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Method for preparing sulfurized isobutylene by combining hydrogen sulfide tail gas in sulfur-phosphoric acid production

A technology for sulfided isobutylene and hydrogen sulfide, applied in hydrogen sulfide, chemical instruments and methods, sulfur compounds, etc., can solve the problems of light color, low odor, and poor economic benefits of hydrogen sulfide gas.

Pending Publication Date: 2021-09-14
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] In view of the above problems, the present invention provides a method for preparing isobutylene sulfide from hydrogen sulfide tail gas combined with phosphoric acid sulfuric acid, aiming at the problem that the hydrogen sulfide gas in the existing phosphoric acid sulfuric acid production process has poor economic benefits and is not fully utilized, without affecting sulfur In the case of phosphoric acid production, after purification of hydrogen sulfide gas, ammonia water is used to realize the safe recovery of hydrogen sulfide, and high-vacuum falling-film heating distillation separation technology is used to treat the isobutylene sulfide produced by the reaction of mother liquor and isobutylene under the condition of not exceeding 140°C Higher content of trisulfide in the obtained sulfurized isobutylene, and the recycling of the mother liquor can be realized, greatly reducing the generation of waste water, and the conversion rate of the process can reach more than 99%, the comprehensive yield can reach more than 96%, and the production efficiency High, avoiding the formation of thioketones, the product has light color, low odor, and the extreme pressure performance and copper corrosion level of the product have good performance

Method used

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  • Method for preparing sulfurized isobutylene by combining hydrogen sulfide tail gas in sulfur-phosphoric acid production
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  • Method for preparing sulfurized isobutylene by combining hydrogen sulfide tail gas in sulfur-phosphoric acid production

Examples

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Effect test

Embodiment 1

[0073] In 200L stainless steel atmospheric pressure kettle, drop into 37.5Kg flake sulfur, ammoniacal liquor (mass content 24%) 100Kg, while stirring, use gas mass flowmeter to measure the input amount of hydrogen sulfide, until the hydrogen sulfide of feeding 9.5Kg, Stirring was continued for 1 h to obtain a clear mother liquor.

[0074] Take the above mother liquor, inject it into a 250L autoclave purged with nitrogen, close the autoclave, raise the temperature to 130°C, feed 52Kg of isobutene within 1 hour, keep the reaction temperature at 130°C, and the maximum pressure in the autoclave is 4.3Mpa. After adding isobutene, the reaction was continued for 2 hours, and then the temperature was naturally lowered to 30°C. Subsequently, open the vent of the autoclave, and release the liquid containing the crude product after there is no pressure in the autoclave. The total weight of the liquid is 197Kg. Get the organic phase (heavy 92.7Kg) in the above liquid, and the water phas...

Embodiment 2

[0080] Drop into 34.9Kg flake sulfur in 200L stainless steel atmospheric pressure kettle, the mother liquor 104.3Kg of ammoniacal liquor (mass content 24%) 6.25Kg and reclaim, while stirring, feed the hydrogen sulfide of 8.15Kg (measurement mode is with embodiment 1) , and continued to stir for 1h to obtain a clear mother liquor.

[0081] Take the above mother liquor and 22.25Kg of recovered light and heavy fractions, inject them into a 250L autoclave after purging with nitrogen, close the body of the autoclave, raise the temperature to 135°C, feed 40Kg of isobutylene within 1 hour, raise the temperature to 145°C and moisturize the reaction. The highest pressure is 3.9Mpa. After adding isobutene, the reaction was continued for 3 hours, then the heating was stopped, and cooling heat transfer oil was introduced into the coil until the temperature in the kettle reached 30°C. Subsequently, open the vent of the autoclave, and release the liquid containing the crude product after t...

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Abstract

The invention discloses a method for preparing sulfurized isobutylene by combining hydrogen sulfide tail gas in sulfur-phosphoric acid production . The method comprises the following steps: purifying the hydrogen sulfide tail gas; introducing hydrogen sulfide gas into a reaction container added with concentrated ammonia water and sulfur sulfur is completely dissolved to serve as mother liquor, and wherein the molar ratio of ammonia to sulfur to hydrogen sulfide is 1: (0.8-1.2): (0.15-0.30); injecting isobutene into the mother liquor at the temperature of 120-140 DEG C, and carrying out reaction for 1-5 hours at the temperature of 120-190 DEG C, wherein the molar ratio of isobutene to hydrogen sulfide is 1: 0.3 to 1: 0.48; after the reaction is finished, cooling to not higher than 30 DEG C, separating liquid, taking an oil phase part, and washing with water; and carrying out high vacuum falling film heating distillation separation on the washed oil phase part, and collecting a fraction at 120-140 DEG C to obtain the product. According to the technical scheme, safe recovery of hydrogen sulfide is achieved, much less wastewater is generated, the process conversion rate and the comprehensive yield are high, the production efficiency is high, the product character and performance are high, and the technological process is simple.

Description

technical field [0001] The invention relates to the technical field of lubricating oil additives, in particular to a method for preparing sulfurized isobutylene by combining sulfuric acid to produce hydrogen sulfide tail gas. Background technique [0002] Sulfurized isobutylene is an extreme pressure and antiwear additive for lubricating oils. It is widely used in gear oils, metalworking oils and greases due to its high sulfur content, extreme pressure and antiwear properties, and good oil solubility. The industrial production process of sulfurized isobutylene mainly includes two-step method and one-step method. The traditional two-step synthesis process uses isobutylene, sulfur monochloride, sulfur, alkali metal or alkaline earth metal sulfide as the main raw materials, undergoes addition reaction and sodium sulfide dechlorination reaction, and finally undergoes alkali refining to obtain a sulfur content of 42 % to 45% of sulfurized isobutylene products, there are problems...

Claims

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Application Information

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IPC IPC(8): C07D341/00C01B17/16
CPCC07D341/00C01B17/168
Inventor 王庆超袁小二徐坤范金凤
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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