CN104593808A - Preparation method of rubber promoter tetramethyl thiuram disulfide - Google Patents
Preparation method of rubber promoter tetramethyl thiuram disulfide Download PDFInfo
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- CN104593808A CN104593808A CN201310520418.0A CN201310520418A CN104593808A CN 104593808 A CN104593808 A CN 104593808A CN 201310520418 A CN201310520418 A CN 201310520418A CN 104593808 A CN104593808 A CN 104593808A
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Abstract
The invention discloses a preparation method of rubber promoter tetramethyl thiuram disulfide. The preparation method comprises following steps: step 1, 30% of sodium hydroxide solution, and 40% of Me2NH solution are delivered into a three-mouth flask, an obtained mixture is stirred uniformly, and is subjected to ice-water bath at 15 DEG C, and at the same time carbon disulfide liquid is added dropwise slowly, after adding, an obtained mixed material is subjected to thermostatic waterbath at 50 DEG C and reaction is carried out for 1h so as to obtain a greenyellow transparent sodium dimethyldithiocarbamate aqueous solution; and step 2, the concentration of the sodium dimethyldithiocarbamate aqueous solution is adjusted to be 30%, the sodium dimethyldithiocarbamate aqueous solution is injected into a H-shaped diaphragm electrolytic cell anode chamber, 50g/L of sodium hydroxide aqueous solution is injected into a cathode chamber, and electrolysis is carried out for 1h at 60 DEG C with electric current density of 0.3A/cm2; and step 3, products obtained via electrolysis are subjected to filtering, washing, drying, and smashing so as to obtain white tetramethyl thiuram disulfide. According to the preparation method, electron is taken as a clean reactant, adding of catalysts is not necessary, reaction conditions are mild, product purity is high, and the preparation method is green and friendly to the environment.
Description
Technical field
The present invention relates to a kind of preparation method of rubber accelerator, be specifically related to a kind of preparation method of tetramethyl-thiuram disulfide.
Background technology
Tetramethyl-thiuram disulfide is natural gum, synthetical glue and latex ultraaccelerator, is the one that in thiuram type accelerator, consumption is maximum.Can produce a large amount of waste gas, waste water and waste liquids in the process of traditional chemical method synthesis tetramethyl-thiuram disulfide, environmental pollution is comparatively large, and security is low.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of rubber accelerator tetramethyl-thiuram disulfide, reaction conditions gentleness, product purity are high, environmental protection.
The preparation method of described rubber accelerator tetramethyl-thiuram disulfide, it comprises the following steps:
One, in there-necked flask, the aqueous sodium hydroxide solution of 30% and the Me of 40% is added
2the NH aqueous solution, is uniformly mixed, and slowly drips nitric sulfid liquid, dropwise, in 50 DEG C of waters bath with thermostatic control, react 1h, obtain the transparent Sodium dimethyldithiocarbamate 40min aqueous solution of yellow-green colour in 15 DEG C of ice-water baths;
Two, the above-mentioned obtained Sodium dimethyldithiocarbamate 40min aqueous solution is deployed into the solution that concentration is 30%, inject H type diaphragm sell anolyte compartment, cathode compartment implantation concentration is the aqueous sodium hydroxide solution of 50g/L, at current density 0.3A/cm
2, electrolysis 1h at electrolysis temperature 60 DEG C;
Three, the product that obtains of electrolysis after filtration, washing, dry, pulverize and obtain white tetramethyl-thiuram disulfide.
The preparation method of rubber accelerator tetramethyl-thiuram disulfide provided by the invention, its beneficial effect is, using electronics as clean reagent, without the need to adding catalyzer, reaction conditions is gentle, product purity is high, environmental protection.
Embodiment
Below in conjunction with an embodiment, the preparation method of rubber accelerator tetramethyl-thiuram disulfide provided by the invention is described in detail.
Embodiment
One, in there-necked flask, the aqueous sodium hydroxide solution of 30% and the Me of 40% is added
2the NH aqueous solution, is uniformly mixed, and slowly drips nitric sulfid liquid, dropwise, in 50 DEG C of waters bath with thermostatic control, react 1h, obtain the transparent Sodium dimethyldithiocarbamate 40min aqueous solution of yellow-green colour in 15 DEG C of ice-water baths;
Two, the above-mentioned obtained Sodium dimethyldithiocarbamate 40min aqueous solution is deployed into the solution that concentration is 30%, inject H type diaphragm sell anolyte compartment, cathode compartment implantation concentration is the aqueous sodium hydroxide solution of 50g/L, anode adopts Pt electrode, negative electrode adopts stainless steel substrates, barrier film employing Nafion400, interpole gap is 2cm, at current density 0.3A/cm
2, electrolysis 1h at electrolysis temperature 60 DEG C;
Three, the product that obtains of electrolysis after filtration, washing, dry, pulverize and obtain white tetramethyl-thiuram disulfide.
Claims (1)
1. a preparation method for rubber accelerator tetramethyl-thiuram disulfide, is characterized in that: it comprises the following steps:
One, in there-necked flask, the aqueous sodium hydroxide solution of 30% and the Me of 40% is added
2the NH aqueous solution, is uniformly mixed, and slowly drips nitric sulfid liquid, dropwise, in 50 DEG C of waters bath with thermostatic control, react 1h, obtain the transparent Sodium dimethyldithiocarbamate 40min aqueous solution of yellow-green colour in 15 DEG C of ice-water baths;
Two, the above-mentioned obtained Sodium dimethyldithiocarbamate 40min aqueous solution is deployed into the solution that concentration is 30%, inject H type diaphragm sell anolyte compartment, cathode compartment implantation concentration is the aqueous sodium hydroxide solution of 50g/L, at current density 0.3A/cm
2, electrolysis 1h at electrolysis temperature 60 DEG C;
Three, the product that obtains of electrolysis after filtration, washing, dry, pulverize and obtain white tetramethyl-thiuram disulfide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520418.0A CN104593808A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter tetramethyl thiuram disulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520418.0A CN104593808A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter tetramethyl thiuram disulfide |
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| CN104593808A true CN104593808A (en) | 2015-05-06 |
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| CN201310520418.0A Pending CN104593808A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter tetramethyl thiuram disulfide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568311A (en) * | 2015-12-31 | 2016-05-11 | 濮阳蔚林化工股份有限公司 | Method for preparing thiuram disulfide vulcanization accelerator |
| CN107638877A (en) * | 2017-09-28 | 2018-01-30 | 晋城天成化工有限公司 | The synthetic method of tetramethylthiuram disulfide |
| CN108179439A (en) * | 2017-12-28 | 2018-06-19 | 湖北兴发化工集团股份有限公司 | The method that electrolysis prepares dimethyl disulfide |
-
2013
- 2013-10-30 CN CN201310520418.0A patent/CN104593808A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568311A (en) * | 2015-12-31 | 2016-05-11 | 濮阳蔚林化工股份有限公司 | Method for preparing thiuram disulfide vulcanization accelerator |
| CN107638877A (en) * | 2017-09-28 | 2018-01-30 | 晋城天成化工有限公司 | The synthetic method of tetramethylthiuram disulfide |
| CN107638877B (en) * | 2017-09-28 | 2020-07-14 | 晋城天成化工有限公司 | Synthesis method of tetramethyl thiuram disulfide |
| CN108179439A (en) * | 2017-12-28 | 2018-06-19 | 湖北兴发化工集团股份有限公司 | The method that electrolysis prepares dimethyl disulfide |
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Application publication date: 20150506 |