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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 friction coefficient (>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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In the 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel, gas filling catheter, add the mixture of perfluoroalkyl iodide wherein 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 benzoyl peroxide initiator, heat to 70°C, start dropping styrene and maintain the reaction temperature at 70-85°C during the dropwise addition of styrene, stop adding styrene dropwise to 70g, and continue the reaction for 4h , move the obtained product into a 2000ml flask, add 800g of isopropanol, 300g of acetic acid, and 65g of zinc powder, stir evenly and then raise the temperature to 90°C for 3 hours of reaction. It has an aromatic smell, the coefficient of friction of skis treated with this fluorine grease is 0.06, it does not freeze at -36°C, does not decompose at 390°C, the water repellency angle is 113°, and the oil repellency can reach the first grade. It is a kind of fluorine ...

Embodiment 2

[0013] Add perfluorooctyl iodide F(CF2)8I 330g in the 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel, gas filling conduit, add initiator benzoyl peroxide 5g, heat to 80°C, add 5g of limonene, start to add styrene dropwise, maintain the reaction temperature at 80-95°C during the dropping process, stop the dropwise addition of styrene when it reaches 65g, continue the reaction for 4h, transfer the obtained product to a 2000ml flask, add 900g Isopropanol, 300g acetic acid, 68g zinc powder, stir evenly, heat up to 90°C and react for 5 hours, the obtained product is filtered, washed with water, dehydrated and separated to obtain the product fluorogrease, which has excellent low temperature resistance and wear resistance after wiping test . This product has lemon-smelling fluorine grease. The friction coefficient of skis treated with this hydrofluoride grease is 0.08. It does not freeze at -40°C and does not decompose at 3...

Embodiment 3

[0015] Add perfluorohexyl iodide F(CF2)6I 404g in the 500ml flask equipped with stirring, electric heating mantle, thermometer, reflux condenser, dropping funnel, gas filling conduit, add initiator benzoyl peroxide 8g, heat to 60 ℃, start to add octene dropwise, maintain the reaction temperature at 60-75°C during the dropwise addition, stop the dropwise addition of octene until 110g, continue the reaction for 3h, move the obtained product to a 2000ml flask, add 1000g isopropanol, 300g Acetic acid, 70g of zinc powder, stir evenly, heat up to 60°C and react for 4 hours, the obtained product is filtered, washed with water, dehydrated and separated to obtain the product fluorogrease. It does not decompose at ℃, the water repellency angle is 110°, and the oil repellency can reach the first grade. 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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