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A kind of preparation method of hexafluoro-1,3-butadiene and its intermediate

A technology of butadiene and hexafluorobutane, which is applied in the field of synthesizing hexafluoro-1,3-butadiene and its intermediates by telomerization, can solve the problems of high equipment requirements and high process safety risks, and achieve improved The effect of selectivity, simple process and mild reaction conditions

Active Publication Date: 2022-03-29
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method has high requirements on equipment and high risk of process safety.

Method used

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  • A kind of preparation method of hexafluoro-1,3-butadiene and its intermediate
  • A kind of preparation method of hexafluoro-1,3-butadiene and its intermediate
  • A kind of preparation method of hexafluoro-1,3-butadiene and its intermediate

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Embodiment 1

[0043] This embodiment provides a preparation method of hexafluoro-1,3-butadiene, the preparation method includes intermediate preparation steps and hexafluoro-1,3-butadiene preparation steps, specifically as follows:

[0044] A1. Preparation of 1,4-dibromo-2,3-dichloro-1,1,2,3,4,4-hexafluorobutane

[0045] Add 150g of acetonitrile, 69.1g (0.25mol) of 1,2-dibromo-1-chloro-1,2,2-trifluoroethane, 69.1g (0.25mol) of diphenylmethane peroxide, Acyl 1.8g (7.5mmol), with high-purity N 2 Purge for 10 minutes, then pour 34.8g (0.30mol) of chlorotrifluoroethylene from the steel cylinder into the reactor, heat up to 80°C under mechanical stirring (300-500r / min), the pressure of the reactor rises to about 0.5MPa, and keep warm for 12 hours to end the reaction.

[0046] The reaction solution was analyzed by GC-MS and calculated: the conversion rate of raw material 1,2-dibromo-1-chloro-1,2,2-trifluoroethane was 98.75%, and the conversion rate of intermediate 1,4-dibromo- The selectivity ...

Embodiment 2

[0051] The operation of this embodiment is the same as that of Embodiment 1, the difference is only in:

[0052] During the preparation of the intermediate, the type of initiator was changed, and the dibenzoyl peroxide in Example 1 was replaced with 1.1 g (7.5 mmol) of di-tert-butyl peroxide. The reaction results are shown in Table 1.

[0053] During the preparation of hexafluoro-1,3-butadiene, the type of catalyst was changed, and 2.5 g of zinc iodide was used instead of elemental iodine in Example 1 to obtain 89.20 g of the product. The results are shown in Table 3.

Embodiment 3

[0055] The operation of this embodiment is the same as that of Embodiment 1, the difference is only in:

[0056] During the preparation of the intermediate, the type of initiator was changed, and the dibenzoyl peroxide in Example 1 was replaced with 0.68 g (7.5 mmol) tert-butyl hydroperoxide; the reaction results are shown in Table 1.

[0057] During the preparation of hexafluoro-1,3-butadiene, the type of catalyst was changed, and 1.5 g of 1,2-dibromoethane was used instead of elemental iodine in Example 1 to obtain 95.0 g of the product. The results are shown in Table 3.

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Abstract

The invention discloses a method for preparing hexafluoro-1,3-butadiene and its intermediates. The method for preparing hexafluoro-1,3-butadiene comprises: A1. in a polar aprotic solvent , under the action of an initiator, 1,2-dibromo-1-chloro-1,2,2-trifluoroethane reacts with trifluorohaloethylene, and the reaction solution is purified by rectification to obtain 1,4-dibromo-2 -Chloro-3-halo-1,1,2,3,4,4-hexafluorobutane; the structural formula of the trifluoroethylene halide is: CF2=CFX, wherein X is Cl, Br or I; the The initiator is selected from at least one of azobisisobutyronitrile, di-tert-butyl peroxide, dibenzoyl peroxide, dicumyl peroxide, tert-butyl hydroperoxide, potassium persulfate, ammonium persulfate species; A2.1,4-dibromo-2-chloro-3-halogenated-1,1,2,3,4,4-hexafluorobutane and zinc powder were dehalogenated to obtain hexafluoro-1,3 ‑Butadiene. The preparation method has the advantages of simple process, mild reaction conditions, suitable for industrial production and the like.

Description

technical field [0001] The invention relates to fluorine-containing electron gas, in particular to a method for synthesizing hexafluoro-1,3-butadiene and its intermediate by telomerization. Background technique [0002] Hexafluoro-1,3-butadiene, whose English name is Hexafluoro-1,3-butadiene, or HFBD for short, has a boiling point of 5.5°C, a freezing point of -130°C, and a liquid density of 1.44kg / L at 15°C. Hexafluoro-1,3-butadiene is a new generation of green dry etching gas with excellent environmental performance and work performance, and its existence time (ALT) in the atmosphere is only 1.9 days, GWP 100 The value is 290. Because hexafluoro-1,3-butadiene has a lower fluorocarbon ratio, it exhibits excellent etching performance. It is used for etching rectifier circuit boards containing Cu and low K dielectric constant. It is mainly used For precise etching of critical dimensions (accuracy up to 100nm), it has better selectivity and aspect ratio than other etching ga...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/278C07C19/10C07C19/14C07C17/25C07C21/20
CPCC07C17/278C07C17/25C07C19/10C07C19/14C07C21/20
Inventor 刘武灿吴海锋谢浩杰赵翀
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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