CN107638877A - The synthetic method of tetramethylthiuram disulfide - Google Patents
The synthetic method of tetramethylthiuram disulfide Download PDFInfo
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- CN107638877A CN107638877A CN201710896996.2A CN201710896996A CN107638877A CN 107638877 A CN107638877 A CN 107638877A CN 201710896996 A CN201710896996 A CN 201710896996A CN 107638877 A CN107638877 A CN 107638877A
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Abstract
The invention discloses a kind of tetramethylthiuram disulfide（TMTD）Synthetic method, comprise the following steps：Catalyst is prepared first, and wherein catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media；Then raw material is added in a kettle, dimethylamine solution, carbon disulfide, methanol and the catalyst that mass concentration is 20 50% are added wherein into reactor, the first mixture is obtained, is subsequently agitated for the first mixture, then to the hydrogen peroxide solution that addition mass concentration is 2 10% in the first mixture；TMTD is finally synthesizing, wherein being passed through oxygen into reactor, and carries out TMTD synthesis, synthesis temperature is 60 80 DEG C, and generated time is 2 10min.The synthetic method of the present invention is used make it that TMTD aggregate velocities are high, synthetic reaction is thorough, while can improve the service life of catalyst.
Description
Technical field
The present invention relates to a kind of synthetic method of thiofide, more particularly to a kind of conjunction of tetramethylthiuram disulfide
Into method.
Background technology
Thiofide TMTD, chemical name are tetramethylthiuram disulfide, are wide variety of both at home and abroad become more meticulous
Product.It is mainly used in natural rubber, synthetic rubber and various latexes and makees ultra fast accelerator.It can be used as agricultural bactericidal
Agent uses, abbreviation thiram.
At present, domestic and international production TMTD method mainly has following several：Natrium nitrosum --- air oxidation process, chlorine
Gas --- air oxidation process, electrolytic oxidation etc..Chlorine --- air oxidation process is high there is production cost, and technological process is multiple
Miscellaneous, technical requirements are high, the problems such as producing waste gas, waste water and the corrosivity to equipment.
Prior art literature 1（CN104744328A）A kind of method for producing TMTD for solvent using isopropanol is disclosed,
In the prior art, one-step oxidation process has been used to prepare TMTD, but there are following problems with the method：1st, oxidation reaction is entered
Row is slower, and the reaction time is generally longer than 3 hours, leverages production efficiency；2nd, reaction is carried out not thorough, is caused after the reaction
Waste water in, the materials such as substantial amounts of dimethylamine, carbon disulfide are also remained, because above-mentioned substance toxicity is larger, so factory also needs
Want special purchase of equipment to carry out sewage disposal to above-mentioned substance, improve the production cost of factory.
Prior art literature 2（CN1299814A）Disclose a kind of TMTD production method, but this method exist it is following
Problem：1st, equally exist oxidation reaction and carry out relatively slow, the halfway problem of reaction progress；2nd, highly basic is added during the course of the reaction
For NaOH to adjust the pH value of reactant, this will cause sewage discharge not up to standard again.
The information for being disclosed in the background section is merely intended to understanding of the increase to the general background of the present invention, without answering
It has been the prior art well known to persons skilled in the art when being considered as recognizing or implying the information structure in any form.
The content of the invention
It is an object of the invention to provide a kind of tetramethylthiuram disulfide（TMTD）Synthetic method, it is existing so as to solve
Have in technology and have that reaction speed is slow, reaction is not thorough, and the problem of pollutant is excessive in reaction product.
To achieve the above object, the invention provides a kind of tetramethylthiuram disulfide（TMTD）Synthetic method, side
Method comprises the following steps：Catalyst is prepared, catalyst is using silica as carrier, using platinum-rhodium alloy as the compound of catalytic media
Material, the preparation method of catalyst are：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, until platinum-rhodium alloy with
The particle diameter of manganese metal is 20-100nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into silica and coagulated
Glue, catalyst pulp is obtained, then, catalyst pulp is spray-dried, obtain catalyst precarsor, finally, in nitrogen gas
Catalyst precarsor is fired under atmosphere, obtains catalyst, wherein, firing temperature is 800-1000 DEG C；Raw material is added in a kettle：To
Dimethylamine solution, carbon disulfide, methanol and the catalyst that mass concentration is 20-50% are added in reactor, obtains the first mixing
Thing, then, the first mixture is stirred, then, the hydrogen peroxide solution that mass concentration is 2-10% is added into the first mixture；Close
Into TMTD：Oxygen is passed through into reactor, and carries out TMTD synthesis, synthetic reaction equation is：
Synthesis temperature is 60-80 DEG C, generated time 2-10min, obtains TMTD.
