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Preparation method of hexachlorobutadiene

A technology of hexafluorobutadiene and synthesis method, which is applied in the field of preparation of hexafluorobutadiene, and can solve problems such as separation difficulties, product yield decline, and difficult extraction of perfluorocyclobutene

Active Publication Date: 2014-04-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been confirmed by experiments that the gas generated in this process is a mixture of perfluorobutadiene and perfluorocyclobutene, and the difference between the boiling points of isomer perfluorocyclobutene and perfluorobutadiene is only 0.8°C, which gives a separation band come with great difficulty
At the same time, the perfluorocyclobutene dissolved in the solvent is difficult to extract, resulting in a decline in product yield

Method used

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  • Preparation method of hexachlorobutadiene

Examples

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preparation example Construction

[0021] Preparation of Grignard reagents:

[0022]A) In a 3L round-bottomed three-necked flask with a condenser, add 108g of magnesium strips (4.5mol), a few grains of iodine, and at the same time add about 500ml of anhydrous ether, heat to boiling, and dissolve 4.5mol of bromobenzene in 200ml of ether solution , first drop a few drops, and after the Grignard reaction is triggered, slowly add the remaining bromophenetole solution dropwise to generate a Grignard reagent with a concentration of about 3 mol / l. By increasing the amount of diethyl ether, different concentrations of bromobenzene and magnesium can be obtained such as 1mol / l, 2mol / , etc. to prepare Grignard reagent.

[0023] B) In a 3L round-bottomed three-necked flask with a condenser, add 27.8g of lithium metal (4.0mol) and a few grains of iodine, and at the same time add about 1000ml of tetrahydrofuran. Add a few drops dropwise to initiate the Grignard reaction, then slowly add the remaining bromobenzenetetrahydrof...

Embodiment 1

[0026] Such as figure 1 In the airtight device shown, 400ml of tetrahydrofuran as a solvent is pre-added in a 2000ml tower kettle 3 with a thermocouple 4 . Add 1000ml (2.0mol) of the Grignard reagent prepared by the above method A and 500ml of 454g (1.0mol) diiodooctafluorobutane with a concentration of 2mol / l into the two dropping funnels 1 and 2 shown in the figure. For tetrahydrofuran solution, nitrogen gas is used to replace all the gases in the equipment and then vacuumize. The vacuum degree is maintained at 300mmHg. Heat the tower kettle to keep the tetrahydrofuran boiling until it reaches full reflux. Slowly add Grignard reagent and diiodooctafluorobutane solution to the middle of the tower at the same time, control the rate of addition, so that the entire solution is added dropwise in about 3-4 hours, collect the crude product in the product collection device 5, and cool it in the product collection device The medium is -90°C. After the reaction is completed, the crud...

Embodiment 2

[0028] As the equipment described in Example 1, add solvent 400ml tetrahydrofuran in 2000ml tower kettle with thermocouple, add respectively concentration be 3mol / l bromobenzene and Mg in 1,2 two dropping funnels according to above-mentioned A The prepared Grignard reagent 1000ml (3.0mol) and 682g (1.5mol) diiodooctafluorobutane solution in 500ml tetrahydrofuran, after all the air in the device was replaced with nitrogen, vacuumed to maintain a vacuum of 100mmHg, heating tower Kettle, keep tetrahydrofuran boiling to total reflux, control the cooling temperature at the top of the tower at 6-7°C, keep a certain amount of reflux in the tower kettle, after the total reflux, slowly drop Grignard reagent and diiodooctafluorobutane from the middle of the tower at the same time Alkanes solution, control the drop rate, so that the whole solution is added dropwise in about 3-4 hours, collect the crude product in a low-temperature cold trap at -90°C, after the reaction is completed, place...

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Abstract

The invention relates to a preparation method of hexachlorobutadiene. Under the existence of a polar solvent, I-CF2-CF2-CF2-CF2-I and a Grignard reagent synthetized by metals of Mg, Zn or Li and the like and aromatic organic compounds react in a rectifying column in manner of reaction distillation, wherein the reaction temperature is the boiling temperature of the corresponding solvent under the reaction condition, and the reaction is carried out in vacuum, or the reaction is carried out at ordinary pressure, and meanwhile, nitrogen purging is utilized in the reaction process. In the invention, the reaction is carried out in manner of reaction distillation; in the reaction process, the maximal steam quantity of steam in a reaction area can be ensured, and meanwhile, under the assistance of the vacuum or nitrogen purging, reaction products are rapidly separated from the solvent, thereby reducing the occurrence of side reaction and effectively increasing the yield and selectivity of the reaction, wherein the highest reaction yield can reach 97.6 percent, and the selectivity can reach 97.78 percent. Meanwhile, after the reaction is ended, the solvent can be recovered in the same device, thereby reducing the equipment investments and reducing the operating steps.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a preparation method of hexafluorobutadiene. Background technique [0002] Electron gas Hexafluorobutadiene (C 4 f 6 ) is the latest laser etchant, it can replace the current laser etchant carbon tetrafluoride (CF 4 ), hexafluoroethane (C 2 f 6 ), octafluoropropane (C 3 f 8 ), Octafluorocyclobutane (C 4 f 8 ) is used for the dry etching process of sharply etching semiconductor capacitor patterns (patterns) with KrF laser, and the etching line width can reach below 90nm. The etching gas Octafluorocyclobutane (C 4 f 8 ) compared to hexafluorobutadiene (C 4 f 6 ) has the advantages of fast degradation in the atmosphere, small greenhouse effect, high aspect ratio and high selectivity. At the same time, hexafluorobutadiene is not only the latest type of laser etchant, but also a synthetic monomer of many new fluororesins, fluoroplastics, and fluororubber...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/20C07C17/23
Inventor 朱璟刘成汪宝和井欣张德立
Owner TIANJIN UNIV
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