CN105566189B - A kind of low impurity solid Sodium Dimethyldithiocarbamate production technology - Google Patents
A kind of low impurity solid Sodium Dimethyldithiocarbamate production technology Download PDFInfo
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- CN105566189B CN105566189B CN201610142295.5A CN201610142295A CN105566189B CN 105566189 B CN105566189 B CN 105566189B CN 201610142295 A CN201610142295 A CN 201610142295A CN 105566189 B CN105566189 B CN 105566189B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/16—Salts of dithiocarbamic acids
Abstract
The invention provides a kind of low impurity solid Sodium Dimethyldithiocarbamate production technology, the synthetic method first adds softened water in synthesis reactor, and stir, add solid sodium hydroxide, treat solid sodium hydroxide all dissolvings, control 10 ~ 25 DEG C of temperature of charge in kettle, then carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin, again gas dimethylamine is passed through from synthesis reactor bottom, carbon disulfide is added from synthesis reactor top, and stirred with agitator, carbon disulfide and gas dimethylamine were added into synthesis reactor in 80 ~ 120 minutes, carbon disulfide and gas dimethylamine are finished, agitator stirring is controlled to continue to react, material in synthesis reactor is put into vacuumfilter, vacuum jet pump is opened to vacuumize, and keep vacuum to be 0.07 ~ 0.09MPa, obtain Sodium Dimethyldithiocarbamate solid.The present invention has purity height, production cost low, and can reduce diformazan amine content in mother liquor, improves the advantage of working environment.
Description
Present patent application is Patent No.：201410025752.3, the applying date is：It is on 01 21st, 2014, entitled：One
Plant the divisional application of the patent of invention of the synthetic method of high-purity solid Sodium Dimethyldithiocarbamate.
Technical field
The present invention relates to new chemical materialses field, more particularly to a kind of low impurity solid Sodium Dimethyldithiocarbamate production technology.
Background technology
Sodium Dimethyldithiocarbamate is used as heavy metal precipitator, emulsion polymerized styrene butadiene rubber, the terminator of styrene-butadiene latex, industrial bactericide, rubber
Vulcanization accelerator and agricultural fungicides of product etc..Sodium Dimethyldithiocarbamate is the good organosulfur compound of bactericidal performance, its function and two
Thiocyanogen methane is similar, soluble in water, and in PH >=7.0, effect is best.Therefore, the cooling water suitably run in the basic conditions
Applied in system.It is used as sterilization algae removal and foundry loam preventing agent in Treatment of Industrial Water, the medicament is compounded with 2-mercaptobenzothiazole
, can also be in oil and paper maker for the control of bacterium, fungi and foundry loam in industrial circulating cooling water tower into 30% aqueous solution
It is used as Biocidal algae-killing agent in industry.Sodium Dimethyldithiocarbamate is agricultural chemicals thiram processed, the intermediate of ziram, is also used for rubber industry accelerator,
Agriculture chemicals fungicide and Coating Antifungal Agents, can also be made the medicated soap that its content accounts for 1% as disinfectant.
At present, domestic solid Sodium Dimethyldithiocarbamate content is generally 95% or so, and has a small amount of SDD two
Polymers etc., in certain applications field as being used as analytical reagent, medicine synthesis, extraordinary fibers material processing, exotic material synthesis
Very big etc. being restricted, user wishes that the solid Sodium Dimethyldithiocarbamate for producing purity more than 99.5% meets the demand of special trade.
My company have submitted a Publication No. " A of CN 103214450 " in application on 04 26th, 2013, entitled
The life for the liquid Sodium Dimethyldithiocarbamate being related in the patent of invention of " process units and its production method of a kind of liquid Sodium Dimethyldithiocarbamate ", the patent
Production method, with the continuous research and development of my scientific research institution of intra-company, with reference to the production method of solid Sodium Dimethyldithiocarbamate in existing technology,
It was found that domestic existing solid Sodium Dimethyldithiocarbamate production method is typically all to use very following process：Water is added in synthesis reactor,
The lower input alkali lye of stirring, 40% dimethylamine solution, are cooled to 10 DEG C or so dropwise addition carbon disulfide, and control drip reacting temperature does not surpass
Cross after 30 DEG C, carbon disulfide completion of dropping, continue to react 1~2h, then stand, separate insoluble residue, obtain Sodium Dimethyldithiocarbamate molten
Liquid, the crystallization that is then concentrated under reduced pressure obtains solid Sodium Dimethyldithiocarbamate.
