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Preparation method of fluorinated acyl fluoride

A technology of acyl fluoride and hydrogen fluoride, which is applied in the field of preparation of acyl fluoride, can solve the problems of cumbersome separation steps, unstable yield, and high requirements for production equipment, and achieve a wide range of raw material sources, reduced production costs, and a high degree of automation Effect

Pending Publication Date: 2022-03-01
科莱博(江苏)科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] (1) European patent document EP623578 reported that trichlorethylene can be oxidized to dichloroacetyl chloride in the presence of an amine catalyst tetramethylpiperidine. The obvious disadvantage of this patent is the generation of by-product halogenated propylene oxide. low utilization
[0008] (2) Chinese patent documents CN1131140 and CN101445445 both reported that trichlorethylene reacted with oxygen in the presence of catalyst azobisisobutyl ester and initiator triethylamine under the environmental conditions of 0.1MPa~0.8MPa and 40℃~180℃. The reaction can produce dichloroacetyl chloride with a yield of 20% to 85%. The patented method has poor reaction stability and unstable yield
[0009] (3) German patent document DE19620018 reported that trichlorethylene can be oxidized to dichloroacetyl chloride by oxygen at 50°C to 200°C. The rate is good, but the requirements for the production equipment are too high
[0010] (4) In 2007, Ou, Hsin-Hung et al. reported that trichlorethylene could be reacted into dichloroacetyl chloride and phosgene by light under the catalysis of platinum-doped carbon dioxide. Phosgene is highly toxic. Due to the extremely active nature of phosgene Chemical properties, if phosgene cannot be completely separated from dichloroacetyl chloride, it will be unfavorable to the preparation of downstream products, so the industrial production of the process technology described in this patent is relatively difficult
In this production process, the oxidation reaction and fluorination reaction are carried out separately, and the reactant hydrofluoric acid is a liquid, and the separation steps are cumbersome.

Method used

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  • Preparation method of fluorinated acyl fluoride
  • Preparation method of fluorinated acyl fluoride
  • Preparation method of fluorinated acyl fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The concrete steps of the preparation method of the difluoroacetyl fluoride of the present embodiment are:

[0049] First, heat the premixer to 110°C to 115°C with heat conduction oil, and heat the reactor filled with the loaded 3-difluoromethyl-1H-methylpyrazole-4-carboxylic acid chromium catalyst to 180°C to 190°C ℃, use nitrogen to purge from the raw material inlet or hydrogen fluoride inlet to ensure that there is no moisture in the entire reaction device.

[0050] Then start the premixer to stir, and start to feed hydrogen fluoride gas into the premixer (flow rate: 5m³ / h). After hydrogen fluoride escapes from the product outlet at the top of the reactor, feed trichlorethylene and dry oxygen into the premixer at the same time (Trichlorethylene flow rate: 1.5m³ / h, oxygen flow rate: 1.8m³ / h), the reactor back pressure is 0.1MPa and the reaction is carried out at 180℃~190℃, and the mixed gas of difluoroacetyl fluoride, hydrogen chloride and hydrogen fluoride can be obt...

Embodiment 2

[0065] The concrete steps of the preparation method of the nonafluorovaleryl fluoride of the present embodiment are:

[0066] Firstly, heat the premixer to 160°C-165°C with heat conduction oil, heat the reactor filled with the loaded complex catalyst to 170°C-175°C, and use nitrogen gas from the raw material inlet or hydrogen fluoride inlet. Purge to ensure that the entire reaction apparatus is free of moisture.

[0067] Then start the premixer to stir, start to feed hydrogen fluoride gas into the premixer (flow rate: 5m³ / h), and after the hydrogen fluoride escapes from the product outlet at the top of the reactor, the 4,5,5,5-decachloropent-1-ene and dry oxygen are simultaneously fed into the premixer (1,1,2,3,3,4,4,5,5,5-decachloropent-1 -Oxygen flow rate: 1.3m³ / h, oxygen flow rate: 1.8m³ / h), reactor back pressure 0.2MPa, react at 170℃~175℃, can stably obtain mixed gas of nonafluorovaleryl fluoride, hydrogen chloride and hydrogen fluoride. The reaction formula is as follow...

Embodiment 3

[0074] The concrete steps of the preparation method of the trifluoroacetyl fluoride of the present embodiment are:

[0075] Firstly, heat the premixer to 120°C~125°C with heat transfer oil, heat the reactor filled with the loaded complex catalyst to 150°C~155°C, and use nitrogen gas from the raw material inlet or hydrogen fluoride inlet. Purge to ensure that the entire reaction apparatus is free of moisture.

[0076] Then start the premixer to stir, start to feed hydrogen fluoride gas into the premixer (flow rate: 5m3 / h), until hydrogen fluoride escapes from the product outlet at the top of the reactor, then feed tetrachlorethylene and dry oxygen into the premixer at the same time ( Tetrachlorethylene: 1.7m³ / h, oxygen flow rate 1.7m³ / h), reactor back pressure 0.1MPa, reaction at 150℃~155℃, can stably obtain the mixed gas of trifluoroacetyl fluoride, hydrogen chloride and hydrogen fluoride. The reaction formula is as follows:

[0077] .

[0078] Since the detection of trif...

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Abstract

The invention relates to a preparation method of fluoroacyl fluoride, which comprises the following steps: reacting halogenated olefin as shown in a formula I, oxygen and hydrogen fluoride under the action of a catalyst to generate fluoroacyl fluoride as shown in a formula II, and the catalyst is 3-difluoromethyl-1H-methylpyrazole-4-chromium formate. The preparation method of the fluoroacyl fluoride is wide in raw material source, simple in process, good in catalytic activity, safe and reliable in reaction, high in automation degree and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of fluoroacyl fluoride, which belongs to the technical field of fine chemicals. Background technique [0002] Acyl halide refers to the product in which the hydroxyl group in a carboxylic acid is replaced by a halogen, and the common ones are acid chloride, acid fluoride, and acid bromide. Acyl halides do not exist in nature and can only be produced through chemical synthesis. At present, acid halides in the chemical field are mainly produced by reacting carboxylic acids with acylating agents. The reaction equation is as follows: [0003] . [0004] In this reaction formula: X can be F, Cl, Br, I, etc.; R can be aliphatic hydrocarbon, aliphatic olefin, aromatic hydrocarbon, aromatic olefin, halogenated aliphatic hydrocarbon, halogenated aromatic hydrocarbon, etc. [0005] Common acylating agents are phosphorus halides, sulfoxide halides, oxalyl halides, triphenylphosphine halides, etc. The shortcomings...

Claims

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Application Information

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IPC IPC(8): C07C51/58C07C53/48C07C53/50C07D231/14B01J31/22B01J35/08B01J37/02B01J37/00B01J37/08
CPCC07C51/58C07D231/14B01J31/223B01J37/0203B01J37/0009B01J37/08B01J2531/62B01J2531/0213B01J35/51C07C53/48C07C53/50Y02P20/584
Inventor 林韦康王明春相雪理朱海蔡以恒杨沫
Owner 科莱博(江苏)科技股份有限公司
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