Modified condensation reduction alkylation catalyst

A catalyst and alkylation technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, amino compound preparation, etc., can solve the problems of high raw material consumption, easy pulverization, waste of raw materials, etc. , to achieve the effects of good anti-powdering ability, side reaction suppression and long service life

Inactive Publication Date: 2012-01-18
郝云青
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Due to the existence of the side reaction of hydrogenation of ketones to alcohols, it not only consumes a large amount of raw material ketones and hydrogen, resulting in waste of raw materials, but also due to the mechanism of the reaction, the side reaction makes the ketone molecules on the surface of the catalyst insufficient, resulting in the formation of ketones The amine condensation intermediate product is difficult, so the content of the main product after hydrogenation cannot be increased, and there are impurities produced by other side reactions at the same time, which brings difficulties to product separation and causes many unqualified products to be produced in the early stage of catalyst use.
[0011] U.S. Patents US3366684, US4043942, etc. have done a lot of work on improving the selectivity of the main reaction and suppressing the side reactions of hydrogenation of ketones, but because of the use of noble metal catalysts, there are still problems with expensive catalysts, high raw material consumption, and large amounts of post-treatment materials. , the disadvantage of troublesome recovery of excess ketone
[0012] The copper-based catalyst described in Chinese patent CN CN200610161327.2 currently has problems such as easy pulverization, serious side reactions of ketone hydrogenation, and long cycle time for qualified products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Dissolve 250g of copper nitrate and 300g of zinc nitrate in 1L of water, heat to 50°C, dissolve 400g of sodium carbonate in 3L of water, and heat to 70°C, then slowly add sodium carbonate dropwise to the copper nitrate and zinc nitrate In the mixed solution, stir rapidly at the same time until pH = 7.5. Continue to stir at 70°C for 1 hour, then add 30g of silicon dioxide powder, stir for another 1 hour, then filter and wash, and dry the solid material at 120°C for 6 hours. Roast at 300°C for 2 hours, then add 2% graphite and 4% water to mix evenly, and press it into a tablet of Ф5×(4.5-5.5) mm with a tablet machine, so that the molar ratio of copper to zinc of the catalyst is 0.94 ; The molar ratio of copper to silicon is 2.1.

Embodiment 2

[0029] Example 2: Dissolve 500g of copper nitrate and 25g of zinc nitrate in 1L of water, heat to 50°C, dissolve 550g of sodium bicarbonate in 3L of water, and heat to 70°C, then slowly add the sodium bicarbonate solution dropwise to the copper nitrate and In the mixed solution of zinc nitrate, stir rapidly at the same time until the pH=7.5. Continue to stir at 70°C for 1 hour, then add 150g of silica powder, stir for another 1 hour, then filter and wash, and dry the solid material at 120°C 6 hours, roasted at 300°C for 2 hours, then add 2% graphite and 4% water to mix evenly, and press it into a tablet of Ф5×(4.5-5.5) mm with a tablet machine, and the catalyst copper zinc prepared in this way The molar ratio is 22.4; the copper-silicon molar ratio is 0.83.

Embodiment 3

[0030] Example 3: Dissolve 200g copper nitrate and 350g zinc nitrate in 1L water, heat to 50°C, dissolve 400g sodium carbonate in 3L water, and heat to 70°C, then slowly add the sodium carbonate solution dropwise to copper nitrate and zinc nitrate Stir rapidly at the same time until pH = 7.5. Continue to stir at 70°C for 1 hour, then add 5.6g of silicon dioxide powder, stir for another 1 hour, then filter and wash, and dry the solid material at 120°C for 6 hour, roasting at 300°C for 2 hours, then add graphite and 2% water to mix evenly, and press it into a tablet of Ф5×(4.5-5.5) mm with a tablet machine, so that the catalyst copper-zinc molar ratio is 0.64; The molar ratio of copper to silicon is 8.9.

[0031] The performance comparison of embodiment catalyst and comparative example catalyst:

[0032] Evaluation method: The laboratory device completely simulates the large-scale industrial production device. The reactor is a Ф32 stainless steel tube with a length of 2m, and 2...

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Abstract

The invention belongs to the technical field of catalysts, and discloses a modified condensation reduction alkylation catalyst used in preparation of a rubber anti-aging agent 4020 by undergoing a hydrogenated reduction alkylation reaction on 4-aminodiphenylamine and methyl isobutyl ketone and preparation of a rubber anti-aging agent 4010NA by undergoing a hydrogenated reduction alkylation reaction on 4-aminodiphenylamine and acetone. The catalyst is a copper-series catalyst, and is mainly characterized in that: the catalyst contains a silicon element; and the molar ratio of copper to silicon is (0.5-10):1. Due to the adoption of the catalyst, a side reaction of ketone hydrogenation for generating an alcohol in the reacting process is suppressed remarkably, raw materials are saved, products 4010NA and 4020 are not required to be passivated by using 4-amino diphenylamine produced by reducing alkali sulfide at an earlier using stage, and unqualified products are avoided; and the catalyst has high intensity and long service life, and is not pulverized easily in the using process.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and is a rubber antioxidant 4020 used for the hydrogenation reduction alkylation reaction of 4-aminodiphenylamine (RT base) and methyl isobutyl ketone, and 4-aminodiphenylamine (RT An improved condensation reduction alkylation catalyst for the preparation of rubber antioxidant 4010NA by hydroreductive alkylation reaction of base) and acetone. Background technique [0002] The condensation reduction alkylation product of RT base and aliphatic ketone is the antioxidant of p-phenylenediamine, which is widely used in industry and has excellent performance. The commonly used ones are 4010NA and 4020. Domestically produced 4010NA and 4020 rubber antioxidants are all used The process of fixed bed catalytic hydrogenation, its chemical reaction formula is: [0003] Primary response: 4010NA [0004] [0005] 4020 [0006] [0007] main side effects [0008] [0009] [0010] Due to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80C07C211/55C07C209/70C08K5/18
Inventor 郝云青
Owner 郝云青
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