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Preparation method of anti-aging agent 264

An anti-aging agent and crystallization technology, which is applied in the field of preparation of anti-aging agent 264, can solve the problems of increasing tar discharge, high energy consumption, and low single-pass yield, and achieves less dangerous waste liquid, small equipment investment, and single-pass yield high effect

Inactive Publication Date: 2018-01-19
郑程
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The rectification of this method needs to consume organic solvents, and about 25% of the anti-aging agent 264 is dissolved in the mother liquor, and the high temperature in the rectification process will produce polymers, which will increase the amount of tar discharge. The problem of low efficiency and high energy consumption
If the organic solvent in the laboratory is used for recrystallization, the yield per pass is lower and the recovery of solvent becomes larger

Method used

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  • Preparation method of anti-aging agent 264
  • Preparation method of anti-aging agent 264

Examples

Experimental program
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Effect test

preparation example Construction

[0011] The preparation method that the present invention adopts sees figure 2 . The specific process is as follows:

[0012] First put p-cresol and concentrated sulfuric acid into the alkylation reaction kettle and pass through isobutylene to carry out the alkylation reaction. Neutralize with sodium hydroxide after the alkylation reaction. Then wash with water in the alkylation reaction kettle, and separate the water layer to obtain the anti-aging agent 264 mother liquor. Add soft water to the anti-aging agent 264 mother liquor to carry out water crystallization and separate the crude product. The crude product is then crystallized, centrifuged, filtered, and dried to obtain antiaging agent 264.

[0013] Among them, the operating conditions of water crystallization: the amount of soft water added is 0.85-2.5 of the volume of the anti-aging agent 264 mother liquor, the crystallization temperature is 40-80 ° C, the stirring speed is 30-50 rpm, the upper layer after standing...

Embodiment 1

[0016] First put 100Kg of p-cresol and 0.3Kg of concentrated sulfuric acid into the alkylation reactor and feed 120Kg of isobutylene to carry out the alkylation reaction. After the alkylation reaction, neutralize with sodium hydroxide to pH=7. Then wash with water in the alkylation reaction kettle, and separate the water layer to obtain the anti-aging agent 264 mother liquor. Add soft water to the anti-aging agent 264 mother liquor to carry out water crystallization and separate the crude product. The crude product is then crystallized, centrifuged, filtered, and dried to obtain antiaging agent 264.

[0017] Among them, the operating conditions for water crystallization: the amount of soft water added is 0.85 of the volume of the anti-aging agent 264 mother liquor, the crystallization temperature is 40-80 ° C, the stirring speed is (30-50) rpm, the upper layer after standing and stratifying is the oil phase, and the oil phase is used Extraction and concentrated treatment, th...

Embodiment 2

[0020] First put 100Kg of p-cresol and 0.3Kg of concentrated sulfuric acid into the alkylation reactor and feed 120Kg of isobutylene to carry out the alkylation reaction. After the alkylation reaction, neutralize with sodium hydroxide to pH=7. Then wash with water in the alkylation reaction kettle, and separate the water layer to obtain the anti-aging agent 264 mother liquor. Add soft water to the anti-aging agent 264 mother liquor to carry out water crystallization and separate the crude product. The crude product is then crystallized, centrifuged, filtered, and dried to obtain antiaging agent 264.

[0021] Among them, the operating conditions for water crystallization: the amount of soft water added is 1.5 of the volume of the anti-aging agent 264 mother liquor, the crystallization temperature is 40-80°C, the stirring speed is (30-50) rpm, the upper layer after standing and stratifying is the oil phase, and vacuum Extraction and concentrated treatment, the lower layer is t...

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Abstract

The invention discloses a preparation method of an anti-aging agent 264. Isobutene, p-cresol and concentrated sulfuric acid are subjected to alkylation reaction; then, sodium hydroxide is used for neutralization; next, soft water is added for product crude separation; a solvent is used for crystallization; centrifugation, filtering and drying are performed. The preparation method is characterizedin that the product crude separation adopts water crystallization. For the product crude separation, an organic solvent is not used during the product crude separation; the water is used and can be repeatedly used; the anti-aging agent 264 is not dissolved in water, so that the once through yield is high; the rectification is not needed, so that high temperature is not needed; the energy consumption is low; the equipment investment is low; the dangerous waste liquid is little.

Description

technical field [0001] The present invention relates to the field of anti-aging agent preparation, in particular, to a preparation method of anti-aging agent 264. Background technique [0002] Anti-aging agent 264 is an important general-purpose phenolic anti-aging agent, which is widely used in various fields. It is a general-purpose phenolic anti-aging agent for rubber, which has a certain protective effect on heat and oxygen aging, and can also inhibit copper damage. It has anti-ozone ability together with anti-ozone base and wax, and can also be used as a stabilizer for post-treatment and storage of synthetic rubber. Anti-aging agent 264 is also an effective anti-aging agent for polymer materials, widely used in polyethylene, polypropylene, polyvinyl ether, polystyrene and its copolymers, celluloid plastics, etc. Antioxidant 264 is an excellent antioxidant additive for various petroleum products. It has good oil solubility and does not affect the color of oil products ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/14C07C37/84
Inventor 郑程
Owner 郑程
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