CN104529937B - The method that solvent applies mechanically serialization purified rubber accelerator M - Google Patents
The method that solvent applies mechanically serialization purified rubber accelerator M Download PDFInfo
- Publication number
- CN104529937B CN104529937B CN201410836572.3A CN201410836572A CN104529937B CN 104529937 B CN104529937 B CN 104529937B CN 201410836572 A CN201410836572 A CN 201410836572A CN 104529937 B CN104529937 B CN 104529937B
- Authority
- CN
- China
- Prior art keywords
- toluene
- accelerator
- cleaning mixture
- washing
- purification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/72—2-Mercaptobenzothiazole
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method that solvent applies mechanically serialization purified rubber accelerator M, accelerator M crude product is added into purification in toluene cleaning mixture, filter after purification, filtrate enters lowered temperature reclamation captax in toluenic mother liquor tank, remaining mother solution Distillation recovery toluene, filter cake is dry after toluene is washed with reclaiming, and obtains rubber vulcanization accelerator M sterling；Toluene cleaning mixture cooling filtrate after washing filter cake is entered in cleaning mixture collecting tank, for the abstraction purification of accelerator M crude product.The inventive method process is simple, toluene can be recycled, reduce the total amount of toluenic mother liquor, energy consumption is reduced, yield, low cost is improve, environmental pollution is little, continuous prodution for captax provides technical support, with economical and environmentally friendly benefit well, meets the requirement of national cleanly production.
Description
Technical field
The present invention relates to a kind of rubber accelerator 2-thiol group benzothiazole（Captax or MBT）Purification process,
Belong to rubber vulcanization accelerator M preparing technical field.
Technical background
Rubber vulcanization accelerator M（Chemical name 2- thiol benzothiazoles）It is the ultra fast accelerator of natural rubber, has increasing concurrently
Effect of modeling agent, its sulfuration critical temperature are low, easily make sizing material cause prevulcanization, can be used alone or with other accelerator simultaneously
With, it is adaptable to tire, rubber overshoes, technically classified rubber product.
Produce that captax generally takes now is acid-base method and solvent method, and acid-base method production captax can produce high salt
Organic wastewater, intractability is big, high cost, is gradually replaced by solvent method.Patent CN200510017513.4 adopts toluene conduct
Extractant purifies M, obtains the finished product M that purify to semi-finished product washing, after drying using fresh toluene.The patent toluene is to promoting
Agent M carries out purification, and toluene also has certain dissolubility to M in addition to the by-product to M has preferable dissolubility, and dissolubility is
0.8g/100mL～1.3g/100mL, therefore when purification is carried out to captax with toluene, a part of captax enters toluene
In, cause the loss of captax.Nobody is reclaimed to this part of M being dissolved in toluene now, is not also reduced
The effective ways of M losses, if being avoided that the loss of captax in toluene purge process, will greatly improve the receipts of captax
Rate.
The content of the invention
It is an object of the invention to provide a kind of method that solvent applies mechanically serialization purified rubber accelerator M, the method
The loss of captax is few, and the consumption of fresh toluene is few, almost without discharging of waste liquid, meets cleanly production requirement.
The present invention is improved and has been optimized to the purifying process of captax, and the toluene produced using washing captax is given up
Liquid replaces " fresh " toluene of abstraction purification captax, because captax in washing process, in toluene, has been dissolved, therefore in extraction
The further dissolving of captax is avoided during taking, the loss of captax is reduced, while decreasing toluenic mother liquor
Amount, alleviates post processing burden.
Concrete technical scheme of the present invention is as follows：
A kind of method that solvent applies mechanically serialization purified rubber accelerator M, comprises the following steps：
（1）Accelerator M crude product is added into purification in toluene cleaning mixture, is filtered after purification, filtrate enters toluenic mother liquor
In tank；
（2）By the filtrate cooling in toluenic mother liquor tank, stand, the accelerator M of precipitation is recovered by filtration, toluenic filtrate steams
Evaporate, reclaim toluene, gained reclaims toluene and enters in toluene collecting tank, for filtering after washing accelerator M purifying crude
The filter cake for arriving, the filtration cakes torrefaction after washing obtain rubber vulcanization accelerator M sterling；
（3）Toluene cleaning mixture after washing filter cake is entered in cleaning mixture collecting tank, for the pure of accelerator M crude product
Change.
