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Method for preparing super branched polyacrylate fluorine and application in finishing agent for textile

A polyacrylate and hyperbranched polyester technology, applied in the direction of physical treatment of paper, etc., can solve the problems of uneven distribution of fluorine atoms on the surface of substrates, many self-polymers in copolymerization products, uneven distribution of fluorine atoms, etc. The effect of novel method, light color and broad industrial application prospect

Inactive Publication Date: 2005-10-26
上海瀛正科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these fluorine-containing acrylate monomers are similar in molecular structure, and there is a common shortcoming when they are copolymerized with hydrocarbon (meth) acrylate monomers: the ratio of fluorine-containing acrylate monomer to hydrocarbon acrylate monomer The reactivity ratio of the body is small, and the surface energy of the carbon-fluorine bond is much lower than that of the carbon-hydrogen bond; resulting in more self-polymers and less alternating copolymers in their copolymerization products; thus in the microstructure On the surface, the distribution of fluorine atoms in the copolymerization product is uneven; this eventually causes the uneven distribution of fluorine atoms on the surface of the substrate, resulting in a decrease in water and oil repellency

Method used

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  • Method for preparing super branched polyacrylate fluorine and application in finishing agent for textile
  • Method for preparing super branched polyacrylate fluorine and application in finishing agent for textile
  • Method for preparing super branched polyacrylate fluorine and application in finishing agent for textile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1. take pentaerythritol as core, prepare polycarboxy polyester by esterification with trimellitic anhydride;

[0038] A 250ml four-necked flask reactor equipped with a magnetic stirrer, a nitrogen inlet and a condenser was used to add 20g (0.147mol) pentaerythritol, 150ml dioxane, 113g (0.588mol) trimellitic anhydride, 0.14g (1000ppm) ) stannous chloride, be warming up to the dioxane reflux state under continuous stirring, react for 8 hours, after the reaction solution is cooled, dioxane is distilled under reduced pressure to obtain a kind of white powder, namely polycarboxy polyester; The yield of the reaction was 96%.

[0039] The obtained product is analyzed by infrared spectrum, and the acid anhydride corresponds to infrared 1810cm -1 The peak disappears. At 1760cm -1 The characteristic peak of ester group appears.

[0040] Using the titration method, the acid value of the product was determined to be 502 mgKOH / g with potassium hydroxide ethanol stand...

Embodiment 2

[0044] Embodiment 2. prepare the hyperbranched polyester of terminal hydroxyl with propylene oxide modified polycarboxyl polyester;

[0045] Adopt a 250ml four-necked flask reactor equipped with a magnetic stirrer, an oil bath and a nitrogen inlet, a condenser and a dropping funnel, add 20g (0.022mol) of polycarboxylated polyester synthesized in Example 1, 100ml of tetrahydrofuran, 15.8g (0.264mol) of propylene oxide and 1.1g (3wt%) of N,N-dimethylbenzylamine were reacted at 65°C for 7 hours, and tetrahydrofuran was distilled under reduced pressure to obtain a colorless viscous liquid, namely terminal hydroxyl group The hyperbranched polyester, its molecular structure is:

[0046]

[0047] The obtained product was analyzed by infrared spectroscopy, and the carboxylic acid corresponds to infrared 1680cm -1 The peak disappears. At 1760cm 1 The characteristic peak of ester group becomes stronger.

[0048] Using the titration method, the acid value of the product was determ...

Embodiment 3

[0052] Example 3. Using the hyperbranched polyester with 8 hydroxyl groups obtained in Example 2 as the core, a "direct method" was used to prepare a hyperbranched polyester with partial acrylated end groups

[0053] Adopt the 250ml three-necked flask reactor equipped with magnetic stirrer, nitrogen inlet and condensing water separator, add 20g (0.015mol) hyperbranched polyester of 8 hydroxyl groups obtained in Example 2, 5.7g (0.078mol) acrylic acid , 100ml toluene and 0.04g (500ppm) p-hydroxyanisole, stir and heat up to 100 ° C, form a transparent solution under nitrogen and continue stirring, add 1g (5wt%) p-toluenesulfonic acid, stir and heat up to toluene reflux state, the reaction is 4-5 hours, and the water output is almost the same as the theoretical value. Cool down, and after the reaction solution is cooled, use saturated NaHCO 3 The aqueous solution washes away residual acrylic monomer and p-toluenesulfonic acid. Separate liquid and use anhydrous Na 2 SO 4 The o...

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Abstract

The present invention relates to a fluorine-contained ultrabranched polyacrylate which can be used in water-proofing oil-proofing fabric finishing agent and its preparation method. Said method includes the following steps: using hydroxyterminated ultrabranched polyester as reaction substrate, adopting 'direct method' or 'indirect method' to modifying its hydroxyl end group into polymerizable active double bond, then adding perfluorinated acyl chlroide or esters, and making it and residual hydroxyl end group of said ultrabranched polyester implement esterification reaction; finally making part of its terminal group form into acrylate double bond and making its another part form into perfluoroalkyl so as to obtain the fluorine-contained ultrabranched polyacrylate. Then said fluorine-contanied ultrabranched polyacrylate and hydrocarbon (methyl) acrylate are undergone the process of emulsion copolymerization so as to obtain the water-proofing oil-proofing fluorine-contained fabric finishing agent emulsion.

Description

[Technical field] [0001] The invention relates to a fluorine-containing hyperbranched polyacrylate which can be used as a water- and oil-repellent fabric finishing agent and a preparation method thereof. [Background technique] [0002] The organic fluorine treatment agent has low interfacial tension, excellent heat resistance and chemical stability, so it can endow leather, textiles, paper and other substrates with excellent waterproof, oil-proof and anti-fouling properties. Acrylic polymers have the characteristics of good film formation and good flexibility of the cured product. After using it as a finishing agent to treat textiles, paper, etc., the treated products have good air permeability and good hand feel. Although polyacrylate has the characteristics of good water resistance, easy availability of raw materials and low cost, it does not have oil resistance. If the perfluoroalkyl group is introduced into the molecular structure of the polyacrylate, the fluorine-conta...

Claims

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Application Information

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IPC IPC(8): C08G63/91
Inventor 徐刚王嘉罗国良郝振文
Owner 上海瀛正科技有限公司
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