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Sulfur-containing palladium/carbon catalyst, preparation method thereof, and preparation method of p-phenylenediamine anti-aging agents

一种对苯二胺类、炭催化剂的技术，应用在催化剂活化/制备、有机化合物的制备、物理/化学过程催化剂等方向，能够解决铂/炭催化剂价格昂贵、酮系催化剂选择性不理想等问题，达到提高产率、良好活性、提高选择性的效果

Active Publication Date: 2013-04-03
JIANGSU SINORGCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the problem of unsatisfactory selectivity of existing ketone catalysts and the high price of platinum / carbon catalysts, the invention provides a method for preparing sulfur-containing palladium / carbon catalysts, thereby preparing a sulfur-containing palladium / carbon catalyst

Method used

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  • Sulfur-containing palladium/carbon catalyst, preparation method thereof, and preparation method of p-phenylenediamine anti-aging agents
  • Sulfur-containing palladium/carbon catalyst, preparation method thereof, and preparation method of p-phenylenediamine anti-aging agents
  • Sulfur-containing palladium/carbon catalyst, preparation method thereof, and preparation method of p-phenylenediamine anti-aging agents

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preparation example Construction

[0029] figure 1 The preparation method of the sulfur-containing palladium / carbon catalyst provided by the invention is shown, comprising the following steps: palladium is loaded on activated carbon to obtain a palladium / carbon catalyst; the palladium / carbon catalyst is mixed with a solvent to make a slurry; The mixture is added to the above slurry, fully stirred at a predetermined temperature; filtered to obtain a sulfur-containing palladium / carbon catalyst. Through the preparation method provided by the invention, palladium is first loaded on the activated carbon, and then the sulfide is used to react with the palladium loaded on the activated carbon, so that the active part of the palladium is passivated, thereby reducing the preparation of p-phenylenediamine rubber antioxidant Reduction of by-products in the process. The inventors have found that it is difficult for sulfide to completely convert the metal target loaded on the activated carbon into palladium sulfide, sulfur...

Embodiment 1

[0051] Weigh 10g of activated carbon, the particle size of activated carbon is 100 mesh, and the specific surface area is 1200m 2 / g, the above-mentioned activated carbon was prepared in 100ml of deionized water into a slurry at a temperature of 80°C, and 10ml of H 2 PdCl 4 solution (the Pd content is 0.05g / ml), stirred for 2h; the pH value of the solution was adjusted to 8 with 10wt% NaOH solution, and the temperature was lowered to room temperature, filtered, and the filter cake was washed to neutrality with deionized water; The cake was configured into a slurry at 40°C, 2ml of 85% hydrazine hydrate solution was added dropwise, stirred for 2 hours, filtered, the filter cake was washed with deionized water until neutral, and vacuum-dried at 100°C; then it was vulcanized, and the Prepare it with 100ml of methanol to make a slurry at 40°C, add 0.1ml of methyl mercaptan dropwise, and stir for 2 hours; filter, and vacuum-dry the filter cake at 100°C to obtain a sulfurized pallad...

Embodiment 2

[0053] Weigh 10g of activated carbon, the particle size of activated carbon is 200 mesh, and the specific surface area is 1400m 2 / g, the above-mentioned activated carbon was prepared in 100ml of deionized water into a slurry at a temperature of 60°C, and 6ml of H 2 PdCl 4 Solution (Pd content is 0.05g / ml), stir 3h; Regulate solution pH value to 8.5 with the NaOH solution of 10wt%, and temperature is dropped to room temperature, filter, and filter cake is washed to neutrality with deionized water; The cake was configured into a slurry at 60°C, 10ml of methanol was added dropwise, stirred for 4 hours, filtered, the filter cake was washed with deionized water until neutral, and dried in vacuum at 90°C; then it was vulcanized, and mixed with 150ml of ethanol Prepare a slurry at 60°C, add 0.1ml of diphenyl sulfide dropwise, and stir for 4 hours; filter, and dry the filter cake in vacuum at 80°C to obtain a sulfurized palladium / activated carbon catalyst.

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Abstract

The invention discloses a sulfur-containing palladium / carbon catalyst, a preparation method thereof, and a preparation method of p-phenylenediamine anti-aging agents. The sulfur-containing palladium / carbon catalyst preparation method comprises the steps that: palladium is loaded on active carbon, such that a palladium / carbon catalyst is prepared; the palladium / carbon catalyst and a solvent are mixed and prepared into slurry; a sulfide is added into the slurry; the mixture is stirred under a preset temperature; and the mixture is filtered, such that the sulfur-containing palladium / carbon catalyst is prepared. When the sulfur-containing palladium / carbon catalyst provided by the invention is applied in the preparation of p-phenylenediamine anti-aging agents, p-phenylenediamine anti-aging agent yield is improved, a phenomenon that raw material is reduced into corresponding alcohol is inhibited, and selectively is improved.

Description

technical field [0001] The invention relates to the field of p-phenylenediamine anti-aging agents, in particular to a palladium-containing activated carbon, its preparation method and a preparation method of p-phenylenediamine anti-aging agents. Background technique [0002] p-Phenylenediamine antioxidants are widely used due to their good protective properties, and an important industrial synthesis method is the reductive alkylation method, which uses p-aminodiphenylamine (RT base) and aliphatic ketones as raw materials to synthesize Methods. For example: rubber anti-aging agent 4020, also known as anti-aging agent DMBPPD, scientific name N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine, it plays an important role in the anti-ozone, anti-oxidation and heat resistance of rubber , Anti-flex cracking and other aspects play an important role. With the popularity of tire meridianization, anti-aging agent 4020 is widely used. Rubber antioxidant 4020 can be prepared by hydrode...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16B01J31/22B01J37/20C07C209/26C07C209/52C07C211/51
CPCC07C211/51C07C209/26B01J31/16B01J31/22B01J23/44B01J2231/32B01J27/045B01J2531/824B01J37/20C07C209/52B01J21/18B01J37/035B01J31/226C07C211/55
Inventor 李小年张群峰陈新民丰枫马磊卢春山李春生
Owner JIANGSU SINORGCHEM TECH CO LTD
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