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Method for producing antioxygen 1076 through noncrystalline method

An antioxidant and non-crystalline technology, applied in the preparation of ester groups and hydroxyl groups, organic chemistry, etc., can solve the problems of high process requirements, long drying time, low solubility, etc., and achieve simple process, good color and high purity Effect

Active Publication Date: 2012-08-22
营口风光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low solubility of the antioxidant 1076 in the solvent, the solubility is low, so the amount of solvent required increases, and the amount of solvent recovered also increases, thereby greatly increasing energy consumption, and the use of a large amount of organic solvents is harmful to the environment. create pollution
In addition, because the melting point range of the antioxidant 1076 is between 49 and 54 °C, it is difficult to dry during the production process, the process requirements are high, the drying time is long, and the energy consumption is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Ingredients: methyl β(3,5-di-tert-butyl-4-hydroxyphenyl)propionate 53.9g

[0018] Octadecanol 45g

[0019] Sodium methoxide 0.45g

[0020] Glacial acetic acid 0.5g

[0021] 2) Chemicals: Add β(3,5-di-tert-butyl-4-hydroxyphenyl)methyl propionate, stearyl alcohol and sodium methoxide to the sealed reaction kettle successively, replace with nitrogen for 3 times, and evacuate to make Keep the vacuum at <-0.1Mpa and heat up the material. When the temperature rises to about 100°C, the material is completely melted and small bubbles appear; when the temperature rises to about 110°C, a large number of bubbles appear. Now turn on the stirring paddle, and the number of revolutions is controlled at 300 revolutions;

[0022] 3) Minimum protection: continue to heat up, and use 2 hours to evenly raise the temperature to about 165°C;

[0023] 4) High protection: contin...

Embodiment 2

[0029] Method is the same as Example 1, except that the ratio of ingredients is different.

[0030] Ingredients: methyl β(3,5-di-tert-butyl-4-hydroxyphenyl)propionate 50.6g

[0031] Octadecanol 40.6g

[0032] Zinc octanoate 0.32g

[0033] Glacial acetic acid 0.22g

[0034] Results: The main content of antioxidant 1076 was 99.3%, the melting point was 52.4°C, and the light transmittance was 98.4%. The yield was 99.1%. Products meet national standards.

Embodiment 3

[0036] The method is the same as in Example 1, except that the ratio of the ingredients is different

[0037] Ingredients: methyl β(3,5-di-tert-butyl-4-hydroxyphenyl)propionate 54.8g

[0038] Octadecanol 48.7g

[0039] Aluminum triisopropoxide 0.55g

[0040] Glacial acetic acid 0.76g

[0041] Results: The main content of antioxidant 1076 was 99.5%, the melting point was 53.7℃, and the light transmittance was 98.6%. The yield was 99.4%. Products meet national standards.

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Abstract

The invention relates to a method for producing an antioxygen 1076 through a noncrystalline method, comprising the following steps of: sequentially adding beta (3,5 di-tertiary-butyl 4-hydroxy phenyl) methyl propionate, octodecyl alcohol and a catalyst to a reaction kettle; displacing nitrogen, and vacuumizing; keeping at air pressure less than -0.1 MPa; heating to 110 DEG C; starting a stirring paddle, and controlling the number of turns to 300 turns / minute; uniformly heating for 2 hours to reach 165 DEG C; then uniformly heating for 2 hours to reach 180 DEG C; reducing the temperature to about 120 DEG C; adding glacial acetic acid in vacuum to carry out neutralization; regulating a pH value to 7; keeping the vacuum at 0.5-1 mmHg, and simultaneously heating to 195 DEG C; controlling the number of turns to about 700 turns / minute; depriving excess beta (3,5 di-tertiary-butyl 4-hydroxy phenyl) methyl propionate for about 2 hours; carrying out heat filtration on a product molten solution; and shifting to a constant-temperature sheeting device to carry out uniform dripping sheeting. The invention has the advantages of simplified process, short production period and high productivity.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for producing antioxidant 1076 by an amorphous method. Background technique [0002] Antioxidant 1076, the chemical name is β-(3,5 di-tert-butyl 4-hydroxyphenyl) octadecyl propionate. It is one of the excellent phenolic antioxidants with good compatibility, high antioxidant efficiency, no pollution, no coloring, low volatility, and water extraction resistance. It has a good effect of preventing discoloration caused by light and heat, and has good heat resistance and water extraction performance. Therefore, it is an antioxidant widely used in polyethylene, polypropylene, polystyrene, ABS resin, polyvinyl chloride, nylon, polyester, polyurethane, cellulose plastic and various rubbers. [0003] However, in the existing production methods, the crystallization method is mainly used. Due to the low solubility of the antioxidant 1076 in the solvent, the solubili...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/732C07C67/03
Inventor 王磊
Owner 营口风光新材料股份有限公司