Being prepared in above-mentioned technique during solid Sodium Dimethyldithiocarbamate mainly has following deficiency：（1）Power consumption is high；（2）Carbon disulfide with
Dimethylamine loss is high；（3）Dimethylamine reaction is incomplete, and residual quantity is more in mother liquor causes last handling process production operation environment
It is poor；（4）Sodium Dimethyldithiocarbamate yield is low, and content is low, and purity is only 95% or so.
Not enough for more than, a kind of my scientific research institution of company purity of exploitation is high, production cost is low, and can improve working environment
Sodium Dimethyldithiocarbamate synthetic method, this method disclosure satisfy that special trade needs, promote industry development, significant.
The content of the invention
The technical problem to be solved in the present invention is that the weak point present in prior art is solid there is provided a kind of low impurity
Body Sodium Dimethyldithiocarbamate production technology, solid Sodium Dimethyldithiocarbamate prepared by this method has purity height, production cost low, and can reduce by two in mother liquor
Methylamine content, improves the advantage of working environment.
The technical solution of the present invention is to provide a kind of following low impurity solid Sodium Dimethyldithiocarbamate production technology, the synthesis
Method is as follows：
（1）Softened water is added in synthesis reactor, turn on agitator stirring added solid sodium hydroxide in 20 ~ 40 minutes,
It it is 10 ~ 25 DEG C after after solid sodium hydroxide all dissolving, controlling temperature of charge in kettle；
（2）Carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin；
（3）Gas dimethylamine is passed through from synthesis reactor bottom, while carbon disulfide is added from synthesis reactor top, and with stirring
The stirring of device, and controlling reaction temperature is 20 ~ 35 DEG C；
（4）Carbon disulfide and gas dimethylamine added synthesis reactor in 80 ~ 120 minutes, and temperature in the kettle is kept during being somebody's turn to do
For 20 ~ 35 DEG C；
（5）Carbon disulfide and gas dimethylamine are finished, and continue to react 40 ~ 60 minutes along with the stirring of agitator, and control
Reaction temperature processed is 20 ~ 35 DEG C；
（6）Material in synthesis reactor is put into vacuumfilter, vacuum jet pump is opened and vacuumizes, and keeps the vacuum to be
0.07 ~ 0.09MPa, obtains Sodium Dimethyldithiocarbamate solid.
Preferably, by above-mentioned synthetic method step（6）Produced in Sodium Dimethyldithiocarbamate solid be put into drying room, 102 ~ 105
Dried at a temperature of DEG C.
Preferably, it is 1 that the reaction mass used in the synthetic method, which is weight ratio,：0.92~1.05：2.01~2.09：
1.19 ~ 1.23 sodium hydroxide, softened water, carbon disulfide and dimethylamine.
Preferably, the step（3）The mixing speed of middle agitator is 60 ~ 80rpm.
Preferably, the step（5）The mixing speed of middle agitator is 100 ~ 130rpm.
Preferably, the step（6）In vacuumized by vacuum jet pump, the vacuum drawn time be 25 ~ 40 minutes.
Preferably, the drying time is 60 ~ 80 minutes, and take out packaging.
Preferably, the content of the high-purity solid Sodium Dimethyldithiocarbamate of the production is 99.06 ~ 99.18%, free alkali is 0.16 ~
0.26%th, pH value is 10.2 ~ 10.8.
Shown in the following chemical molecular formula of reaction principle in the synthetic method：
。
Using the beneficial effect of low impurity solid Sodium Dimethyldithiocarbamate production technology of the present invention：
Using high-concentration sodium hydroxide solution, accelerate under the same terms than low-concentration sodium hydroxide reaction speed, and promote
The precipitation of the Sodium Dimethyldithiocarbamate crystal of generation.
