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Synthesis process of 1-chloro octane

A synthesis method and technology of chlorooctane, applied in the field of synthesis of 1-chlorooctane, can solve the problems of inconvenient and accurate measurement of phosgene, difficulty in storage and transportation, pollution, etc., achieve great implementation value and social and economic benefits, eliminate The effect of great safety hazards and advanced process routes

Inactive Publication Date: 2007-03-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The product obtained by the phosphorus oxychloride process contains a large amount of by-product phosphoric acid, and phosphorus oxychloride is used as a chlorinated reagent to seriously corrode the equipment, a large amount of phosphorus-containing wastewater is difficult to handle, serious pollution problems, and prominent environmental problems
Although the yield of phosgene is high, phosgene is a highly toxic gas, which is not easy to store and transport. At the same time, it is not convenient to accurately measure phosgene as a gas, especially when the laboratory needs a small amount of accurate quantitative phosgene, excessive use prone to side effects
The hydrogen chloride gas method has strict requirements on equipment, and it is difficult to realize industrial production

Method used

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  • Synthesis process of 1-chloro octane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The amount ratio of feed material n-octanol: two (trichloromethyl) carbonates: organic amine catalyst is 1: 0.36: 0.2, and the feeding amount of n-octanol is 6.5g (0.05mol), two (trichloromethyl) The charging amount of carbonate is 5.35g (0.018mol), the organic solvent is chlorobenzene, and the consumption is 0.5 times of n-octanol quality, and the organic amine catalyst is triethylamine, and the consumption is 1.01g (0.01mol).

[0021] Dissolve bis(trichloromethyl)carbonate in the above-mentioned chlorobenzene, transfer to the constant pressure dropping funnel at low temperature, then transfer n-octanol to another constant pressure dropping funnel after diluting n-octanol with the same solvent At 60-110°C, slowly add it dropwise to a solution of triethylamine diluted with chlorobenzene, and keep this temperature for 4-9 hours. The reaction solution was naturally cooled to room temperature, neutralized with an alkaline solution to neutrality, then washed 3 times with ta...

Embodiment 2

[0023] The amount ratio of the feed material is n-octanol: two (trichloromethyl) carbonate: catalyst is 1: 0.4: 0.4, and the feeding amount of n-octanol is 6.5g (0.05mol), two (trichloromethyl) carbonate The feeding amount is 5.94g (0.02mol), the organic solvent is chlorobenzene, and the consumption is 0.3 times of n-octanol mass, and the catalyst is triethylamine, and the consumption is 2.02g (0.02mol).

[0024] Reaction temperature is 67~72 ℃, other operation is the same as embodiment 1, obtains product 5.58g, product yield 75.1%, purity 96.0%, boiling point 182~186 ℃.

Embodiment 3

[0026] The amount ratio of feed material is n-octanol: two (trichloromethyl) carbonate: catalyst is 1: 0.36: 0.6, and the feeding amount of n-octanol is 6.5g (0.05mol), two (trichloromethyl) carbonate The feeding amount is 5.35g (0.018mol), the organic solvent is chlorobenzene, the catalyst is triethylamine, and the consumption is 3.04g (0.03mol).

[0027] Reaction temperature is 80~85 ℃, other operation is the same as embodiment 1, obtains product 6.48g, product yield 87.2%, purity 98.4%, boiling point 182~186 ℃.

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Abstract

The present invention is synthesis process of 1-chloro octane with bis(trichloromethyl) carbonate as one of the materials. Under the action of organic amine catalysis, n-octanol and bis(trichloromethyl) carbonate react in organic solvent at 60-150 deg.c for 4-9 hr to obtain 1-chloro octane. The present invention has advanced technological path, reasonable technological conditions, high safety, high yield, low cost, no environmental pollution and simple post-treatment.

Description

(1) Technical field [0001] The invention relates to a synthesis method of 1-chlorooctane, in particular to a synthesis method using bis(trichloromethyl)carbonate as one of the raw materials. (2) Background technology [0002] The haloalkane compound 1-chlorooctane is n-chlorooctane, which is the main intermediate for the synthesis of UV absorber UV-531 and PVC high-efficiency non-toxic organotin heat stabilizer. In addition to being used as organic solvent and raw material for organic synthesis, it is also used as Used as a printing detergent. [0003] Before the present invention was given, the chemical synthesis methods of 1-chlorooctane in the prior art were mostly prepared by n-octanol and phosphorus oxychloride, phosgene, hydrogen chloride gas or thionyl chloride. As in Green Chemistry, 2006, 8, 437-438 with alcohol and SOCl 2 The reaction produces 1-chlorooctane and so on. Using the thionyl chloride process, a large amount of sulfur dioxide gas is released in the ta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/01C07C17/00
Inventor 苏为科陈志卫王博
Owner ZHEJIANG UNIV OF TECH
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