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Preparation method of 2-bromine-3,3,3-trifluoropropene

A technology of trifluoropropene and liquid bromine, applied in the direction of dehydrohalogenation preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalyst, etc. Recycling and reuse and other issues to achieve the effects of simplified operation, fast response, and cost reduction

Active Publication Date: 2014-02-05
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction time period of this method is long, and the iron trichloride catalyst of the bromination reaction cannot be recycled and reused, and it needs to be removed by alkali washing and water washing.

Method used

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  • Preparation method of 2-bromine-3,3,3-trifluoropropene

Examples

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preparation example Construction

[0011] Catalyst preparation:

[0012] 1. Preparation of Mesoporous Sulfonic Acid Catalyst

[0013] Phenyltrimethoxysilane (phenyltfimethoxysilane) and tetraethoxysilane (tetraethylorthosilicate) were added to 20mL ethanol solution at a ratio of 3:7, 35mL of 0.1mol / L HCl solution was gradually added, and vigorously stirred at 60°C for 4h. After cooling to room temperature, 80 mL of ethanol and 135 mL of cyclohexane solution were added to the solution, and then 180 mL of water and 18 mL of concentrated ammonia solution were added, while stirring was maintained. Then a transparent gel appeared in the reaction vessel, and after the stirring was stopped, the obtained The solid gel was aged at room temperature for 7 days, then vacuum-dried and calcined to obtain a phenyl polysiloxane precursor. Soak the obtained precursor in tetrachloroethane solution overnight, then transfer it into a sulfonation reaction bottle, add 30% sulfur trioxide solution, the reaction is strongly exothermi...

Embodiment 1

[0018] (1) Add 1.6g of mesoporous sulfonic acid and 160g (1mol) of liquid bromine into a three-neck flask equipped with a thermometer, air guide tube and reflux condenser, heat up to 35°C under stirring, and start to introduce 91.2g (0.95mol) 3,3,3-Trifluoropropene was passed through for about 2 hours, and the reaction was continued to stir for 0.5 hours at a temperature of 35° C., cooled to room temperature, and the catalyst was filtered out to obtain a reaction liquid. The filtered catalyst can be reused.

[0019] (2) In a three-neck flask equipped with a thermometer, a constant pressure dropping funnel and an atmospheric distillation device, add 200 g of 25% aqueous sodium hydroxide solution, heat up to 75°C to 85°C under stirring, and add dropwise the obtained product in step (1). The reaction solution was distilled at the same time, and the fraction at 32-36°C was received to obtain 2-bromo-3,3,3-trifluoropropene. The yield of 2-bromo-3,3,3-trifluoropropene was 94.1%, and...

Embodiment 2

[0021] (1) Add 160g (1mol) of liquid bromine and 4.8g of montmorillonite K-10 into a three-neck flask equipped with a thermometer, an air guide tube and a reflux condenser, heat up to 20°C under stirring, and start to introduce 96g (1.0mol) ) 3,3,3-trifluoropropene, pass through for about 4 hours, continue to stir and react at a temperature of 20° C. for 0.5 hours, cool to room temperature, filter out the catalyst, and obtain a reaction liquid.

[0022] (2) The operation steps are the same as step (2) of Example 1, and the yield of the obtained 2-bromo-3,3,3-trifluoropropene is 90.6%, and the purity is 99.7%.

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Abstract

The invention discloses a preparation method of 2-bromine-3,3,3-trifluoropropene. The preparation method solves a problem of long reaction period. The preparation method utilizes 3,3,3-trifluoropropene as a raw material and comprises the following steps: (1) liquid bromine is added into a reaction bottle in the presence of solid acids and 3,3,3-trifluoropropene gas is fed into the reaction bottle with stirring at a temperature of from 20 to 60 DEG C, wherein a feeding time is in a range of 1 to 6 hours; after the 3,3,3-trifluoropropene gas is fed completely, the 3,3,3-trifluoropropene gas reacts further with the liquid bromine for 0.5 hours and the reaction products are cooled to room temperature; and a catalyst is removed from the reaction products by filtering and a reaction solution is collected; and (2) a 25% of sodium hydroxide aqueous solution is putted into a reaction bottle with a distillation device and is heated with stirring to a temperature of from 75 to 85 DEG C; the reaction solution obtained from the step (1) is dropwise added into the 25% of sodium hydroxide aqueous solution with distillation at a temperature of from 75 to 85 DEG C and a fraction at a temperature of from 32 to 36 DEG C is collected thus 2-bromine-3,3,3-trifluoropropene is obtained. The preparation method provided by the invention is utilized mainly for preparing 2-bromine-3,3,3-trifluoropropene.

Description

technical field [0001] The invention relates to a preparation method of 2-bromo-3,3,3-trifluoropropene, which belongs to the field of organic synthesis. Background technique [0002] 2-Bromo-3,3,3-trifluoropropene can be used as refrigerant, fire extinguishing material, etc., and is also an important fluorine-containing building block, which can be used as raw materials and intermediates of fluorine-containing medicines, pesticides, dyes, etc. The synthesis and application of 2-bromo-3,3,3-trifluoropropene published in "New Chemical Materials", 33(7), 27-30(2005) discloses a 2-bromo-3,3,3 -The synthetic method of trifluoropropene, this method uses iron trichloride as catalyst, under dark conditions, 3,3,3-trifluoropropene is passed into liquid bromine, and the passage time is 15.3h, obtains 1,2- Dibromo-3,3,3-trifluoropropane, yield 95.2%, then 1,2-dibromo-3,3,3-trifluoropropane was dehydrobrominated under basic conditions to give 2-bromo -3,3,3-trifluoropropene, the yield...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/25B01J27/188B01J31/06B01J21/16
Inventor 谷玉杰吕剑万红李凤仙杜咏梅李春迎刘波马辉张伟杨建明
Owner XIAN MODERN CHEM RES INST
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