In said method, step（1）Middle accelerator M crude product is 1 with the ratio of toluene cleaning mixture：1～4.
In said method, after accelerator M crude product adds toluene cleaning mixture, 1-6h is stirred.
In said method, step（2）In, toluenic mother liquor is stood at a temperature of 0-25 DEG C, for reclaiming accelerator M.
In said method, step（3）In, toluene cleaning mixture is stored for future use at a temperature of 0-30 DEG C, reduces the volatilization of toluene.
In said method, used by washing, toluene is suitable with the amount of toluene cleaning mixture used by extraction.
Said method can be used for industrialization and continuously produce in accelerator M, and the recovery toluene obtained by rectification both can be with
For the washing of this batch filter cake, it is also possible to for the washing of next batch filter cake.Toluene cleaning mixture in cleaning mixture collecting tank
For the purification of next batch accelerator M crude product.
In said method, the accelerator M crude product is obtained in aniline, Carbon bisulfide and sulfur as raw material reaction
Crude product.
The present invention has advantages below：
1st, the inventive method process is simple, and energy consumption is low, and low cost, environmental pollution are little, is that the continuous prodution of captax is carried
Technical support is supplied, with economical and environmentally friendly benefit well, has met the requirement of national cleanly production.
2nd, using the toluene cleaning mixture after last batch cleaning product as the extractant of extraction captax crude product, reduce
Dissolving of the captax in toluene.Meanwhile, the toluenic mother liquor after extraction can further be lowered the temperature to settle and be reclaimed product, redistillation
Fresh toluene is obtained, the washing of captax is back to.The continuous of captax is realized by the continuous recycled of toluene
Change purification, reduce the consumption of toluene, reduce the total amount of toluenic mother liquor, reduce the distillation amount of toluene, reduce energy consumption, save
The about energy.
3rd, toluene can be recycled, the consumption of toluene when can increase washing, improve product quality, purity 98% with
On.
4th, reclaimed the part captax being dissolved in toluenic mother liquor by cooling, using toluene cleaning mixture to thick
Product are extracted, and reduce the loss of M, and product average yield improves about 1.5%.
5th, keep washing toluene suitable with extraction toluene amount so that washing toluene can be realized using reuse as extraction toluene
Recycling for toluene, reduces the toluenic mother liquor for needing to distill to greatest extent, reduces production cost.
Specific embodiment
Below, the present invention is further detailed by specific embodiment, the description below is merely to explain this
It is bright, its content is not limited.
In following embodiments, captax crude product used is with Carbon bisulfide, sulfur, aniline as raw material, in High Temperature High Pressure
Lower to react the captax crude product for obtaining, in the crude product, captax mass content is 88%-91%.
Embodiment 1
Upper batch toluene cleaning mixture 800L inputs extraction kettle is taken from cleaning mixture collecting tank, 700kg captax crude products are taken
Into in extraction kettle, stirring 1h after filter, the filtrate after filtration enter toluenic mother liquor tank in, filtrate be first cooled to 20-25 DEG C, it is quiet
Putting separates out the captax of dissolving, then reclaims captax by way of filtering, and what toluenic filtrate Jing distilled fresh returns
Toluene is received, for the washing of next batch captax, M crude products filter cake last batch reclaims the fresh toluene for obtaining and washed
Wash, at 20-30 DEG C, filtrate enters in cleaning mixture collecting tank the toluene cleaning mixture temperature control after washing, promotees for next batch
Enter the clarification of agent M crude products, the filter cake convection drying after washing is promoted agent M sterlings 605.5kg, and Jing HPLC detections promote
The purity for entering agent M is 98.2%, with captax crude product rate of collecting as 86.5%.
