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Method for preparing anti-aging agent 4010NA through modification-catalytic hydrogenation

A technology for catalytic hydrogenation and anti-aging agent, which is applied in the directions of reductive alkylation preparation, organic chemistry, and bulk chemical production, etc. The effect of polyalkyl reduction and alkylation side reactions, suppression of side reactions, and saving of operating costs

Inactive Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When RT base and acetone are used as raw materials to produce anti-aging agent 4010NA by catalytic hydrogenation with copper catalyst, the selectivity of the main reaction is low, and the product purity is low. 92% purity
In addition, the catalytic hydrogenation will significantly amplify side reactions, and acetone will be completely converted into isopropanol after the hydrogenation reaction
This not only increases the consumption of raw material acetone, but also reduces its concentration which affects the speed of the main reaction
The recovered isopropanol needs to be dehydrogenated again at high temperature to make acetone, which greatly increases the production cost

Method used

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  • Method for preparing anti-aging agent 4010NA through modification-catalytic hydrogenation
  • Method for preparing anti-aging agent 4010NA through modification-catalytic hydrogenation
  • Method for preparing anti-aging agent 4010NA through modification-catalytic hydrogenation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add RT base, acetone and [Bmim]BF to the ingredients tank 4 , stirred evenly to form a raw material solution, wherein the molar ratio of RT base to acetone is 1:5.5, acetone and [Bmim]BF 4 The volume ratio is 1000:2.5.

[0028] Install the granular C?207 copper-based catalyst in the fixed bed, pass in hydrogen, and adjust the pressure in the fixed bed to 4MPa, and then input acetone solvent at a speed of 50ml / hour. After the solvent is mixed with hydrogen, after pre- The heater then enters the fixed bed reactor. Slowly increase the temperature of the preheater and the fixed bed, and when the temperature reaches 180°C, keep it for several hours until the solvent fills the fixed bed reactor. At this temperature, the system pressure was adjusted to 2.0MPa, the material was replaced with raw material solution, the feed rate was adjusted to 20ml / hour, and the reducing solution after the catalytic hydrogenation reaction overflowed from the top of the fixed-bed reactor. Mov...

Embodiment 2

[0034] Concrete operation condition is the same as embodiment 1, just ionic liquid is made of [Bmim] BF 4 Change to [Bmim]BF 4 With [Bzmim] BF 4 Mixed solution (volume ratio 1:1), the copper-based catalyst was changed from C?207 to F04. The test results are shown in the comparison table 2.

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Abstract

The invention belongs to the technical field of organic synthesis and particularly relates to a method for preparing anti-aging agent 4010NA through modification-catalytic hydrogenation. The method is characterized by comprising following steps: (1) preparing a raw material solution with raw materials including 4-aminodiphenylamine, acetone and an ionic liquid; (2) filling a fixed bed reactor with a copper-based catalyst; and (3) feeding the raw material solution to the fixed bed reactor for preparing the high-purity anti-aging agent 4010NA through catalytic hydrogenation, wherein a ketone-alcohol ratio after the hydrogenation reaction is significantly increased. The method is simple in operation, is high in conversion rate, is good in selectivity and is high in yield. Side reactions, such as multi-alkyl reduction hydrocarbonylation and acetone hydrogenation with isopropanol generated, are significantly inhibited. The method is beneficial to industrial preparation of the high-purity anti-aging agent 4010NA and increase of the ketone-alcohol ratio after the hydrogenation reaction, can reduce consumption of acetone and significantly reduces a production cost.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically relates to a method for preparing high-purity antioxidant 4010NA through modification and catalytic hydrogenation. Background technique [0002] Rubber Anti-Aging Agent 4010NA is a general-purpose excellent anti-aging agent. It has excellent protection against ozone and flex cracks. It is suitable for natural rubber, styrene-butadiene rubber, butadiene rubber, neoprene, nitrile rubber and latex. Anti-aging agent 4010NA is the most outstanding and perfect representative so far. It has comprehensive protective effect, high anti-ozone and flex resistance, and has inhibitory effect on heat, oxygen, and harmful metals (such as copper, manganese, etc.), and is widely used. Used in tire treads and sidewalls, rubber hoses, cables, seals, etc. Because the toxicity, volatility, washing loss rate, solvent extraction resistance and skin irritation of antiaging agent 4010NA are gre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/55C07C209/26
CPCY02P20/54
Inventor 杨怀青黄伟管庆宝张帆张蓉蓉吴结华
Owner CHINA PETROLEUM & CHEM CORP
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