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Preparation process of flame-retardant polyester resin and application of flame-retardant polyester resin in flame-retardant coatings

A technology of flame retardant polyester and preparation process, applied in polyester coatings, fire retardant coatings, coatings, etc., can solve problems such as changes in coating properties, changes in resin structure, and reduction in flame retardant properties of coatings, and achieves high activity and strong performance. Effect

Active Publication Date: 2021-04-02
宁波顺声通讯设备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because polyester resin contains ester groups, it is easy to be hydrolyzed, and the acid gas dissolved in water will catalyze the hydrolysis and breakage of resin ester bonds more quickly, so that the structure of polyester resin will change and affect the performance of the prepared coating. In the prior art, the resin is directly cross-linked by a cross-linking agent to form a network cross-linked structure. Since the position of the cross-linking group on the resin is fixed, it is located on the carboxyl side or the hydroxyl side of the ester group, so the ester group is hydrolyzed The non-crosslinked side generates free small molecular substances, which in turn causes changes in the resin structure and changes in the properties of the prepared coatings.
[0003] Existing polyester resins are widely used in the preparation of coatings. For flame retardant polyester resins, flame retardants are usually added directly, but after the flame retardants are added, they are mixed by mechanical stirring. Many flame retardants are mixed with the matrix resin. The compatibility between them is poor, resulting in the reduction of the flame retardant performance of the coating

Method used

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  • Preparation process of flame-retardant polyester resin and application of flame-retardant polyester resin in flame-retardant coatings

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The specific preparation process of flame retardant reinforcing agent is as follows:

[0032] Step 1: Add 265mL of acetone, 283g of cupric chloride and 72g of isobutyraldehyde into the reaction kettle, stir and react at 8°C for 83h, then heat to evaporate the solvent and cool down to 0°C, then filter and recover cuprous chloride to obtain chlorinated Isobutyraldehyde; Chloroisobutyraldehyde 1 HNMR spectrum analysis, δ=1.75ppm is -CH 3 group 1 Absorption peak of H, δ=9.72ppm aldehyde group 1 H absorption peak;

[0033] Step 2: Add 500mL of benzene and 1mol of dimethyl phosphite into the reaction kettle at the same time, and then add a methanol solution of sodium methoxide to it. The amount of sodium methoxide added is 1mol. After stirring evenly, the temperature is raised to 60°C, and 0.98mol of N- Allylmethylamine, control the dropwise addition within 1 hour, reflux reaction for 4 hours after the addition, then adjust the pH of the solution to 7-7.5, then add the pr...

Embodiment 2

[0037] The specific preparation process of brominated adipic acid is as follows: Add 1 mol of adipic acid into 150 mL of benzene and stir to dissolve, then raise the temperature to 80°C, add 100 mL of bromine and 4.8 mL of phosphorus trichloride dropwise, and heat the reaction until no longer Red bromine liquid vapor appears, then slowly raise the temperature to 100°C and keep it warm for 4 hours, then carry out vacuum distillation and cooling crystallization on the product to obtain brominated adipic acid; brominated adipic acid 1 Spectrum analysis of HNMR, δ=4.23ppm and δ=12.22ppm are carboxyl groups 1 H absorption peak.

Embodiment 4

[0039] The specific preparation process of dihydroxyacetophenone is as follows: 1mol of 4-aminoacetophenone, 50mL of acetic acid solution with a mass concentration of 35% and 160mL of ethanol are simultaneously added to the reactor and stirred to dissolve, and then 2.4mol of Propylene oxide, control the dropwise addition within 2 hours, then raise the temperature to 30°C for 2 hours, then raise the temperature to 110°C for 7 hours, and remove unreacted propylene oxide and solvent by rotary evaporation to obtain dihydroxyacetophenone; Keto 1 Spectrum analysis of HNMR, δ=2.5ppm and δ=5.37ppm are -CH in the benzene ring connected to the ethyl ketone group 3 and hydroxyl 1 H absorption peak;

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Abstract

The invention discloses a preparation process of flame-retardant polyester resin, which is characterized by comprising the following steps: adding a flame-retardant reinforcing agent, absolute ethyl alcohol and a sodium hydroxide solution with the mass concentration of 18% into a reaction kettle, stirring to dissolve, adding saturated polyester resin liquid, reacting for a period of time, adding asaturated solution of sodium carbonate, dropwise adding diaminosilane after stirring and reacting for 4 hours, continuously adding diethylene glycol monoethyl ether acetate in the reaction process, carrying out rotary evaporation to recover the solvent, and washing the product to be neutral to obtain the flame-retardant polyester resin. According to the flame-retardant polyester resin prepared bythe invention, the saturated polyester resin is subjected to cross-linking polymerization by virtue of a flame-retardant enhancer, and two amino groups in the diaminosilane added into the saturated polyester resin can be subjected to addition reaction with olefin groups, so that the polyester resinis cross-linked with flame-retardant enhancer and then cross-linked by virtue of the diaminosilane to form a reticular structure; therefore, the prepared resin has relatively strong performance.

Description

technical field [0001] The invention belongs to the field of paint preparation, and relates to a preparation process of flame-retardant polyester resin and its application in flame-retardant paint. Background technique [0002] Polyester resins are usually prepared by esterification and polycondensation of dibasic acids and dibasic alcohols. A common feature of this type of polymer structure is that the chains of its macromolecules are connected by ester groups, so they are commonly called polyesters. Polyester has the advantages of bright, plump, high hardness, good physical and mechanical properties, chemical corrosion resistance, adhesion, impact resistance and wear resistance. With the development of science and technology, more and more saturated polyester resin products are used in high-performance fields. However, because polyester resin contains ester groups, it is easy to be hydrolyzed, and the acid gas dissolved in water will catalyze the hydrolysis and breakage ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/682C08G63/91C09D167/02C09D161/20C09D5/18C09D7/61
CPCC08G63/6826C08G63/916C08K2003/3045C08L2201/02C09D5/18C09D167/02C09D7/61C08L61/20C08K3/30
Inventor 吴春秋
Owner 宁波顺声通讯设备有限公司
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