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Method for efficiently preparing lubricant additive T321 in pollution-free manner by employing medium-pressure solvothermal method

A technology of lubricating oil additives and solvothermal method, which is applied in the field of organic sulfide synthesis, can solve the problems of high equipment requirements, serious environmental pollution, and difficulty in control, and achieve the effects of reducing pollution, reducing production costs, and less pollution

Inactive Publication Date: 2014-03-05
ANHUI UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main disadvantage is that the pollution is serious and difficult to control
There are a lot of dark-colored and foul-smelling sodium sulfide and sodium polysulfide in the wastewater, and there is a lot of hydrogen sulfide gas in the waste gas, which seriously pollutes the environment; in addition, the reaction is carried out under high pressure (generally greater than 10MPa), and the equipment requirements higher

Method used

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  • Method for efficiently preparing lubricant additive T321 in pollution-free manner by employing medium-pressure solvothermal method
  • Method for efficiently preparing lubricant additive T321 in pollution-free manner by employing medium-pressure solvothermal method
  • Method for efficiently preparing lubricant additive T321 in pollution-free manner by employing medium-pressure solvothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The ratio of sulfur to ene is 2:1. Add 9.71Kg of elemental sulfur into the reactor, 18Kg of solvent with a mass fraction of 5% ammonia water and an alcohol ratio of 9:1, raise the temperature to 200°C, add 8.5Kg of isobutylene intermittently, and keep the pressure at 3.5-4.5MPa After the addition, the reaction was continued for 6 hours, and then cooled to 60°C, and the mixture was pressed out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed and distilled to obtain the lubricating oil additive T321 product with a yield of 90%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling. The product obtained in this embodiment is analyzed to obtain an infrared spectrogram ( figure 1 ), the gas chromatogram ( figure 2 ).

[0027] Synthetic lubricating oil additive T321 specification...

Embodiment 2

[0030] Sulfurene ratio 1.5:1. Add 7.29Kg of elemental sulfur into the reactor, 18Kg of solvent with a mass fraction of 10% ammonia water and alcohol in a ratio of 9:1, raise the temperature to 180°C, add 8.5Kg of isobutylene intermittently, and keep the pressure at 3.5-4.5MPa After the addition, the reaction was continued for 5 hours, and then cooled to 60°C, and the mixture was pressed out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed and distilled to obtain the lubricating oil additive T321 product with a yield of 88%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling.

[0031] Synthetic lubricating oil additive T321 specification parameters are as follows:

[0032]

Embodiment 3

[0034] Sulfurene ratio 1.5:1. Add 7.29Kg of elemental sulfur into the reactor, 18Kg of solvent with a mass fraction of 10% ammonia water and alcohol in a ratio of 9:1, raise the temperature to 200°C, add 8.5Kg of isobutylene intermittently, and keep the pressure at 3.5-4.5MPa After the addition, the reaction was continued for 4 hours, and then cooled to 60°C, and the mixture was pressed out of the reaction vessel using residual pressure. The mixture was allowed to stand for liquid separation, and the organic phase was filtered, washed and distilled to obtain the lubricating oil additive T321 product with a yield of 85%. After analyzing the ammonia concentration of the inorganic phase, add fresh ammonia water to make it reach the original concentration before recycling.

[0035]

[0036]

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Abstract

The invention discloses a method for efficiently preparing a lubricant additive T321 in a pollution-free manner by employing a medium-pressure solvothermal method and belongs to the technical field of synthesis of an organic sulfide of an acyclic unsaturated carbon frame. The synthesis method comprises the following steps: adding elemental sulfur and solvents to a reaction kettle; heating to 160-200 DEG C, and after agitating and reacting for 0.5 hours, intermittently adding isobutene into the reaction kettle; controlling the pressure at 3.5-4.5MPa all the time, continuing to react for 3-6 hours, cooling to 60 DEG C; pressing a reaction mixture out of the reaction kettle by using overbottom pressure; standing and skimming the product, filtering, washing and distilling an organic phase, so as to obtain the lubricant additive T321; after analyzing an inorganic phase, supplying a fresh solvent until the original concentration is reached so that the solvent can be reused, wherein the solvents are ammonia solutions with different concentrations. Thus, the method has the advantages of being green and environment-friendly, low in cost, high in product yield, low in demands on equipment and the like and solves the problem in the prior art.

Description

technical field [0001] The invention belongs to the technical field of organic sulfide synthesis of acyclic unsaturated carbon frame, and in particular relates to a green and efficient method for preparing lubricating oil additive T321 by a medium-pressure solvothermal method. Background technique [0002] Lubricating oil additive T321 is an excellent extreme pressure and anti-wear additive for lubricating grease. Because of its high sulfur content, it has strong extreme pressure and anti-wear properties, good oil solubility, low copper corrosion, low toxicity, light color, and dosage In particular, adjusting the sulfur index of the vulcanizing agent in production can produce vulcanized isobutylene (ie T321) products with different sulfur content and different activities, so it is widely used in gear oils, metal processing oils and lubricating greases. The mainstream product of sulfur agent in extreme pressure antiwear agent. [0003] In the traditional production process o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D341/00
CPCC07D341/00
Inventor 牛和林潘文胜吴绪虎李平
Owner ANHUI UNIVERSITY
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