A kind of preparation method of fluorine-containing polyacrylate soap-free emulsion

A technology of polyacrylate and soap-free emulsion, which is applied in the preparation of fluorine-containing polyacrylate soap-free emulsion and the preparation of cationic soap-free fluorine-containing water and oil repellent, which can solve the problems of increased production cost, low solubility, environmental pollution, etc. problem, to achieve the effect of improving waterproof and oil-proof performance and good placement stability

Inactive Publication Date: 2016-04-06
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low solubility of fluorine-containing monomers in the water phase, a large amount of solvents (such as acetone, etc.) are usually added during the polymerization process, which will lead to increased production costs and environmental pollution

Method used

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  • A kind of preparation method of fluorine-containing polyacrylate soap-free emulsion

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Preparation of fluorine-containing terpolymer.

[0032] First, 40 g of dodecafluoroheptyl acrylate, 20 g of N-butyldiallylamine, and 40 g of N-methyldiallylamine were uniformly mixed to prepare mixed monomer A.

[0033] Add mixed monomer A and 200 g of dioxane into a four-neck flask equipped with a stirring device, a reflux device and a thermometer. The temperature of the solution was raised to 65° C., and 1 g of azobisisobutyronitrile was added to initiate a polymerization reaction. The polymerization time was 8 hours.

[0034] After the polymerization reaction is completed, the solvent is distilled off under reduced pressure to obtain a terpolymer with a vacuum degree of 10mmHg-20mmHg.

[0035] 2. Preparation of cationic soap-free fluorine-containing emulsion.

[0036] Mix 50 g of dodecafluoroheptyl methacrylate and 50 g of methyl acrylate to prepare mixed monomer B.

[0037] The terpolymer prepared above and water were added to the mixed monomer B. Th...

Embodiment 2

[0040] 1. Preparation of fluorine-containing terpolymer.

[0041] First, 60 g of dodecafluoroheptyl methacrylate, 10 g of N-butyldiallylamine, and 30 g of N-methyldiallylamine were uniformly mixed to prepare the mixed monomer A.

[0042] Add mixed monomer A and 300 g of dioxane into a four-neck flask equipped with a stirring device, a reflux device and a thermometer. The temperature of the solution was raised to 65° C., and 3 g of azobisisobutyronitrile was added to initiate a polymerization reaction. The polymerization time was 6 hours.

[0043] After the polymerization reaction is completed, the solvent is distilled off under reduced pressure to obtain a terpolymer with a vacuum degree of 10mmHg-20mmHg.

[0044] 2. Preparation of cationic soap-free fluorine-containing emulsion.

[0045] Mix 50 g of dodecafluoroheptyl acrylate and 50 g of butyl acrylate to prepare mixed monomer B.

[0046] The terpolymer prepared above and water were added to the mixed monomer B....

Embodiment 3

[0049] 1. Preparation of fluorine-containing terpolymer.

[0050] Firstly, 60 g of dodecafluoroheptyl acrylate, 10 g of N-dodecyl diallylamine, and 30 g of N-methyl diallyl amine were uniformly mixed to prepare the mixed monomer A.

[0051] Add mixed monomer A and 400 g of dioxane into a four-neck flask equipped with a stirring device, a reflux device and a thermometer. The temperature of the solution was raised to 85° C., and 5 g of azobisisobutyronitrile was added to initiate a polymerization reaction. The polymerization time was 4 hours.

[0052] After the polymerization reaction is completed, the solvent is distilled off under reduced pressure to obtain a terpolymer with a vacuum degree of 10mmHg-20mmHg.

[0053] 2. Preparation of cationic soap-free fluorine-containing emulsion.

[0054] Mix 50 g of hexafluorobutyl acrylate, 40 g of methyl acrylate, and 10 g of lauryl acrylate to prepare mixed monomer B.

[0055] The terpolymer prepared above and water were ad...

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Abstract

The invention relates to a preparation method of a cation polyacrylate soap-free emulsion containing fluorine. The preparation method comprises following steps: dodecafluorhe-ptylacrylate or dodecafluoroheptyl methacrylate, N-alkyl diene propyl amine, and methyldiallylamine are mixed so as to obtain a mixed monomer A; oil soluble initiator azodiisobutyronitrile is added, an obtained mixture is heated to a certain temperature for polymerization, and a terpolymer is obtained; organic fluorine monomer and acrylate monomer are mixed so as to obtain a mixed monomer B; the terpolymer and water are added so as to obtain a monomer pre-emulsification liquid C; and water soluble initiator azobis(2-methylpropionamidine) dihydrochloride is added, and finished products are obtained via polymerization. The cation polyacrylate soap-free emulsion containing fluorine is a white emulsion; pH value ranges from 4.0 to 7.0; when the cation polyacrylate soap-free emulsion containing fluorine is mixed with water at a ratio of 9:1, no delamination is caused in 24 hours; and the cation polyacrylate soap-free emulsion containing fluorine possesses excellent storage stability, and can be stored at room temperature for 6 months without deterioration. The cation polyacrylate soap-free emulsion containing fluorine is capable of improving water resistance and oil resistance of paper or leather significantly.

Description

(1) Technical field [0001] The invention relates to a preparation technology of a cationic soap-free fluorine-containing waterproof and oil-repellent agent, in particular to a preparation method of a fluorine-containing polyacrylate soap-free emulsion, which belongs to the technical field of light industry. (2) Background technology [0002] Since the C-F bond of the fluoroalkyl side chain has large bond energy and strong polarity, and is oriented outward during the film formation process, it has a strong shielding and protecting effect on the C-C main chain. Therefore, fluoropolyacrylate has excellent hydrophobic and oleophobic properties, thermal stability and chemical corrosion resistance. In recent years, fluorinated polyacrylates have been widely used in the fields of leather, papermaking, textiles, protection of ancient buildings and controlled drug release. [0003] Emulsion polymerization is a commonly used method for preparing fluoroacrylate emulsions. For example...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F265/04C08F265/06C08F271/00C08F220/22C08F220/14C08F220/18C08F226/02C08F212/08D21H19/20C09D151/00D06M15/21C14C11/00
Inventor 靳丽强魏延伟徐清华王玉路
Owner QILU UNIV OF TECH
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