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Method for preparing high-purity diethyl disulfide

A high-purity technology of diethyl disulfide, which is applied in the field of petrochemical industry, can solve the problems of inability to prepare high-purity diethyl disulfide in large quantities, reduce the discharge of three wastes and environmental pollution, reduce production costs, simplify The effect of the production process

Active Publication Date: 2014-06-25
NINGBO ZHONGYI PETROCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method realizes the separation of disulfide and lye by controlling the gas-liquid volume ratio, operating temperature, operating pressure, and the speed of the supergravity machine. Although the method realizes the refined separation of disulfide, the obtained disulfide is still Mixture, unable to prepare high-purity diethyl disulfide in large quantities

Method used

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  • Method for preparing high-purity diethyl disulfide

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Embodiment 1

[0020] Such as figure 1 As shown, a method for preparing high-purity diethyl disulfide described in the embodiment of the present invention, its production process is: the petrochemical raw material rich in ethanethiol is subjected to the step of sweetening mercaptan with lye, and the step of catalytic oxidation of sulfur-containing and rich alkali , disulfide pre-distillation impurity removal step and disulfide rectification step to obtain high-purity diethyl disulfide;

[0021] The lye demercaptan step is as follows: mix ethanethiol-rich petrochemical raw materials with NaOH solution according to the volume ratio (1:1~5:1) and react at 25~45°C for 1~30 minutes to prepare mercaptan Sodium lye, its chemical reaction formula is: CH 3 -CH 2 -SH+NaOH→CH 3 -CH 2 -S-Na+H 2 O;

[0022] The described sulfur-containing alkali-rich catalytic oxidation step is: adding a phthalocyanine cobalt catalyst and an oxidant to the above-mentioned thiol-containing sodium lye for catalytic o...

Embodiment 2

[0027] Take 1L of crude oil with high ethanethiol content (100-20000??g / g) (represented by South Pass crude oil, but not limited thereto) or coking liquefied gas and mixed liquefied gas with high ethanethiol content during processing One of intermediate products such as gas, light naphtha, oil gas, condensate, etc., prepare 0.2L of NaOH solution with a concentration of 15-30%wt, and 10%wt of dinuclear phthalocyanine cobalt ammonium sulfonate catalyst solution as the experimental material 0.1 L; The oil product containing ethanethiol and NaOH solution are carried out sweetening reaction in the fiber liquid membrane or other similar high-efficiency mass transfer reactors according to the ratio of 5:1. After standing for 30 minutes, ethanethiol is converted into sodium mercaptide and separated into the lye phase; after the lye and oil are completely separated, add 20-2000?g of lye rich in sodium mercaptide to the catalyst / g, into the lye containing the catalyst, air or oxygen th...

Embodiment 3

[0029]After crude oil containing different sulfur forms is refined and processed, the total sulfur in the coking liquefied gas is 3800??g / g, of which ethanethiol accounts for 53% of the total sulfur. First, the coking liquefied gas is eluted with alkali to remove the mercaptan Then, the sulfide in the rich lye after sweetening is catalyzed and oxidized, and most of ethanethiol and a small amount of other mercaptans are finally converted into a disulfide mixture mainly composed of diethyl disulfide. Preliminary distillation is carried out on the disulfide separated by enrichment, and after most of the impurities such as sodium ions and cobalt ions are separated, the crude disulfide obtained is subjected to rectification or high gravity separation and purification. The difference is that the number of theoretical plates used in disulfide rectification is 40, the reflux ratio is 15, and the diethyl disulfide with a purity of 98.2% is obtained.

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Abstract

The invention relates to a method for preparing high-purity diethyl disulfide. The method comprises the following steps: mixing an ethanethiol-enriched petrochemical raw material with NaOH solution in a volume ratio of (1:1)-(5:1), and reacting for 1-30 minutes at 25-45 DEG C to prepare a sodium mercaptide-containing alkaline solution; adding cobalt phthalocyanine catalysts and an oxidant in the sodium mercaptide-containing alkaline solution, carrying out catalytic oxidation at 35-40 DEG C, and reacting for 1-8 hours to obtain a disulphide mixture; primarily distilling the disulphide mixture to obtain a disulphide crude product; rectifying and purifying the disulphide crude product to obtain the high-purity diethyl disulfide finished product. The method disclosed by the invention has the following beneficial effects that the production cost of diethyl disulfide is reduced, the production process is simplified, and the three-waste discharge and environmental pollution during the preparation process for the diethyl disulfide are reduced.

Description

technical field [0001] The invention relates to the field of petrochemical technology, in particular to a method for purifying disulfides. Background technique [0002] The production and preparation of diethyl disulfide in the prior art mainly adopts the method of chemical synthesis, puts sodium sulfide solution in the reactor earlier, feeds in sulfur powder according to sodium sulfide: sulfur=1:1 (molar ratio), sandwiches Heat up the cover, under stirring, when the temperature reaches 80-95°C, keep it warm for 1h to form disodium disulfide (Na 2 S 2 ) solution, then pump in the disodium disulfide solution in the alkylation kettle, start stirring, and wait until the reaction kettle is vacuumed to (2~3.3)×10 4 Pa closed the vacuum valve and began to feed ethyl chloride, the reaction temperature was controlled at 75-90°C, and the pressure was controlled at (1.17-1.18)×10 5 Pa, the feed ratio (molar ratio) is disodium disulfide: ethyl chloride = 1:2, after passing through t...

Claims

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Application Information

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IPC IPC(8): C07C321/14C07C319/24
Inventor 王德志高秀祁永生夏桂友聂通元梁玮蔡喜洋朱易峰王铭高帅
Owner NINGBO ZHONGYI PETROCHEM TECH
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