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Method for synthesizing sulfurized isobutylene

A technology of sulfurized isobutylene and synthesis method, which is applied in the field of synthesis of sulfur olefins, can solve the problems of high production cost, high impurity content, and strong pungent odor, and achieve the effects of stable product quality, low activation reaction temperature, and reduced production cost

Inactive Publication Date: 2013-11-27
SHENYANG GUANGDA CHEM
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

Solved the problems of the existing T321 high-pressure synthesis method, such as strong pungent odor, high impurity content, and high production cost

Method used

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Experimental program
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Effect test

Embodiment 1

[0015] The content of the present invention will be described in detail below. The synthesis method of this sulfurized isobutylene comprises the following steps: at normal temperature, add 32 kg of elemental sulfur powder and an aqueous solution containing 31 kg of sodium sulfide into a reactor evacuated by inert gas (such as nitrogen, helium), and gradually heat up to make it Activate the reaction at 25~100°C to make the solution orange-red and transparent, that is, sodium sulfide and elemental sulfur completely react to form sodium polysulfide. Then, slowly feed isobutene into the reactor through a high-pressure metering pump, control the flow rate of isobutene, continue to raise the temperature and control the reaction temperature at 115~204°C, and the pressure at 1.0~6.9MPa. After the reaction, cool to room temperature and add After reacting for 8~10h, discharge the sulfurized isobutylene.

Embodiment 2

[0017] At normal temperature, add 32kg of elemental sulfur powder and 28kg of sodium sulfide aqueous solution into a reaction kettle evacuated by inert gas (such as nitrogen, helium), and gradually raise the temperature to activate the reaction at 45~90°C. The solution is orange-red transparent. Then, slowly feed 196kg of isobutene into the reactor through a high-pressure metering pump, control the flow rate of isobutene, continue to heat up and control the reaction temperature at 125~195°C, and the pressure at 2.2~5.5MPa. After the reaction, cool to room temperature, add After 10-12 hours of combined reaction, the sulfurized isobutylene is discharged.

Embodiment 3

[0019] At normal temperature, add 32kg of elemental sulfur powder and 32kg of sodium sulfide aqueous solution into a reaction kettle evacuated by inert gas (such as nitrogen, helium), and gradually raise the temperature to activate the reaction at 75~87°C. The solution is orange-red transparent. Then, slowly feed 84kg of isobutene into the reactor through a high-pressure metering pump, control the flow rate of isobutene, continue to heat up and control the reaction temperature at 130~180°C, and the pressure at 2.5~4.5MPa. After the reaction, cool to room temperature, add Discharge the sulfurized isobutylene after 1~3 hours of combined reaction.

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Abstract

The invention provides a method for synthesizing sulfurized isobutylene, for solving the problems of products prepared by the existing T321 high-pressure synthesis method, such as strong sharp aroma, high impurity content and high production cost. The method disclosed by the invention comprises the following steps of: adding elemental sulphur and sodium sulphide solution into a reaction kettle without oxidation treatment in the normal temperature state, gradually increasing the temperature, and carrying out activating reaction at temperature from normal temperature to 100 DEG C till the solution is of an orange red color and is transparent; and introducing isobutene into the reaction kettle, continuously increasing the temperature, controlling reaction temperature to be 100-204 DEG C, controlling pressure to be 1.0-6.9 MPa, and discharging sulfurized isobutylene after carrying out addition reaction for 1-16h, wherein the molar ratio of elemental sulphur to isobutene is 1.0:(0.5-3.5). The method for synthesizing sulfurized isobutylene disclosed by the invention has the advantages of high yield and product quality, low production cost, clean and odorless reaction process and the like.

Description

technical field [0001] The invention belongs to a synthesis method of sulfur olefins, specifically a synthesis method of sulfurized isobutylene, more specifically a high-purity T321 odorless high-pressure synthesis method. Background technique [0002] Sulfurized isobutylene extreme pressure antiwear agent, product code T321, this product has high sulfur content, good oil solubility in mineral oil, excellent extreme pressure activity and thermal stability. Due to the superior characteristics of T321, it is widely used by domestic and foreign manufacturers to prepare gear oils, metal processing oils, greases and anti-wear hydraulic oils that meet different specifications. However, because the reaction process produces a large amount of foul-smelling waste liquid and waste gas, which seriously pollutes the environment, production was once stopped abroad. [0003] The prior art mainly includes normal pressure and high pressure synthesis to produce sulfurized isobutylene, but n...

Claims

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Application Information

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IPC IPC(8): C07D341/00
Inventor 王宪法苗凤琴付志强付守法张铁华
Owner SHENYANG GUANGDA CHEM
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