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Flexible reaction device and method for trifluoroethanol/trifluoroethyl methacrylate

A technology of trifluoroethyl methacrylate and trifluoroethanol, which is applied in the field of fluorine-containing fine chemicals, can solve problems such as unsatisfactory reaction rate and product yield, reduced income, and difficult separation, and achieve production capacity The effect of high utilization rate, stable product quality and simple process

Active Publication Date: 2020-07-28
新元化学(山东)股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

US2868846 uses water and dihydric alcohol as solvents to synthesize trifluoroethanol by reacting alkali metal acetate with R-133a at 225-300°C, 3.4-18MPa and pH 4-7; US4590310 at 223°C and 9MPa Under certain conditions, trifluoroethanol is synthesized by reacting an aqueous solution of R-133a and metal acetate, wherein the metal acetate is prepared by metal hydroxide, water and acetic acid. The problem of the above two methods is that the metal chloride in the reaction product It is difficult to separate from excess unreacted metal acetate or alkali metal salt catalyst, which will easily cause waste of raw materials and reduce revenue
Moreover, the stirring form and stirring equipment of the reaction mostly adopt traditional stirring reactors, which makes the reaction rate and product yield not very satisfactory.
In the prior art, there is a lack of a flexible device that can produce both trifluoroethanol and trifluoroethyl methacrylate. At the same time, there is a lack of equipment for optimizing the reaction form of material mixing to increase the reaction rate and product yield. and product quality, for this reason, propose the present invention

Method used

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  • Flexible reaction device and method for trifluoroethanol/trifluoroethyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Such as figure 1 As shown, a flexible reaction device of trifluoroethanol / trifluoroethyl methacrylate, the device includes R-133a metering tank 1, R-133a metering pump 2, raw material mixing kettle 3, raw material feeding pump 4, Venturi Injector 5, reactor 6, reaction circulation pump 7, filter 14, distillation kettle 15, distillation condenser 16, receiving tank 17, tail gas condenser 18, bottom feeding pump 19;

[0050] The Venturi injector 5 is arranged on the upper end of the reactor 6, and the suction port of the Venturi injector 5 is communicated with the side top of the reactor 6 by an air duct; the R-133a metering tank 1 is passed through the R-133a metering pump 2 It is connected with the feed port of the reactor 6, the raw material mixing tank 3 is connected with the feed port of the reactor 6 through the raw material feeding pump 4, and the feed port at the lower end of the reactor 6 passes through the inlet of the reaction circulation pump 7 and the Venturi...

Embodiment 2

[0055] A flexible reaction device of trifluoroethanol / trifluoroethyl methacrylate as described in Example 1, the difference is: the medium of the tail gas condenser 18 provided at the upper end of the receiving tank 17 is -35°C to -30°C °C frozen brine. The outer side of the raw material mixing kettle 3 is provided with a heating or cooling jacket, and the raw material mixing kettle 3 is provided with a stirring device. A heating or cooling jacket is provided on the outside of the still 15, and a stirring device is provided on the still 15.

Embodiment 3

[0057] Utilize the method for producing trifluoroethanol by the production device described in embodiment 1 or 2, comprise steps as follows:

[0058] (1) first open the second valve 9 and the third valve 10 on the filter, close the first valve 8, the fourth valve 11, the fifth valve 12, the sixth valve 13, through the raw material mixing kettle 3, to the reactor 6 and Squeeze metered N-methylpyrrolidone solvent into the filter 14, then close the second valve 9 and the third valve 10, open the first valve 8, start the reaction circulation pump 7 to circulate, and form the injection reaction loop; 48wt%KOH After the aqueous solution and N-methylpyrrolidone solvent are mixed in the raw material mixing tank 3, they are pumped into the reactor 6 by the raw material feeding pump 4, and then the R-133a is injected into the R-133a metering tank 1 through the R-133a metering pump 2 Reactor 6; the molar ratio of KOH to N-methylpyrrolidone is 1:5~6, and the molar ratio of R-133a to KOH i...

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Abstract

The invention relates to a flexible reaction device and method for trifluoroethanol / trifluoroethyl methacrylate. The device comprises an R-133a metering tank, an R-133a metering pump, a raw material mixing kettle, a raw material ramming pump, a venturi ejector, a reactor, a reaction circulating pump, a filter, a distillation kettle, a distillation condenser, a receiving tank, a tail gas condenser,a kettle bottom ramming pump and the like. The venturi ejector is arranged at the upper end of the reactor, and a suction inlet of the venturi ejector is communicated with the side top of the reactorthrough a gas guide pipe to form a venturi ejection reactor and an ejection loop reaction system is formed. Flexible switching production can be achieved through the production device with the specific structure and connection relation, and the device has the advantages of being simple in process, high in reaction rate, high in product yield, stable in product quality, dual-purpose, higher in capacity utilization rate, lower in comprehensive cost and suitable for flexible industrial production of trifluoroethanol / trifluoroethyl methacrylate.

Description

technical field [0001] The invention belongs to the field of fluorine-containing fine chemicals, in particular to a flexible reaction device and method of trifluoroethanol / trifluoroethyl methacrylate. Background technique [0002] Trifluoroethanol is an important aliphatic fluorine-containing fine chemical, which is widely used in the fields of fluorine-containing medicines, pesticide synthesis, advanced solvents, dyes and energy. Its structure is: [0003] CF 3 CH 2 Oh [0004] There are many synthetic methods of trifluoroethanol, including trifluorochloroethane (R-133a) hydrolysis method, trifluoroethane oxidation method, trifluoroacetic acid (derivative) reduction method, trifluoroacetaldehyde (derivative) reduction method , Vinylidene fluoride oxidation and other processes. Among them, the R-133a hydrolysis method has the advantages of low raw material cost, safety and reliability. US2868846 uses water and dihydric alcohol as solvents to synthesize trifluoroethanol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C31/38C07C67/08C07C69/54C01D3/04C01D3/14B01J19/26C07C29/76C07C67/48
CPCC07C29/124C07C67/08C01D3/04C01D3/14B01J19/26C07C29/76C07C67/48C07C31/38C07C69/54
Inventor 解乐福邵军强杜辉田志钢孙程刘晓敏赵伟洁
Owner 新元化学(山东)股份有限公司
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