CN1321637A - Preparation method of tellurium diethyl dithiocarbamate - Google Patents
Preparation method of tellurium diethyl dithiocarbamate Download PDFInfo
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- CN1321637A CN1321637A CN 01105884 CN01105884A CN1321637A CN 1321637 A CN1321637 A CN 1321637A CN 01105884 CN01105884 CN 01105884 CN 01105884 A CN01105884 A CN 01105884A CN 1321637 A CN1321637 A CN 1321637A
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- tellurium
- diethyl dithiocarbamate
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- thiocarb
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Abstract
A preparation method of tellurium diethyldithiocarbamate uses tellurium oxide as raw material and adopts the following steps: using caustic alkali to dissolve tellurium oxide, controlling a certain reaction condition, making alkaline solution of tellurium and sodium diethyldithiocarbamate produce reaction to prepare and obtain homogeneous phase tellurium diethyl dithiocarbamate with uniform grain size. Said method is simple and convenient in operation, and easy to implement.
Description
The present invention relates to the preparation method of tellurium diethyl dithiocarbamate.
Tellurium diethyl dithiocarbamate is called for short TDEC, is the additive in the ethylene-propylene diene copolymer production of articles process.Its structural formula is:
Because ethylene-propylene diene copolymer has outstanding anti-ozone, higher thermostability (485 ℃), good heat aging property, weather, chemicals-resistant, oil resistant and outstanding electrical insulation capability, make it be mainly used in hot material conveyor belt, electric wire, cable, seal washer etc.Tellurium diethyl dithiocarbamate (TDEC) is to belong to dithiocarbamate(s) high-speed vulcanization promotor, and it not only can improve the sulfuration efficient of ethylene-propylene diene copolymer, cuts down the consumption of energy, and importantly it can improve the uniform in foaming and the physical strength of goods.Therefore, TDEC is an important auxiliary agent in the different third glue production of articles of ternary.
At present, TDEC generally is that tellurium salt and Thiocarb reaction by solubility obtains.But because solubility tellurium salt such as sulfurous acid tellurium, tellurium tetrachloride equistability are poor, be easy to be hydrolyzed into tellurium oxide, when reacting, can not obtain homogeneous tellurium diethyl dithiocarbamate with Thiocarb.Therefore, because the minimizing of active principle and usage quantity increases in this auxiliary agent, make the production cost of goods improve and the waste of resource in the different third glue production of articles process of ternary.
The object of the present invention is to provide a kind of new method for preparing tellurium diethyl dithiocarbamate, this method can obtain homogeneous tellurium diethyl dithiocarbamate, thereby can overcome the above-mentioned defective of existing in prior technology.
Technical conceive of the present invention is such:
The present invention is a raw material with the tellurium oxide of good stability, with caustic alkali such as sodium hydroxide or potassium hydroxide dissolved oxygen tellurium, control the certain reaction condition then, the tellurium diethyl dithiocarbamate that the alkaline solution and the Thiocarb prepared in reaction of tellurium obtained homogeneous phase and even particle size.
Realize the technical scheme of the object of the invention:
The said method of the present invention comprises the steps:
1. the preparation of tellurium solution:
With alkali lye dissolved oxygen tellurium, make it to become the solution of tellurium, the concentration of alkali lye is 0.1～2moll
-1The concentration of alkali is less than 0.1moll
-1, tellurium oxide can not be dissolved in the caustic solution fully; And greater than 2moll
-1The time, the tellurate of formation is easily separated out, and can not obtain the alkaline solution of uniform tellurium;
The concentration of tellurium there is no substantial influence to next step reaction in the alkaline solution of tellurium, but generally with 0.02～0.08moll
-1Be advisable;
Said alkali comprises one or more in sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or the saleratus;
Preferably sodium hydroxide or potassium hydroxide;
2. tellurium diethyl dithiocarbamate is synthetic:
The alkaline solution and the Thiocarb of the tellurium that 1. step is obtained react, and reaction conditions is as follows:
20～80 ℃ of pH=7～11, temperature of reaction;
In the alkaline solution of tellurium and the Thiocarb reaction process, pH is between 7～11 in control.Less than 7, the alkaline solution of Thiocarb and tellurium easily decomposes as pH, can not obtain tellurium diethyl dithiocarbamate; Greater than 11, tellurium can not precipitate fully as pH, and yield descends.
