A kind of anti-aging agent 4020 continuous production process

A production process and anti-aging agent technology, which is applied in the continuous production process of anti-aging agent 4020, can solve the problems of affecting catalyst life and single-pass output, catalyst activation is easy to deactivate over temperature, and the consumption of methyl isobutyl ketone is large, and it is easy to achieve Disassembly and assembly, good sealing performance and low cost

Inactive Publication Date: 2011-11-30
NANJING ENVIRO CHEM ENG DESIGN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The heating steam of the preheater E101 is 3.5MPa superheated steam, and the following problems often occur in the production process: (1) When the catalyst is activated in one pass (activation temperature ≤ 150°C), due to the relatively high steam pressure and temperature, SP101 controls It is difficult to achieve self-control, and the temperature of TRC/101 fluctuates greatly (±10°C), so it will easily cause over-temperature deactivation when the catalyst is activated, which also directly affects the life of the catalyst and the single-pass yield; (2) due to the steam pressure The fluctuation of TRC/101 is relatively large, which causes the relatively large fluctuation of TRC/101 temperature (±5°C), which directly affect

Method used

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  • A kind of anti-aging agent 4020 continuous production process
  • A kind of anti-aging agent 4020 continuous production process
  • A kind of anti-aging agent 4020 continuous production process

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Such as figure 1 As shown, the gas-liquid-solid three-phase fixed-bed hydrogenation reactor used in the continuous production process of anti-aging agent 4020 in this embodiment includes a main container, namely a cylinder, a discharge port, a clean port, a feed pre-distributor, The upper head, the lower head, the upper support, the lower support and the temperature measuring port. The main container is a cylinder with a height of 14.6m and a diameter of 1200mm. The feed pre-distributor is a pipe-type pre-distributor. , installed in the lower part of the reactor and surrounded by ceramic balls, the nozzle of the calandria pre-distributor faces downward, the upper head is an elliptical head, the lower head is an elliptical head, and the main container is There is a manhole at the bottom of the catalyst layer, which makes it more convenient to replace the catalyst. The main body of the reactor is made of stainless steel composite plate. This reactor is used for the produc...

Embodiment 2

[0025] The gas-liquid-solid three-phase fixed-bed hydrogenation reactor used in this example is the same as that in Example 1.

[0026] Such as figure 2 As shown, when 4020 is produced, the ratio of ketone to amine is 2:1, and the ratio of hydrogen to oil is 2000:1. The raw materials 4-aminodiphenylamine, hydrogen and methyl isobutyl ketone first enter the jacketed tube heated by heat transfer oil. The static mixer consists of a preheater E101 which is preheated to 150°C. After part of the raw materials are vaporized, they enter the static mixer H101, and then the materials enter the reactor R101 through the calandria predistributor. The liquid material fills the reactor, and hydrogen bubbles in the liquid material. Under the action of nickel catalyst, under the condition of reaction temperature of 165°C and pressure of 6MPa, it gradually reacts with the raw material, and the reacted material is discharged through the discharge port. The conversion rate can reach 95.1%.

Embodiment 3

[0028] The gas-liquid-solid three-phase fixed-bed hydrogenation reactor used in this example is the same as that in Example 1.

[0029] Such as figure 2 As shown, when 4020 is produced, the ratio of ketone to amine is 4:1, and the ratio of hydrogen to oil is 5000:1. The raw materials 4-aminodiphenylamine, hydrogen and methyl isobutyl ketone first enter the jacketed tube heated by heat transfer oil. The static mixer consists of a preheater E101 which is preheated to 220°C. After part of the raw materials are vaporized, they enter the static mixer H101, and then the materials enter the reactor R101 through the calandria predistributor. The liquid material fills the reactor, and hydrogen bubbles in the liquid material. Under the action of the nickel catalyst, the reaction temperature is 230 ° C and the pressure is 5.8 MPa, and the raw material is gradually reacted. The reacted material is discharged through the discharge port. The reaction conversion rate can reach 97%.

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Abstract

The invention discloses a continuous producing process of an anti-aging agent 4020, which has the advantages of stability and reliability in operation and high production efficiency. The process comprises the following steps of: adopting 4-aminodiphenylamine, methyl isobutyl ketone and hydrogen as raw materials; mutually preheating all raw materials by a preheater E101; enabling the preheated rawmaterials to enter a reactor; and carrying out catalytic hydrogenation reaction on the raw materials at a high pressure under the effect of a catalyst so as to obtain the anti-aging agent 4020, wherein the reactor is a gas-liquid-solid three-phase fixed bed hydrogenation reactor; the hydrogenation reaction is continuous operation carried out by using the gas-liquid-solid three-phase fixed bed hydrogenation reactor; the gas-liquid-solid three-phase fixed bed hydrogenation reactor comprises a main body container, a discharging opening, a completely discharging opening, a feed pre-distributor, an upper seal head, a lower seal head, an upper support, a lower support and a temperature measuring opening, wherein the feed pre-distributor is an exhaust pipe type pre-distributor which is mounted at the lower part of the main body container; the upper seal head is an elliptical seal head; and the lower seal head is also an elliptical seal head; and the temperature is 165-230 DEG C, the pressureis 5.5-6.0 MPa, the keto-amine ratio is 2-4:1 and the hydrogen-oil ratio is 2000-5000:1 during reaction.

Description

technical field [0001] The present invention relates to a production process of anti-aging agent, more specifically relates to a continuous production process of anti-aging agent 4020. Background technique [0002] Anti-aging agent is an important part of rubber additives, which plays an irreplaceable role in the anti-ozone, anti-oxidation, heat resistance and flex resistance of rubber. Among the many products in the p-phenylenediamine series, antioxidants 4010NA and 4020 are widely used all over the world. Antiaging agent 4020 [N-(1,3-dimethylbutyl)-N'-phenylenediamine] belongs to p-phenylenediamine antiaging agent with comprehensive protection effect, especially good durability, and is the current antiaging agent It is widely used in rubber products such as tires and cables. The existing synthesis process is generally prepared by catalytic hydrogenation condensation of 4-aminodiphenylamine and methyl isobutyl ketone under high pressure. The fixed-bed hydrogenation react...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/68B01J8/02C08K5/18
Inventor 吴员鸿唐文麒吴翔
Owner NANJING ENVIRO CHEM ENG DESIGN
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