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Preparation method of alkylsalicylic acid and/or alkylsalicylate

A technology of alkyl salicylate and alkyl salicylic acid, applied in the field of alkyl salicylate and alkyl salicylic acid, can solve the problems of harsh reaction conditions and high processing cost, and achieve relatively mild reaction conditions , high conversion rate, easy to recycle

Active Publication Date: 2018-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] It can be seen from the above patents that when salicylic acid and olefins directly synthesize alkyl salicylic acid, the reaction conditions are relatively harsh, and the cost of catalyst post-treatment is high. Therefore, the method for synthesizing alkyl salicylic acid needs further improvement

Method used

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  • Preparation method of alkylsalicylic acid and/or alkylsalicylate
  • Preparation method of alkylsalicylic acid and/or alkylsalicylate
  • Preparation method of alkylsalicylic acid and/or alkylsalicylate

Examples

Experimental program
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Effect test

preparation Embodiment 1

[0036] Synthesis of IL-1 as catalyst of 1-methyl-3-butylimidazole boron tetrafluoride salt-metaphosphoric acid-sodium dodecylbenzenesulfonate

[0037] Add 1mol N-methylimidazole and 1.05mol 1-bromobutane into a three-necked flask, 2 After purging for 20mim, start stirring and heat to 85°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of ethyl acetate was added to the lower layer liquid to wash, and then the ethyl acetate was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous 1-methyl-3-butylimidazolium bromide.

[0038] The obtained 1-methyl-3-butylimidazolium bromide was dissolved in dichloromethane, and NaBF was added thereto 4 Aqueous solution with a content of 1mol was stirred and reacted at room temperature ...

preparation Embodiment 2

[0041]Synthesis of IL-2 Catalyst of 1-Methyl-3-Butylimidazolium Sulfate-Tripolyphosphoric Acid-Sodium Caprate

[0042] In the three-necked flask, add 1mol N-methylimidazole, 1.05mol 1-bromo-n-butane, pass through N 2 After purging for 20mim, start stirring and heat to 85°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of ethyl acetate was added to the lower layer liquid to wash, and then the ethyl acetate was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous 1-methyl-3-butylimidazolium bromide.

[0043] Dissolve the obtained 1-methyl-3-butylimidazolium bromide in methanol, add NaHSO 4 Aqueous solution with a content of 1mol was stirred and reacted at room temperature for 24h. Then suction filtration, the filter...

preparation Embodiment 3

[0046] Synthesis of IL-3 as Catalyst of N-Butylpyridine Trifluoromethanesulfonate-Pyrophosphoric Acid-Dodecylbenzenesulfonate Catalyst

[0047] In a three-necked flask, add 1 mol of pyridine and 1.05 mol of 1-chlorobutane, pass through N 2 After purging for 20mim, start stirring and heat to 75°C for 30-36h. After the reaction was completed, it was left to cool down to room temperature, the lower layer of the solution was light yellow, and the upper layer was unreacted raw materials. The upper layer liquid was decanted, 3 times the volume of diethyl ether was added to the lower layer liquid to wash, and then the diethyl ether was separated to remove unreacted raw materials. After washing, dry at 70°C for 24 hours to obtain light yellow viscous N-butylpyridinium chloride salt.

[0048] Mix the obtained N-butylpyridinium chloride salt and 1mol trifluoromethanesulfonic acid in a three-necked flask, stir at 50°C for 24 hours, extract and purify with ether, then spin to remove the...

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Abstract

The invention provides a preparation method of alkylsalicylic acid and / or alkylsalicylate. The preparation method of alkylsalicylic acid and / or alkylsalicylate comprises the following steps: alpha-olefin, salicylic acid and / or salicylate are subjected to an alkylation reaction under the action of a catalyst, and a product is collected, wherein the catalyst is prepared from an ionic liquid, polyphosphoric acid and organic acid salt by mixing at 30-100 DEG C for 1-12 h. The method has the advantages of high conversion rate, good product selectivity, relatively mild reaction conditions, easily recovered catalyst and the like, and is a green and pollution-free preparation process.

Description

technical field [0001] The invention relates to alkyl salicylic acid and alkyl salicylate, in particular to a preparation method of alkyl salicylic acid and alkyl salicylate. Background technique [0002] Calcium alkyl salicylate is one of the lubricating oil detergents that appeared in the early 1940s. It has good high-temperature detergency, acid neutralization ability, high thermal stability, certain low-temperature dispersion ability and anti-oxidation and anti-corrosion Excellent performance, free of sulfur, phosphorus and other elements, especially suitable for use as a detergent for internal combustion engine oil. [0003] There are many problems in the production process of traditional alkyl salicylate, among which the more prominent problem is that the preparation process of alkyl salicylic acid follows the Kolbe-Schmidt reaction, and alkylphenol is used as the initial raw material. To prepare calcium alkyl salicylate, there are five or six steps of reaction, more ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/05C07C51/353C07C69/84C07C67/343B01J31/02
CPCC07C51/353C07C67/343B01J27/16B01J31/0225B01J31/0284B01J2231/4205B01J35/19C07C65/05C07C69/84Y02P20/584
Inventor 刘依农段庆华张耀
Owner CHINA PETROLEUM & CHEM CORP