Preferably, in above-mentioned technical proposal, the particle diameter of platinum-rhodium alloy and manganese metal is 30-80nm.
Preferably, in above-mentioned technical proposal, dimethylamine solution, carbon disulfide, methanol, catalyst, the thing of hydrogen peroxide solution
Expect that ratio is 1-5:1-5:10-20:0.1-0.3:1-5.
Preferably, in above-mentioned technical proposal, firing temperature is 900-950 DEG C.
Preferably, in above-mentioned technical proposal, in TMTD steps are synthesized, synthesis temperature is 70-75 DEG C.
Preferably, in above-mentioned technical proposal, in TMTD steps are synthesized, generated time 2-3min.
Preferably, in above-mentioned technical proposal, dimethylamine solution, carbon disulfide, methanol, catalyst, the thing of hydrogen peroxide solution
Material is than being 2:2:15:0.2:2.
Preferably, in above-mentioned technical proposal, firing temperature is 920-930 DEG C.
Preferably, in above-mentioned technical proposal, in TMTD steps are synthesized, the generated time is 2min.
Preferably, in above-mentioned technical proposal, in TMTD steps are synthesized, the synthesis temperature is 72-73 DEG C.
Compared with prior art, the present invention has the advantages that：1st, inventor has surprisingly found that, by reacting
The platinum-rhodium alloy catalyst using silica as carrier is added in journey, one-step oxidation process synthesis TMTD conjunction can be increased substantially
Into speed, and synthetic reaction is carried out more thorough, it is slow so as to overcome reaction speed in the prior art, in reaction product
The defects of pollutant is excessive；2nd, by increasing Ball-milling Time, to adjust the particle diameter of platinum-rhodium alloy, and matched somebody with somebody by adjusting material
Than, can further improve the speed of synthetic reaction, and further such that synthetic reaction carry out it is more thorough；3rd, control is passed through
Catalyst firing temperature, and manganese metal is added, catalyst poisoning can be prevented, improves the service life of catalyst；4th, by
Oxygen is passed through in building-up process, and improves reaction temperature（In the prior art, reaction temperature is below 50 DEG C, what the present invention made an exception
Reaction temperature is brought up to 60-80 DEG C, inventor has found simultaneously, improves reaction temperature and is not adversely affected for synthetic reaction）,
The generation of synthetic reaction can be promoted, improve the speed of synthetic reaction.
Embodiment
It is described in detail with reference to the embodiment of the present invention, it is to be understood that protection scope of the present invention is simultaneously
Do not limited by embodiment.
Explicitly indicated that unless otherwise other, otherwise in entire disclosure and claims, term " comprising " or its change
Change such as "comprising" or " including " etc. and will be understood to comprise stated element or part, and do not exclude other members
Part or other parts.
Chemical reagent used in the present invention can be purchased from chemical article shop, and the oxygen used is that general industry is used
Pure oxygen, the sintering reaction of catalyst are carried out in sintering furnace, and it is the state of the art that spray-on process, which prepares catalyst,（Such as join
See prior art literature 3：CN106423189A）.
Embodiment 1
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, until the grain of platinum-rhodium alloy and manganese metal
Footpath is 20-100nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into silica dioxide gel, urged
Agent slurry, then, catalyst pulp is spray-dried, obtains catalyst precarsor, finally, fired urge in a nitrogen atmosphere
Agent precursor, obtains catalyst, wherein, firing temperature is 1000 DEG C；Raw material is added in a kettle：Matter is added into reactor
Dimethylamine solution, carbon disulfide, methanol and the catalyst that concentration is 20 are measured, obtains the first mixture, then, stirring first is mixed
Compound, then, the hydrogen peroxide solution that mass concentration is 2% is added into the first mixture；Synthesize TMTD：It is passed through into reactor
Oxygen, and TMTD synthesis is carried out, synthesis temperature is 60 DEG C, generated time 10min, obtains TMTD, dimethylamine solution, two sulphur
It is 1 to change carbon, methanol, catalyst, the material ratio of hydrogen peroxide solution:1:10:0.1:1.Then in measure waste water material content to push away
Reaction carry out degree is calculated, by determining and calculating, more than 95% material is finished with reaction.
