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Prepn process of calcium alkyl salicylate

A technology of base value calcium alkyl salicylate and alkylphenol calcium salt, which is applied in the field of lubricating oil, can solve problems such as lack of control means, high cost, and inability to adapt to production development, so as to achieve good social and economic benefits and improve The effect of lubricating oil acid neutralization ability and good high temperature detergency

Inactive Publication Date: 2005-09-28
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional preparation process of alkyl salicylate is relatively complicated. The preparation of alkyl salicylate from phenol and α-olefin is divided into seven steps, and after the alkylation reaction is completed, unreacted substances need to be distilled off. After alkalization, the solvent needs to be distilled off, so there are nine processes in total
From the problems exposed in production, it can be seen that the current process is very complicated, lack of production process control means, dark product color, high cost and serious environmental protection problems. Although many improvements and perfections have been made to the process over the years, the fundamental problem The reason is that the existing process route can no longer adapt to production development, and has directly affected the development of alkyl salicylate series products and the economic benefits of additive manufacturers
There are many patents related to the production and preparation of alkyl salicylate, but they mainly focus on the optimization of the high alkalinity process, while the preliminary preparation technology of alkyl salicylate starts from the raw materials of alkylphenol and olefins. The patent technology of alkyl salicylate is seldom seen in report, only relevant patents such as JP 61282336 (1986) of Japan Maruzen Co., Ltd., French patent FR 2587353 (1987) have reported that take ethylene glycol as promotor, in The preparation process of next-step metallization at a certain pressure has been reported, but the product synthesized under this process is a neutral salt product with a base value between 80-110, which cannot meet the high alkalinity requirements of oil products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: drop into 300.0 gram alkylphenols (ortho position about 60%, para position about 40%), 400.0 gram nonylphenol ( The ortho position is about 5%, the para position is about 95%), 51.0 grams of calcium hydroxide, and 72.0 grams of 300ZN base oil are added at the same time, the stirring is started, 54.0 grams of ethylene glycol is added, the temperature is raised to about 110 ° C, and N 2 , react at 120-130°C, 2.0Mpa for 3 hours. Cool down to about 80°C, move the crude product to a 2000ml three-necked flask with a condensation dehydrator and distill under reduced pressure to 230°C (residual pressure 2.0Kpa) to remove the water, ethylene glycol and most of the unreacted nonyl Base phenol, obtain neutral alkyl phenol calcium salt product (base number 139mgKOH / g, calcium content is 4.87%).

[0018] Move the above-mentioned alkylphenol calcium salt product into an autoclave and heat up to about 160°C, introduce carbon dioxide gas, react at 170-180°C, 2.0Mpa for 4...

Embodiment 2

[0020] Embodiment 2: drop into 300.0 gram alkylphenols (ortho position about 60%, para position about 40%), 400.0 gram dodecyl phenols in the 2000ml autoclave that has agitator, condenser, gas inlet pipe and thermometer socket Phenol (ortho position is about 5%, para position is about 95%), 51.0 grams of calcium hydroxide, and 72.0 grams of 300ZN base oil are added at the same time, stirring is started, 54.0 grams of ethylene glycol is added, the temperature is raised to about 110 ° C, and N 2 , react at 120-130°C, 2.0Mpa for 3 hours. Cool down to about 80°C, move the crude product to a 2000ml three-necked flask with a condensation dehydrator and distill under reduced pressure to 230°C (residual pressure 2.0Kpa) to remove the water, ethylene glycol and most of the unreacted nonyl Base phenol, obtain neutral alkyl phenol calcium salt product (base number 129mgKOH / g, calcium content is 4.62%).

[0021] Move the above-mentioned alkylphenol calcium salt product into an autoclave ...

Embodiment 3

[0023] Embodiment 3: drop into 300.0 gram alkylphenols (ortho position about 60%, para position about 40%), 400.0 gram dodecyl phenols in the 2000ml autoclave that has stirrer, condenser, gas inlet pipe and thermometer socket Phenol (ortho position is about 5%, para position is about 95%), 51.0 grams of calcium hydroxide, and 72.0 grams of 300ZN base oil are added at the same time, stirring is started, 54.0 grams of ethylene glycol is added, the temperature is raised to about 110 ° C, and N 2 , react at 120-130°C, 2.0Mpa for 3 hours. Cool down to about 80°C, move the crude product to a 2000ml three-necked flask with a condensation dehydrator and distill under reduced pressure to 230°C (residual pressure 2.0Kpa) to remove the water, ethylene glycol and most of the unreacted nonyl Base phenol, obtain neutral alkyl phenol calcium salt product (base number 129mgKOH / g, calcium content is 4.62%).

[0024] Move the above-mentioned alkylphenol calcium salt product into an autoclave a...

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PUM

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Abstract

The present invention describes one kind of calcium alkyl salicylate as metal detergent and its preparation process. Under the condition of certain pressure and in the presence of glycol as promoter, the materials including alkyl phenol, calcium hydroxide, etc. are made to pass through the three-step process including neutralization, carboxylation and high alkalinity reaction to synthesize medium alkalinity carboxylation calcium alkyl salicylate product with alkalinity over 160 mg KOH / g. The product of the present invention has excellent high temperature detergency, excellent low temperature dispersivity, certain antioxidant anticorrosion, extreme pressure antiwear performance and excellent compatibility with sulfonate detergent, and is one lubricant oil additive with excellent performance.

Description

(1) Technical field [0001] The invention relates to a method for preparing a lubricating oil additive with a medium alkali value calcium alkyl salicylate, in particular to a method for preparing a metal detergent product with a medium alkali value calcium alkyl salicylate, belonging to the field of lubricating oil. (2) Background technology [0002] As we all know, lubricating oil metal detergent is mainly used in engine oil, it can inhibit the oxidative deterioration of lubricating oil or reduce the formation of high temperature deposits on the surface of piston ring area (piston, piston ring, cylinder liner, ring groove) under high temperature conditions, so that The interior of the engine (combustion chamber and crankcase) is kept clean. Metal detergents are generally stable loading micelles and free surfactant molecules composed of carbonate (or borate) and surfactants adsorbed on the surface of carbonate (or borate). An oil solution composed of micelles, which mainly i...

Claims

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Application Information

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IPC IPC(8): C07C51/15C07C65/10
Inventor 姚文钊付兴国
Owner PETROCHINA CO LTD
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