Catalyst and diphenylamine alkylation method

A technology of alkylation and catalyst, which is applied in the field of catalyst and alkylation of diphenylamine, which can solve the problems of poor catalyst reusability and large amount of catalyst, and achieve the effect of good reusability and increased production

Active Publication Date: 2010-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to overcome the disadvantages of more catalyst consumption and poor catalyst reusability in the above-mentioned

Method used

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  • Catalyst and diphenylamine alkylation method

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preparation example Construction

[0016] The preparation method of the catalyst provided by the invention comprises contacting an acid aqueous solution with a concentration of 20% by weight or less with activated clay, dehydrating and drying.

[0017] According to the preparation method provided by the present invention, preferably, the concentration of the acid is lower than 20% by weight, preferably 1-12% by weight, more preferably 1-10% by weight. And the acid may be various acids known to those skilled in the art, such as water-soluble mineral acid and / or p-toluenesulfonic acid. Wherein the water-soluble inorganic acid can be selected from one or more of sulfuric acid, phosphoric acid, hydrochloric acid, phosphotungstic acid and phosphomolybdic acid. The selected acid is preferably one or more of sulfuric acid, phosphoric acid, hydrochloric acid and p-toluenesulfonic acid.

[0018] According to the preparation method provided by the present invention, preferably, the temperature of the immersion is 20-80°...

Embodiment 1

[0034] 1. Preparation of catalyst

[0035] Adopt equal volume impregnation method to impregnate activated clay (Jinzhou Yixian Petroleum Clay Co., Ltd. product) in the sulfuric acid that temperature keeps on 20 ℃, concentration is 2% by weight, soaks 2 hours, then distills off water, dries at 100 ℃ for 2 hours hours, the catalyst was obtained.

[0036] 2. Preparation of alkylated diphenylamine

[0037] Add 50.7 g of diphenylamine, 60.5 g of diisobutylene, and 2 g of the catalyst prepared above into a 250 ml autoclave, and replace the reaction system with nitrogen three times. Start to heat up, and start stirring at a speed of 200 rpm when the temperature reaches 100°C. When the temperature is raised to 170° C. and the pressure of the reaction system is 0.30 MPa, the timing starts. After 10 hours of reaction, the pressure gradually decreases to 0.17 MPa as the reaction progresses. The residual diphenylamine content is lower than 4 wt. %, the reaction ends at this point. The...

Embodiment 2

[0039] 1. Preparation of catalyst

[0040] Adopt equal volume impregnation method to impregnate activated clay (Jinzhou Yixian Petroleum Clay Co., Ltd. product) in the sulfuric acid that temperature keeps on 30 ℃, concentration is 4% by weight, soaks 3 hours, distills off water then, dries at 120 ℃ for 3 hours hours, the catalyst was obtained.

[0041] 2. Preparation of alkylated diphenylamine

[0042] Add 50.7 g of diphenylamine, 67.2 g of diisobutylene, and 3 g of the catalyst prepared above into a 250 ml autoclave, and replace the reaction system with nitrogen three times. Start to heat up, and start stirring at a speed of 200 rpm when the temperature reaches 100°C. When the temperature is raised to 170° C. and the pressure of the reaction system is 0.38 MPa, the timing starts. After the reaction is carried out for 12 hours, the pressure gradually decreases to 0.15 MPa as the reaction progresses. The residual diphenylamine content is lower than 4 wt. %, the reaction ends...

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Abstract

The invention provides a method for preparing a catalyst. The method comprises the steps of allowing aqueous solution of acid in a concentration of less than 20 percent by weight to be in contact with activated clay, dehydrating and drying the obtained product. The invention also provides a diphenylamine alkylation method, which comprises the steps of subjecting diphenylamine and diisobutylene to contact reaction under alkylation conditions in the presence of the catalyst in an inert gas atmosphere, wherein the catalyst is obtained by the method provided by the invention. According to the method provided by the invention, the catalyst is low in consumption, and increases the yield of final products compared with the prior art. In addition, the catalyst is good in reusability, can be directly used after the catalyst is removed from the final products, and can be repeatedly reused.

Description

technical field [0001] The invention relates to a catalyst and an alkylation method of diphenylamine. Background technique [0002] During use, mineral oil and synthetic oil will undergo a chemical reaction when in contact with oxygen in the air and metal surfaces, oxidize and deteriorate, and generate acidic substances, resulting in corrosion of machinery and equipment. In order to delay the oxidation process of the oil and improve the performance, usually the most effective method is to add antioxidants to the oil. [0003] Alkylated diphenylamine is an octyl-butyl mixed alkyl-substituted amine antioxidant, which is characterized by good oil solubility, good compatibility with other types of functional additives, and can be used under higher temperature conditions. It still has an excellent antioxidant effect, especially when used in combination with phenolic ester antioxidants. At the same time, as the quality of lubricating oil is upgraded, it is increasingly required ...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J27/053C07C209/60C07C211/55
Inventor 张辉李新华段庆华李华杨永璧
Owner CHINA PETROLEUM & CHEM CORP
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