Preparation method of tellurium diethyl dithiocarbamate

A technology of diethyldithiocarbamate and sodium diethyldithiocarbamate is applied in the field of preparation of rubber vulcanization accelerators, and can solve the problems of environmental and human harm, unqualified product quality, large amount of waste water and the like, Achieve the effect of avoiding harmful gases, reducing production costs and simplifying processes

Inactive Publication Date: 2014-01-22
FIRST RARE MATERIALS CO LTD
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Problems solved by technology

However, there is a direct addition of quantitative acid to regulate pH in the above-mentioned method, which easily decomposes diethyldithiocarbamate, and then produces harmful gases to the environment and the human body; There are soluble tellurium salts that are easily hydrolyzed, resulting in unstable product quality; and direct use of buffer solution to control pH has problems such as large amount of waste water, high price of pure tellurium and tellurium oxides, etc.

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  • Preparation method of tellurium diethyl dithiocarbamate

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[0015] The preparation method of tellurium diethyldithiocarbamate according to the present invention comprises the steps of: heating the tellurium-containing waste with alkali to dissolve and remove impurities to obtain an alkali metal tellurite solution; Sodium formate is dissolved in the buffer solution to obtain a buffer solution containing sodium diethyldithiocarbamate; alkali metal tellurite solution and hydrochloric acid solution are added to the buffer solution containing sodium diethyldithiocarbamate, so that two Sodium ethyl dithiocarbamate reacts with alkali metal tellurite, wherein the buffer solution is one of boric acid-borax solution, borax-disodium hydrogen phosphate solution, and disodium hydrogen phosphate-sodium hydroxide solution; after the reaction is completed Aging; followed by cooling, filtration, washing and drying to obtain diethyl dithiocarbamic acid tellurium.

[0016] In the method for preparing tellurium diethyldithiocarbamate according to the pres...

Embodiment 1

[0027] Ball mill 8.25g semiconductor refrigeration waste (43% tellurium content) to 0.325mm, mix with 7.5g sodium hydroxide and 3.1g sodium carbonate in a crucible and melt to 650°C, keep the temperature for 1h; add 2.1g nitric acid in batches Sodium and stir the melt, keep warm for 1h, take out and cool, break the obtained yellow product to 0.15mm, leaching with hot water at 80°C, liquid-solid ratio (mass ratio between hot water and broken yellow product) 4:1, finally Obtain 50ml sodium tellurite solution, the analysis concentration is 0.49mol / L.

[0028] 18.5g DDTC was dissolved in 130ml borax-disodium hydrogen phosphate buffer solution (pH=9.0) in a round bottom flask, heated to a temperature of 50°C, and 31.5ml sodium tellurite solution (0.49 mol / L) and 65ml hydrochloric acid solution (1mol / L), the relative speed of dropping is 1:2 in terms of droplets (0.05ml per drop), the temperature of the reaction process is controlled at 50°C, the dropping time is 1.5h, and then Age...

Embodiment 2

[0030] 6.95g of cadmium telluride waste (53% tellurium content) was ball-milled to 0.125mm, mixed with 8.1g of potassium hydroxide and 4.6g of potassium carbonate in a crucible and melted to 640°C, kept at constant temperature for 1h; g sodium nitrate and stir the melt, keep it warm for 1h, take it out and cool, break the obtained product to 0.15mm, leaching with hot water at 100℃, liquid-solid ratio (mass ratio between hot water and broken product) 3:1, filter Finally, 50 ml of potassium tellurite solution was obtained with an analytical concentration of 0.50 mol / L.

[0031] Dissolve 18.5g of DDTC in 130ml of boric acid-borax buffer solution (pH=8.4) in a round bottom flask, heat to a temperature of 50°C, and simultaneously add 31.25ml of potassium tellurite solution (0.50mol / L) and 70ml of hydrochloric acid solution (1mol / L), the relative speed of dropping is 1:2 in terms of droplets (0.05ml per drop), the temperature of the reaction process is controlled at 50°C, the dropp...

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Abstract

The invention provides a preparation method of tellurium diethyl dithiocarbamate. The preparation method comprises the following steps of: removing impurities from a tellurium-containing waste through alkali heating alkali fusion so as to obtain an alkali metal tellurite solution; dissolving sodium diethyl dithiocarbamate in a buffer solution to obtain a buffer solution containing sodium diethyl dithiocarbamate, and adding the alkali metal tellurite solution and hydrochloric acid solution into the buffer solution containing sodium diethyl dithiocarbamate to ensure that sodium diethyl dithiocarbamate reacts with alkali metal tellurite, wherein the buffer solution is one of a boric acid-borax solution, borax-disodium hydrogen phosphate solution, and disodium hydrogen phosphate-sodium hydroxide solution; performing aging after reaction; then cooling, filtering, washing and drying to obtain tellurium diethyl dithiocarbamate. The preparation method provided by the invention can simplify the process, reduce the production cost and avoid the generation of harmful gas, and a product is high in purity and controllable in particle size.

Description

technical field [0001] The method relates to a preparation method of a rubber vulcanization accelerator, in particular to a preparation method of tellurium diethyldithiocarbamate. Background technique [0002] Adding the accelerator to the rubber can accelerate the vulcanization speed, shorten the vulcanization time, lower the vulcanization temperature, and reduce the amount of vulcanizing agent. Tellurium diethyldithiocarbamate (TDEC for short), belongs to the vulcanization accelerator of dithiocarbamate. This kind of accelerator is an acidic accelerator, which has a very strong accelerating effect and a very fast vulcanization speed. It is called an "ultra-speed accelerator". It is usually used for low-temperature vulcanization and can endow rubber with great elongation strength. [0003] At present, the synthesis method of TDEC is mainly prepared by the reaction of soluble tellurium salt and sodium diethyldithiocarbamate (DDTC), and it is also prepared by using pure tell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/16
Inventor 高远潘惠娟李长龙黄娟
Owner FIRST RARE MATERIALS CO LTD
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