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Preparation process of high-base value sulfurized alkyl salicylate

A technology for sulfurizing alkyl salicylate and alkyl salicylic acid, which is applied in the petroleum industry, additives, lubricating compositions, etc., to achieve the effects of easy operation, mild reaction conditions, good high-temperature detergency and hydrolysis stability

Inactive Publication Date: 2019-04-26
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the total base value of the product recorded in the patents of sulfurized alkyl salicylate is mostly lower than 300mgKOH / g, but there is no report on the patent of sulfurized alkyl salicylate with high base value (TBN>350)

Method used

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  • Preparation process of high-base value sulfurized alkyl salicylate
  • Preparation process of high-base value sulfurized alkyl salicylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The present embodiment 1 provides a kind of preparation technology of alkyl salicylic acid solution, specifically:

[0035] Add 160g of salicylic acid, 400g of a mixture of n-hexadecene, n-octadecene and n-eicosene into the flask, and 80g of polar catalyst methanesulfonic acid, heat the system to 130°C, stir and keep it warm for 15h, after the reaction Add 500g of 200# solvent oil, leave standstill for 48h and then separate layers, centrifuge to remove the lower layer of methanesulfonic acid, and the upper layer is solvent-containing alkyl salicylic acid, get the upper layer sample and do gas chromatography, and record the content of the alkyl salicylic acid solution. The acid content is 50%.

Embodiment 2

[0037] Step 1: Preparation of alkyl salicylic acid products

[0038] Using the samples and data from Example 1, a solvent-containing alkyl salicylic acid product was prepared.

[0039] Step 2: Preparation of high alkali value sulfurized alkyl salicylate

[0040] Add 150g of alkyl salicylic acid products (acid content 50%), 10g of polyisobutylene succinimide, 50g of hydrogenated base oil, 10g of calcium oxide, and 9g of sulfur in the flask, start heating and slowly heat up, at 130°C Maintain 3h. Add 30g of ethylene glycol to the flask for vulcanization reaction, keep the system at 155°C for 6h, then put in 25g of calcium oxide (adding in 4 times) and introduce carbon dioxide to start the high alkalinization reaction, keep the carbon dioxide aeration time at 5h, and the aeration ends After cooling down to 100°C, add 100g of 200# solvent oil and use a filter aid to filter and remove the slag. The filtrate is distilled under reduced pressure to remove ethylene glycol and solvent...

Embodiment 3

[0042] The present embodiment 3 provides a kind of preparation technology of high alkali value sulfurized alkyl salicylate, specifically comprises the following several steps:

[0043] Step 1: Preparation of alkyl salicylic acid products

[0044] Using the samples and data from Example 1, a solvent-containing alkyl salicylic acid product was prepared.

[0045] Step 2: Preparation of high alkali value sulfurized alkyl salicylate

[0046] Add 150g of alkyl salicylic acid products (acid content 50%), 5g of polyisobutylene succinic anhydride, 50g of hydrogenated base oil, 10g of calcium oxide, and 9g of sulfur into the flask, start heating and slowly raise the temperature, and maintain it at 150°C for 2h . Add 30g of ethylene glycol to the flask for vulcanization reaction, keep the system at 160°C for 6h, then add 25g of calcium oxide (adding in 4 times) and carbon dioxide to start the high alkalinization reaction, the carbon dioxide aeration time is kept at 5h, and the aeration...

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Abstract

The invention discloses a preparation process of high-base value sulfurized alkyl salicylate. The preparation process comprising the following steps: firstly taking salicylic acids and long-chain alkenes as initiators, performing alkylation reaction under the action of a polar catalyst to prepare alkyl salicylate and preparing a high-base value (TBN) 350 mgKOH / g) sulfurized alkyl salicylate product through neutralization, vulcanization and high alkalization reactions of the alkyl salicylate. The preparation process disclosed by the invention has the benefits that a continuous synthesis processis adopted, reaction conditions are mild, the product has a higher base value, contains no free phenol and has excellent high temperature detergency, oxidation resistance and abrasion resistance, thereby being a comprehensive, environmentally-friendly and energy-saving product.

Description

technical field [0001] The invention relates to a preparation process of high alkali value sulfurized alkyl salicylate. Background technique [0002] Alkyl salicylate has excellent high-temperature detergency and hydrolytic stability, and is widely used in internal combustion engine oil and marine oil. With the rapid development of the lubricating oil field, higher requirements are placed on the quality and performance of oil additives. [0003] The preparation technology of sulfurized alkyl salicylate mainly contains two kinds, a kind of is that alkylphenol is a starting material, introduces carboxyl group on the benzene ring of alkylphenol through Kolbe-Schmitt reaction after ripening, obtains neutral alkyl water Salicylate, and then through sulfuration and carbonation reaction to obtain sulfurized basic alkyl salicylate; the other is to use alkyl salicylic acid as the reaction raw material, under the action of accelerators, surfactants, etc., through curing, Sulfurizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M159/22C10M135/26C10N30/06C10N30/10
CPCC10M135/26C10M159/22C10M2201/043C10M2201/062C10M2209/08C10M2217/024C10N2030/06C10N2030/10C10N2030/64C10N2030/66
Inventor 任晓琳万新水范金凤王学义
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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