CN107286910A - A kind of harmless treatment process of spent resin - Google Patents
A kind of harmless treatment process of spent resin Download PDFInfo
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- CN107286910A CN107286910A CN201710518047.0A CN201710518047A CN107286910A CN 107286910 A CN107286910 A CN 107286910A CN 201710518047 A CN201710518047 A CN 201710518047A CN 107286910 A CN107286910 A CN 107286910A
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- spent resin
- temperature
- liquid
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- pyrolysis
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Materials Engineering (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of harmless treatment process of spent resin, comprise the following steps：Pre-add heat treatment is carried out to the spent resin produced in di-mercaptobenzothiazolby production process, the spent resin for obtaining liquid is standby；Low-temperature catalytic pyrolysis processing is carried out to above-mentioned standby liquid spent resin, 70 200 DEG C are maintained the temperature at, pressure is kept in 1 0MPa, 10 20 hours of catalytic pyrolysis；Pintsch process processing is carried out, 200 450 DEG C are maintained the temperature at, keeps pressure in 1 0MPa, pyrolysis time is 20 40 hours；Separate and collect processing：The above-mentioned gaseous breakdown distillate isolated is passed through and handled by liquid caustic soda, NaHS is produced by chemically reacting；Remaining component heterocyclic compound after cracking is passed through in the holding vessel of water, taken out after solidification to be cooled, fill bag.The invention realizes resource recycling, greatly reduces production cost, economizes on resources, enhances the competitiveness of product.
Description
Technical field
The present invention relates to di-mercaptobenzothiazolby production and process field, more particularly to a kind of harmless treatment of spent resin
Technique.
Background technology
Produce di-mercaptobenzothiazolby（Captax）Conventional method have two kinds of acid-base method and solvent method, but at present, this
Two ways can produce about 20% spent resin in process of production, and this spent resin is sticky, smell is big, inflammable poisonous, right
Body is harmful to, and this spent resin pollutes environment, is classified as hazardous solid waste by environmental administration, at present, contains in resin
Study a lot of on the extraction and application of a small amount of captax, but for lacking environmental consciousness in the processing of product spent resin, due to useless
Carbon disulfide containing 0.5%-1% in resin, 1%-2% toluene, 1%-2% aniline, 1%-2% captax, 3%-5% benzene
And thiazole, 30%-40% benzothiazole azo, 20%-30% benzothiazole diazol and some baroque jeterocyclic chemistries
Compound, these materials are presented with polymeric form, the mutual embedding company of molecule, formation macromolecular glass state material, and most life at present
Production producer is roughly divided into two kinds in the method for handling this spent resin, and one kind is barrelling storage, concentrates burial processing；It is another to be
It is handed over to disposal centre and makees burning processing, the former causes waste material cumulative, causes waste in resource and to soil horizon
Harm is larger, and the latter is direct burning, can produce secondary air pollution, does not carry out recycling recycling to waste, and often
About 3000 yuan of the spent resin of one ton of processing, forms the phenomenon of waste of resource to a certain extent.
The content of the invention
In view of the above-mentioned problems of the prior art, the invention provides a kind of harmless treatment process of spent resin, should
Invention is carried out this kind of waste resin after harmless treatment, the solid product ultimately formed reaches insoluble by a series of flows
Yu Shui, tasteless, non-ignitable purpose, and can be used as a kind of raw material of waterproof material, gaseous state distillate is after cooled
The production of di-mercaptobenzothiazolby can be continued to participate in as raw material, economic benefit and society's effect are being produced as waterproof material sale
While beneficial, it is thus also avoided that the problem of hazardous waste long term storage and directly burning processing generation secondary pollution the problem of.