Compared with using Ordinary Compression air, when can substantially prevent conveying carbon disulfide using nitrogen, have in air
The presence of oxygen adds speed, carbon disulfide can be made to occur the other compounds of the reaction generation such as oxidation, so that in synthesis reactor
The purity of other final Sodium Dimethyldithiocarbamate solids of compounds affect is inside further generated with dimethylamine, sodium hydroxide reaction.
Using gas dimethylamine as raw material, dimethylamine gas is added from synthesis reactor bottom, and dimethylamine almost all is participated in
Reaction, the dimethylamine amount remained in reaction system is seldom；At the same time carbon disulfide is added from synthesis reactor top, due to two sulphur
Change carbon ratio weight larger, it is natural to be settled to synthesis reactor bottom, spread with from synthesis reactor bottom up, the dimethylamine of dissolving is contacted,
Reacted rapidly in liquid caustic soda.Plus the effect of stirring, sodium hydroxide, dimethylamine and carbon disulfide three are able to fully react.
Phase, later stage use different speeds of agitator before the reaction.Early stage is reacted, material relative concentration is higher, reaction speed
Comparatively fast, relatively low speed of agitator can be used；React the later stage, material concentration is reduced, it is necessary to accelerate mixing speed to strengthen material
Heat and mass, promotes reaction speed to accelerate.
The Sodium Dimethyldithiocarbamate solid and liquid of generation are separated by the way of vacuum filtration, even if being deposited in the material that synthesis reactor is released
There is a small amount of unreacted dimethylamine, dimethylamine can be also drawn into hydraulic jet pump water under vacuum, dissolved with dimethylamine
Water may return to synthesis reactor and be continuing with, it is to avoid because the taste that there is amine at operation scene causes operating environment difference etc..
The mother liquor that vacuum filtration is obtained, which is continued back in synthesis reactor, to be used, and whole system is without any three waste discharge.
Phase, later stage use different speeds of agitator before the reaction.It is step to react early stage（3）Stage, key reaction material
Sodium hydroxide relative concentration is higher, and dimethylamine and carbon disulfide are added after synthesis reactor, and reaction speed is very fast, relatively low speed of agitator
Also it can guarantee that reaction is completed in a short time；It is step to react the later stage（5）Stage, key reaction material sodium hydroxide relative concentration
Step-down, dimethylamine and carbon disulfide are added after synthesis reactor, and three kinds of raw molecule collision probabilities for participating in reaction are reduced, it is necessary to improve
Mixing speed increases touch opportunity with the heat and mass for strengthening material in synthesis reactor, accelerates reaction process, shortens the reaction time.
Because the mass fraction using sodium hydroxide lye is 50% or so, adds and added respectively from synthesis reactor bottom, top
Dimethylamine, carbon disulfide, material are added while reacting, and reaction speed is accelerated than other feed way, single device life
Production capacity power improves 35%, and product integrated cost reduction by 3% produces the solid Sodium Dimethyldithiocarbamate of purity more than 99%, further expands good fortune
The application field of U.S. sodium.
Embodiment
For purposes of illustration only, being done specifically to the low impurity solid Sodium Dimethyldithiocarbamate production technology of invention with reference to specific embodiment
It is bright.
Embodiment 1：
Choose volume and be 2000L synthesis reactor, and it is 525 to prepare weight ratio：525：1060：635 solid sodium hydroxide,
Softened water, carbon disulfide and dimethylamine.
