Method for preparing 3, 3, 3-trifluoropropyne through gas-phase dehydrohalogenation

A technology for dehydrohalogenation and trifluoropropyne, which is applied in the direction of dehydrohalogenation preparation, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of harsh use conditions, low selectivity, and environmental pollution, and achieve single-pass production The effect of high efficiency and high selectivity

Active Publication Date: 2021-06-22
泉州宇极新材料科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0013] The above liquid-phase dehydrohalogenation route has the following problems: (1) All belong to the batch process, and the synthesis efficiency is low; (2) A large amount of reaction solvent is used, which will generate a large amount of waste liquid, thereby seriously polluting the environment; (3) Using A large number of alkaline dehydrohalogenation reagents (such as potassium hydroxide, n-butyllithium, lithium diisopropylamide, etc.) will produce a large amount of waste solids, which will seriously pollute the environment; (4) use n-butyllithium or Lithium diisopropylamide is used as a reagent for dehydrohalogenation. Although the yield of 3,3,3-trifluoropropyne is very high, n-butyllithium is expensive, and the use conditions are harsh, requiring anhydrous and oxygen-free operation. And flammable and explosive, difficult to safe experimental operation
[0019] The route of above-mentioned gas-phase dehydrohalogenation has the following problems: the catalytic activity of the catalyst is very low, showing the shortcomings of low conversion rate and low selectivity, and it is difficult to meet the requirements of industrial production

Method used

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  • Method for preparing 3, 3, 3-trifluoropropyne through gas-phase dehydrohalogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051]Catalyst preparation: (1) Dissolve barium chloride in water, then add ammonia water dropwise until the pH value is 7-9, then age for 16 hours, filter, wash, and dry at 100°C for 16 hours to obtain a solid, pulverize, Press molding to obtain the precursor barium hydroxide; (2) The obtained precursor is roasted at 400°C for 12 hours in a nitrogen atmosphere; Gas activation for 16 hours to obtain barium fluoride; (3) according to the mass percentage of cesium fluoride and barium fluoride composition 10%:90%, the alkali metal fluoride is dissolved in water, and the barium fluoride carrier is added to the impregnating solution , impregnated at room temperature for 12 hours, filtered, dried at 100° C. for 16 hours, and calcined at 400° C. for 12 hours under a nitrogen atmosphere to obtain a catalyst.

[0052] A tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm was filled with 10 ml of the catalyst prepared above. The temperature o...

Embodiment 2

[0054] The same operation as in Example 1, the difference is that "composition of 10% according to the mass percentage of cesium fluoride and barium fluoride: 90%" is changed to "composition of 20% according to the mass percentage of cesium fluoride and barium fluoride: 80% %", change the reaction temperature to 350°C. The reaction results are as follows: the conversion rate of Z-1-chloro-3,3,3-trifluoropropene is 13.8%, the selectivity of 3,3,3-trifluoropropyne is 96.8%, and the selectivity of E-1-chloro-3 , The sum of the selectivities of 3,3-trifluoropropene and 2-chloro-3,3,3-trifluoropropene was 3.1%.

Embodiment 3

[0056] The same operation as in Example 1, except that "composition of 10% according to the mass percentage of cesium fluoride and barium fluoride: 90%" was changed to "composition of 30% according to the mass percentage of cesium fluoride and barium fluoride: 70% %", change the reaction temperature to 450°C. The reaction results are as follows: the conversion rate of Z-1-chloro-3,3,3-trifluoropropene is 25.4%, the selectivity of 3,3,3-trifluoropropyne is 93.1%, and the selectivity of E-1-chloro-3 , The sum of the selectivities of 3,3-trifluoropropene and 2-chloro-3,3,3-trifluoropropene was 6.8%.

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Abstract

The invention discloses a method for preparing 3, 3, 3-trifluoropropyne through gas-phase dehydrohalogenation. The method comprises the following steps: taking 1-halogen-3, 3, 3-trifluoropropene or/and 2-halogen-3, 3, 3-trifluoropropene (halogen = F or Cl or Br or I) as a raw material, and carrying out gas-phase dehydrohalogenation reaction in the presence of a catalyst to obtain the 3, 3, 3-trifluoropropyne. The method disclosed by the invention is mainly used for producing the 3, 3, 3-trifluoropropyne in a gas-phase continuous circulation manner at a high conversion rate and high selectivity.

Description

technical field [0001] The present invention relates to a method for preparing 3,3,3-trifluoropropyne by gas-phase dehydrohalogenation, in particular to a method using E-1-halo-3,3,3-trifluoropropene or / and Z-1- Halogen-3,3,3-trifluoropropene or / and 2-halogen-3,3,3-trifluoropropene (halogen = F or Cl or Br or I) as raw materials, in the presence of catalyst, dehalogenation in gas phase Hydrogen reaction to obtain 3,3,3-trifluoropropyne method. Background technique [0002] At present, there are two main synthetic methods of 3,3,3-trifluoropropyne: [0003] (1) Liquid phase dehydrohalogenation [0004] EP2143702 reported that in ethanol solvent, 130.5g of Z-1-chloro-3,3,3-trifluoropropene was reacted with 61.7g of potassium hydroxide at 38°C for 2.5 hours, then Z-1-chloro-3,3 , The conversion rate of 3-trifluoropropene was 99.2%, and the selectivity of 3,3,3-trifluoropropyne was 98.4%. [0005] JP6032085 reported that in aqueous potassium hydroxide solution, Z-1-chloro-3,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/25C07C21/22B01J27/138B01J37/03B01J37/08B01J37/26B01J37/02
CPCB01J27/138B01J37/0201B01J37/031B01J37/082B01J37/26C07C17/25C07C21/22
Inventor 权恒道张呈平董利刘冬鹏
Owner 泉州宇极新材料科技有限公司
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