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Network-structure short-chain fluorine-containing waterproof and oil-proof copolymer and preparation method thereof

A waterproof and oil-proof, network structure technology, applied in the direction of fiber type, textile and papermaking, fiber processing, etc., can solve the problems of high price, difficult degradation of PFOA/PFOS, bioaccumulative environmental hazards, etc., to achieve large steric hindrance, Good waterproof and oil-proof effect

Active Publication Date: 2021-04-30
TAICANG BAONI IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the deepening of relevant research, people gradually realize that PFOA / PFOS is difficult to degrade, bioaccumulate and harm the environment in the application process, so this kind of fluorine-containing compounds is restricted and banned
[0003] Short-chain alkyl fluorine water repellent, that is, C6 or C4 water repellent commonly used in the industry, has extremely low bioaccumulation and almost non-toxicity. Current research is considered to be a good substitute for long-chain alkyl fluorine water and oil repellents products, but they are expensive

Method used

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  • Network-structure short-chain fluorine-containing waterproof and oil-proof copolymer and preparation method thereof
  • Network-structure short-chain fluorine-containing waterproof and oil-proof copolymer and preparation method thereof
  • Network-structure short-chain fluorine-containing waterproof and oil-proof copolymer and preparation method thereof

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preparation example Construction

[0041] In a preferred embodiment, the present invention provides a kind of preparation method of network structure short-chain fluorine-containing waterproof and oil-repellent copolymer, it comprises the steps:

[0042] 1) dissolving the nonionic surfactant and the cationic surfactant in a mixed solution of water and an organic solvent to prepare a solution;

[0043] 2) adding the pre-mixed solution of the comonomer into the solution of step 1), and high shearing to make a pre-emulsion;

[0044] 3) Warm up the pre-emulsion in step 2) to 70-90°C, add an initiator to initiate, and keep warm for 2-4h;

[0045] 4) Cool down to room temperature, adjust pH to 2-4 with acetic acid and collect.

[0046] In a more preferred embodiment, said nonionic surfactant comprises isomerism (C 10 -C 13 ) alcohol polyoxyethylene ether (5-20EO), C 8 -C 20 Fatty alcohol polyoxyethylene ether (15-40EO), or their mixture; the cationic surfactant includes dodecyltrimethylammonium chloride, dodecyl...

Embodiment 1

[0068] 21g of 1,3,5-benzenetricarboxylic acid and 38g of 1,14-tetradecanediol were reacted at 220°C for 4 hours under the catalysis of 0.12g of tetra-n-butyl titanate, and then 7.92g of acrylic acid and 0.1g of titanic acid were added Tetra-n-butyl ester and 0.4 g of hydroquinone were reacted at 220° C. for 3 h and cooled to room temperature to be used as comonomer 1.

[0069] Stir and dissolve 1.0g fatty alcohol polyoxyethylene ether (10EO) and 0.8g cetyltrimethylammonium bromide in a mixed solution of 68.8g deionized water and 7g ethylene glycol monobutyl ether, then mix 10g of the above Comonomer 1, 3.5g of octadecyl acrylate, 6.0g of perfluorobutyl ethyl acrylate, 0.5g of hydroxyethyl acrylate were mixed evenly and then added, the temperature was raised to 70°C, and after complete dissolution, high shear was used to obtain pre-emulsion 1 .

[0070] Add 2.4g of 10% azobisisobutylamidine hydrochloride solution slowly (control the stable change not to be higher than 5°C) dro...

Embodiment 2

[0072] 21g of 1,3,5-benzenetricarboxylic acid and 24g of 1,3-octanediol were reacted at 220°C for 4h under the catalysis of 0.1g of tetra-n-butyl titanate, and then 7.92g of acrylic acid and 0.1g of tetra-titanate were added. n-Butyl ester and 0.4g of hydroquinone were reacted at 220°C for 3h, then cooled down to room temperature, as comonomer 2.

[0073] 0.9g of isomeric tridecyl alcohol polyoxyethylene ether (15EO), 0.7g of octadecyltrimethylammonium chloride were stirred and dissolved in 70g of deionized water and 6g of propylene glycol mixture, and then 11.4g of the above-mentioned comonomer 2. 3.3g of n-butyl acrylate, 4.5g of perfluorohexyl ethyl acrylate, and 0.8g of glycidyl acrylate were mixed evenly and then added, the temperature was raised to 70°C, and after complete dissolution, pre-emulsion 2 was obtained by high shearing.

[0074] Add 2.4g of 10% azobisisobutylamidine hydrochloride solution slowly (control the stable change not to be higher than 5°C) dropwise in...

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Abstract

The invention provides a network-structure short-chain fluorine-containing waterproof and oil-proof copolymer and a preparation method thereof. The network-structure short-chain fluorine-containing waterproof and oil-proof copolymer comprises the following copolymerization units: 1) 35-65 wt% of copolymerization units derived from a condensation polymer of 1, 3, 5-benzenetricarboxylic acid, alkyl glycol and acrylic acid; 2) 15-35 wt% of copolymerized units derived from a short chain fluorinated acrylate; 3) 10-40 wt% of copolymerized units derived from an acrylate; and 4) 1-10 wt% of copolymerized units derived from functional monomers. The copolymer is of a reticular structure, has good waterproof and oil-proof effects, can be comparable with a long-chain perfluoroacrylate waterproof and oil-proof agent, and can be used for waterproof and oil-proof finishing of various substrates such as fabrics, leather, paper and the like.

Description

technical field [0001] The invention relates to the field of functional additives, in particular to the field of water and oil repellents. Background technique [0002] Fluorine-containing acrylate copolymer emulsion is the only water and oil repellent finishing agent commonly used in the market. Acrylic polymers with perfluorocarbon chains (-CnF2n+1, n≥8) based on perfluorooctanoic acid (PFOA) or perfluorooctane sulfonic acid (PFOS) are usually called long-chain alkyl perfluorinated waterproof and oil-proof agent. With the deepening of relevant research, people have gradually realized that PFOA / PFOS is difficult to degrade, bioaccumulates in the application process, and is harmful to the environment. Therefore, this type of fluorine-containing compounds is restricted and banned. [0003] Short-chain alkyl fluorine water repellent, that is, C6 or C4 water repellent commonly used in the industry, has extremely low bioaccumulation and almost non-toxicity. Current research is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/06C08F220/18C08F220/24C08F220/20C08F220/32C08F220/34D06M15/277D06M15/263D06M15/273D06M101/32
CPCC08F290/061D06M15/277D06M15/263D06M15/273D06M2200/11D06M2200/12D06M2101/32C08F220/1818C08F220/24C08F220/20C08F220/1804C08F220/325C08F220/1812C08F220/34
Inventor 姚敏敏李正雄
Owner TAICANG BAONI IND CO LTD
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