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Preparation method for vulcanized alkylphenol

A technology for sulfurizing alkyl phenols and alkyl phenols, applied in the petroleum industry, additives, lubricating compositions, etc., can solve problems such as affecting product performance and not being well solved, and achieve the effect of excellent oxidation resistance

Active Publication Date: 2014-04-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above inventions relate to the preparation method of sulfurized alkylphenols. Different vulcanizing agents and some post-treatment measures are used. However, some impurities in the vulcanization reaction will affect the performance of the product, such as corrosiveness, high temperature detergency, etc., the above problems has not been well solved, therefore, the existing technology needs to be further improved

Method used

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  • Preparation method for vulcanized alkylphenol

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Embodiment 1 (adopt methanol solution to process three times, adopt two kinds of demulsifiers at every turn)

[0042]Add 100 grams of dodecylphenol and 75 grams of 150SN into a three-necked flask equipped with electric stirring, and stir for 15 minutes after adding, then add 4 grams of 20% ammonia solution and 10 grams of sulfur powder, and heat up to 150°C after adding , react at constant temperature for 5 hours, after the reaction, cool down to 35°C, then add 200 grams of 35% methanol aqueous solution, mix and stir for 30 minutes, at this time the solution is partially emulsified, and the emulsified layer accounts for about 6% of the water layer, add T1001 and T901, its addition amount is 120ppm of the total mass of dodecylphenol, the mass ratio between the two is 1:1, the emulsified layer does not completely disappear after standing, and about 2% of the water phase volume is the emulsified layer, and the water is separated Layer and emulsification layer, add 200 gram...

Embodiment 2

[0043] Embodiment 2 (using methanol solution to process three times, each adopting three kinds of demulsifiers)

[0044] Add 100 grams of dodecylphenol and 75 grams of 150SN into a three-necked flask equipped with electric stirring, and stir for 15 minutes after adding, then add 4 grams of 20% ammonia solution and 10 grams of sulfur powder, and heat up to 150°C after adding , react at constant temperature for 5 hours, cool down to 35°C after the reaction, then add 200 grams of 40% methanol aqueous solution, mix and stir for 30 minutes at 30-35°C, at this time, the solution is partially emulsified, and the emulsified layer accounts for about 6% of the water layer. %, add the mixture of T1001, T901 and polyisobutylene 1, the addition amount is 140ppm of the total mass of dodecylphenol, the mass ratio between T1001 and T901, polyisobutylene in the demulsifier mixture is 1:1:1, static The emulsified layer is almost invisible after putting it on. After separating the water layer, a...

Embodiment 3

[0045] Embodiment 3 (using methanol solution to process three times, each adopting three kinds of demulsifiers)

[0046] Add 100 grams of nonylphenol and 73 grams of 150SN into a three-necked flask equipped with electric stirring, stir for 15 minutes after adding, then add 2.6 grams of 20% sodium hydroxide solution, 9.6 grams of sulfur powder, and heat up to 145 ° C after adding, React at constant temperature for 5 hours. At this time, hydrogen sulfide gas is released from the three-necked bottle, absorb hydrogen sulfide gas with 20% potassium hydroxide solution, cool down to 30°C after reaction, then add 190 grams of 35% methanol aqueous solution, Mix and stir for 30 minutes. After standing, the solution has partial emulsification. The emulsified layer is 4% of the water layer. Add the demulsifier mixture of KR-12, T901 and polyisobutylene 2, and its addition is 1% of the total mass of dodecylphenol 140ppm, wherein the mass ratio between KR-12, T901, and polyisobutylene 2 is ...

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Abstract

The invention provides a preparation method for vulcanized alkylphenol. The method disclosed by the invention comprises the following steps: (1) mixing alkylphenol and a vulcanizing agent with inorganic alkaline or an aqueous solution of the inorganic alkaline, and conducting vulcanization reaction; (2) adding low-molecular-weight alcohol aqueous solution into a reaction product obtained in the step (1), mixing and stirring, then adding a demulsifier, separating an oil phase, and collecting a product. The vulcanized alkylphenol prepared by using the preparation method disclosed by the invention is excellent in antioxidant activity, corrosion inhibition and high-temperature detergency and is a lubricating oil antioxidant with comprehensive performance.

Description

technical field [0001] The invention relates to a sulfurized alkylphenol, in particular to a preparation method of a sulfurized alkylphenol antioxidant. Background technique [0002] Antioxidants are a type of additives commonly used in lubricating oils, mainly to prevent oils from oxidative decay at high temperatures. Commonly used antioxidants are divided into metal-containing and ashless antioxidants, among which zinc dialkyldithiophosphate is a commonly used metal-based antioxidant. The ashless antioxidants include alkylarylamine type, alkylphenol, sulfurized alkylphenol type, alkylphenol ester type and the like. Among them, the sulfurized alkylphenol antioxidant has high sulfur content and comprehensive performance, and can be used in gear oil and hydraulic oil. [0003] There are many patents on the preparation method of sulfurized alkylphenols. For example, U.S. Patent No. 2,916,454 introduces a method for preparing alkylphenol metal salts containing sulfur bridges ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M159/22C10N30/10C10N30/12C10N30/04
Inventor 刘依农段庆华张耀李玲
Owner CHINA PETROLEUM & CHEM CORP
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