Embodiment 2
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, until the grain of platinum-rhodium alloy and manganese metal
Footpath is 20-100nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into silica dioxide gel, urged
Agent slurry, then, catalyst pulp is spray-dried, obtains catalyst precarsor, finally, fired urge in a nitrogen atmosphere
Agent precursor, obtains catalyst, wherein, firing temperature is 800 DEG C；Raw material is added in a kettle：Matter is added into reactor
Dimethylamine solution, carbon disulfide, methanol and the catalyst that concentration is 30% are measured, obtains the first mixture, then, stirring first
Mixture, then, the hydrogen peroxide solution that mass concentration is 3% is added into the first mixture；Synthesize TMTD：Lead into reactor
Enter oxygen, and carry out TMTD synthesis, synthesis temperature is 80 DEG C, generated time 2min, obtains TMTD, dimethylamine solution, two
Nitric sulfid, methanol, catalyst, the material ratio of hydrogen peroxide solution are 5:5:20:0.3:5.Then measure waste water in material content with
Reaction carry out degree is calculated, by determining and calculating, more than 95% material is finished with reaction.
Embodiment 3
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, carries out long-time ball milling, until platinum rhodium closes
The particle diameter of gold and manganese metal is 30-80nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into titanium dioxide
Silica hydrogel, catalyst pulp is obtained, then, catalyst pulp is spray-dried, obtain catalyst precarsor, finally, in nitrogen
Catalyst precarsor is fired under gas atmosphere, obtains catalyst, wherein, firing temperature is 900 DEG C；Raw material is added in a kettle：To
Dimethylamine solution, carbon disulfide, methanol and the catalyst that mass concentration is 40% are added in reactor, obtains the first mixture,
Then, the first mixture is stirred, then, the hydrogen peroxide solution that mass concentration is 5% is added into the first mixture；Synthesize TMTD：
Oxygen is passed through into reactor, and carries out TMTD synthesis, synthesis temperature is 70 DEG C, generated time 3min, obtains TMTD, two
Methylamine solution, carbon disulfide, methanol, catalyst, the material ratio of hydrogen peroxide solution are 2:2:15:0.2:2.Then in measure waste water
Material content is to calculate reaction carry out degree, and by determining and calculating, more than 95% material is finished with reaction.
Embodiment 4
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, until the grain of platinum-rhodium alloy and manganese metal
Footpath is 20-100nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into silica dioxide gel, urged
Agent slurry, then, catalyst pulp is spray-dried, obtains catalyst precarsor, finally, fired urge in a nitrogen atmosphere
Agent precursor, obtains catalyst, wherein, firing temperature is 950 DEG C；Raw material is added in a kettle：Matter is added into reactor
Dimethylamine solution, carbon disulfide, methanol and the catalyst that concentration is 50% are measured, obtains the first mixture, then, stirring first
Mixture, then, the hydrogen peroxide solution that mass concentration is 10% is added into the first mixture；Synthesize TMTD：Lead into reactor
Enter oxygen, and carry out TMTD synthesis, synthesis temperature is 75 DEG C, generated time 3min, obtains TMTD, dimethylamine solution, two
Nitric sulfid, methanol, catalyst, the material ratio of hydrogen peroxide solution are 2:2:15:0.2:2.Then measure waste water in material content with
Reaction carry out degree is calculated, by determining and calculating, more than 95% material is finished with reaction.
Comparative example 1
Raw material is added in a kettle：Dimethylamine solution, carbon disulfide, methanol that mass concentration is 50% are added into reactor
And catalyst, the first mixture is obtained, then, the first mixture is stirred, then, mass concentration is added into the first mixture
For 10% hydrogen peroxide solution；Synthesize TMTD：Oxygen is passed through into reactor, and carries out TMTD synthesis, synthesis temperature 75
DEG C, generated time 3h obtains TMTD, and dimethylamine solution, carbon disulfide, methanol, catalyst, the material ratio of hydrogen peroxide solution are
2:2:15:0.2:2.Without using catalyst in the comparative example.Then material content is reacted into stroke with calculating in measure waste water
Degree, by determining and calculating, only 70% or so material reaction finishes.Noxious material is more in waste water.And it was found that reaction production
Thing TMTD is oxidized, and product quality is poor.Therefrom it can be found that when being added without catalyst, reaction temperature not above