1, adds softened water 525Kg in synthesis reactor, turn on agitator stirring, and solid hydroxide was added in 30 minutes
Sodium 525Kg, is passed through cooling medium chilled brine, temperature is generally 3 ~ 10 DEG C, and controls temperature of charge in kettle to synthesis reactor chuck
For 20 ~ 25 DEG C, solid sodium hydroxide is all dissolved the mass fraction after sodium hydroxide is completely dissolved and be slightly below 50%, generally
49.5%；
2. 1060Kg carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin；
3. gas dimethylamine 635Kg is passed through from synthesis reactor bottom, while adding carbon disulfide, regulation from synthesis reactor top
The mixing speed of agitator is 63rpm, and controlling reaction temperature is 25 ~ 30 DEG C；
4. carbon disulfide and gas dimethylamine added synthesis reactor in 90 minutes, should during keep temperature in the kettle be 25 ~
30℃；
5. carbon disulfide and gas dimethylamine are finished, the mixing speed of agitator is controlled to adjust in the case of 100rpm
Continue to react 50 minutes, controlling reaction temperature is 25 ~ 30 DEG C；,
6. material in synthesis reactor is put into vacuumfilter, opens vacuum jet pump and vacuumize, and keep the vacuum to be
0.07~0.08MPa, the vacuum drawn time is 30 minutes, to release the mother liquor in vacuumfilter bottom in operation in time, together
When obtain Sodium Dimethyldithiocarbamate solid.
Sodium Dimethyldithiocarbamate solid in vacuumfilter is finally put into drying room, regulation drying room temperature is 102 ~ 105 DEG C, dries 60 points
Clock, packaging.
Seen as shown in table 1 by the quality index of the solid Sodium Dimethyldithiocarbamate prepared by embodiment 1.
Table 1：
| Index name | Index | Testing result |
| Outward appearance | White crystalline body or solid | White crystalline body |
| Content %, >= | 99 | 99.12 |
| Free alkali（In terms of NaOH）, % ,≤ | 0.5 | 0.26 |
| PH values | 9.5~11.5 | 10.2 |
By table 1, the solid Sodium Dimethyldithiocarbamate that the embodiment is produced meets industry index, and the solid good fortune produced
U.S. sodium high purity 99.12%, higher than professional standard.
Embodiment 2：
Choose volume and be 2000L synthesis reactor, and it is 475 to prepare weight ratio：475：970：578 solid sodium hydroxide,
Softened water, carbon disulfide and dimethylamine.
1. softened water 475Kg is added in synthesis reactor, turn on agitator stirring added solid hydroxide in 25 minutes
Sodium 475Kg, cooling medium is passed through to synthesis reactor chuck, and it is 10 ~ 20 DEG C to control temperature of charge in kettle, makes solid sodium hydroxide whole
Dissolving；
2. 970Kg carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin；
3. gas dimethylamine 578Kg is passed through from synthesis reactor bottom, while adding carbon disulfide, regulation from synthesis reactor top
The mixing speed of agitator is 63rpm, and controlling reaction temperature is 25 ~ 30 DEG C；
4. carbon disulfide and gas dimethylamine added synthesis reactor in 100 minutes, it is 25 that temperature in the kettle is kept during being somebody's turn to do
~30℃；
5. carbon disulfide and gas dimethylamine are finished, the mixing speed of agitator is controlled to adjust in the case of 110rpm
Continue to react 60 minutes, controlling reaction temperature is 25 ~ 30 DEG C；
6. material in synthesis reactor is put into vacuumfilter, opens vacuum jet pump and vacuumize, and keep the vacuum to be
0.08~0.09MPa, the vacuum drawn time is 30 minutes, while obtaining Sodium Dimethyldithiocarbamate solid.
Sodium Dimethyldithiocarbamate solid in vacuumfilter is finally put into drying room, regulation drying room temperature is 102 ~ 105 DEG C, dries 70 points
Clock, packaging.
Seen as shown in table 2 by the quality index of the solid Sodium Dimethyldithiocarbamate prepared by embodiment 2.
Table 2：
| Index name | Index | Testing result |
| Outward appearance | White crystalline body or solid | White crystalline body |
| Content %, >= | 99 | 99.18 |
| Free alkali（In terms of NaOH）, % ,≤ | 0.5 | 0.22 |
| PH values | 9.5~11.5 | 10.4 |
By table 2, the solid Sodium Dimethyldithiocarbamate that the embodiment is produced meets industry index, and the solid good fortune produced
U.S. sodium high purity 99.18%, higher than professional standard.
