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Preparation method of perfluoroalkyl ethanol

A technology of perfluoroalkylethanol and perfluoroalkylethylene, which is applied in the field of preparation of perfluoroalkylethanol, can solve the problems of harsh conditions, complicated process and high cost, and achieve simple operation, readily available raw materials and low cost Effect

Pending Publication Date: 2021-06-04
四川上氟科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the current preparation process of perfluoroalkyl alcohol, there are problems of high cost, complex process and harsh conditions

Method used

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  • Preparation method of perfluoroalkyl ethanol
  • Preparation method of perfluoroalkyl ethanol

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[0018] The invention provides a kind of preparation method of perfluoroalkyl alcohol, comprising the steps of:

[0019] S1 Perfluoroalkylethylene and methanol undergo electrophilic addition reaction under the catalysis of inorganic acid. The molar ratios of perfluoroalkylethylene to methanol and inorganic acid are 1:10-40 and 1:1-6, respectively. The reaction pressure is 1-1.5MPa, the temperature is 40-100°C, and the time is 1h-6h; after the reaction, carry out vacuum distillation and purification to obtain perfluoroalkyl ethyl methyl ether;

[0020] S2 blends the perfluoroalkyl ethyl methyl ether in S1 with hydroiodic acid, reacts at 20-120°C for 2-8 hours, distills off the by-products after the reaction is completed, and then purifies it by vacuum distillation to obtain perfluoroalkyl ether Alkylethanol.

[0021] In the present invention, the preparation reaction equation of perfluoroalkyl alcohol is:

[0022]

[0023] Among them, R f It refers to a straight-chain perf...

Embodiment 1

[0033] S1 Add 692g of perfluorohexylethylene (2mol), 1280g of methanol (40mol) and 1000mL (3mol / L) of hydrochloric acid solution into a high-pressure stainless steel reactor with a capacity of 5L, and seal the reactor. The high-pressure stainless steel reactor is equipped with electric stirrer, thermocouple, cooling coil and shaft seal cooling water. Start the stirring process, raise the temperature to 60°C, react at a pressure of 1-1.5 MPa for 3 hours, cool to room temperature and discharge to obtain the crude product of perfluorohexyl ethyl methyl ether. Under the system pressure of -0.1MPa~-0.096MPa and temperature of 80~180℃, the crude product was purified by vacuum distillation to obtain 673g of colorless and transparent perfluorohexyl ethyl methyl ether, the purity of which was detected by gas chromatography was 96.5 %, the yield is 85.9%.

[0034] S2 is the hydriodic acid solution that adds 1960g purified perfluorohexyl ethyl methyl ether (5mol) and 1000mL (5mol / L) to ...

Embodiment 2

[0036] S1 Add 692g of perfluorohexylethylene (2mol), 1600g of methanol (50mol) and 1000mL (3mol / L) of hydrochloric acid solution into a high-pressure stainless steel reactor with a capacity of 5L, and seal the reactor. The high-pressure stainless steel reactor is equipped with electric stirrer, thermocouple, cooling coil and shaft seal cooling water. Start the stirring process, raise the temperature to 60°C, react at a pressure of 1-1.5 MPa for 3 hours, cool to room temperature and discharge to obtain the crude product of perfluorohexyl ethyl methyl ether. Under the system pressure of -0.1MPa~-0.096MPa and temperature of 80~180℃, the crude product was purified by vacuum distillation to obtain 686g of colorless and transparent perfluorohexyl ethyl methyl ether, the purity of which was detected by gas chromatography was 97.2 %, the yield is 88.2%.

[0037] S2 is the hydriodic acid solution of 1960g purified perfluorohexyl ethyl methyl ether (5mol) and 1200mL (5mol / L) in the 5L ...

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Abstract

The present invention relates to the technical field of fluorine-containing alcohol preparation, and discloses a perfluoroalkyl ethanol preparation method, which comprises: S1, carrying out an electrophilic addition reaction on perfluoroalkyl ethylene and methanol under the catalytic effect of an inorganic acid, with the molar ratio of perfluoroalkyl ethylene to methanol to inorganic acid being 1:10-40 and 1:1-6, the reaction pressure being 1-1.5 MPa, the temperature being 40-100 DEG C, and the time being 1-6 h; after the reaction, carrying out reduced pressure distillation and purification to obtain perfluoroalkyl ethyl methyl ether; S2, blending the perfluoroalkyl ethyl methyl ether in the S1 with hydroiodic acid, reacting at 20-120 DEG C for 2-8 hours, distilling the reaction product to remove byproducts after reaction is finished, and performing reduced pressure distillation and purification to obtain the perfluoroalkyl ethanol. The preparation method can reduce the production cost, digest production waste, and is safe, environment-friendly and simple to operate.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing alcohols, and in particular relates to a preparation method of perfluoroalkyl alcohols. Background technique [0002] Perfluoroalkylethanol is an important class of aliphatic fluorine-containing compounds. It is an important intermediate for the preparation of advanced antifouling coatings such as fluorine-containing surfactants, fluorine-containing fabric treatment agents, and water and oil repellent agents. At the same time, it also has excellent and unique properties such as high surface activity, high chemical stability, and both water and oil repellency, so it is widely used in the fields of textile dyes, pharmaceutical synthesis, and chemical anticorrosion. [0003] At present, the industrial preparation methods of perfluoroalkylethanol mainly include the direct hydrolysis reaction of perfluoroalkylethyl iodide and the indirect hydrolysis reaction of perfluoroalkyl...

Claims

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Application Information

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IPC IPC(8): C07C29/10C07C31/38C07C41/06C07C43/12
CPCC07C41/06C07C29/10C07C43/12C07C31/38
Inventor 孙道德何喜春
Owner 四川上氟科技有限公司
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