50 DEG C, it otherwise can not obtain the product of high quality.
Comparative example 2
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, shortens Ball-milling Time, platinum-rhodium alloy and gold
The particle diameter for belonging to manganese is more than 200nm, obtains catalyst metal particles, then, catalyst metal particles is dissolved in into silica and coagulated
Glue, catalyst pulp is obtained, then, catalyst pulp is spray-dried, obtain catalyst precarsor, finally, in nitrogen gas
Catalyst precarsor is fired under atmosphere, obtains catalyst, wherein, firing temperature is 950 DEG C；Raw material is added in a kettle：To reaction
Dimethylamine solution, carbon disulfide, methanol and the catalyst that mass concentration is 50% are added in kettle, obtains the first mixture, with
Afterwards, the first mixture is stirred, then, the hydrogen peroxide solution that mass concentration is 10% is added into the first mixture；Synthesize TMTD：
Oxygen is passed through into reactor, and carries out TMTD synthesis, synthesis temperature is 75 DEG C, generated time 3min, obtains TMTD, two
Methylamine solution, carbon disulfide, methanol, catalyst, the material ratio of hydrogen peroxide solution are 2:2:15:0.2:2.Then in measure waste water
Material content is to calculate reaction carry out degree, and by determining and calculating, 60% or so material reaction finishes.Inventor's discovery, instead
It is due to catalyst poisoning that it is relatively low that degree, which should be carried out, is caused under optimum condition, and reaction carry out degree is relatively low.
Comparative example 3
Prepare catalyst, catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, catalyst
Preparation method be：Platinum-rhodium alloy is put into ball grinder and carries out ball milling, shortens Ball-milling Time, the particle diameter of platinum-rhodium alloy is 20-
100nm, catalyst metal particles are obtained, then, catalyst metal particles are dissolved in silica dioxide gel, obtain catalyst slurry
Material, then, catalyst pulp is spray-dried, obtains catalyst precarsor, finally, before firing catalyst in a nitrogen atmosphere
Body, catalyst is obtained, wherein, firing temperature is 950 DEG C；Raw material is added in a kettle：Mass concentration is added into reactor
For 50% dimethylamine solution, carbon disulfide, methanol and catalyst, the first mixture is obtained, then, stirs the first mixture,
Then, the hydrogen peroxide solution that mass concentration is 10% is added into the first mixture；Synthesize TMTD：Oxygen is passed through into reactor,
And carry out TMTD synthesis, synthesis temperature is 75 DEG C, generated time 3min, obtains TMTD, dimethylamine solution, carbon disulfide,
Methanol, catalyst, the material ratio of hydrogen peroxide solution are 2:2:15:0.2:2.Without addition manganese metal in the comparative example.Then
Material content is to calculate reaction carry out degree in measure waste water, and by determining and calculating, 60% or so material reaction finishes.Hair
A person of good sense has found that relatively low reaction carry out degree is due to catalyst poisoning, is caused under optimum condition, and reaction carry out degree is relatively low.
Comparative example 4
Catalyst firing temperature is 700 DEG C.Other experiment conditions are same as Example 4.Then measure waste water in material content with
Reaction carry out degree is calculated, by determining and calculating, 60% or so material reaction finishes.Inventor has found, reacts carry out degree
Relatively low is due to catalyst poisoning, is caused under optimum condition, and reaction carry out degree is relatively low.
Comparative example 5
When carrying out TMTD synthesis, synthesis temperature is 40 DEG C, generated time 3min, and other experiment conditions are same as Example 4.
Then material content is to calculate reaction carry out degree in measure waste water, and by determining and calculating, 70% or so material reaction is complete
Finish.
Comparative example 6
When carrying out TMTD synthesis, synthesis temperature is 90 DEG C, generated time 1min, and other experiment conditions are same as Example 4.
Then material content is to calculate reaction carry out degree in measure waste water, and by determining and calculating, 70% or so material reaction is complete
Finish.Product TMTD is oxidized, and product quality is poor.
Comparative example 7
When carrying out TMTD synthesis, oxygen is not passed through, other experiment conditions are same as Example 4.Then material in measure waste water
Content is to calculate reaction carry out degree, and by determining and calculating, 85% or so material reaction finishes.
