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Method for synthesizing perfluoroalkyl propanol

A technology of perfluoroalkyl propanol and synthesis method, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem that perfluoroalkyl iodide is expensive, unfavorable for industrial production, and high production cost problem, to achieve the effect of low cost, excellent performance and cost saving

Inactive Publication Date: 2012-08-15
锦州恒通氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some problems in this method: 1) The raw material perfluoroalkyl iodide is expensive, and allyl alcohol is a strong irritant and toxic substance
2) The hydrogenation reaction requires the use of noble metal catalysts, resulting in high production costs
3) There are many steps and complicated operation, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 615g of perfluorobutylethylene (2.5mol), 1600g of methanol (50mol) and 6g of benzoyl peroxide into a 5L high-pressure stainless steel reactor with electric stirrer, thermocouple, cooling coil, and shaft seal cooling water (0.025mol). The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, raise the temperature to 90°C-100°C, react for 1 hour under a pressure of 1.2MPa-1.4MPa, cool to room temperature and discharge to obtain a crude product. Under the system pressure of -0.097MPa~-0.095MPa and temperature of 80℃~85℃, the crude product was purified by vacuum distillation to obtain 685g (2.464mol) of colorless and transparent liquid perfluorobutylpropanol, which was detected by gas chromatography The purity is 99.5%, and the yield is 98.1%.

Embodiment 2

[0020] Add 865g of perfluorohexylethylene (2.5mol), 2400g (75mol) of methanol and 7.4g of tertiary peroxybenzoic acid to a 5L high-pressure stainless steel reactor with electric stirrer, thermocouple, cooling coil, and shaft seal cooling water. Butyl ester (0.038 mol). The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, raise the temperature to 120°C-130°C, react for 2 hours under a pressure of 1.4MPa-1.6MPa, cool to room temperature and discharge to obtain a crude product. Under the system pressure of -0.099MPa~-0.098MPa and the temperature of 95℃~100℃, the crude product was purified by vacuum distillation to obtain 925g of colorless and transparent liquid perfluorohexylpropanol, the purity of which was 99.3% by gas chromatography. The yield was 97.2%.

Embodiment 3

[0022] Add 1615g of perfluorodecylethylene (2.5mol), 3200g (100mol) of methanol and 4.5g of tert-butylperoxide into a 5L high-pressure stainless steel reactor equipped with electric stirrer, thermocouple, cooling coil, and shaft seal cooling water. Hydrogen oxide (0.05 mol). The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, raise the temperature to 180°C-190°C, react for 3 hours under a pressure of 1.8-2.0MPa, cool to room temperature and discharge to obtain a crude product. Under the system pressure of -0.1MPa~-0.099MPa and temperature of 125℃~130℃, the crude product was purified by vacuum distillation to obtain 1635g of white solid perfluorodecylpropanol, the purity of which was detected by gas chromatography was 99.1%. The rate is 95.6%.

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Abstract

The invention relates to a method for synthesizing perfluoroalkyl propanol. The method comprises the following steps: carrying out free radical addition reaction on perfluoroalkyl ethylene and methyl alcohol in the presence of organic peroxide initiator, wherein the molar ratios of perfluoroalkyl ethylene to methyl alcohol and perfluoroalkyl ethylene to the organic peroxide are respectively 1:20-1:40 and 1:0.01-1:0.02, the pressure is 1.2MPa-2.0MPa, the temperature is 90-190 DEG C and the time is 1-3h; and after reacting, purifying through reduced-pressure distillation to obtain perfluoroalkyl propanol. The method has the advantages of easily-obtained materials, low cost, safety and environmental friendliness; methyl alcohol is used as the reactant and solvent, is low in cost and can be recycled; the operation process is simple, safe and stable without generating by-products, the purity of the finished product is 99.1-99.5% and the yield is 95.6-98.1%; and perfluoroalkyl propanol has excellent performance, has the water and oil resistance, corrosion resistance and weather resistance similar to perfluoroalkyl ethanol, and is a good substitute for perfluoroalkyl ethanol.

Description

technical field [0001] The invention belongs to the field of fluorine-containing compounds and derivatives thereof, in particular to a method for synthesizing perfluoroalkyl propanol. Background technique [0002] Perfluoroalkyl propanol (general formula R f CH 2 CH 2 CH 2 OH, where R f It is a straight-chain perfluoroalkyl group with a carbon number of 4~n), which has the characteristics of water resistance, oil resistance, corrosion resistance, and weather resistance similar to perfluoroalkyl alcohols. Active agents, fluorine-containing fabric treatment agents, and important intermediates of advanced antifouling materials such as fluorine-containing coatings, are good substitutes for perfluoroalkyl alcohols with complex preparation processes. [0003] At present, perfluoroalkyl propanol is prepared by reacting perfluoroalkyl iodide with allyl alcohol through multi-step reactions of addition, elimination and hydrogenation. There are some problems in this method: 1) T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C29/44
Inventor 杨华杰魏奇谷峰
Owner 锦州恒通氟化学有限公司
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