Preparation method of fluorine resin

A perfluoroalkyl iodide and product technology, applied in the field of fluorocarbon preparation, can solve the problems of low friction coefficient, low molecular weight, poor stain resistance, etc., and achieve low friction coefficient, high selectivity, and no by-products Effect

Active Publication Date: 2011-08-17
JINZHOU DPF TH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002]Existing fluorine grease is mostly used in deep-sea drilling, mining of combustible ice, aerospace technology and other fields. Due to its small carbon-hydrogen bond energy and low molecular weight, its Short service time, poor high and low temperature resistance, unusable due to freezing below -30°C, poor stain resistance, large f

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0010] Example 1

[0011] Add the mixture of perfluoroalkyl iodide into a 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel, and gas-filled tube, where F(CF 2 )12I 315g, F(CF 2 )14I 90g, F(CF 2 )16I 31.5g, F(CF 2 )18I 9g, F(CF 2 ) 20I 4.5g, add 3g of the initiator benzoyl peroxide, heat to 70°C, start to add styrene dropwise while maintaining the reaction temperature at 70-85°C, add dropwise styrene to 70g, stop dropping, continue the reaction for 4h , Move the obtained product to a 2000ml flask, add 800g isopropanol, 300g acetic acid, 65g zinc powder, stir evenly, and then heat to 90°C for 3 hours. The obtained product is filtered, washed with water, and dehydrated to obtain fluorine grease. It has a fragrant odor. The friction coefficient of the skis treated with the fluorine grease is 0.06, -36℃ does not freeze, 390℃ does not decompose, the water repellent angle is 113°, and the oil repellency can reach one level. It is ...

Example Embodiment

[0012] Example 2

[0013] Add 330g of perfluorooctyl iodide F(CF2)8I to a 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel, and gas-filled tube, add 5g of initiator benzoyl peroxide, and heat to At 80°C, add 5g of limonene, start to add styrene and maintain the reaction temperature at 80-95°C during the dropwise addition. When styrene is added dropwise to 65g, stop the dripping, continue the reaction for 4h, transfer the obtained product to a 2000ml flask, and add 900g Isopropanol, 300g acetic acid, 68g zinc powder, stir evenly, and then heated to 90℃ to react for 5h. The product obtained is filtered, washed with water, dehydrated and separated to obtain the product fluorine grease. The fluorine grease has excellent low temperature resistance and abrasion resistance after wiping test . The product has a lemon-scented fluorine grease. The friction coefficient of skis treated with this hydrofluoride grease is 0.08, does n...

Example Embodiment

[0014] Example 3

[0015] Add 404g of perfluorohexyl iodide F(CF2)6I to a 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel and gas-filled tube, add 8g of initiator benzoyl peroxide, and heat to 60 ℃, start to add octene while maintaining the reaction temperature at 60-75℃, octene is dripped to 110g, stop dripping, continue the reaction for 3h, move the obtained product to a 2000ml flask, add 1000g isopropanol, 300g Acetic acid, 70g zinc powder, stir evenly, heat up to 60℃ and react for 4h. The product obtained is filtered, washed with water, dehydrated and separated to obtain the product fluorine grease. The friction coefficient of skis treated with this fluorine grease is 0.1, -35℃ does not freeze, 380 It does not decompose at ℃, the water repellency angle is 110°, and the oil repellency can reach one level. It is a kind of fluorine grease with excellent performance.

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PUM

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Abstract

The invention discloses a preparation method of fluorine resin, comprising the following steps of: mixing 33-62 parts by weight of perfluoroalkyl iodide and 0.3-0.8 parts by weight of initiator, and then heating to 60-100 DEG C, wherein the initiator is benzoyl peroxide or azobisisobutyronitrile; dropping 7-14 parts by weight of olefin, wherein the olefin is one or two of styrene, octylene, pinene and limonene; reacting at 60-100 DEG C for 3-5 hours; then adding 75-100 parts by weight of solvent, 28-33 parts by weight of acetic acid and 65-70 parts by weight of zinc powder, wherein the solvent is isopropanol or xylene; reacting at 60-100 DEG C for 3-5 hours to obtain a product; and filtering, water-washing, dehydrating and separating the product to obtain a target product. A continuous adding manner is adopted in the method, the reaction is easy to control, no byproduct is generated, the obtained product is easy to separate, and has high selectivity, low frictional factor (0.05-0.1), a water repellence angle of over 110 DEG and high oil repellency up to the first grade, does not freeze at 35 DEG C below zero, and does not decompose at 350 DEG C; and the fluorine resin can be used in the fields such as deep-sea drilling, ignitable ice exploiting, astronautical technology, equipment lubrication under the working condition of permanent freezing layers, and the like.

Description

technical field [0001] The invention relates to a preparation method of fluorocarbons, in particular to a preparation method of fluorogrease. Background technique [0002] The existing fluorine grease is mostly used in deep sea drilling, mining of combustible ice, aerospace technology and other fields. Due to its small carbon-hydrogen bond energy and low molecular weight, it has a short service life and poor high and low temperature resistance. Unusable due to freezing, poor stain resistance, high coefficient of friction (>0.1). With the development of science and technology in recent years, the lubrication of equipment under the condition of permafrost needs to have lubricating performance at -35°C to 350°C and a low friction coefficient (0.05-0.1), which cannot be met by the existing lubricating grease made of fluorine grease. Require. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of...

Claims

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Application Information

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IPC IPC(8): C10M169/00C10M177/00C08F112/08C08F110/14C08F132/08C10N50/10
Inventor 魏奇孙百开魏潇
Owner JINZHOU DPF TH CHEM CO LTD
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