Pretreating process for preparing copper base catalyst of p-phenylenediamine anti-aging agent

A copper-based catalyst, p-phenylenediamine technology, applied in catalyst activation/preparation, physical/chemical process catalyst, reductive alkylation preparation, etc., to shorten the preliminary process, reduce the failure rate, and improve the production level.

Active Publication Date: 2010-06-16
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Activation pretreatment is an important factor affecting catalyst activity. How to activate and pretreat copper-based catalysts used in the preparation of p-phenylenediamine antioxidants has not been systematically studied.
And there is no relevant report on the activation pretreatment of this kind of catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a continuous tubular reactor with a volume of 100 milliliters, a copper-based catalyst weighing 150 grams, including 38.93% by weight of CuO, 40.84% ​​of ZnO, and 10.49% of Al 2 o 3 . Feed inert gas nitrogen into the reactor to fill the reactor with nitrogen and keep the pressure at 2.5 MPa, and control the flow of nitrogen by controlling the tail discharge device to form a gas flow, maintain the gas-liquid ratio, and promote gas-liquid mass transfer. Start the heating program to heat the reactor, the heating rate is 10° C. / hr, and the copper-based catalyst enters the heating dehydration step. Slowly raise the temperature when it is close to 100°C, and maintain it in the temperature range of 100-120°C for about 5 hours to remove the physical water in the copper-based catalyst as much as possible. When the temperature rises to 120-125°C, a small amount of hydrogen is introduced. At this time, the temperature of the reactor will rise and the reaction will be exotherm...

Embodiment 2

[0028] In a continuous tubular reactor with a volume of 100 milliliters, 150 grams of the same copper-based catalyst as in Example 1 were charged. Feed inert gas nitrogen into the reactor to fill the reactor with nitrogen and keep the pressure at 2.5 MPa, and control the flow of nitrogen by controlling the tail discharge device to form a gas flow, maintain the gas-liquid ratio, and promote gas-liquid mass transfer. Start the heating program to heat the reactor, the heating rate is 10° C. / hr, and the copper-based catalyst enters the heating dehydration step. Slowly raise the temperature when it is close to 100°C, and maintain it in the range of 100-120°C for about 5 hours to remove the physical water in the copper-based catalyst as much as possible. When the temperature rises to 120-125°C, a small amount of hydrogen is introduced. At this time, the temperature of the reactor will rise and the reaction will be exothermic. At this time, adjust the temperature control to avoid the...

Embodiment 3

[0030] In the reactor for producing p-phenylenediamine anti-aging agent 4020, 8 tons of the same copper-based catalysts as in Example 1 were loaded into the reactor. Nitrogen is replaced so that the entire reactor is filled with nitrogen, the pressure is maintained at 2.5 MPa, and the gas cycler is started. Raise the temperature at a rate of 10-15°C / hr, and stabilize it for 4-6 hours when the temperature rises to 110°C, and remove the water inside the copper-based catalyst. Pass hydrogen into the reactor. At this time, the temperature of the copper-based catalyst gradually rises. Control the temperature of the copper-based catalyst bed, and pay attention to the system pressure and temperature at all times to prevent the copper-based catalyst bed from overheating. The initial flow rate of hydrogen accounts for 0.5% by volume of the total gas flow rate. As the hydrogenation reduction reaction of the copper-based catalyst proceeds, the concentration of hydrogen gas is gradually i...

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PUM

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Abstract

The invention provides a pretreating process for preparing a copper base catalyst of a p-phenylenediamine anti-aging agent. Before use, the main active component copper of the copper base catalyst exists in an oxide form. The process comprises the following steps: (1) heating and dewatering step: heating a copper base catalyst bed to remove the water content contained in the copper base catalyst; (2) hydrogenation reducing step: introducing hydrogen to the copper base catalyst after dewatering to reduce the copper base catalyst and obtain the activated copper base catalyst, wherein, water generated in reaction is carried over; and (3) passivating treatment step: passivating the activated copper base catalyst so that the activity and selectivity thereof are suitable for N-alkylation reaction. The pretreating process of the invention can enable the copper base catalyst to reach the activity and selectivity required by reaction in a short time, shorten the pretreating time of the copper base catalyst, reduce the reject ratio of the p-phenylenediamine anti-aging agent products, and even eliminate rejected products.

Description

technical field [0001] The invention relates to a catalyst pretreatment process, in particular to a copper-based catalyst pretreatment process for preparing p-phenylenediamine antioxidants. Background technique [0002] P-phenylenediamine antioxidant is a kind of rubber antioxidant with excellent performance. It is the most widely used general-purpose antioxidant in the tire rubber industry. It is widely used in tires, tapes and many other industrial rubber products. P-phenylenediamine anti-aging agent has a protective effect on the damage of thermal oxygen, cracking and flexing aging, and it is also a stabilizer for synthetic rubber such as styrene-butadiene rubber and isoprene rubber. The production of p-phenylenediamine anti-aging agents is huge in the world, and the main types of p-phenylenediamine anti-aging agents include N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine (anti-aging Agent 4020), N-isopropyl-N'-phenyl-p-phenylenediamine (antiaging agent 4010NA), N-sec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/00B01J37/18B01J37/08C07C209/26C07C211/55
Inventor 王志刚
Owner JIANGSU SINORGCHEM TECH CO LTD
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