Embodiment 3：
Choose volume and be 3000L synthesis reactor, and it is 750 to prepare weight ratio：775：1530：900 solid sodium hydroxide,
Softened water, carbon disulfide and dimethylamine.
1. softened water 750Kg is added in synthesis reactor, turn on agitator stirring added solid hydroxide in 40 minutes
Sodium 775Kg, cooling medium is passed through to synthesis reactor chuck, and it is 20 ~ 25 DEG C to control temperature of charge in kettle, makes solid sodium hydroxide whole
Dissolving；
2. 1530Kg carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin；
3. gas dimethylamine 900Kg is passed through from synthesis reactor bottom, while adding carbon disulfide, regulation from synthesis reactor top
The mixing speed of agitator is 80rpm, and controlling reaction temperature is 25 ~ 35 DEG C；
4. carbon disulfide and gas dimethylamine added synthesis reactor in 110 minutes, it is 25 that temperature in the kettle is kept during being somebody's turn to do
~35℃；
5. carbon disulfide and gas dimethylamine are finished, the mixing speed of agitator is controlled to adjust in the case of 100rpm
Continue to react 50 minutes, controlling reaction temperature is 25 ~ 35 DEG C；
6. material in synthesis reactor is put into vacuumfilter, opens vacuum jet pump and vacuumize, and keep the vacuum to be
0.08~0.09MPa, the vacuum drawn time is 40 minutes, while obtaining Sodium Dimethyldithiocarbamate solid.
7. Sodium Dimethyldithiocarbamate solid in vacuumfilter is put into drying room, regulation drying room temperature is 102 ~ 105 DEG C, dries 80 points
Clock, packaging.
Seen as shown in table 3 by the quality index of the solid Sodium Dimethyldithiocarbamate prepared by embodiment 3.
Table 3：
| Index name | Index | Testing result |
| Outward appearance | White crystalline body or solid | White crystalline body |
| Content, %, >= | 99 | 99.06 |
| Free alkali（In terms of NaOH）, % ,≤ | 0.5 | 0.16 |
| PH values | 9.5~11.5 | 10.8 |
By table 3, the solid Sodium Dimethyldithiocarbamate that the embodiment is produced meets industry index, and the solid good fortune produced
U.S. sodium high purity 99.06%, higher than professional standard.
In summary, the solid Sodium Dimethyldithiocarbamate that preparation is produced described in embodiment 1 ~ 3 meets as defined in current industry after testing,
Quality index, and reach as high as 99.18% by the solid Sodium Dimethyldithiocarbamate purity prepared described in method of the present invention, and state
Interior existing solid Sodium Dimethyldithiocarbamate purity is generally below 95%, and purity is higher by current industry index more than 4%, and pH value is all higher than 7.0, product
Quality is high, and practical performance is good, and embodiment 2 is a kind of optimal technical scheme.
In the above-described embodiments, the preferred forms to the present invention are described, it is obvious that in the invention structure of the present invention
Under think of, many changes can be still made.Here, it should be noted that any change made under the inventive concept of the present invention all will
Fall within the scope of protection of the present invention.
