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Recovery method for mother liquor of cyclohexyl disulfide

A technology of dicyclohexyl disulfide and recovery method, which is applied in the directions of sulfur compounds, chemical instruments and methods, hydrogenated polysulfide/polysulfide preparation, etc., can solve problems such as rare reports on mother liquor treatment, and eliminate potential safety hazards. , Save the cost of raw materials and ensure the effect of safe production

Active Publication Date: 2018-11-06
山东戴瑞克新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the previous reports on dicyclohexyl disulfide focused on its synthesis method, but there were few reports on the treatment of the resulting mother liquor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Concentrate 1000L mother liquor to the state where sodium sulfide is about to be saturated in an environment of 90°C. At this time, part of sodium chloride is precipitated. At this temperature, use centrifugal filtration, filter tank suction filtration or pressure filtration to perform the filtration operation. 55.54 kg of sodium chloride crystals were isolated. The crystallized NaCl crystals were washed with NaCl saturated solution, consuming 56.30 kg of NaCl saturated solution, and detected by HPLC, the purity of the obtained sodium chloride was 92.10%. In this process, the quality of the steamed water is 821.2kg.

[0033] 2, add 32wt% sodium hydroxide solution in the filtrate, make NaHS all change into sodium sulfide, the amount of the added sodium hydroxide solution is 75.22kg.

[0034] 3. Cool down to 0°C for crystallization. After no crystals are precipitated, use centrifugal filtration, filter tank suction filtration or pressure filtration at this temperature...

Embodiment 2

[0040] 1. Concentrate 1000L of the mother liquor at 80°C until the sodium sulfide is about to be saturated. At this time, some sodium chloride is precipitated. Use centrifugal filtration, filter tank suction filtration or pressure filtration to separate the chloride 54.01kg of sodium crystals. Wash the NaCl saturated solution to the crystallized NaCl saturated solution, and consume 55.68kg NaCl saturated solution. Detected by HPLC, the purity of the obtained sodium chloride was 90.95%. In this process, the quality of the steamed water is 802.92kg.

[0041] 2, add 32wt% sodium hydroxide solution in the filtrate, make NaHS all change into sodium sulfide, the amount of the added sodium hydroxide solution is 75.22kg.

[0042] 3. Cool down to 10°C for crystallization. After no crystals are precipitated, use centrifugal filtration, filter tank suction filtration or pressure filtration at this temperature to perform filtration operations to separate Na 2 S crystallization 100.01kg...

Embodiment 3

[0048] 1. Concentrate 1000L of mother liquor at 85°C to the state where sodium sulfide is about to be saturated. At this time, part of sodium chloride is precipitated. Use centrifugal filtration, filter tank suction filtration or pressure filtration to separate the chloride 54.87kg of sodium crystals. Wash the NaCl saturated solution to the crystallized NaCl saturated solution, and consume 55.91kg NaCl saturated solution. Detected by HPLC, the purity of the obtained sodium chloride was 91.56%. In this process, the quality of the steamed water is 817.56kg.

[0049] 2, add 32wt% sodium hydroxide solution in the filtrate, make NaHS all change into sodium sulfide, the amount of the added sodium hydroxide solution is 75.22kg.

[0050] 3. Cool down to 25°C for crystallization. After no crystals are precipitated, use centrifugal filtration, filter tank suction filtration or pressure filtration at this temperature to perform filtration operations to separate Na 2 S crystallization ...

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Abstract

The invention discloses a recovery method for a mother liquor of cyclohexyl disulfide. The recovery method comprises the following steps: carrying out evaporation concentration on the mother liquor ofcyclohexyl disulfide, so as to dissolve out sodium chloride crystals, and stopping concentration until saturation or near saturation of sodium sulfide; separating out sodium chloride crystals, and adding a sodium hydroxide solution into the residual mother liquor so as to remove NaHS, then cooling to 0 to 25 DEG C for crystallization, so as to separate out sodium sulfide crystals. According to the recovery method provided by the invention, sodium hydrosulfide is changed to be sodium sulfide by using the sodium hydroxide solution, then according to the differences of solubilities of sodium sulfide and sodium chloride under impacts of temperature variation, a pure physical way is adopted for recovering sodium sulfide and sodium chloride in the mother liquor, an acidation process in a traditional process is avoided, no hydrogen sulfide is produced, the technological process is simplified, raw material cost, equipment cost and field cost are reduced greatly, and environmental protection is achieved.

Description

technical field [0001] The invention relates to a method for recovering mother liquor, in particular to a method for recovering dicyclohexyl disulfide mother liquor with simple operation, and belongs to the technical field of post-synthesis treatment of dicyclohexyl disulfide. Background technique [0002] The structural formula of dicyclohexyl disulfide (referred to as disulfide) is , can be used as food spices, used in dyes, medicines, pesticides, organic synthesis, etc.; in the rubber additive industry, dicyclohexyl disulfide is a synthetic anti-scorch agent CTP One of the important intermediates of amines. Modern rubber processing technology is developing in the direction of high temperature and high speed. The role of anti-scorch agents is becoming more and more prominent, and the status of the intermediate product dicyclohexyl disulfide is becoming more and more important. [0003] At present, the main method of synthesizing disulfides is: Na 2 S, S and chlorocyclo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/04C01B17/34C07C319/24C07C321/22
CPCC01B17/34C01D3/04C01P2006/80C07C319/24C07C2601/14C07C321/22
Inventor 郑崇纳李宪索方风芹纪艳宇卢杰马亚敏赵丹丹徐晓兰刘红王兴军丁述辉
Owner 山东戴瑞克新材料有限公司
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