Catalyst for catalytically preparing tert-dodecanethiol, and preparation method thereof

A tertiary dodecyl mercaptan, catalytic preparation technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the difficulty of catalyst preparation, high Corrosiveness, high toxicity and other problems, to achieve the effect of easy operation and handling, mild reaction conditions

Inactive Publication Date: 2020-03-13
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1983, in order to increase the chlorine content of the catalytic system, the United WEB Chemical Plant proposed to use AlCl 3 -Toluene-HCl mixture as a catalyst has achieved good results, but it uses highly toxic and highly corrosive hydrogen chloride gas, which greatly increases the difficulty of catalyst preparation

Method used

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Experimental program
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Effect test

specific Embodiment approach 1

[0023] A catalyst for catalyzing the preparation of tertiary dodecyl mercaptan, said catalyst for catalyzing the preparation of tertiary dodecyl mercaptan is mainly composed of anhydrous aluminum chloride, aromatic hydrocarbon additives, chlorinated alkane additives Made, the molar ratio of described anhydrous aluminum chloride, described aromatic hydrocarbon auxiliary agent, described chlorinated alkanes auxiliary agent is 1:5:1.

[0024] In the catalyst used to catalyze the preparation of tert-dodecyl mercaptan described in this embodiment, the aromatic hydrocarbon additive is benzene.

[0025] In the catalyst used to catalyze the preparation of tert-dodecylmercaptan described in this embodiment, the chlorinated alkane additive is monochloromethane.

specific Embodiment approach 2

[0027] A kind of preparation method for the catalyst that is used to catalyze the preparation of tertiary dodecyl mercaptan according to specific embodiment one, comprises the steps:

[0028] Step 1. Take a certain mass of anhydrous aluminum chloride, aromatic hydrocarbon additives, and chlorinated alkane additives according to the molar ratio, and wait for use; Step 2. Add the weighed aromatic hydrocarbon additives in step 1 to batches while stirring Quickly add the weighed anhydrous aluminum chloride, and mix evenly; step 3, add the weighed chlorinated alkane additive dropwise under the condition of temperature control and stirring, and the dropping time is 0.5h. After the dropping is completed, continue to control Warmly stirred and reacted for 0.5 h, and returned to room temperature to obtain the above-mentioned acidic liquid catalyst for catalyzing the preparation of tert-dodecyl mercaptan.

[0029] In the method for preparing a catalyst for the catalytic preparation of t...

specific Embodiment approach 3

[0032] The application of a catalyst for catalyzing the preparation of tertiary dodecyl mercaptan according to the first embodiment is used for catalyzing the synthesis reaction of tetrapropylene and hydrogen sulfide.

[0033] The application of a catalyst for the catalytic preparation of tert-dodecyl mercaptan described in this embodiment is to add 100 g of tetrapropylene into a 250 ml four-necked flask, and add 9 g of the prepared one for catalysis dropwise under stirring. Prepare the catalyst for tert-dodecyl mercaptan, control the amount of hydrogen sulfide introduced to 30g / h, control the temperature of the reaction solution in the four-necked flask at 20-25°C, stop feeding hydrogen sulfide after 1h, and continue stirring for 20 minutes to obtain 126.2g Reaction solution, sampling analysis, the weight composition of reaction solution is: dodecene accounts for 11.73wt%, tertiary dodecyl mercaptan 79.64wt%, dodecyl sulfide 1.41wt%, and the remaining 7.22wt% is mainly catalys...

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PUM

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Abstract

The invention discloses a catalyst for catalytically preparing tert-dodecanethiol, and a preparation method thereof, and belongs to the field of catalysts for catalytically preparing tert-dodecanethiol. The catalyst is an acidic liquid prepared from anhydrous aluminum chloride, an aromatic hydrocarbon auxiliary agent and a chloroalkane auxiliary agent, a molar ratio of the anhydrous aluminum chloride to the aromatic hydrocarbon auxiliary agent to the chloralkane auxiliary agent is 1:(0.5-5):(0.1-1), the aromatic hydrocarbon auxiliary agent is benzene, methylbenzene, ethylbenzene, xylene, chlorobenzene or nitrobenzene, and the chloralkane auxiliary agent is monochloromethane, dichloromethane, trichloromethane, monochloroethane or dichloroethane. The method comprises the following steps: rapidly adding the anhydrous aluminum chloride into the aromatic hydrocarbon auxiliary agent in batches while stirring, dropwise adding the chloralkane auxiliary agent under a temperature-controlled stirring condition, and continuously carrying out a temperature-controlled stirring reaction for a certain time after the drop-by-drop addition is completed so as to prepare the catalyst for catalyticallypreparing tert-dodecanethiol. The preparation selectivity of the tert-dodecanethiol is 98% or above, and the catalysis reaction conditions are mild.

Description

technical field [0001] The invention belongs to the field of catalysts used for catalytic reactions of tert-dodecyl mercaptans; in particular, it relates to a catalyst for catalyzing the preparation of tertiary-dodecyl mercaptans and a preparation method thereof. Background technique [0002] Tertiary dodecyl mercaptan is mainly used in the polymerization reaction process of ABS resin, styrene-butadiene rubber, nitrile rubber, and high-impact polystyrene products, as a molecular weight regulator, and can also be used as a polyvinyl chloride, polyethylene, etc. Olefin stabilizers and antioxidants can also be used to synthesize certain drugs, non-ionic surfactants, lubricating oil additives, insecticides, fungicides, spices and other products. [0003] Tertiary dodecyl mercaptan is generally synthesized by addition reaction of mixed dodecene (tetrapolypropylene or trimeric isobutylene) and hydrogen sulfide. The main catalysts are: Lewis acid catalyst, zeolite molecular sieve,...

Claims

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Application Information

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IPC IPC(8): B01J31/26B01J27/125C07C319/04C07C321/04
CPCB01J31/26B01J27/125C07C319/04
Inventor 田勇韩大维李猛胡永玲曹龙海于振王文彬黎庆
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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