Embodiment 2
Upper batch toluene cleaning mixture 2500L inputs extraction kettle is taken from cleaning mixture collecting tank, 700kg captax crude products are taken
Into in extraction kettle, filter after stirring 3h, the filtrate after filtration is entered in toluenic mother liquor tank, and filtrate is first cooled to 10-15 DEG C of analysis
Brilliant recovery captax, the recovery toluene that remaining filtrate Jing distills fresh, for the washing of next batch captax, M is thick
Product filter cake last batch reclaims the fresh toluene for obtaining and is washed, and the toluene cleaning mixture temperature control after washing is in 10-15
DEG C, filtrate is entered in cleaning mixture collecting tank, and for the clarification of next batch captax crude product, the filter cake after washing is direct
It is dried, is promoted agent M sterlings 607.6kg, the purity of Jing HPLC detection captaxs is 98.5%, is collected with captax crude product
Rate is 86.8%.
Embodiment 3
Upper batch toluene cleaning mixture 3300L inputs extraction kettle is taken from cleaning mixture collecting tank, 700kg captax crude products are taken
Into in extraction kettle, filter after stirring 6h, the filtrate after filtration is entered in toluenic mother liquor tank, and filtrate is first cooled to 0-5 DEG C of crystallize
Reclaim captax, the recovery toluene that remaining filtrate Jing distills fresh, for the washing of next batch captax, filter cake use
Last batch reclaims the fresh toluene for obtaining and is washed, toluene cleaning mixture temperature control 0-5 DEG C after washing, and filtrate enters and washes
Wash in liquid collecting tank, for the clarification of next batch captax crude product, the filter cake convection drying after washing, be promoted
Agent M sterlings 612.5kg, the purity of Jing HPLC detection captaxs is 99.1%, with captax crude product rate of collecting as 87.5%.
Claims (5)
1. a kind of method that solvent applies mechanically serialization purified rubber accelerator M, is characterized in that comprising the following steps：
（1）Accelerator M crude product is added into purification in toluene cleaning mixture, is filtered after purification, filtrate is entered in toluenic mother liquor tank；
（2）By the filtrate cooling in toluenic mother liquor tank, stand, the accelerator M of precipitation be recovered by filtration, toluenic filtrate distills,
Toluene is reclaimed, gained reclaims toluene and enters in toluene collecting tank, for what is be filtrated to get after washing accelerator M purifying crude
Filter cake, the filtration cakes torrefaction after washing obtain rubber vulcanization accelerator M sterling；
（3）Toluene cleaning mixture after washing filter cake is entered in cleaning mixture collecting tank, for the purification of accelerator M crude product；
Step（1）In, accelerator M crude product is 1 with the mass values of toluene cleaning mixture:1～4, step（2）In, toluene is female
Liquid temp control is stood at 0-25 DEG C.
2. method according to claim 1, is characterized in that：The recovery toluene of distillation gained both can be used for this batch filter cake
Washing, it is also possible to for the washing of next batch filter cake.
3. method according to claim 1, is characterized in that：Toluene in cleaning mixture collecting tank is used for next batch sulfuration and promotees
Enter the purification of agent M crude products.
4. the method according to any one of claim 1-3, is characterized in that：Step（1）In, accelerator M crude product adds
After entering toluene cleaning mixture, 1-6h is stirred.
