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Diphenylamine alkylation catalyst and preparation method thereof

A technology of diphenylamine alkane and catalyst, which is applied in the field of acid-containing solid diphenylamine alkylation catalyst and preparation thereof, can solve the problems of poor activity, large amount of catalyst used, no mention of diphenylamine content, etc. The effect of good repeated use performance and low dosage

Active Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method uses a lot of catalyst, up to about 20% by weight of the amount of diphenylamine, and will carry more products when removing the catalyst, thus reducing the output of the final product
In addition, the reusability of the activated clay catalyst is poor, and when it is reusable once, the content of residual diphenylamine in the reaction product is as high as 5% by mass or more.
[0010] CN1995904A discloses a method for synthesizing dialkyl diphenylamines, including the use of Hβ zeolite and γ-Al 2 o 3 The composition of the catalyst, the reaction temperature is 175 ~ 185 ° C, the reaction pressure is 0.8 ~ 1.0MPa, using a fixed bed for continuous production, the catalyst is used for more than 300 hours, and the content of 4,4-di-tert-octyldiphenylamine in the obtained product is less than 20%, the catalyst can be recycled, but the content of unreacted diphenylamine in the product is not mentioned in the article
The catalyst is used for the alkylation reaction of diphenylamine, the activity is still poor, the residual amount of diphenylamine in the reaction product is relatively high, and the repeated service life of the catalyst is not long

Method used

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  • Diphenylamine alkylation catalyst and preparation method thereof
  • Diphenylamine alkylation catalyst and preparation method thereof

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preparation example Construction

[0017] The preparation method of the catalyst provided by the invention comprises the steps of saturated impregnating molecular sieves with aqueous acid solution, followed by dehydration and drying.

[0018] The aqueous solution concentration of the acid used in the method of the present invention is preferably 1-20% by mass, preferably 1-12% by mass, more preferably 1-10% by mass. The temperature of saturated impregnation is 20-80°C, and the impregnation time is preferably 2-7 hours. The drying temperature is 90-200°C. The saturated impregnation means that the volume of the impregnating liquid used is equal to the saturated adsorbed water amount of the impregnated carrier, and the impregnating liquid just wets the surface of the carrier completely.

[0019] The method for alkylating diphenylamine of the present invention comprises making diphenylamine contact and react with an alkylating agent at 140-250° C., 0.2-0.5 MPa, and an inert gas environment in the presence of the c...

example 1

[0030] (1) Preparation of catalyst

[0031] Take the HY type molecular sieve, press the liquid / solid ratio of 0.80ml / g at 20 DEG C, impregnate with the sulfuric acid solution saturation that concentration is 2 mass % for 2 hours, then distill off the water, dry 2 hours at 100 DEG C, obtain catalyst A, wherein sulfuric acid The content is 1.54% by mass, and the content of HY molecular sieve is 98.46% by mass.

[0032] (2) Preparation of alkylated diphenylamine

[0033]In a 250 ml autoclave, add 50.7 g of diphenylamine, 60.5 g of diisobutylene, and 2 g of catalyst A, and replace the reaction system with nitrogen three times. Stirring was started after the temperature was raised to 100°C, and the heating was continued to raise the temperature to 170°C. When the pressure of the reaction system reached 0.30 MPa, the reaction was timed for 10 hours. As the reaction progressed, the pressure was gradually reduced to 0.17 MPa, and when the content of diphenylamine in the reaction sys...

example 2

[0035] (1) Preparation of catalyst

[0036] Take the HY type molecular sieve, press the liquid / solid ratio of 0.78ml / g at 30 DEG C, impregnate with the sulfuric acid solution saturation that concentration is 4 mass % for 3 hours, then distill off water, 120 DEG C dry for 3 hours, obtain catalyst B, wherein sulfuric acid The content is 3.10% by mass, and the content of HY molecular sieve is 96.90% by mass.

[0037] (2) Preparation of alkylated diphenylamine

[0038] In a 250 ml autoclave, 50.7 g of diphenylamine, 67.2 g of diisobutylene, and 3 g of catalyst B were added, and the reaction system was replaced with nitrogen three times. After heating up to 100°C, start stirring, continue to heat up to 170°C, and when the pressure of the reaction system reaches 0.38MPa, time the reaction for 12 hours. As the reaction progresses, the pressure gradually decreases to 0.15MPa. When the diphenylamine content is less than 4% by mass, the reaction is terminated. Cool the material, and ...

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Abstract

The invention relates to a diphenylamine alkylation catalyst. The catalyst comprises, by mass, 85-99% of a molecular sieve and 1-15% of an acid, wherein the molecular sieve comprises faujasite and / or a MFI-type molecular sieve, the acid comprises an inorganic acid containing oxygen or a heteropoly acid. The catalyst is prepared by adopting an acid-containing solution to carry out saturated immersion for the molecular sieve, and carrying out treatments of dehydration and drying. The catalyst is used for the diphenylamine alkylation reaction, and has high reaction activity and reusability.

Description

technical field [0001] The invention relates to a diphenylamine alkylation catalyst and a preparation method thereof, in particular to an acid-containing solid diphenylamine alkylation catalyst and a preparation method thereof. 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, the most effective way is to add antioxidants to the oil. [0003] Alkylated diphenylamine is a kind of octyl and butyl mixed alkyl substituted amine antioxidant, which is characterized by good oil solubility, good compatibility with other types of functional additives, and is still effective at higher temperatures. Excellent antioxidant effect, especially when used in combination with phenolic ester anti...

Claims

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Application Information

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IPC IPC(8): B01J29/80B01J29/08B01J29/40C07C209/68C07C211/55
Inventor 张辉李新华段庆华李华杨永璧
Owner CHINA PETROLEUM & CHEM CORP
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