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Polyester type fluorine-containing block polymer as well as preparation method and application thereof

A block polymer, polyester technology, used in polyester coatings, coatings, powder coatings, etc., can solve the problem of reducing surface tension and leveling speed. Long-chain fluorocarbon acrylate, long-chain fluorocarbon chain Poor compatibility of monomer homopolymers, low utilization of fluorocarbons, etc., to achieve wide compatibility, wide application range and the effect of reducing surface tension

Active Publication Date: 2020-07-14
上海深竹化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The disadvantages of the prior art are: the existing fluorine-containing leveling agent technologies are all based on acrylates, which have limited applicability, especially limited compatibility with some polyester and alkyd matrix resins; in addition, the existing Fluorine-containing leveling agent technology is mostly based on ordinary free radical technology, and the utilization rate of fluorocarbons is not high. Although CN101448865A uses active polymerization to prepare block polymers, the compatibility of long-chain fluorocarbon chain monomer homopolymers is too high. Poor, only short-chain fluorocarbon acrylate can be used, but its effect of reducing surface tension and leveling speed is not as good as long-chain fluorocarbon acrylate

Method used

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  • Polyester type fluorine-containing block polymer as well as preparation method and application thereof
  • Polyester type fluorine-containing block polymer as well as preparation method and application thereof
  • Polyester type fluorine-containing block polymer as well as preparation method and application thereof

Examples

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preparation example Construction

[0032] In the preparation method of the polyester-type fluorine-containing block polymer of the present invention, first prepare the polyester block M: monoalcohol, such as lauryl alcohol, and ε-caprolactone and δ-valerolactone Put it into a three-necked flask, add a ring-opening polymerization catalyst, such as dibutyltin dilaurate or stannous octoate, pass nitrogen or argon, heat up to 120-180°C, keep warm until the conversion rate reaches more than 99.5%, and the conversion rate can be It is obtained by testing the solid content, and then the first block polyester can be obtained by lowering the temperature, and its number-average molecular weight and molecular weight distribution can be tested by gel chromatography.

[0033]Prepare the block polyester containing vinyl bonds in the following way: the first block polyester, ε-caprolactone and α-methylene-γ-butyrolactone, polymerization inhibitor, catalyst, etc. are added in proportion to In the flask, pass nitrogen or argon,...

Embodiment 1

[0039] Put 3.9 parts of lauryl alcohol, 54.7 parts of ε-caprolactone, 12 parts of δ-valerolactone, and 0.02 parts of stannous octoate into a three-necked flask, start stirring, replace nitrogen, raise the temperature to 140°C, and keep it warm for 12 to 16 hours. When the solid content of the monitoring system reached the theoretical value, the reaction was stopped, and the polyester A1 was cooled down to a light yellow viscous flowable liquid. The molecular weight and molecular weight distribution were tested by GPC, Mn=3800, PDI=1.8.

[0040] Add 22.8 parts of ε-caprolactone and 5.9 parts of α-methylene-γ-butyrolactone to polyester A1, start stirring, replace nitrogen, add 0.15 parts of diphenylphosphoric acid, stir at room temperature for 12 hours, and monitor the solids of the system After reaching the theoretical value, stop the reaction, and cool down to light yellow viscous flowable polyester B1. Take a sample to test the molecular weight and molecular weight distributi...

Embodiment 2

[0042] Example 2: Put 3.9 parts of lauryl alcohol, 54.7 parts of ε-caprolactone, 24 parts of δ-valerolactone, and 0.02 parts of stannous octoate into a three-necked flask, start stirring, replace nitrogen, heat up to 140°C, and keep warm for 12 ~16h, monitor the solid content of the system to the theoretical value, stop the reaction, and cool down to light yellow viscous flowable liquid polyester A2. The molecular weight and molecular weight distribution were tested by GPC, Mn=4200, PDI=1.6.

[0043] Add 22.8 parts of ε-caprolactone and 2 parts of α-methylene-γ-butyrolactone to polyester A2, start stirring, replace nitrogen, add 0.15 parts of diphenylphosphoric acid, stir at room temperature for 10 hours, and monitor the solids of the system When it reaches the theoretical value, stop the reaction, and cool down to light yellow viscous flowable polyester B2. Take a sample to test the molecular weight and molecular weight distribution, Mn=5300, PDI=1.3.

[0044] Add 7.6 parts ...

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Abstract

The present invention discloses a polyester type fluorine-containing block polymer, a preparation method and an application thereof, a general formula is R1-[M]-[N], R1 is C1-C22 branched or straightchain alkyl alcohol; [M] is a polyester chain obtained by polycondensation or ring opening polymerization of one or more hydroxy acids or hydroxy acid lactones; wherein [N] is a chain segment obtainedby carrying out random copolymerization on epsilon-caprolactone and alpha-methylene-gamma-butyrolactone and then carrying out a click reaction on the chain segment and sulfydryl-vinyl containing fluorine-containing mercaptan, the structural formula of [N] is as follows: x and y are polymerization degrees, the ratio of x to y is 3: 1-10: 1, and y is greater than or equal to 1 and less than or equal to 20; R2 is a fluorine-containing organic matter, the compound is selected from CnF2n+1(CH2)m<->, ACnF2n(CH2)m<->, CnF2n+1(CH2)m <->(OCH2CHR2)P<->, ACnF2n(CH2)m <->(OCH2CHR3)P<->, wherein A is H, Cl, Br, I, C1-12 alkyl or C1-12 alkoxy, n is greater than or equal to 2 and less than or equal to 20, m is greater than or equal to 0 and less than or equal to 4, and p is greater than or equal to 0 and less than or equal to 20. The polyester type fluorine-containing block polymer has wide compatibility, wide application range and excellent leveling property, and a smooth surface can be obtained after the polyester type fluorine-containing block polymer is used.

Description

technical field [0001] The invention relates to the technical field of polyester-type block polymers, in particular to a polyester-type fluorine-containing block polymer, a preparation method and an application thereof. Background technique [0002] After the coating or ink is applied, it is usually desired to obtain a smooth and uniform solid film without shrinkage, not only to meet the visual aesthetic requirements, but more importantly, for some functional coatings, such as anti-corrosion coatings, conductive coatings, insulating coatings, etc., If the surface has shrinkage cavities or is not covered by the coating, it will affect the performance of the product and significantly reduce the functionality of the coating. [0003] When coating or ink is applied on a solid surface, if the surface tension of the substrate is low, and the surface tension of the liquid system is high, it is not easy to coat, and an uncovered surface will result. During the construction and film...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C09D7/47C09D5/03C09D167/00C09D167/08
CPCC08G63/912C08L2205/02C08L2205/03C09D5/033C09D167/00C09D167/08C09D7/47C08L67/04
Inventor 孙丽莉程德书金逐中罗菊香
Owner 上海深竹化工科技有限公司