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Preparation method of quaternary ammonium salt modified polyester resin for antibacterial powder coating

A technology of modified polyester and antibacterial powder, applied in the field of powder coatings, can solve the problems of easy migration of antibacterial agents, unsatisfactory economy and safety, decreased antibacterial effect, etc., to reduce costs, safety risks, and requirements of reaction conditions. Low, excellent antibacterial effect

Active Publication Date: 2021-04-13
ZHEJIANG GUANGHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The antibacterial powder coating prepared by this method is in a free state, so the antibacterial agent is easy to migrate to the coating surface, and the antibacterial effect will decrease over time.
[0004] In order to improve the stability of quaternary ammonium salt antibacterial agents, researchers grafted quaternary ammonium salt antibacterial groups on insoluble polymer carriers to form polymer quaternary ammonium salts. The quaternary ammonium salt antibacterial groups were concentrated on the surface of the carrier. Larger, faster sterilization and higher efficiency, but the existing technology generally uses solution polymerization to synthesize high-molecular quaternary ammonium salts, which requires the use of a large amount of solvents, which is not very ideal from the perspective of economy and safety

Method used

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  • Preparation method of quaternary ammonium salt modified polyester resin for antibacterial powder coating
  • Preparation method of quaternary ammonium salt modified polyester resin for antibacterial powder coating
  • Preparation method of quaternary ammonium salt modified polyester resin for antibacterial powder coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0051] The quaternary ammonium salt-modified polyester resin in the examples of this group is a carboxyl-terminated quaternary ammonium salt-modified polyester resin.

[0052] Its preparation comprises the following steps:

[0053] Step S1: After heating the polyol and esterification catalyst with continuous stirring and melting, add polybasic acid and / or acid anhydride, and gradually raise the temperature to 180°C under the protection of nitrogen. During this period, the distillation column is used to distill out the esterification water, and the temperature of the distillation column is controlled at the top of the column. The temperature does not exceed 102°C to prevent the distillation of materials other than esterified water;

[0054] Step S2: After the temperature in step S1 rises to 220°C to 250°C, keep warm, wait until the material is clear and transparent, and basically no esterified water distills out, then cool down to 190°C to 210°C, add an end-capping agent, and c...

Embodiment 6～10

[0080] The difference between this group of examples and Examples 6-10 is that the end-capping agent in this group of examples is isophthalic acid.

[0081] The materials and molar amounts of each component in each embodiment are shown in Table 3 below.

[0082] The relevant performances of the carboxyl-terminated quaternary ammonium salt-modified polyester resins prepared in each embodiment were tested, and the test results are shown in Table 3 below.

[0083] Use the carboxyl-terminated quaternary ammonium salt-modified polyester resin prepared in Examples 6-10 to prepare powder coatings and coatings.

[0084] Preparation of powder coating: a, the carboxyl-terminated quaternary ammonium salt modified polyester resin prepared in 558g embodiment 6~10, 42gTGIC, 250g titanium dioxide, 136g precipitated barium sulfate, 10g leveling agent, 4g benzoin weighed and Pre-mixing; b. Melting and extruding the pre-mixed mixture through an extruder; c. Cooling and pressing tablets; d. Cru...

Embodiment 11～15

[0097] The quaternary ammonium salt-modified polyester resin in this group of examples is a hydroxyl-terminated quaternary ammonium salt-modified polyester resin.

[0098] Its preparation comprises the following steps:

[0099] Step S1: After the polyol and esterification catalyst are heated and continuously stirred and melted, the polybasic acid and / or acid anhydride is added, heated to 180°C under the protection of nitrogen, and the temperature is gradually raised. Prevent distillation of materials other than esterification water;

[0100] Step S2: keep warm when the temperature rises to 220-250°C, wait until the material is clear and transparent, and basically no esterification water distills out;

[0101] Step S3: Cool down to 200°C, add halomethyl carboxylic acid compound, keep warm at 220°C-240°C for 1-2h, then distill under reduced pressure at -0.095MPa--0.1MPa for 1-2h, take samples to measure the acid value, when acid After the value is below 5mgKOH / g, return to nor...

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Abstract

The invention discloses a preparation method of quaternary ammonium salt modified polyester resin for an antibacterial powder coating, and belongs to the technical field of powder coatings; the quaternary ammonium salt modified polyester resin is formed by bulk polymerization of a carboxylic acid compound, a tertiary amine compound, a comonomer and an esterification catalyst in a heating molten state; the carboxylic acid compound is a carboxylic acid compound with halomethyl, the comonomer comprises polybasic acid and / or anhydride and polyhydric alcohol, no solvent participates in the whole process, a solvent which is high in price, high in toxicity and volatile is avoided, and meanwhile multiple complex post-treatment processes such as filtering, washing, drying and crystallizing after the reaction are completed are avoided; waste liquid treatment cost is saved, strict explosion-proof workshops are not needed, environmental impact assessment requirements can be met more easily, personal safety of operators is guaranteed better, no by-product is produced in the whole process of esterification water removal, yield is high, requirements for reaction conditions are low, pressurization is not needed, preparation steps are simplified, cost and safety risks are reduced, and large-scale production is easy to achieve.

Description

【Technical field】 [0001] The invention relates to the technical field of powder coatings, in particular to a preparation method of a quaternary ammonium salt-modified polyester resin used for antibacterial powder coatings. 【Background technique】 [0002] Powder coating is an environmentally friendly, economical, high-efficiency, green coating with no VOC emissions. It has been developing very well since it came out. Antibacterial powder coatings have their market space, especially in some public places, such as hospitals, stations, schools, airports and other places where there is a large flow of people, it is necessary to use antibacterial coating products. Brief introduction of quaternary ammonium salt antibacterial agent: quaternary ammonium salt is also a kind of chemically synthesized antibacterial agent. It has strong antibacterial power, broad-spectrum antibacterial, convenient and easy to obtain, and has a wide range of uses. After the quaternary ammonium salt is in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C08G63/183C08G63/78C09D167/02C09D5/03C09D5/14
CPCC08G63/916C08G63/183C08G63/78C09D167/02C09D5/03C09D5/14C08G2150/20
Inventor 褚海涛贾林孙杰风许国徽
Owner ZHEJIANG GUANGHUA NEW MATERIALS
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