Claims (1)
1. a kind of low impurity solid Sodium Dimethyldithiocarbamate production technology, it is characterized in that：Synthetic method is as follows：
（1）Choose volume and be 2000L synthesis reactor, and it is 525 to prepare weight ratio：525：1060：635 solid sodium hydroxide,
Softened water, carbon disulfide and dimethylamine；
（2）Softened water 525Kg is added in synthesis reactor, turn on agitator stirring added solid sodium hydroxide in 30 minutes
525Kg, cooling medium chilled brine is passed through to synthesis reactor chuck, and temperature is generally 3 ~ 10 DEG C, and controls the temperature of charge in kettle to be
20 ~ 25 DEG C, make solid sodium hydroxide all dissolvings；
（3）1060Kg carbon disulfide nitrogen is pressed into carbon disulfide head tank from basin；
（4）Gas dimethylamine 635Kg is passed through from synthesis reactor bottom, while adding carbon disulfide, regulation stirring from synthesis reactor top
The mixing speed of device is 63rpm, and controlling reaction temperature is 25 ~ 30 DEG C；
（5）Carbon disulfide and gas dimethylamine added synthesis reactor in 90 minutes, and it is 25 ~ 30 that temperature in the kettle is kept during being somebody's turn to do
℃；
（6）Carbon disulfide and gas dimethylamine are finished, and control to adjust the mixing speed of agitator in the case of 100rpm to continue
Reaction 50 minutes, controlling reaction temperature is 25 ~ 30 DEG C；
（7）Material in synthesis reactor is put into vacuumfilter, vacuum jet pump is opened and vacuumizes, and keep vacuum for 0.07~
0.08MPa, the vacuum drawn time is 30 minutes, to release the mother liquor in vacuumfilter bottom in operation in time, obtain simultaneously
Sodium Dimethyldithiocarbamate solid；
（8）Sodium Dimethyldithiocarbamate solid in vacuumfilter is finally put into drying room, regulation drying room temperature is 102 ~ 105 DEG C, dries 60 points
Clock, packaging；
The content of the solid Sodium Dimethyldithiocarbamate of the production, it is 99.12% to calculate in parts by weight；
Free alkali is in terms of NaOH in the solid Sodium Dimethyldithiocarbamate of the production, and it is that 0.26%, pH value is 10.2 to calculate in parts by weight.
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| CN201410025752.3A CN103819375B (en) | 2014-01-21 | 2014-01-21 | A kind of synthetic method of high-purity solid Sodium Dimethyldithiocarbamate |
| CN201610142295.5A CN105566189B (en) | 2014-01-21 | 2014-01-21 | A kind of low impurity solid Sodium Dimethyldithiocarbamate production technology |
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| CN201610142292.1A Expired - Fee Related CN105566188B (en) | 2014-01-21 | 2014-01-21 | A kind of short solid Sodium Dimethyldithiocarbamate synthesis technique of drying time |
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| CN201610142292.1A Expired - Fee Related CN105566188B (en) | 2014-01-21 | 2014-01-21 | A kind of short solid Sodium Dimethyldithiocarbamate synthesis technique of drying time |
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| CN106139812A (en) * | 2015-04-20 | 2016-11-23 | 兰州信元新型材料有限责任公司 | Carbon disulfide Special desulfurizing agent and preparation method thereof |
| CN105949099A (en) * | 2016-05-10 | 2016-09-21 | 株洲福美实业有限公司 | Novel preparation technology for sodium dimethyl dithiocarbamate as heavy metal treating agent |
| CN106423027A (en) * | 2016-11-30 | 2017-02-22 | 湖南福尔程环保科技有限公司 | Production device and production method for sodium dimethyl dithiocarbamate |
| CN109265383A (en) * | 2018-10-08 | 2019-01-25 | 泰山医学院 | A kind of synthetic method of good fortune U.S. potassium and application in the treatment of waste water |
| CN114105843A (en) * | 2021-11-11 | 2022-03-01 | 江西坤奇实业有限公司 | Preparation method for synthesizing high-purity solid sodium ferbamate by one-step method |
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| CN1935788A (en) * | 2006-10-08 | 2007-03-28 | 河北冠龙农化有限公司 | Method for preparing ziram |
| CN101723973B (en) * | 2009-12-09 | 2012-09-26 | 浙江新安化工集团股份有限公司 | Method for preparing glyphosate dimethylamine salt solid |
| CN102321890A (en) * | 2011-09-13 | 2012-01-18 | 南开大学 | Method for preparing thiram by direct-electrochemical-oxidation |
| CN103214405B (en) * | 2013-04-26 | 2016-01-20 | 青岛中科荣达新材料有限公司 | A kind of production equipment of liquid Sodium Dimethyldithiocarbamate and production method thereof |
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| CN103819375B (en) | 2016-04-13 |
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| CN105693580A (en) | 2016-06-22 |
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