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Method for preparing oil soluble antimony dithiocarbamate

A technology based on dithiocarbamic acid and dithioamine, which is applied in the field of preparation of oil-soluble antimony dithiocarbamate, which can solve the problems of difficult purification of products, equipment corrosion, high energy consumption, and low yield. , to achieve the effects of short production time, low production energy consumption and simple preparation process

Inactive Publication Date: 2009-06-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the shortcomings of low yield, high energy consumption, difficult to purify the product and high corrosion to equipment in the previous preparation technology, and provide a kind of high yield, low preparation energy consumption, easy purification of the product, and the preparation process is easy to use. Preparation method of oil-soluble antimony dithiocarbamate with little equipment corrosion

Method used

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  • Method for preparing oil soluble antimony dithiocarbamate
  • Method for preparing oil soluble antimony dithiocarbamate
  • Method for preparing oil soluble antimony dithiocarbamate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of Antimony Dioctyldithioaminodithiocarbamate

[0028] Add 15.3g of sodium di-n-octyl dithiocarbamate and 50ml of water into a three-neck flask equipped with stirring, start stirring, and add the aqueous solution of antimony nitrate (7.275g) and manna alcohol (2.73g) dropwise within 15min , reacted at room temperature for 1 hour. 50ml of chloroform was added, the organic phase was separated, washed three times with water, dried with anhydrous sodium sulfate, filtered, and the solvent was removed by rotary evaporation to obtain 15.2g of light yellow powder. Yield 94.7%, antimony content (theoretical value: 11.38%): 11.7%.

Embodiment 2

[0030] Preparation of antimony dihexyldithiocarbamate

[0031] Add 12.7g of sodium di-n-hexyldithiocarbamate and 50ml of water into a three-necked flask equipped with stirring, start stirring, and add an aqueous solution of antimony nitrate (7.275g) and mannacol (2.73g) dropwise within 15min. React at room temperature for 1 hour. Add 50ml of chloroform, separate the organic phase, wash with water three times, add anhydrous sodium sulfate to dry, filter, remove the solvent by rotary evaporation, recrystallize with chloroform and ethanol, 12.72g of light yellow flaky crystals. Yield 93.9%, antimony content (theoretical value: 13.49%): 13.7%.

Embodiment 3

[0033] Preparation of Antimony Dibenzylaminodithiocarbamate

[0034] Add 13.8g of sodium dibenzyldithiocarbamate and 50ml of water into a three-necked flask equipped with stirring, start stirring, and add an aqueous solution of antimony nitrate (7.275g) and mannacol (2.73g) dropwise within 15min. React at room temperature for 1 hour. Add 50ml of chloroform, separate the organic phase, wash with water three times, add anhydrous sodium sulfate to dry, filter, remove the solvent by rotary evaporation, and recrystallize with chloroform and ethanol to obtain 13.32g of light yellow crystals. Yield 94.6%, antimony content (theoretical value: 12.97%): 13.5%.

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Abstract

The invention discloses a method for preparing oil-soluble antimony dithiocarbamate, which comprises: antimony compound and an accelerant are dissolved into water, and added with dithiocar-bamate aqueous solution to carry out reaction at a temperature of between 0 and 50 DEG C for 0.5 to 3 hours in the presence of a reaction solvent or without the reaction solvent, and products are extracted by an extraction method or a filtration method. The method has the advantages of low reaction temperature, short time, simple preparation, high yield, pure products and so on.

Description

technical field [0001] The invention relates to a preparation method of oil-soluble antimony dithiocarbamate Background technique [0002] Oil-soluble antimony dithiocarbamate has a high thermal decomposition temperature, excellent tribological properties and anti-oxidation properties, and can be used to prepare aviation engine lubricating oil, turbine oil for generators, heavy-duty diesel engine oil and gear oil for tanks, Internal combustion engine oil and gear oil for trucks and high-end cars can also be used for the preparation of hydraulic oil, guide rail oil, worm gear oil and extreme pressure anti-wear and anti-friction grease. The preparation of oil-soluble antimony dithiocarbamate has been widely concerned at home and abroad. [0003] In the past, antimony dialkylaminodithioformates have been prepared by direct reaction of antimony halides such as antimony trichloride and antimony nitrate with dialkylaminodithioformic acid. This method has two obvious disadvantage...

Claims

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Application Information

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IPC IPC(8): C07C333/16
Inventor 刘维民方建孙玉彬梁永民
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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