Rare earth dithiocarbamate vulcanization acalerator and its preparation method

A technology of dithiocarbamic acid and vulcanization accelerator is applied in the field of rare earth complexes, which can solve the problems of toxicity, poor vulcanization stability, easy scorch, etc., and achieve the effects of mild reaction conditions, good performance and easy acquisition.

Inactive Publication Date: 2003-12-10
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, a convenient, quick and energy-saving "one-step synthesis method" is mainly provided for the synthesis of diethylamine dithiocarbamate rare earth complex accelerator; this kind of rare earth accelerator has diethylamine dithiocarbamate in structure Substitute carbamic acid ligands, and the vulcanization reaction rate is fast; but there are also disadvantages such as easy scorch, poor vulcanization stability and certain toxicity.

Method used

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  • Rare earth dithiocarbamate vulcanization acalerator and its preparation method
  • Rare earth dithiocarbamate vulcanization acalerator and its preparation method
  • Rare earth dithiocarbamate vulcanization acalerator and its preparation method

Examples

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Effect test

Embodiment 1

[0023] (1) In a three-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, using THF as a solvent, add 1.00 mol of dibenzylamine, 1.12 mol of NaOH and 1.20 mol of CS in sequence 2 , control the reaction temperature at 50±2°C, stir the reaction for 2.5h; evaporate the solvent to obtain a white solid, wash with ether three times to obtain 280.5g of the white ligand.

[0024] (2) In a 500mL Erlenmeyer flask, dissolve 0.60mol of the ligand obtained in reaction (1) into 250mL of water, add 0.20mol of solid lanthanum chloride under stirring at 60°C, continue stirring for 5h, and filter to obtain a white powder .

[0025] (3) Dissolve the product of step (2) in acetone at normal temperature, and slowly drop 0.43mol of hexamethylene phosphoramide under stirring conditions; react for 2h, and naturally volatilize the solvent to obtain the lanthanum rare earth complex of the present invention thing.

Embodiment 2

[0027] (1) In a three-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, using tetrahydrofuran as a solvent, add 1.00 mol of dibenzylamine, 1.10 mol of NaOH and 1.40 mol of CS 2 , control the reaction temperature at 50±2°C, stir the reaction for 3h; evaporate the solvent to obtain a white solid, wash with ether 3 times to obtain 279.4g of the white ligand.

[0028] (2) In a 500mL Erlenmeyer flask, dissolve 0.63mol of the ligand obtained in reaction (1) in 250mL of water, add 0.22mol of solid neodymium chloride under stirring at 60°C, continue stirring for 4 hours, and filter to obtain light blue color powder.

[0029] (3) Dissolve the product of step (2) in acetone at normal temperature, slowly drop into 0.45mol of hexamethylene phosphoramide under stirring conditions; react for 1.9h, and naturally volatilize the solvent to obtain neodymium rare earth of the present invention Complexes.

Embodiment 3

[0031] (1) In a three-necked flask equipped with an electric stirrer, a thermometer and a reflux condenser, using tetrahydrofuran as a solvent, add 1.00 mol of dibenzylamine, 1.20 mol of NaOH and 1.32 mol of CS 2 , control the reaction temperature at 50±2°C, stir the reaction for 2h; evaporate the solvent to obtain a white solid, wash with ether 3 times to obtain 281.5g of the white ligand.

[0032] (2) In a 500mL Erlenmeyer flask, take 0.66mol of the ligand obtained in reaction (1) and dissolve it in 250mL of water, add 0.24mol of solid samarium chloride under stirring at 70°C, continue stirring for 5h, and filter to obtain pink powder.

[0033] (3) Dissolve the product of step (2) in acetone at normal temperature, slowly drop into 0.484mol hexamethylene phosphoramide under stirring condition; react for 2.1h, and naturally volatilize the solvent to obtain the samarium rare earth of the present invention Complexes.

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Abstract

The present invention relates to a dithiocarbamic acid rare earth sulfofication accelerant and its preparation method. It includes the following steps: firstly, using dibenzylamine, NaOH and CS2 as raw material to prepare ligand, then making the ligand react with rare earth chloride to prepare rare earth dibenzyl dithiocarbamate coordination compound intermediate body, and making said intermediate body react with hexamethylphosphoramide to obtain the required product.

Description

(1) Technical field [0001] The invention relates to a rare earth complex containing a dithiocarbamic acid structure which can be used as a vulcanization accelerator, and relates to a preparation method thereof. (2) Technical background [0002] The rubber vulcanization accelerators currently used can be divided into two categories: inorganic and organic accelerators. Dithiocarbamate is the main type of inorganic accelerators, and generally has strong accelerator activity. It is widely used in the rubber industry. called superaccelerators. Most of the reported compounds are salts of transition metals and alkaline earth metals, and they generally have disadvantages such as poor vulcanization stability, easy scorch and certain toxicity during application. Relatively speaking, there are not many studies on the synthesis and structural properties of dithiocarbamic acid rare earth complexes. This is mainly because the trivalent rare earth ions in the ground state, whose 4f orbit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/39
Inventor 章伟光张启交
Owner SOUTH CHINA NORMAL UNIVERSITY
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