5. the method according to any one of claim 1-3, is characterized in that：Step（3）In, toluene cleaning mixture is in cleaning mixture
Temperature control in collecting tank is at 0-30 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410836572.3A CN104529937B (en) | 2014-12-30 | 2014-12-30 | The method that solvent applies mechanically serialization purified rubber accelerator M |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410836572.3A CN104529937B (en) | 2014-12-30 | 2014-12-30 | The method that solvent applies mechanically serialization purified rubber accelerator M |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104529937A CN104529937A (en) | 2015-04-22 |
| CN104529937B true CN104529937B (en) | 2017-04-05 |
Family
ID=52845614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410836572.3A Active CN104529937B (en) | 2014-12-30 | 2014-12-30 | The method that solvent applies mechanically serialization purified rubber accelerator M |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104529937B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674041B (en) * | 2017-10-13 | 2021-01-22 | 山东尚舜化工有限公司 | Continuous production device for purifying rubber vulcanization accelerator M by solvent method |
| CN116283826B (en) * | 2023-01-29 | 2024-06-18 | 山东尚舜化工有限公司 | Process method for efficiently recovering MBT from liquid resin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002077126A1 (en) * | 2001-03-27 | 2002-10-03 | Exxonmobil Research And Engineering Company | Tuning fuel composition for driving cycle conditions in spark ignition engines |
| CN101693701A (en) * | 2009-10-21 | 2010-04-14 | 山东阳谷华泰化工股份有限公司 | Purification process for vulcanization accelerator 2-mercaptobenzothiazole |
| CN102408393A (en) * | 2011-10-18 | 2012-04-11 | 中国石油化工集团公司 | Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole |
| CN102850292A (en) * | 2011-06-30 | 2013-01-02 | 鹤壁市恒瑞橡塑材料有限公司 | Totally enclosed clean production system for rubber vulcanization accelerator 2-mercaptobenzothiazole |
-
2014
- 2014-12-30 CN CN201410836572.3A patent/CN104529937B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002077126A1 (en) * | 2001-03-27 | 2002-10-03 | Exxonmobil Research And Engineering Company | Tuning fuel composition for driving cycle conditions in spark ignition engines |
| CN101693701A (en) * | 2009-10-21 | 2010-04-14 | 山东阳谷华泰化工股份有限公司 | Purification process for vulcanization accelerator 2-mercaptobenzothiazole |
| CN102850292A (en) * | 2011-06-30 | 2013-01-02 | 鹤壁市恒瑞橡塑材料有限公司 | Totally enclosed clean production system for rubber vulcanization accelerator 2-mercaptobenzothiazole |
| CN102408393A (en) * | 2011-10-18 | 2012-04-11 | 中国石油化工集团公司 | Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104529937A (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102241606B (en) | Clean production method of N-cyanoethylaniline | |
| CN105460972B (en) | A kind of its recovery method as resource of circuit board tin-stripping waste liquid | |
| CN102408393A (en) | Method for continuously purifying vulcanization accelerator 2-mercaptobenzothiazole | |
| CN102206196B (en) | Method for recovering morpholine from acidic waste water containing morpholine | |
| CN104193751A (en) | Method for treating mother liquid discharged in glycine production | |
| CN104529937B (en) | The method that solvent applies mechanically serialization purified rubber accelerator M | |
| CN103333052A (en) | Method for preparing pure p-cresol and pure m-cresol by separating industrial mixed p-cresol and m-cresol | |
| CN106006676B (en) | A kind of method of NaOH in recovery H soda acid process of smelting | |
| CN102351809B (en) | Method for recovering 2-mercaptobenzothiazole from crystallization mother liquor of ceflriarone sodium | |
| CN110157538B (en) | Waste oil treatment based on green solvent | |
| CN109053627B (en) | Comprehensive recovery method of 2-mercaptobenzothiazole, triethylamine and dichloromethane in ceftriaxone sodium dichloromethane mother liquor | |
| CN103467252B (en) | Method for increasing purity of di-trimethylolpropane | |
| CN101134824A (en) | Method for reclaiming solvent from aramid fiber polymeric compound | |
| CN102242267A (en) | Method for recycling valuable metal in manganese-rich slag | |
| CN104086398A (en) | Method for separating and recovering oxalic acid from waste oxalic acid liquor | |
| CN108164069B (en) | Treatment method of tetraethylammonium tetrafluoroborate production wastewater | |
| CN102746134A (en) | Method for decreasing content of sodium chloride impurities in recovered sodium formate | |
| CN215479737U (en) | Sodium thiosulfate waste liquid purification device | |
| CN210826005U (en) | 1, 2-benzisothiazole-3-ketone production system | |
| CN105111088A (en) | Method for recycling triethylamine from wastewater containing triethylamine hydrochloride | |
| CN105037082A (en) | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor | |
| CN108558704A (en) | A kind of process of methyl carbamate wastewater treatment | |
| CN101525287B (en) | Method for refining sebacic acid | |
| CN102718728B (en) | Refining process of rubber vulcanization accelerator MBT | |
| CN108409536B (en) | Method for recovering pentaerythritol from alcohol hydrolysis liquid filter residue of antioxidant 1010 mother liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |