for esterification reaction, after the materials are added, gradually heating from 135 ℃ to 185 ℃ at a heating rate of 10-12 ℃/h, and carrying out heat preservation esterification dehydration reaction for 3-5 h;
B. when the acid value of the polymer is less than 90mgKOH/g, adding 2-ethyl-1, 3-hexanediol with the formula amount, starting a nitrogen blowing system, gradually heating to 210-220 ℃ at the heating rate of 5-7 ℃/h under the protection of nitrogen, and carrying out heat preservation reaction until no obvious distillate is evaporated, wherein the acid value of the reactant is less than 35 mgKOH/g;
C. adding the antioxidant with the formula amount, starting a vacuum system, keeping the vacuum degree of-0.098 Mpa to-0.095 Mpa, reacting for 1-3h, promoting the further chain extension reaction of the polyester resin, and stopping vacuumizing when the acid value is reduced to be below 12 mgKOH/g;
D. when the temperature is reduced to 200 ℃, adding adipic acid with the formula amount to carry out carboxyl end capping reaction, heating to 225-230 ℃ at the speed of 10 ℃/h to carry out esterification end capping reaction for 2-4h, and stopping the reaction when the acid value of the reactant is 20-30 mgKOH/g;
E. then cooling to 100-;
F. sampling and detecting, stopping the reaction when the epoxy equivalent of the polymer in the reaction kettle is 600g/mol together with 500-; the sampling detection is to carry out detection after filtering salt and removing solvent of the sample.
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