To achieve the above object, the present invention is realized in：A kind of harmless treatment process of spent resin, including it is following
Step：
（1）Pre-add is heat-treated：By the spent resin centralized collection produced in di-mercaptobenzothiazolby production process, take and be put into right amount
In pre- thermal reactor, pre- thermal reactor is cylindrical tube shape, and preheating reactor bottom and top are respectively equipped with heater and cooling
Device, heater carries out preliminary preheating to spent resin and melted, and controls the temperature of reactor at 50-70 DEG C, the time is 3-5
Hour, the spent resin of liquid is obtained, it is standby；Pass through the fugitive constituent for setting cooling device to avoid spent resin from being produced in heating process
Effusion, fugitive constituent is mainly toluene, dimethylbenzene and carbon disulfide, and the amount of the toluene, dimethylbenzene and carbon disulfide accounts for above-mentioned add
Plus the ratio of spent resin total content is respectively 1-2%, 1-2%, 0.5-1%, belongs to inflammable, explosive, poisonous chemical substance, heating-up temperature control
System can be realized spent resin being melted into liquid completely, be easy to next step to transmit at 50-70 DEG C, and can realize by cooling down dress
Control fugitive constituent toluene, the effusion of carbon disulfide to greatest extent are put, the output end of cooling device is connected with external storage case, just
The reproduction of di-mercaptobenzothiazolby is carried out in centralized collection；
（2）Low-temperature catalytic pyrolysis processing：By above-mentioned steps（1）The standby liquid resin produced, spy is transferred into by booster pump
In the catalytic cracking reaction device of system, catalytic pyrolysis；Catalytic cracking reaction device bottom and top are respectively equipped with heater and cooling
Device, catalyst uses palladium-nickel alloy mesh catalyst, and heater maintains the temperature at 70-200 DEG C, keeps pressure in -1-
0MPa, the catalytic pyrolysis time is 10-20 hour, and the gas component cracked out has：Carbon disulfide, toluene, dimethylbenzene, aniline,
Benzothiazole, the carbon disulfide, toluene, dimethylbenzene, aniline, the amount of benzothiazole gas account for the ratio of above-mentioned standby liquid resin
Example is respectively 0.5-1%, 1-2%, 1-2%, 1-2%, 3-5%；Discharged through catalytic cracking reaction device top, it is cooled down through cooling device
Afterwards, collected by external storage case, be convenient for the reproduction of di-mercaptobenzothiazolby；Softening point is higher and composition is relatively single
Stable heterocyclic compound component exists in liquid form, and key component is 25-30% heterocyclic compound, 20-30% benzo
The benzothiazole azo of thiazole diazol, 30-40%, 3-5% sulphur is standby；
（3）Pintsch process processing：By step（2）Remaining liquid component high-temperature pyrolysis reactor is transferred into by booster pump
In, heater is provided with high-temperature pyrolysis reactor, heater maintains the temperature at 200-450 DEG C, keeps pressure in -1-
0MPa, catalyst uses nickel-cobalt alloy mesh catalyst, and pyrolysis time is 20-40 hour, after treating that cracking is fully completed,
Gaseous pyrolysis product is mainly hydrogen sulfide, the liquid caustic soda liquid reserve tank in the external world is escaped into by pipeline, both chemically react
NaHS is generated, product packaging sale can be made；By liquid substance remaining in high-temperature pyrolysis reactor, main component is pitch
The heterocyclic compound of shape, it is standby；
（4）Collection is handled：By step（3）Remaining liquid hetero-ring compounds, are transferred into by booster pump and store water and close
In the holding vessel of envelope, treat that the heterocyclic compound of pitch shape is cooled to normal temperature, become blocks of solid, afterwards take out blocks of solid,
Dress bag, can be used as the raw material for manufacturing waterproof material；
（5）Gas is recycled：Pre-add is heat-treated, low-temperature catalytic pyrolysis processing, the gas produced in Pintsch process processing procedure
After body component is condensed through cooling device, centralized collection, the reproduction for di-mercaptobenzothiazolby.
It is preferred that, the heater is anti-explosion electric heater.
It is preferred that, the catalytic cracking reaction device is the WXY-4304-1 type catalytic cracking reaction devices of customization version, and buying is certainly
The unrestrained pharmaceutical chemical industry equipment Co., Ltd of Wuxi City snow.
It is preferred that, the cooling device is gas trap.
It is preferred that, the holding vessel is irony holding vessel.
The present invention has the following advantages that：This kind of waste resin is carried out innoxious place by the invention by a series of flows
After reason, the solid product ultimately formed reaches water insoluble, tasteless, non-ignitable purpose, and can be used as a kind of waterproof material
Raw material is used, and gaseous state distillate can continue to participate in the production of di-mercaptobenzothiazolby after cooled as raw material, as anti-
The sale of water material is producing economic benefit and while social benefit, it is thus also avoided that the problem of hazardous waste long term storage and directly
The problem of burning processing produces secondary pollution, spent resin transfers to the processing of hazardous waste treating stations to deliver 3000 yuan/ton, and the work
About 1000 yuan/ton of the processing cost of skill, waste realizes repetition recycling, also greatlys save cost, and the technical process is real
Cracking section product is given birth to di-mercaptobenzothiazolby as raw material again, realized by the totally enclosed operation of row, pollution-free, no danger
Recycling, greatly reduces production cost, economizes on resources, enhance the competitiveness of product.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Embodiment
With reference to specific embodiment, the invention is further described.
