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Method for preparing 1-alkoxy-1,1,2,2-tetrafluoroethane

A technology of tetrafluoroethane and alkoxy, which is applied in the field of preparation of fluorine-containing ether compounds, can solve problems such as difficult separation of products and catalysts, difficulty in catalyst recovery, environmental pollution, etc., and achieves excellent low-temperature reaction activity and comprehensive alkalinity Strengthen and reduce the effect of pollution

Active Publication Date: 2015-06-03
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The catalysts used in the above patents and literature technologies are mainly alkali metal compounds, which have disadvantages such as difficulty in catalyst recovery, high slag content, and difficulty in separating the product from the catalyst due to fine solid particles. At the same time, it is easy to cause environmental pollution due to the use of a large amount of solvents.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]A preparation method of 1-methoxy-1,1,2,2-tetrafluoroethane, comprising the following steps:

[0033] Step 1: Add 100Kg of sodium methoxide and [bmim]BF to a 300L reactor 4 10Kg of ionic liquid, stirred for 2h, then added 80Kg of fluorine-intercalated hydrotalcite (LDH-F, the mass percentages of Ni, Mg, F and Al were 23%, 16%, 3% and 58%), at 120 Reaction at ℃ for 8 hours, after the reaction, the basic compound supported by fluorine intercalation hydrotalcite and [bmim]BF 4 Composite catalysts for ionic liquids.

[0034] Step 2: Add 100Kg of methanol and 30Kg of the composite catalyst prepared in the above step (1) into a 500L stainless steel autoclave, close the feeding port, replace the air in the autoclave with nitrogen, and then introduce tetrafluoroethylene monomer, heat up to start the reaction , the reaction temperature is controlled at 40°C, and the tetrafluoroethylene is metered into the reactor. When 300Kg of tetrafluoroethylene monomer is introduced, the rea...

Embodiment 2

[0036] A preparation method of 1-methoxy-1,1,2,2-tetrafluoroethane, comprising the following steps:

[0037] Step 1: Add 100Kg of sodium methoxide and [bmim]BF to a 300L reactor 4 10Kg of ionic liquid, stirred for 2 hours, then added 40Kg of fluorine intercalated hydrotalcite (LDH-F, the mass percentages of Ni, Mg, F and Al were 30%, 15%, 1% and 54% respectively), at 200 Reaction at ℃ for 5 hours, after the reaction, the basic compound supported by fluorine intercalation hydrotalcite and [bmim]BF 4 Composite catalysts for ionic liquids.

[0038] Step 2: Add 100Kg of methanol and 30Kg of the composite catalyst prepared in the above step (1) into a 500L stainless steel autoclave, close the feeding port, replace the air in the autoclave with nitrogen, and then introduce tetrafluoroethylene monomer, heat up to start the reaction , the reaction temperature is controlled at 70°C, and the tetrafluoroethylene is metered into the reactor. When 300Kg of tetrafluoroethylene monomer is ...

Embodiment 3

[0040] A preparation method of 1-methoxy-1,1,2,2-tetrafluoroethane, comprising the following steps:

[0041] Step 1: Add 100Kg of sodium methoxide and [bmim]BF to a 300L reactor 4 10Kg of ionic liquid, stirred for 2h, then added 100Kg of fluorine intercalated hydrotalcite (LDH-F, the mass percentages of Ni, Mg, F and Al were 20%, 20%, 5% and 55%), at 80 Reaction at ℃ for 20 hours, after the reaction, the basic compound supported by fluorine intercalation hydrotalcite and [bmim]BF 4 Composite catalysts for ionic liquids.

[0042] Step 2: Add 100Kg of methanol and 30Kg of the composite catalyst prepared in the above step (1) into a 500L stainless steel autoclave, close the feeding port, replace the air in the autoclave with nitrogen, and then introduce tetrafluoroethylene monomer, heat up to start the reaction , the reaction temperature is controlled at 30°C, and the tetrafluoroethylene is metered into the reactor. When 300Kg of tetrafluoroethylene monomer is introduced, the r...

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PUM

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Abstract

The invention discloses a method for preparing 1-alkoxy-1,1,2,2-tetrafluoroethane. The method comprises the following steps of (1) carrying out reaction on an alkali compound, [bmim]BF4 ionic liquid and fluorine intercalation hydrotalcite according to the mass ratio of 1:(0.05-0.2):(0.4-1), wherein the reaction temperature is 80-200 DEG C, the reaction time is 5-20 hours; after reaction, obtaining fluorine intercalation hydrotalcite loaded alkali compound and compound catalyst of [bmim]BF4 ionic liquid, and reserving for later use; (2) adding alcohol and the compound catalyst prepared in step (1)10-50% the mass of alcohol into a reaction kettle, sealing the reaction kettle, replacing the air in the reaction kettle with nitrogen, then aerating tetrafluoroethylene monomer, rising the temperature and beginning to react, wherein the reaction temperature is controlled to be 30-70 DEG C; finishing the reaction when tetrafluoroethylene monomer 100-400% mass of the alcohol is aerated, filtering and recycling the compound catalyst, washing and rectifying the filtrate so as to obtain the 1-alkoxy-1,1,2,2-tetrafluoroethane. The method has the advantages that the catalyst has good activity and can be recycled, few three wastes are generated, and the method is environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing ether compounds, in particular to a preparation method of 1-alkoxy-1,1,2,2-tetrafluoroethane. Background technique [0002] 1-Alkoxy-1,1,2,2-tetrafluoroethane has excellent properties such as low toxicity, low global warming potential and low greenhouse effect, compared with long carbon chain perfluoroalkyl compounds, It has fewer fluorine atoms, low price, and low long-term residual rate in the environment. It can be used as a refrigerant with excellent cleaning performance, foaming agent, cleaning agent, aerosol and waterproof drying solvent, and can also be used to produce polyurethane Foam or polyisocyanurate foam blowing agent, its performance is under development, the market prospect is promising. [0003] The preparation routes of 1-alkoxy-1,1,2,2-tetrafluoroethane mainly include: hydroalkoxylation of unsaturated hydrocarbons and alcohols, and alkylation of acid fluorides (car...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/12C07C41/06B01J27/128B01J31/02
CPCY02P20/584
Inventor 王金明吴晓晋杨海波宋小弦
Owner JUHUA GROUP TECH CENT