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Synthetic process for sulfurized calcium alkyl phenolate clearing agent

A technology of sulfurized alkylphenol calcium and sulfurized alkylphenol, which is applied in additives, petroleum industry, lubricating compositions, etc., can solve problems such as hydrogen sulfide poisoning, and achieve the effect of easy alkali value

Inactive Publication Date: 2017-02-01
朝阳中联化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a synthesis process of sulfurized alkylphenol calcium detergent, which can avoid the unsafe factors of high-temperature spontaneous combustion of sulfur dust and the occurrence of hydrogen sulfide poisoning accidents caused by hydrogen sulfide leakage, and solve the problem of alkylphenol in Discharge of waste gas and waste water during the vulcanization process, and can recycle by-products

Method used

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  • Synthetic process for sulfurized calcium alkyl phenolate clearing agent
  • Synthetic process for sulfurized calcium alkyl phenolate clearing agent
  • Synthetic process for sulfurized calcium alkyl phenolate clearing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1), add 51.2g of dodecylphenol into the there-necked flask with stirring, install the condenser tube and the absorption bottle, add 22.4g of calcium oxide and 18g of water in the absorption bottle and stir well;

[0044] (2) Weigh 13.5g of sulfur monochloride with a dropping bottle, raise the temperature of dodecylphenol in the three-necked bottle to 120°C, and start adding sulfur monochloride dropwise to the three-necked bottle; continue to heat up after all the drops are completed 180 ℃ ~ 190 ℃, constant temperature for 2 hours for vulcanization; after the vulcanization is completed, take samples for the total acid value, control the total acid value to be greater than 210KOHmg / g, and pour it into the neutralization tank after passing the test;

[0045] (3) After pouring the sulfurized alkylphenol into the neutralization tank, add 32.35g of base oil and 30g of calcium chloride aqueous solution, according to the acid value of the sulfurized alkylphenol, add 20g of calc...

Embodiment 2

[0052] (1), add 51.2g of dodecylphenol into the there-necked flask with stirring, install the condenser tube and the absorption bottle, add 22.4g of calcium oxide and 18g of water in the absorption bottle and stir well;

[0053] (2) Weigh 13.5g of sulfur monochloride with a dropping bottle, raise the temperature of dodecylphenol in the three-necked bottle to 120°C, and start adding sulfur monochloride dropwise to the three-necked bottle; continue to heat up after all the drops are completed 170 ℃ ~ 180 ℃, constant temperature for 1 hour for vulcanization; after the vulcanization is completed, take samples for the total acid value, control the total acid value to be greater than 210KOHmg / g, and pour it into the neutralization tank after passing the test;

[0054] (3) After pouring the sulfurized alkylphenol into the neutralization tank, add 32.35g of base oil and 30g of calcium chloride aqueous solution, according to the acid value of the sulfurized alkylphenol, add 20g of calci...

Embodiment 3

[0061] (1), add 51.2g of dodecylphenol into the there-necked flask with stirring, install the condenser tube and the absorption bottle, add 22.4g of calcium oxide and 18g of water in the absorption bottle and stir well;

[0062] (2) Weigh 13.5g of sulfur monochloride with a dropping bottle, raise the temperature of dodecylphenol in the three-necked bottle to 120°C, and start adding sulfur monochloride dropwise to the three-necked bottle; continue to heat up after all the drops are completed 150 ℃ ~ 160 ℃, constant temperature for 2 hours for vulcanization; after the vulcanization is completed, take samples for the total acid value, control the total acid value to be greater than 210KOHmg / g, and pour it into the neutralization tank after passing the test;

[0063] (3) After pouring the sulfurized alkylphenol into the neutralization tank, add 32.35g of base oil and 30g of calcium chloride aqueous solution, according to the acid value of the sulfurized alkylphenol, add 20g of calc...

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Abstract

The invention provides a synthetic process for a sulfurized calcium alkyl phenolate clearing agent. The synthetic process comprises the following steps: adding dodecylphenol into a three-neck bottle with a stirring function, mounting a condenser tube and an absorption bottle and adding sulfur monochloride into the three-neck bottle for sulfuration so as to obtain sulfurized alkyl phenate; pouring sulfurized alkyl phenate into a neutralization kettle, adding base oil and an aqueous solution of calcium chloride and adding calcium oxide for a neutralization reaction; after completion of neutralization, adding the solvent glycol, stearic acid and calcium oxide, introducing CO2 and carrying out carbonation once; after completion of carbonation, adding calcium oxide into the neutralization kettle, introducing CO2 and continuing carbonation twice to three times; and carrying out pressure-reduced distillation and filtering so as to obtain the product sulfurized calcium alkyl phenolate. The synthetic process has the advantages that the process is simple and rational, can prevent the unsafe factor of spontaneous combustion of sulfur dust at high temperature and the accident of hydrogen sulfide poisoning caused by leakage of hydrogen sulfide, overcomes the problem of emission of exhaust gas and waste water in the process of sulfuration of alkylphenol, and enables by-products to be recycled.

Description

technical field [0001] The invention belongs to the field of preparation of lubricating oil additives, in particular to a synthesis process of sulfurized alkylphenate calcium detergent. Background technique [0002] Sulfurized calcium alkylphenate has good neutralization ability, detergency, good anti-oxidation and anti-corrosion ability, and has good water separation and compatibility, which plays a significant role in controlling carbon deposits on the top ring and skirt of the piston. It is one of the main ingredients of engine lubricating oil, especially marine engine oil and heavy-duty diesel engine oil functional additives. [0003] At present, the production process of sulfurized alkylphenol calcium (T115B) is that dodecylphenol, sulfide (sulfur powder), and calcium hydroxide are first neutralized and vulcanized to generate sulfurized alkylphenol neutral salt and release hydrogen sulfide. The base value depends on the number of carbonation reactions and the amount of...

Claims

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Application Information

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IPC IPC(8): C10M135/30C10N30/02C10N30/04
CPCC10M135/30C10M2219/02C10N2010/04C10N2020/02C10N2030/04
Inventor 张晓东张国华
Owner 朝阳中联化工有限公司
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