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Preparation method of low free phenol content sulfurized calcium alkyl phenolate

A technology for sulfurized calcium alkyl phenate and preparation process, which is applied in the petroleum industry, additives, lubricating compositions, etc., can solve the problems of troublesome process, secondary pollution, complicated process and the like, and achieves simple and easy process operation and mild reaction conditions. , the effect of improving water separation

Inactive Publication Date: 2019-01-11
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Although this process removes most of the free alkylphenols in sulfurized calcium alkylphenate, the process is cumbersome and will produce a large amount of waste solvents, causing secondary pollution
Patent CN105462652B is to add solvents such as alcohol and ketone after the carbonation reaction of sulfurized alkylphenol calcium to extract free alkylphenols to achieve the purpose of removing free alkylphenols. Similarly, this process is also cumbersome and consumes a large amount of extraction solvent
[0005] At present, in view of the increasingly severe environmental protection situation, experts and scholars in this field at home and abroad have tried to reduce the content of free alkylphenol in sulfurized calcium alkylphenate calcium by various means, but the results are not ideal. A simple and effective process is invented to prepare low-free phenol Calcium sulfurized alkylphenate products are imminent

Method used

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  • Preparation method of low free phenol content sulfurized calcium alkyl phenolate
  • Preparation method of low free phenol content sulfurized calcium alkyl phenolate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1 (comparative experiment):

[0032] Add 60g of alkylphenol, 55g of base oil, 15g of sulfur, 10g of calcium oxide, 2g of tetradecanoic acid, and 1g of polyisobutylene succinic anhydride into a 500mL four-necked bottle, raise the temperature to 100°C for neutralization reaction for 1 hour, and continue to heat up to 160°C , add 9g accelerator ethylene glycol to carry out vulcanization reaction for 5 hours, then add 12g calcium oxide (adding in three times), charge carbon dioxide 5.5L to carry out carbonation reaction. After the reaction was completed, the temperature was lowered to 120° C., and 5 g of filter aid was added to remove the slag by filtration to obtain 149 g of finished sulfurized calcium alkylphenate.

Embodiment 2

[0034] Add 60g of alkylphenol, 60g of base oil, 15g of sulfur, 10g of calcium oxide, 2g of tetradecanoic acid, and 1g of polyisobutylene succinic anhydride into a 500mL four-necked bottle, raise the temperature to 100°C for neutralization reaction for 1 hour, and continue to heat up to 160°C , add 9g accelerator ethylene glycol to carry out vulcanization reaction for 5 hours, add calcium oxide 12g again (adding in three times), charge carbon dioxide 5.5L to carry out carbonation reaction. After the reaction, the temperature of the system was lowered to 30-60°C, 5.5g of polyisobutylene succinimide and 1.0g of paraformaldehyde were added, and the temperature was raised slowly, controlling the heating time for 4 hours to raise the temperature to 220°C, during which the water generated by the reaction was removed. After the reaction was completed, the temperature was lowered to 100° C., and 5 g of filter aid was added to remove the slag by filtration to obtain 158 g of finished pro...

Embodiment 3

[0036]Add 60g of alkylphenol, 60g of base oil, 15g of sulfur, 10g of calcium oxide, 2g of tetradecyl carbonic acid, and 1g of octadecanol into a 500mL four-necked bottle, raise the temperature to 100°C for neutralization reaction for 1 hour, and continue to heat up to 160°C. Add 9g of accelerator ethylene glycol to carry out vulcanization reaction for 5 hours, add 12g of calcium oxide again (adding in two times), and charge 5.5L of carbon dioxide to carry out carbonation reaction. After the reaction, the temperature of the system was lowered to 30-60°C, 1.2g of diethylenetriamine and 0.5g of paraformaldehyde were added, and the temperature was raised slowly. The heating time was controlled for 2 hours and the temperature was raised to 160°C, during which the water generated by the reaction was removed. After the reaction was completed, the temperature was lowered to 120° C., and 5 g of filter aid was added to remove the slag by filtration to obtain 152 g of finished product of ...

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Abstract

The invention discloses a preparation method of a low free phenol content sulfurized calcium alkyl phenolate. The preparation method comprises following steps: 1, alkylphenol, a base oil, calcium oxide, and sulphur are subjected to neutralization and sulfuration reaction under the effect of a promoter, and then carbon dioxide gas is introduced for carbonation reaction; 2, after carbonation reaction, amine and aldehyde are added for further Mannich reaction of alkylphenol which is not sulfurized completely; and 3, after Mannich reaction, filtering is adopted to remove residue so as to obtain the low free phenol content sulfurized calcium alkyl phenolate finished product. According to the preparation method, the content of free phenol in the low free phenol content sulfurized calcium alkyl phenolate is lower than 1.0%; the preparation method is simple and convenient in operation; the reaction conditions are mile; no secondary pollution is caused; it is shown by performance evaluation that the cleanliness, the oxidation resistance, and the water separation performance of the finished product are improved at different degrees.

Description

technical field [0001] The invention relates to a preparation process of sulfurized alkylphenate calcium with low free phenol content. Background technique [0002] Calcium sulfurized alkylphenate is an excellent lubricating oil detergent. It has strong acid neutralization ability, high temperature detergency, and also has certain anti-oxidation and anti-wear properties. One of the main additives of marine oil. [0003] The currently well-known preparation process of sulfurized calcium alkylphenate is: alkylphenol, base oil, calcium oxide, sulfur and reaction additives undergo neutralization and vulcanization reactions under the action of accelerators, and then carbon dioxide is charged to carry out carbonation reactions. After centrifugation or filtration to remove impurities, the finished product of sulfurized alkylphenate calcium can be obtained. Alkylphenol is an important raw material for the preparation of sulfurized alkylphenol calcium. It is not easy to degrade in ...

Claims

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Application Information

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IPC IPC(8): C10M159/22C10N30/04C10N30/10
CPCC10M159/22C10M2219/089C10N2030/04C10N2030/10C10N2010/04
Inventor 范金凤万新水乔庆文
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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