The control of pH can realize by adding the pH regulator agent, as adding pH buffered soln, mineral acid example hydrochloric acid, acetic acid, nitric acid etc.;
Temperature of reaction is 20～80 ℃, is lower than 20 ℃ as temperature of reaction, and reaction can not be complete, and the yield of TDEC descends; And temperature of reaction is greater than 80 ℃, and speed of response is too fast, forms the TDEC gel, aftertreatment is added to the difficulties, and granular size is inhomogeneous;
Thiocarb preferably is mixed with solution earlier, concentration with 5～20wt% for well;
3. separate:
Adopt conventional method,, from reaction mixture, separate TDEC as methods such as filtration, washing, dryings.
The TDEC that adopts above-mentioned disclosed preparation method to obtain, can obtain homogeneous tellurium diethyl dithiocarbamate, for the production cost that reduces the different third glue goods of ternary provides condition, and as seen by above-mentioned disclosed technical scheme, method of the present invention, easy and simple to handle, easy to implement, its yield can be higher than 96%.
Below will the present invention is further illustrated by EXAMPLE Example.
Embodiment 1
With 40gTeO
2Join 500ml 1mol l
-1In the NaOH solution, be heated to TeO
2Dissolving fully.Get 10% (wt) 2260g Thiocarb solution, control reaction temperature is 50 ℃, drips the NaOH solution of above-mentioned tellurium under stirring condition to Thiocarb solution.In the dropping process, be between the 8-9 with the pH of borax-dipotassium hydrogen phosphate buffered soln (pH is 8.4) regulation system, the aureus precipitation is TDEC.Washing 80 ℃ of following vacuum-dryings, obtains 182gTDEC after filtration, and wherein tellurium content is 16.9%, and fusing point is 110-118 ℃, granular size 2-10 μ m.
Embodiment 2
With 40gTeO
2Join 1000ml 0.5mol l
-1In the KOH solution, be heated to TeO
2Dissolving fully.Get 10% (wt) 2260g Thiocarb solution, control reaction temperature is 50 ℃, is added dropwise under stirring condition in the KOH solution of above-mentioned tellurium.In the dropping process, use 0.1mol l
-1The pH of HCl regulation system is between the 8-10, and the aureus precipitation is TDEC.Washing 80 ℃ of following vacuum-dryings, obtains 177.5gTDEC after filtration, and wherein tellurium content is 18%, and fusing point is 113-117 ℃, granular size 2-8 μ m.
Embodiment 3
Adopt and embodiment 1 identical operations method, the mixing solutions replacement NaOH with KOH and NaOH (1: 1 quality) obtains 174gTDEC, and wherein tellurium content is 18.5%, and fusing point is 113-117 ℃, granular size 2-8 μ m.
Embodiment 4
Adopt and embodiment 1 identical operations method, replace NaOH with sodium carbonate solution, obtain 160gTDEC, wherein tellurium content is 19.5%, and fusing point is 113-117 ℃, granular size 2-8 μ m.
Embodiment 5
Adopt and embodiment 1 identical operations method, replace NaOH with solution of potassium carbonate, obtain 161gTDEC, wherein tellurium content is 19.0%, and fusing point is 113-117 ℃, granular size 2-8 μ m.
Claims (8)
1. the preparation method of a tellurium diethyl dithiocarbamate is characterized in that, comprises the steps:
1. the preparation of tellurium solution: with alkali lye dissolved oxygen tellurium, the concentration of alkali lye is 0.1～2moll
-1
2. tellurium diethyl dithiocarbamate is synthetic: the condition and the Thiocarb of alkaline solution in pH=7～11 of the tellurium that 1. step is obtained reacts;
3. separate: adopt conventional method from reaction mixture, to separate TDEC.
2. the method for claim 1 is characterized in that, said alkali comprises one or more in sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or the saleratus.
3. method as claimed in claim 2 is characterized in that, said alkali is sodium hydroxide or potassium hydroxide.
