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A kind of synthetic method of di-tert-butyl terminated chain polysulfide

A technology of di-tert-butyl encapsulation and synthesis method, which is applied in the field of preparation of organic sulfides, and can solve problems such as low conversion rate of isobutylene and product yield, low activity of alumina, difficulty in recycling catalysts, etc.

Inactive Publication Date: 2016-03-30
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Lubrizol Company of the United States uses n-propylamine or triethylamine as a catalyst to catalyze the reaction of sulfur, isobutylene and hydrogen sulfide to prepare chain di-tert-butyl polysulfide (US4119549, US4119550, US4191659, US4344854), and the catalyst is difficult to recycle.
Ethyl Company of the United States uses alumina as a catalyst to catalyze the reaction of sulfur, isobutylene and hydrogen sulfide to prepare chain di-tert-butyl polysulfide (EP0554011, US5250737). The disadvantage is that the activity of alumina is low, and the conversion rate of isobutene and product yield are low.

Method used

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  • A kind of synthetic method of di-tert-butyl terminated chain polysulfide
  • A kind of synthetic method of di-tert-butyl terminated chain polysulfide
  • A kind of synthetic method of di-tert-butyl terminated chain polysulfide

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Experimental program
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Effect test

Embodiment 1

[0030] Add 367.0g (11.44mol) of sulfur into a 2.5-liter reactor, add 0.734g of NH 2 - MIL-53(Al) catalyst (0.2% by mass based on sulfur), followed by a reinforced seal. Purge 3 times with 2.0MPa high-purity nitrogen, and finally release to normal pressure. Feed H into the above reaction kettle 2 S (129.8g, 3.81mol), heat up and control the temperature to 140oC, start stirring (rotating speed is about 320rpm). Start the metering pump, inject isobutene (427.6g, 7.62mol), adjust the flow rate of the metering pump so that the injection time of isobutene is 1h, and continue to react for 1h after the injection of isobutene is completed. Keep this temperature constant, release the pressure in the kettle and purging with nitrogen for 0.5h, and cool the tail gas with a primary condenser (ice water bath) and a secondary condenser (dry ice acetone bath) to recover by-products tert-butyl mercaptan and di-tert-butyl mono Sulfur ether, the cooled tail gas uses a fixed bed desulfurizer to...

Embodiment 2

[0032] Add 555.84g (17.37mol) of sulfur into a 2.5-liter reactor, add 0.556g of NH 2 -MIL-101(Al) catalysis

[0033]

[0034] When the mol ratio of hydrogen sulfide, sulfur and isobutylene was 1:3:2, the average chain length of the product was 4, and tetrasulfide was the main product in the product. When the mol ratio of hydrogen sulfide, sulfur and isobutylene was 1:2: When 2, the average chain length of the product is 3, and trisulfide is the main product in the product.

[0035] Although isobutene can be 100% converted, the by-products tert-butyl mercaptan and di-tert-butyl monosulfide are inevitably generated. Nitrogen stripping is carried out at 100 ° C, and the tail gas is passed through a primary condenser (ice-water bath) and a secondary The condenser (dry ice acetone bath) cools and recovers the by-products tert-butyl mercaptan and di-tert-butyl monosulfide, which can continue to react with sulfur to form chain di-tert-butyl polysulfide. The reaction formula is as...

Embodiment 3

[0039] Add 243.8g (7.62mol) of sulfur into a 2.5-liter reactor, add 0.975g of NH 2 - MIL-101 (Al) catalyst (0.4% by mass based on sulfur), followed by a reinforced seal. Purge 3 times with 2.0MPa high-purity nitrogen, and finally release to normal pressure. Feed H into the above reaction kettle 2 S (129.8g, 3.81mol), heat up and control the temperature at 150oC, and start stirring (rotation speed is about 320rpm). Start the metering pump, inject isobutene (427.6g, 7.62mol), adjust the flow rate of the metering pump so that the injection time of isobutene is 1h, and continue to react for 1h after the injection of isobutene is completed. Keep this temperature constant, release the pressure in the kettle and purging with nitrogen for 0.5h, and cool the tail gas with a primary condenser (ice water bath) and a secondary condenser (dry ice acetone bath) to recover by-products tert-butyl mercaptan and di-tert-butyl mono Sulfur ether, the cooled tail gas uses a fixed bed desulfuriz...

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Abstract

The invention provides a method for synthesizing a di-tert-butyl-terminated chain polysulfide, which is characterized in that it comprises the following steps: putting elemental sulfur and a catalyst (a metal-organic framework microporous material based on an amino group) into a reaction kettle , Use nitrogen to replace the air in the reactor, then inject hydrogen sulfide, stir and heat up to 120-160°C, slowly inject isobutylene into the reactor, after the addition, the reaction pressure is 4-7MPa, react for 2-6 hours, and then cool the reaction product to 100°C , purging with nitrogen, the low boiling point by-products tert-butyl mercaptan and di-tert-butyl monosulfide are recovered after condensation and can be reused as raw materials, and the product is cooled to room temperature and filtered to obtain di-tert-butyl-terminated chain polysulfide Ether products, the filtered catalyst is reused. The synthesis method provided by the invention has the advantages of high yield, reusable catalyst, close to 100% reaction atom economy, zero pollution and zero discharge, and belongs to the environment-friendly synthesis method.

Description

technical field [0001] The present invention belongs to the preparation method of organic sulfide, specifically, the present invention is a kind of synthetic method of preparing di-tert-butyl terminated chain polysulfide. Background technique [0002] Di-tert-butyl-terminated chain polysulfides have a wide range of uses, and their chemical composition is a mixture. When the average sulfur chain length is 3, it can be used as extreme pressure and antiwear agent for lubricating oil. It is characterized by high sulfur content (46wt%), strong extreme pressure and antiwear performance, good oil solubility, and low corrosion to non-ferrous metal copper. , widely used in the preparation of vehicle gear oil, industrial gear oil, but also for anti-wear hydraulic oil, extreme pressure grease. When the chain length of flat sulfur is 4, it can be used as a vulcanizing agent for pre-sulfurization of hydrogenation catalysts. It is characterized by high flash point (closed at 100°C), low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C321/14C07C319/24B01J31/22
Inventor 姜恒刘鹏宇李飞赵杉林李萍宫红张凤华
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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