Embodiment 1：A kind of harmless treatment process of spent resin, comprises the following steps：
（1）Pre-add is heat-treated：By the spent resin centralized collection produced in di-mercaptobenzothiazolby production process, take and be put into right amount
In pre- thermal reactor, pre- thermal reactor is cylindrical tube shape, and preheating reactor bottom and top are respectively equipped with heater and cooling
Device, heater is anti-explosion electric heater, and cooling device is gas trap, and heater carries out preliminary pre-add to spent resin
Heat is melted, and controls the temperature of reactor at 50-70 DEG C, the time is 3-5 hour, obtains the spent resin of liquid, standby；By setting
The fugitive constituent effusion that cooling device avoids spent resin from being produced in heating process is put, fugitive constituent is mainly toluene, dimethylbenzene and two
Nitric sulfid, the ratio that the amount of the toluene, dimethylbenzene and carbon disulfide accounts for above-mentioned addition spent resin total content is respectively 1-2%, 1-
2%th, 0.5-1%, belongs to inflammable, explosive, poisonous chemical substance, and heating and temperature control can be realized at 50-70 DEG C and melt spent resin completely
Liquid is melted into, is easy to next step to transmit, and can realize fugitive constituent toluene, carbon disulfide are controlled by cooling device to greatest extent
Effusion, the output end of cooling device is connected with external storage case, is easy to centralized collection to carry out the regeneration of di-mercaptobenzothiazolby
Production；
（2）Low-temperature catalytic pyrolysis processing：By above-mentioned steps（1）The standby liquid resin produced, spy is transferred into by booster pump
In the catalytic cracking reaction device of system, catalytic pyrolysis；Catalytic cracking reaction device is anti-for the WXY-4304-1 type catalytic pyrolysis of customization version
Device is answered, buying avenges unrestrained pharmaceutical chemical industry equipment Co., Ltd from Wuxi City；Catalytic cracking reaction device bottom and top are filled provided with heating
Put and cooling device, catalyst uses palladium-nickel alloy mesh catalyst, heater maintains the temperature at 70-200 DEG C, keeps pressure
Power is 10-20 hour in -1-0MPa, catalytic pyrolysis time, and the gas component cracked out has：Carbon disulfide, toluene, diformazan
Benzene, aniline, benzothiazole, the carbon disulfide, toluene, dimethylbenzene, aniline, the amount of benzothiazole gas account for above-mentioned standby liquid
The ratio of resin is respectively 0.5-1%, 1-2%, 1-2%, 1-2%, 3-5%；Discharge, filled through cooling through catalytic cracking reaction device top
Put after cooling, collected by external storage case, be convenient for the reproduction of di-mercaptobenzothiazolby；Softening point is higher and composition
Heterocyclic compound component with respect to single stable exists in liquid form, key component be respectively 25-30% heterocyclic compound,
20-30% benzothiazole diazol, 30-40% benzothiazole azo, 3-5% sulphur is standby；
（3）Pintsch process processing：By step（2）Remaining liquid component high-temperature pyrolysis reactor is transferred into by booster pump
In, heater is provided with high-temperature pyrolysis reactor, heater maintains the temperature at 200-450 DEG C, keeps pressure in -1-
0MPa, catalyst uses nickel-cobalt alloy mesh catalyst, and pyrolysis time is 20-40 hour, after treating that cracking is fully completed,
Gaseous pyrolysis product hydrogen sulfide, the liquid caustic soda liquid reserve tank in the external world is escaped into by pipeline, and both occur chemical reaction generation sulphur
Sodium hydride, can make product packaging sale；By liquid substance remaining in high-temperature pyrolysis reactor, main component is miscellaneous for pitch shape
Cycle compound, it is standby；
（4）Collection is handled：By step（3）Remaining liquid hetero-ring compounds, are transferred into by booster pump and store water and close
In the holding vessel of envelope, holding vessel is irony holding vessel, and the heterocyclic compound of pitch shape is cooled to normal temperature, becomes blocks of solid, it
Blocks of solid is taken out afterwards, bag is filled, the raw material for manufacturing waterproof material can be used as；
（5）Gas is recycled：Pre-add is heat-treated, low-temperature catalytic pyrolysis processing, the gas produced in Pintsch process processing procedure
After body component is condensed through cooling device, centralized collection, the reproduction for di-mercaptobenzothiazolby.
