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Production method of antioxidizer 300

A production method and technology for antioxidants, applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfides, etc., can solve the problems of hydrogen chloride not being released, corroding equipment, etc., and achieve the effect of improving purity and reducing the difficulty of treatment.

Active Publication Date: 2019-04-19
淄博万科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The reaction between alkylphenol and sulfur chloride generates hydrogen chloride, and the generated hydrogen chloride gas is absorbed and treated with water, but there will be a lot of hydrogen chloride remaining in the reaction material that cannot be released, which will corrode the equipment in the subsequent process, and the residual hydrogen chloride needs to be removed Clean or neutralize with alkali

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The same device and steps as in Comparative Example 1, the difference is: change the petroleum ether to a saturated aliphatic hydrocarbon solvent oil with a boiling range of 130-140 ° C; Oil-water separation device, then add 100 ml of methanol to the reaction material, heat up, when the temperature slowly rises to 115±5°C, stop heating when there is no distilled liquid, and obtain 137 ml of azeotrope, including 112 ml of methanol phase; Cool to room temperature under stirring, drop 1 drop of ammonia water reagent, when the color of the material turns gray, test slightly alkaline with pH test paper; filter to obtain the crude product.

[0029] Compared with the amount of ammonia water added in Comparative Example 1, calculated by 1 drop of 0.05 milliliters, the amount of ammonia water added in Example 1 is reduced by 99.72%.

[0030] During the experiment, the amount of ammonia water added dropwise is usually between 1-5 drops, thus reducing the amount of hydrogen chlori...

Embodiment 2

[0032] The device and steps are the same as in Example 1, except that the petroleum ether is changed to a saturated aliphatic solvent oil with a boiling range of 130-140° C., methanol is changed to absolute ethanol, and the amount added is 50 milliliters. The temperature is raised to 115° C. and directly distilled out Alcohol-aliphatic hydrocarbon solvent oil azeotropic liquid 85 milliliters, wherein ethanol phase is 48 milliliters. After cooling to room temperature, drop 1 drop of ammonia water reagent, the color of the material solution changes, and the pH test paper test is slightly alkaline; compared with Example 1, the amount of ammonia water added is reduced by 99.72%.

Embodiment 3

[0034] The device and steps are the same as in Example 1, except that the petroleum ether is changed to a saturated aliphatic solvent oil with a boiling range of 130-140° C., methanol is replaced with isopropanol, and the addition amount is 50 milliliters, and the alcohol-aliphatic hydrocarbon solvent is directly distilled out Oil azeotropic liquid, stop heating when the temperature rises to 125°C, distill out the total amount of azeotrope 107.5 ml, the azeotrope has no phase separation, after the material is cooled to room temperature, drop 2 ml of ammonia water reagent, pH test paper to test slightly alkaline , this shows that residual alkyd is more in the material, but compared with comparative example 1, the quantity of ammoniacal liquor added reduces by 88.89%, this shows that after using isopropanol as a cosolvent, it greatly reduces the residual hydrogen chloride in the material Quantity works just as well.

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PUM

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Abstract

The invention relates to a production method of an antioxidizer 300 and belongs to the technical field of manufacturing of an alkylphenol sulfide antioxidizer. The production method comprises the following steps that 1, saturated aliphatic hydrocarbon solvent oil with high boiling range is used as a solvent, 6-tert-butyl-m-cresol and sulfur chloride conduct a sulpho reaction, and 4,4'-sulpho bis(6-tert-butyl-m-cresol) is generated; 2, after the sulpho reaction is completed, low-molecular-weight alcohol is added; 3, the temperature is increased, hydrogen chloride and alcohol are generated through evaporation and then cooled to the normal temperature, a weak base aqueous solution is added, the pH value of the material is adjusted to be neutral, and through filtering, a coarse product is obtained. The production method is scientific, reasonable, simple and easy to implement, the small amount of residual hydrogen chloride which needs to be neutralized is only produced in the production process, and the produced antioxidizer 300 coarse product has few impurities and is high in purity.

Description

technical field [0001] The invention relates to a production method of antioxidant 300, belonging to the technical field of alkylphenol sulfide antioxidant manufacture. Background technique [0002] The reaction between alkylphenol and sulfur chloride generates hydrogen chloride, and the generated hydrogen chloride gas is absorbed and treated with water, but there will be a lot of hydrogen chloride remaining in the reaction material that cannot be released, which will corrode the equipment in the subsequent process, and the residual hydrogen chloride needs to be removed Clean or neutralize with alkali. [0003] As stated in the invention patent CN1318401C: Judging from the current technology adopted by domestic manufacturers, it is generally used at 5 ° C to 15 ° C, sulfur dichloride and 5-methyl-2-tert-butylphenol The reaction was carried out in the medium of petroleum ether as a solvent to obtain the crude product of antioxidant 300, and then the fine product was obtained...

Claims

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Application Information

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IPC IPC(8): C07C319/14C07C321/30C07C319/28
CPCC07C319/14C07C319/28C07C321/30
Inventor 王文举朱永国黄东华张青郝仲华崔华松张胜传姜翠平邹文旭
Owner 淄博万科化工有限公司
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