The description of the foregoing specific illustrative embodiment to the present invention is to illustrate and the purpose of illustration.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned teaching, can be much changed
And change.The purpose of selecting and describing the exemplary embodiment is that explain that the certain principles of the present invention and its reality should
With so that those skilled in the art can realize and utilize the present invention a variety of exemplaries and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
- A kind of 1. tetramethylthiuram disulfide（TMTD）Synthetic method, it is characterised in that：The synthetic method includes as follows Step：Prepare catalyst：The catalyst is the composite using silica as carrier, using platinum-rhodium alloy as catalytic media, institute The preparation method for stating catalyst is：Platinum-rhodium alloy and manganese metal are put into ball grinder and carry out ball milling, until the platinum-rhodium alloy Particle diameter with the manganese metal is 20-100nm, obtains catalyst metal particles, and then, the catalyst metal particles are dissolved in Silica dioxide gel, catalyst pulp is obtained, then, the catalyst pulp is spray-dried, obtains catalyst precarsor, Finally, the catalyst precarsor is fired in a nitrogen atmosphere, obtains the catalyst, wherein, firing temperature is 800-1000 DEG C；Raw material is added in a kettle：It is 20-50% dimethylamine solution, curing that mass concentration is added into the reactor Carbon, methanol and catalyst, the first mixture is obtained, then, stir first mixture, then, to the described first mixing The hydrogen peroxide solution that mass concentration is 2-10% is added in thing；Synthesize TMTD：Oxygen is passed through into reactor, and carries out TMTD synthesis, the synthetic reaction equation is：Synthesis temperature is 60-80 DEG C, generated time 2-10min, obtains TMTD.
- 2. synthetic method according to claim 1, it is characterised in that：The particle diameter of the platinum-rhodium alloy and the manganese metal is 30-80nm。
- 3. synthetic method according to claim 1, it is characterised in that：The dimethylamine solution, carbon disulfide, methanol, urge Agent, the material ratio of hydrogen peroxide solution are 1-5:1-5:10-20:0.1-0.3:1-5.
- 4. synthetic method according to claim 1, it is characterised in that：Firing temperature is 900-950 DEG C.
- 5. synthetic method according to claim 1, it is characterised in that：In TMTD steps are synthesized, the synthesis temperature is 70-75℃。
- 6. synthetic method according to claim 1, it is characterised in that：In TMTD steps are synthesized, the generated time is 2-3min。
- 7. synthetic method according to claim 3, it is characterised in that：The dimethylamine solution, carbon disulfide, methanol, urge Agent, the material ratio of hydrogen peroxide solution are 2:2:15:0.2:2.
- 8. synthetic method according to claim 4, it is characterised in that：Firing temperature is 920-930 DEG C.
- 9. synthetic method according to claim 1, it is characterised in that：In TMTD steps are synthesized, the generated time is 2min。
- 10. synthetic method according to claim 5, it is characterised in that：In TMTD steps are synthesized, the synthesis temperature is 72-73℃。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624946A (en) * | 2020-12-30 | 2021-04-09 | 山东尚舜化工有限公司 | Method for synthesizing promoter TMTD by continuous method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5015752A (en) * | 1984-10-27 | 1991-05-14 | Akzo N.V. | Thiuram polysulfide |
| CN1096024A (en) * | 1992-12-30 | 1994-12-07 | 孟山都公司 | catalytic oxidation |
| CN1944505A (en) * | 2006-10-30 | 2007-04-11 | 濮阳市蔚林化工有限公司 | Method for producing tetra benzyl thiuram disulfide as rubber vulcanizing accelerator |
| CN104593808A (en) * | 2013-10-30 | 2015-05-06 | 青岛旺裕橡胶制品有限公司 | Preparation method of rubber promoter tetramethyl thiuram disulfide |
| CN106966935A (en) * | 2017-03-30 | 2017-07-21 | 山东斯递尔化工科技有限公司 | A kind of method that utilization micro-reaction device continuously prepares tetramethylthiuram disulfide |
-
2017
- 2017-09-28 CN CN201710896996.2A patent/CN107638877B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5015752A (en) * | 1984-10-27 | 1991-05-14 | Akzo N.V. | Thiuram polysulfide |
| CN1096024A (en) * | 1992-12-30 | 1994-12-07 | 孟山都公司 | catalytic oxidation |
| CN1944505A (en) * | 2006-10-30 | 2007-04-11 | 濮阳市蔚林化工有限公司 | Method for producing tetra benzyl thiuram disulfide as rubber vulcanizing accelerator |
| CN104593808A (en) * | 2013-10-30 | 2015-05-06 | 青岛旺裕橡胶制品有限公司 | Preparation method of rubber promoter tetramethyl thiuram disulfide |
| CN106966935A (en) * | 2017-03-30 | 2017-07-21 | 山东斯递尔化工科技有限公司 | A kind of method that utilization micro-reaction device continuously prepares tetramethylthiuram disulfide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624946A (en) * | 2020-12-30 | 2021-04-09 | 山东尚舜化工有限公司 | Method for synthesizing promoter TMTD by continuous method |
| CN112624946B (en) * | 2020-12-30 | 2023-07-14 | 山东尚舜化工有限公司 | Method for synthesizing accelerator TMTD by continuous method |
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