Under normal operating condition, the invention is carried out this kind of waste resin after harmless treatment, most by a series of flows
End form into solid product reach water insoluble, tasteless, non-ignitable purpose, and can make as a kind of raw material of waterproof material
With gaseous state distillate can continue to participate in the production of di-mercaptobenzothiazolby after cooled as raw material, be used as waterproof material pin
Sell and producing economic benefit and while social benefit, it is thus also avoided that the problem of hazardous waste long term storage and direct burning processing
The problem of producing secondary pollution, the technical process carries out totally enclosed operation, pollution-free, no danger, by cracking section product weight
New work is that raw material gives birth to di-mercaptobenzothiazolby, realizes recycling, greatly reduces production cost, economize on resources, enhances
About 30% or so material in the competitiveness of product, the spent resin that di-mercaptobenzothiazolby production is produced is changed into continuing to produce two
The raw material of mercaptobenzothiazoler, remaining most of product is converted to solid material and can used as waterproof material, all becomes
Useful product, greatlys save the resources of production；Spent resin is produced in the di-mercaptobenzothiazolby production process that the present invention is provided
Harmless treatment process tool have great advantage, environmental protection contribution is big, passes through the spent resin for producing di-mercaptobenzothiazolby and producing
In various poisonous and harmful, volatile materials extract, make di-mercaptobenzothiazolby production produce spent resin it is no longer right
Environmental danger, fundamentally solves the environmental pollution problem that spent resin processing is produced；And in whole processing procedure, do not have
There are waste water, waste gas to produce, it is to avoid secondary environmental pollution.
For the ordinary skill in the art, simply the present invention is exemplarily described for specific embodiment,
The obvious present invention, which is implemented, to be not subject to the restrictions described above, and is entered as long as employing the inventive concept and technical scheme of the present invention
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical scheme directly apply to other occasions
, within protection scope of the present invention.
Claims (5)
1. a kind of harmless treatment process of spent resin, it is characterised in that：Comprise the following steps：
（1）Pre-add is heat-treated：By the spent resin centralized collection produced in di-mercaptobenzothiazolby production process, take and be put into right amount
In pre- thermal reactor, the bottom and top of pre- thermal reactor are respectively equipped with heater and cooling device, and heater is to useless tree
Fat carries out preliminary preheating and melted, and maintains the temperature at 50-70 DEG C, the time is 3-5 hour, obtains the spent resin of liquid, standby；
Plus thermogenetic fugitive constituent is mainly toluene, dimethylbenzene and carbon disulfide, the amount of the toluene, dimethylbenzene and carbon disulfide is accounted for
The ratio for stating addition spent resin total content is respectively 1-2%, 1-2%, 0.5-1%, passes through cooling device condensation process, the cooling
The output end of device is also associated with extraneous storage bin；
（2）Low-temperature catalytic pyrolysis processing：By above-mentioned steps（1）The standby liquid resin produced, spy is transferred into by booster pump
In the catalytic cracking reaction device of system, catalytic pyrolysis；Catalytic cracking reaction device bottom and top are respectively equipped with heater and cooling
Device, catalyst uses palladium-nickel alloy mesh catalyst, and heater keeps the temperature of reactor at 70-200 DEG C, keeps pressure
Power is 10-20 hour in -1-0MPa, catalytic pyrolysis time, and the gas component cracked out has：Carbon disulfide, toluene, diformazan
Benzene, aniline, benzothiazole, the carbon disulfide, toluene, dimethylbenzene, aniline, the amount of benzothiazole gas account for above-mentioned standby liquid
The ratio of resin is respectively 0.5-1%, 1-2%, 1-2%, 1-2%, 3-5%；Cooling device of the cracked gas through catalytic cracking reaction device
Cooling, the output end of the cooling device is also associated with extraneous storage bin；Softening point is higher and composition is miscellaneous with respect to single stable
Cycle compound component exists in liquid form, and key component is respectively 25-30% heterocyclic compound, 20-30% benzothiazole
The benzothiazole azo of diazol, 30-40%, 3-5% sulphur is standby；
（3）Pintsch process processing：By step（2）Remaining liquid component high-temperature pyrolysis reactor is transferred into by booster pump
In, the bottom of high-temperature pyrolysis reactor is provided with heater, and heater keeps the temperature of reactor at 200-450 DEG C, kept
Pressure is in -1-0MPa, and catalyst uses nickel-cobalt alloy mesh catalyst, and pyrolysis time is 20-40 hour, treats cracking all
After completion, gaseous pyrolysis product is mainly hydrogen sulfide, and the liquid caustic soda liquid reserve tank in the external world is escaped into by pipeline；Pintsch process
Remaining liquid substance in reactor, main component is the heterocyclic compound of pitch shape, standby；
（4）Separate and collect processing：By step（3）Remaining liquid hetero-ring compounds, are transferred into by booster pump and store water
And sealedly treat that the heterocyclic compound of pitch shape is cooled to normal temperature in holding vessel, become blocks of solid, afterwards take blocks of solid
Go out, fill bag；
（5）Gas is recycled：Pre-add is heat-treated, low-temperature catalytic pyrolysis processing, the gas produced in Pintsch process processing procedure
After body component is condensed through cooling device, centralized collection, the reproduction for di-mercaptobenzothiazolby.
