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Method for preparing fluorine-silicon containing polyurethane and acrylate emulsion

A technology of acrylate and polyurethane, applied in the field of preparation of water-based polyurethane, can solve the problems of poor hydrolysis resistance, poor pollution resistance, etc., and achieve the effects of low surface energy, good hydrophobicity, and simple preparation method

Active Publication Date: 2012-05-02
JIAXING HEXIN CHEM IND
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0003] The present invention aims to propose a preparation method of fluorine-containing silicon polyurethane-acrylate emulsion, so that the prepared water-based polyurethane resin can overcome the shortcomings of ordinary water-based polyurethane resin such as poor hydrolysis resistance and poor pollution resistance.

Method used

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  • Method for preparing fluorine-silicon containing polyurethane and acrylate emulsion
  • Method for preparing fluorine-silicon containing polyurethane and acrylate emulsion
  • Method for preparing fluorine-silicon containing polyurethane and acrylate emulsion

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preparation example Construction

[0013] The preparation method of this fluorine-containing silicon polyurethane-acrylate emulsion comprises the following steps:

[0014] (1) Under the protection of nitrogen, add acid fluoride dropwise to the ether solution of trimethylolpropane, reflux for 6 to 8 hours, wash with water, and distill under reduced pressure to remove residual water and unreacted raw materials to obtain fluorine-containing bismuth Alcohol; its reaction formula is as follows:

[0015]

[0016] where Rf is -C 7 f 15 、-C 2 f 5 or -CF(CF 3 ) (OCF 2 CF(CF 3 )) m OCF 2 CF 2 CF 3 , m is an integer of 0-3.

[0017] (2) Use a three-necked flask device with a reflux condenser and a constant pressure funnel, add the toluene solution of hydrogen-containing silicone oil to the constant pressure funnel, add fluorine-containing acrylate, dienyl acrylate and anhydrous Ethanol (absolute ethanol only acts as a cocatalyst), stir and mix evenly, control the temperature at 60-100°C, add Pt catalyst, sl...

Embodiment 1

[0034] 1) Preparation of fluorine-containing diols

[0035]Add 26.8g of trimethylolpropane and 50ml of anhydrous ether to a three-necked flask equipped with a reflux condenser and a constant pressure funnel, and add 89.5g of perfluoro 2,5-dimethyl-3,6 - Dioxononanoyl fluoride, reflux reaction for 6 hours, washed with water, and distilled off under reduced pressure to remove residual water and unreacted raw materials to obtain 102.5 g of fluorine-containing dihydric alcohol. Wherein, the molar ratio of trimethylolpropane to perfluoro 2,5-dimethyl-3,6-dioxononanoyl fluoride is 0.9.

[0036] 2) Preparation of fluorine-containing silicone oil

[0037] In a three-necked flask equipped with a reflux condenser and a constant pressure funnel (pumping and baking 3 times), add 20ml of a toluene solution of 18.5g of hydrogen-containing silicone oil to the constant pressure funnel; add 4.5g of methacrylic acid deca Difluoroheptyl ester, 1.2 g of dipropylene glycol diacrylate and 2 g of ...

Embodiment 2

[0047] 1) Preparation of fluorine-containing diols

[0048] Add 26.8g of trimethylolpropane and 50ml of anhydrous ether to a three-necked flask equipped with a reflux condenser and a constant pressure funnel, and add 89.5g of perfluoro 2,5-dimethyl-3,6 - Dioxononanoyl fluoride, reflux reaction for 6 hours, washed with water, and distilled off under reduced pressure to remove residual water and unreacted raw materials to obtain 102.5 g of fluorine-containing dihydric alcohol. Wherein, the molar ratio of trimethylolpropane to perfluoro 2,5-dimethyl-3,6-dioxononanoyl fluoride is 0.9.

[0049] 2) Preparation of fluorine-containing silicone oil

[0050] In a three-necked flask equipped with a reflux condenser and a constant pressure funnel (pumping and baking 3 times), add 20ml of a toluene solution of 18.5 hydrogen-containing silicone oil to the constant pressure funnel; add 4.5g of hexafluoromethacrylate to the three-necked flask Butyl ester, 3.2g dipropylene glycol diacrylate ...

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Abstract

The invention relates to a method for preparing fluorine-silicon containing polyurethane and acrylate emulsion, which comprises the following steps of: preparing fluorine-silicon containing oil from hydrogen-silicon containing oil, fluorine containing acrylate, divinyl acrylate and absolute ethyl alcohol; and carrying out chain extension reaction of a pre-polymer obtained by reacting isocyanate, polyether glycol and polyester glycol, fluorine containing glycol, chain extension agent and hydrophilic chain extension agent, dispersing and emulsifying by adding water, decompressing, distilling and removing an organic solvent to obtain aqueous polyurethane emulsion, then adding acrylate and the fluorine-silicon containing oil to disperse at high speed, adding catalyst, increasing the temperature and polymerizing to obtain the fluorine-silicon containing polyurethane and acrylate emulsion. The fluorine-silicon containing polyurethane and acrylate emulsion prepared by using the method disclosed by the invention has the advantages of being better in integral performance, low in surface energy, better hydrophobic performance, high in solid content, controllable in solid content, simple andconvenient in preparation method, flexible and the like.

Description

technical field [0001] The invention relates to a preparation method of water-based polyurethane and a preparation method of fluorine-containing silicon polyurethane-acrylate emulsion. Background technique [0002] Polyurethane is the abbreviation of polyurethane, which means that the main chain of the macromolecule contains repeated urethane units. In addition to containing a large number of urethane bonds, it may also contain ester bonds, ether bonds, urea bonds, and allophanic acid. Ester bonds, isocyanurate bonds, hydrogen bonds between macromolecules, etc. Polyurethane is a block polymer composed of flexible soft segments composed of polyester or polyether and rigid hard segments such as carbamate and urea groups alternately connected; due to the thermodynamic incompatibility of soft and hard segments, soft Segment and hard segment aggregate in the polymer respectively to form soft segment phase and hard segment phase, and microphase separation occurs. Due to the uniq...

Claims

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Application Information

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IPC IPC(8): C08F283/00C08G18/66C08G18/48C08G18/42C08G18/12C08G18/32C08G18/61C08G77/385C09D151/08
Inventor 郦聪纪尚超徐欣欣石磊沈连根朱崇恩李寿伟
Owner JIAXING HEXIN CHEM IND
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