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Core-shell type short-chain fluorine-containing acrylate emulsion and preparation method thereof

A technology of acrylate and butyl acrylate, applied in the direction of plant fiber, coating, fiber treatment, etc., can solve the problems of water and oil repellency of polymer, water and oil repellency, etc., to improve water and oil repellency. Good water and oil repellency effect, cost reduction effect

Inactive Publication Date: 2016-03-30
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) Compared with conventional emulsion polymerization, the core-shell emulsion greatly reduces the amount of fluorine monomer, but judging by the contact angle, its water and oil repellency effect is slightly reduced, which needs to be improved, such as literature 1 and literature 2, 3 Case
[0009] (2) In the same core-shell emulsion polymerization, after the main functional monomer fluorine monomer is changed from C8 to C6, the water and oil repellency effect of the polymer decreases, as in the case of Document 2 and Document 3

Method used

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  • Core-shell type short-chain fluorine-containing acrylate emulsion and preparation method thereof
  • Core-shell type short-chain fluorine-containing acrylate emulsion and preparation method thereof
  • Core-shell type short-chain fluorine-containing acrylate emulsion and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Seed emulsion: in the 250ml four-necked flask that electric stirrer, condensation pipe, thermometer, nitrogen gas introduction device are housed, add the compound surfactant 0.48g (m(SDS) of metering: m(OP-10)= 2:1) and 75g of deionized water, nitrogen, stirred for 15min and then heated to 50°C. Then add 27g of the core phase (mass ratio BA:MMA=2:1) ​​and 0.48g of NMA into the above-mentioned flask, blow nitrogen, and stir for 25 minutes to pre-emulsify. Dissolve the initiator 0.16g KPS in 15g deionized water and add 2 / 3 to the above-mentioned four-necked flask. The temperature was raised to 70°C, and the reaction was stirred for 2h. That is, the seed emulsion is obtained.

[0035] (2) Shell core emulsion: take 0.06g of compound surfactant (m(SDS):m(OP-10)=2:1), take 2.7g of FMA6, 1.62g of long carbon chain acrylate, and 10g of deionized water Pre-emulsify for 30 minutes to obtain the shell monomer pre-emulsion, then mix it with the remaining 1 / 3 KPS aqueous solu...

Embodiment 2

[0040] (1) Seed emulsion: in the 250ml four-necked flask that electric stirrer, condensation pipe, thermometer, nitrogen gas introduction device are housed, add the compound surfactant 0.51g (m(SDS) of metering: m(OP-10)= 2:1) and 75g of deionized water, nitrogen, stirred for 15min and then heated to 50°C. Then add 23.8g of the core phase (mass ratio BA:MMA=2:1) ​​and 0.34g of NMA into the above-mentioned flask, blow nitrogen, and stir for 25 minutes to pre-emulsify. Dissolve the initiator 0.51g KPS in 15g deionized water and add 2 / 3 to the above-mentioned four-necked flask. The temperature was raised to 70°C, and the reaction was stirred for 2h. That is, the seed emulsion is obtained.

[0041] (2) Core-shell emulsion: take 0.15g of compound surfactant (m(SDS):m(OP-10)=2:1), take 6.8g of FMA6, 3.06g of long carbon chain acrylate, and 10g of deionized water Pre-emulsify for 30 minutes to obtain the shell monomer pre-emulsion, then mix it with the remaining 1 / 3 KPS aqueous so...

Embodiment 3

[0044] (1) Seed emulsion: add metered compound surfactant 0.95g (m(SDS):m(OP-10)= 1:1) and 75g of deionized water, nitrogen, stirred for 15min and then heated to 50°C. Then add 27g of the core phase (mass ratio BA:MMA=1:1) and 0.48g of NMA into the above-mentioned flask, blow nitrogen gas, and stir for 25 minutes to pre-emulsify. Dissolve the initiator 0.16g KPS in 15g deionized water and add 2 / 3 to the above-mentioned four-necked flask. The temperature was raised to 70°C, and the reaction was stirred for 2h. That is, the seed emulsion is obtained.

[0045] (2) Shell-core emulsion: take 0.13g of compound surfactant (m(SDS):m(OP-10)=1:1), take 2.7g of FMA6, 1.62g of long carbon chain acrylate, and 10g of deionized water Pre-emulsify for 30 minutes to obtain the shell monomer pre-emulsion, then mix it with the remaining 1 / 3 KPS aqueous solution, add it dropwise to the seed emulsion with a temperature control of 75°C with a titration funnel, control the drop for about 2 hours,...

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Abstract

The present invention discloses core-shell short-chain fluorine-containing acrylate emulsion and a preparation method thereof. A series of core-shell short-chain fluorine-containing acrylate emulsion are synthesized from methyl methacrylate (MMA) and butyl acrylate (BA) copolymer as a core and a short fluorocarbon chain 2-(perfluorohexyl) ethyl methacrylate (FMA6) and non-fluoro alkyl methacrylate copolymer as a shell by a multi-step emulsion polymerization method. The core-shell short-chain fluorine-containing acrylate emulsion solves the environmental problem caused by a C8 fluorine-containing monomer as an essential functional monomer used in a main three-control finishing agent, and meanwhile makes up the defect of shortage of product water-repellent and oil-repellent effects when an environmentally friendly C6 fluorine-containing monomer is used as an essential functional monomer. The product has a core-shell structure, the shell layer is rich in a fluorine-containing acrylate component, the amount of the fluorine monomer in the emulsion can be greatly reduced, cost is reduced, water contact angle and oil contact angle of a product latex film are large, and the core-shell short-chain fluorine-containing acrylate emulsion used in textile finishing exhibits excellent water and oil repellency.

Description

technical field [0001] The invention belongs to the technical field of polymer chemistry, and in particular relates to a preparation method of a core-shell type short-chain fluorine-containing acrylate emulsion, which can be used in the fields of fabric finishing, water-based paint, solid surface modification and the like. Background technique [0002] Due to the unique properties of fluorine atoms, fluorine-containing polymers have excellent low surface properties. Compared with aliphatic hydrocarbons and silicone-based water repellents, fluorine-containing finishing agents can not only obtain excellent waterproof, oil-proof, In addition to anti-fouling properties, it can also maintain a good soft feel and excellent air permeability and moisture permeability of the fabric. [0003] Long carbon chain perfluoroalkyl compounds (C8 for short) with greater than or equal to 8 carbons have always been the mainstream of "three-proof" finishing agents for organic fluorine series fab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F220/14C08F220/24C08F220/58C08F2/26C08F2/30D06M15/277C09D133/16D06M101/06
Inventor 张跃军唐敏
Owner NANJING UNIV OF SCI & TECH
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