2. a kind of harmless treatment process of spent resin according to claim 1, it is characterised in that：The heater is
Anti-explosion electric heater.
3. a kind of harmless treatment process of spent resin according to claim 1, it is characterised in that：The catalytic pyrolysis is anti-
It is WXY-4304-1 type catalytic cracking reaction devices to answer device.
4. a kind of harmless treatment process of spent resin according to claim 1, it is characterised in that：The cooling device is
Gas trap.
5. a kind of harmless treatment process of spent resin according to claim 1, it is characterised in that：The holding vessel is iron
Matter holding vessel.
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| CN201710518047.0A CN107286910A (en) | 2017-06-29 | 2017-06-29 | A kind of harmless treatment process of spent resin |
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| CN201710518047.0A CN107286910A (en) | 2017-06-29 | 2017-06-29 | A kind of harmless treatment process of spent resin |
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| CN201710518047.0A Pending CN107286910A (en) | 2017-06-29 | 2017-06-29 | A kind of harmless treatment process of spent resin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073317A (en) * | 2019-12-19 | 2020-04-28 | 山东省交通科学研究院 | Composite modified asphalt and preparation method thereof |
| CN111103422A (en) * | 2020-01-08 | 2020-05-05 | 中国辐射防护研究院 | Waste resin pyrolysis test device |
| CN112919469A (en) * | 2021-01-28 | 2021-06-08 | 河南乾瑞化工科技有限公司 | Recycling method of waste resin of accelerator M |
| CN117660039A (en) * | 2023-11-07 | 2024-03-08 | 东莞市高誉机械设备有限公司 | Cracking oil production device and cracking oil production process for waste resin powder |
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| CN1898220A (en) * | 2003-12-23 | 2007-01-17 | 杜斯乐联合股份公司 | Method of obtaining 2-mercaptobenzothiazole |
| CN102603668A (en) * | 2012-02-21 | 2012-07-25 | 刘炤 | Method for treating 2-mercaptobenzothiazole production waste |
| CN106243059A (en) * | 2016-07-26 | 2016-12-21 | 濮阳蔚林化工股份有限公司 | A kind of method extracting benzothiazole from 2 benzothiazolyl mercaptans production by-products |
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2017
- 2017-06-29 CN CN201710518047.0A patent/CN107286910A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1898220A (en) * | 2003-12-23 | 2007-01-17 | 杜斯乐联合股份公司 | Method of obtaining 2-mercaptobenzothiazole |
| CN102603668A (en) * | 2012-02-21 | 2012-07-25 | 刘炤 | Method for treating 2-mercaptobenzothiazole production waste |
| CN106243059A (en) * | 2016-07-26 | 2016-12-21 | 濮阳蔚林化工股份有限公司 | A kind of method extracting benzothiazole from 2 benzothiazolyl mercaptans production by-products |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073317A (en) * | 2019-12-19 | 2020-04-28 | 山东省交通科学研究院 | Composite modified asphalt and preparation method thereof |
| CN111103422A (en) * | 2020-01-08 | 2020-05-05 | 中国辐射防护研究院 | Waste resin pyrolysis test device |
| CN112919469A (en) * | 2021-01-28 | 2021-06-08 | 河南乾瑞化工科技有限公司 | Recycling method of waste resin of accelerator M |
| CN117660039A (en) * | 2023-11-07 | 2024-03-08 | 东莞市高誉机械设备有限公司 | Cracking oil production device and cracking oil production process for waste resin powder |
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Application publication date: 20171024 |