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Preparation method of perfluorohexyl propyl acrylate and application of the perfluorohexyl propyl acrylate in fabric waterproof and oil-proof agent

A technology of fluorohexylpropyl acrylate and perfluoroalkylethylene, which is applied in the field of fluorine-containing acrylate preparation, can solve the problems of long reaction time, unfavorable long-term large-scale industrial production, high requirements for reaction conditions, etc., and achieve good water and oil resistance Effect, strong emulsification system, 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

However, the reaction conditions are relatively high, and the long reaction time is not conducive to long-term large-scale industrial production

Method used

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  • Preparation method of perfluorohexyl propyl acrylate and application of the perfluorohexyl propyl acrylate in fabric waterproof and oil-proof agent
  • Preparation method of perfluorohexyl propyl acrylate and application of the perfluorohexyl propyl acrylate in fabric waterproof and oil-proof agent
  • Preparation method of perfluorohexyl propyl acrylate and application of the perfluorohexyl propyl acrylate in fabric waterproof and oil-proof agent

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preparation example Construction

[0021] First, the invention provides a kind of preparation method of perfluorohexyl propyl acrylate, comprising the steps:

[0022] S1 Perfluoroalkylethylene and methanol undergo free radical addition reaction under the triggering action of organic peroxide. The molar ratios of perfluoroalkylethylene to methanol and organic peroxide are 1:20 and 1:0.02, respectively. The reaction pressure is 1.0-2MPa, the temperature is 80°C, and the time is 3h; after the reaction, the first vacuum distillation purification is carried out to obtain perfluoroalkyl ethyl propanol;

[0023] S2 Dissolve the perfluoroalkyl ethyl propanol in S1 in tert-butanol, and carry out esterification reaction with excess acrylic acid under the action of a catalyst. The reaction temperature is 70-100°C, and the reaction time is 2-8h. After the reaction, the tert-butanol was recovered, and then purified by the second vacuum distillation to obtain perfluorohexylpropyl acrylate.

[0024] In the present invention,...

Embodiment 1

[0043] S1 Add 692g of perfluorohexylethylene (2mol), 1280g of methanol (40mol) and 4.72g of acetyl peroxide (0.04mol) 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 80°C, react for 3 hours under a pressure of 1.2-2MPa, cool to room temperature and discharge to obtain the crude product of perfluorohexylpropanol. Under the system pressure of -0.1MPa~-0.096MPa and temperature of 80~180°C, the crude product was purified by vacuum distillation to obtain 706g of colorless and transparent perfluorohexylpropanol, the purity of which was detected by gas chromatography was 96.10%. The rate is 89.74%.

[0044] S2 Add 779g of purified perfluorohexylpropanol (2mol) and 2L of tert-butanol to a glass reactor with a capacity of 5L and stir for 2min, then add 288g of...

Embodiment 2

[0046]S1 Add 692g of perfluorohexylethylene (2mol), 1280g of methanol (40mol) and 4.72g of acetyl peroxide (0.04mol) 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 80°C, react for 3 hours under a pressure of 1.2-2MPa, cool to room temperature and discharge to obtain the crude product of perfluorohexylpropanol. Under the system pressure of -0.1MPa~-0.096MPa and temperature of 80~180°C, the crude product was purified by vacuum distillation to obtain 706g of colorless and transparent perfluorohexylpropanol, the purity of which was detected by gas chromatography was 96.10%. The rate is 89.74%.

[0047] S2 Add 779g of purified perfluorohexylpropanol (2mol) and 2L of tert-butanol to a glass reactor with a capacity of 5L and stir for 2min, then add 288g of ...

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Abstract

The invention relates to the technical field of preparation of fluorine-containing acrylate, and discloses a preparation method of perfluorohexyl propyl acrylate, which comprises the following steps: perfluoroalkyl ethylene and methanol are subjected to free radical addition reaction under the initiation action of organic peroxide; after the reaction, performing first reduced pressure distillation purification to obtain perfluoroalkyl ethyl propanol; then dissolving perfluoroalkyl ethyl propanol in tert-butyl alcohol, carrying out esterification reaction with excessive acrylic acid under the action of a catalyst, recovering the tert-butyl alcohol after the esterification reaction is finished, and carrying out second vacuum distillation purification to obtain the perfluorohexyl propyl acrylate. According to the preparation method, perfluorohexyl ethylene is taken as a raw material, perfluorohexyl propyl acrylate is prepared through a two-step method, the requirement for reaction conditions is lower, safety and environment friendliness are achieved, and the production cost can be saved. The waterproof and oil-proof agent can be directly used for preparing waterproof, oil-proof and antifouling finishing agents for fabrics and anti-corrosion agents for large-scale integrated circuits and the like, wherein the effects are obviously superior to that of a traditional waterproof and oil-proof additive.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing acrylates, and in particular relates to a preparation method of perfluorohexylpropyl acrylate and the application of perfluorohexylpropyl acrylate in fabric waterproof and oil-repellent agents. Background technique [0002] The fluorine-containing acrylate produced by the esterification reaction of polyfluoroalcohol and acrylic acid is an important comonomer for preparing fabric waterproof, oil-proof and anti-fouling finishing agents. This unsaturated ester polymer can also be used as a resist for large-scale integrated circuits, as well as outer sheath materials for plastics and optical fibers. [0003] At present, the method for preparing perfluoroalkyl acrylates in industry mainly includes the reaction of perfluoroalkyl ethyl iodide and acrylic acid metal salts to generate corresponding perfluoroalkyl ethyl acrylates, such as U.S. Patent No. 06660803B1. The alkyl iod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/44C07C31/38D06M15/295D06M101/32D06M101/34
CPCC07C29/44C07C67/08D06M15/295D06M2101/32D06M2101/34D06M2200/11D06M2200/12C07C69/54C07C31/38
Inventor 孙道德何喜春
Owner 四川上氟科技有限公司
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