4. the method for claim 1 is characterized in that, 2. step adds the pH of pH regulator agent with control solution in the building-up process of tellurium diethyl dithiocarbamate.
5. the method for claim 1 is characterized in that, said pH regulator agent comprises pH buffered soln or mineral acid.
6. the method for claim 1 is characterized in that, the concentration of tellurium is 0.02～0.08moll in the alkaline solution of tellurium
-1
7. the method for claim 1 is characterized in that, Thiocarb concentration is the solution of 5～20wt%.
8. as the arbitrary described method of claim 1～7, it is characterized in that temperature of reaction is 20～80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01105884 CN1202080C (en) | 2001-04-09 | 2001-04-09 | Preparation method of tellurium diethyl dithiocarbamate |
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| CN 01105884 CN1202080C (en) | 2001-04-09 | 2001-04-09 | Preparation method of tellurium diethyl dithiocarbamate |
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| CN1321637A true CN1321637A (en) | 2001-11-14 |
| CN1202080C CN1202080C (en) | 2005-05-18 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524390A (en) * | 2012-07-05 | 2014-01-22 | 广东先导稀材股份有限公司 | Preparation method of tellurium diethyl dithiocarbamate |
| CN103910665A (en) * | 2013-01-05 | 2014-07-09 | 广东先导稀材股份有限公司 | Tellurium diethyldithiocarbamate preparation method |
| CN104447456A (en) * | 2014-11-05 | 2015-03-25 | 宁波硫华聚合物有限公司 | Preparation method of tellurium diethyl dithiocarbamate, pre-dispersing masterbatch particles comprising tellurium diethyl dithiocarbamate and preparation method thereof |
| CN104529850A (en) * | 2014-12-25 | 2015-04-22 | 湖南大学 | Method for preparing (Z) type tellurium-sulfur olefin compound |
| CN105399652A (en) * | 2014-08-29 | 2016-03-16 | 广东先导稀材股份有限公司 | Preparation method of rubber vulcanization accelerator of dimethyldithiocarbamate selenium |
| CN105669508A (en) * | 2014-11-05 | 2016-06-15 | 宁波硫华聚合物有限公司 | Preparation method of tellurium diethyl dithiocarbamate |
| CN107903198A (en) * | 2017-11-30 | 2018-04-13 | 清远先导材料有限公司 | A kind of method of recycling TDEC |
-
2001
- 2001-04-09 CN CN 01105884 patent/CN1202080C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524390A (en) * | 2012-07-05 | 2014-01-22 | 广东先导稀材股份有限公司 | Preparation method of tellurium diethyl dithiocarbamate |
| CN103910665A (en) * | 2013-01-05 | 2014-07-09 | 广东先导稀材股份有限公司 | Tellurium diethyldithiocarbamate preparation method |
| CN103910665B (en) * | 2013-01-05 | 2016-03-23 | 广东先导稀材股份有限公司 | The preparation method of tellurium diethyl dithiocarbamate |
| CN105399652A (en) * | 2014-08-29 | 2016-03-16 | 广东先导稀材股份有限公司 | Preparation method of rubber vulcanization accelerator of dimethyldithiocarbamate selenium |
| CN104447456A (en) * | 2014-11-05 | 2015-03-25 | 宁波硫华聚合物有限公司 | Preparation method of tellurium diethyl dithiocarbamate, pre-dispersing masterbatch particles comprising tellurium diethyl dithiocarbamate and preparation method thereof |
| CN105669508A (en) * | 2014-11-05 | 2016-06-15 | 宁波硫华聚合物有限公司 | Preparation method of tellurium diethyl dithiocarbamate |
| CN104447456B (en) * | 2014-11-05 | 2016-08-17 | 宁波硫华聚合物有限公司 | The preparation method of tellurium diethyl dithiocarbamate, the pre-dispersed masterbatch particles including it and preparation method thereof |
| CN104529850A (en) * | 2014-12-25 | 2015-04-22 | 湖南大学 | Method for preparing (Z) type tellurium-sulfur olefin compound |
| CN107903198A (en) * | 2017-11-30 | 2018-04-13 | 清远先导材料有限公司 | A kind of method of recycling TDEC |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1202080C (en) | 2005-05-18 |
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