CN112063405B - Pyrolysis-based waste tire treatment method - Google Patents
Pyrolysis-based waste tire treatment method Download PDFInfo
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- CN112063405B CN112063405B CN202010961146.8A CN202010961146A CN112063405B CN 112063405 B CN112063405 B CN 112063405B CN 202010961146 A CN202010961146 A CN 202010961146A CN 112063405 B CN112063405 B CN 112063405B
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- swelling
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/07—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of solid raw materials consisting of synthetic polymeric materials, e.g. tyres
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
- Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
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- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
A pyrolysis-based waste tire treatment method comprises the following steps: step 1: feeding the swelling solvent and the rubber particles of the waste tire into a swelling tank for swelling treatment; step 2: after the swelling treatment is finished, pouring the proppant powder into the mixture of the swelling rubber and the swelling solvent, and stirring and mixing to enable the proppant to enter the pore channels of the swelling rubber; and step 3: carrying out treatment of evaporating swelling solvent on the mixture obtained in the step 2; and 4, step 4: after the evaporation treatment is finished, obtaining a mixture of the swollen rubber particles, the carbon black and the residual propping agent, filtering the mixture, and separating the swollen rubber particles; and 5: taking the swollen rubber particles obtained by filtering as a pyrolysis raw material, and carrying out pyrolysis operation to finish the harmless treatment of the swollen rubber; by adding the proppant powder after the swelling treatment of the waste tire rubber particles, the volume shrinkage of the swelling rubber in the solvent evaporation process is avoided.
Description
Technical Field
The invention relates to the field of swelling treatment, in particular to a pyrolysis-based waste tire treatment method.
Background
With the development of the automobile field, a large number of automobiles are replaced every year, wherein a large number of waste tires are generated every year in the world along with the replacement of the automobiles, and the main components of the waste tires are natural rubber, styrene butadiene rubber, butadiene rubber and the like. If the waste rubber tires are not treated in time, a large amount of land resources are occupied, mosquitoes and flies are bred, the possibility of spreading diseases is improved, on the other hand, the hidden danger of fire is buried, and serious environmental protection problems and social problems are caused, so that the waste rubber tires must be subjected to harmless treatment or processed and recycled.
Because the main component of the waste tire is rubber, the rubber can be treated by a pyrolysis process at present, and the pyrolysis process comprises supercritical pyrolysis, microwave pyrolysis, catalytic pyrolysis and vacuum pyrolysis technologies. In order to shorten the time consumption of the pyrolysis process, the waste rubber tires are crushed into small particles and then pyrolyzed.
But the junked tire pyrolysis technology of present mainstream because the coefficient of heat conductivity of rubber is lower, and in the initial stage of pyrolysis, the heat can't be conducted the inside of rubber granule fast, leads to in the pyrolysis initial stage, and the conversion efficiency of energy is low, leads to some technological and engineering problems, for example can cause the operating mode production difference that opens and stop stage and middle pyrolysis stage for the quality of pyrolysis product is unstable etc..
In order to further improve the pyrolysis efficiency of waste tires, two methods are mainly used at present, one of which is to increase the specific surface area of rubber particles by further reducing the particle size of the rubber particles, but the method crushes the waste rubber in a cryogenic environment and consumes a large amount of energy; secondly, the specific surface area of the waste rubber is increased by increasing the pore size distribution and the number of pore channels of the material, and more pore structures are favorable for pyrolysis atmosphere to rapidly enter the inside of the particles. The second treatment method can be realized by swelling rubber, wherein the swelling of rubber refers to the phenomenon that the volume of a rubber high molecular polymer is expanded in a solvent; the non-polymer materials in the waste tires do not participate in the swelling process and are discharged during the swelling process of the rubber, such as carbon black and the like. After the swelling treatment, the internal pore structure of the rubber becomes more developed, but the swollen rubber rapidly shrinks back to the original state along with the evaporation of the solvent. In the pyrolysis reaction, the swollen state of the rubber cannot be maintained for a long time, whether the solvent is evaporated in advance or the swollen rubber with the solvent is directly put into the reactor. It is therefore necessary to find a method which allows the rubber after completion of swelling to maintain the swollen state after the solvent has evaporated off.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide a pyrolysis-based waste tire treatment method, which is used for filling materials in a pore channel of swelling rubber to keep the swelling of the rubber and maintain the pore channel so as to facilitate the pyrolysis of the rubber.
A pyrolysis-based waste tire treatment method comprises the following steps:
step 1: feeding the swelling solvent and the rubber particles of the waste tire into a swelling tank for swelling treatment;
step 2: after the swelling treatment is finished, pouring the proppant powder into the mixture of the swelling rubber and the swelling solvent, and stirring and mixing to enable the proppant to enter the pore channels of the swelling rubber;
and step 3: carrying out treatment of evaporating swelling solvent on the mixture obtained in the step 2;
and 4, step 4: after the evaporation treatment is finished, obtaining a mixture of the swollen rubber particles, the carbon black and the residual propping agent, filtering the mixture, and separating the swollen rubber particles;
and 5: and (3) taking the swollen rubber particles obtained by filtering as a pyrolysis raw material, and carrying out pyrolysis operation to finish the harmless treatment of the swollen rubber.
Further, in the step 2, the proppant powder comprises one or any combination of lithium chloride, potassium chloride, silicon dioxide, calcium dioxide, aluminum oxide, iron oxide, titanium oxide, copper oxide, carbon nanotubes, artificial ceramic particles and resin-coated sand.
Further, the particle size range of the propping agent powder in the step 2 is 500nm-800 μm, and the mass ratio of the added propping agent powder to the mass of the waste tire rubber particles in the step 1 is 0.1% -150%.
Further, the particle size range of the proppant powder in the step 2 is 50-200 μm, and the mass ratio of the added proppant powder to the mass of the waste tire rubber particles in the step 1 is 8-15%.
Further, the swelling treatment in step 1 is performed at normal temperature or at elevated temperature.
Further, the swelling treatment is carried out in an environment of increasing temperature, and the maximum temperature does not exceed 300 ℃.
Further, the swelling solvent comprises one or any combination of toluene, benzene, xylene, chloroform, carbon tetrachloride, cyclohexane, heptane, methanol, ethanol, n-butanol, acetone, cyclohexanone, methyl ethyl ketone, ethyl acetate, amyl acetate, kerosene, gasoline and diesel oil.
Further, the stirring in the step 2 is ultrasonic stirring.
Further, the stirring speed in the step 2 is in the range of 500 r/min-700 r/min.
Further, the evaporation treatment in step 3 may be heating evaporation or vacuum drying evaporation or a combination of the two, wherein the temperature of the heating evaporation does not exceed 200 ℃.
The invention has the beneficial effects that:
after swelling treatment of the waste tire rubber particles is completed, adding the propping agent powder to mix the propping agent powder into the pore channels of the swelling rubber and support the pore channels, so that the volume shrinkage of the swelling rubber in the process of solvent evaporation is avoided, the specific surface area of the solid swelling rubber particles obtained after solvent evaporation and the initial waste tire rubber particles is increased, the pyrolysis reaction of the swelling rubber is facilitated, the swelling rubber particles can be uniformly and rapidly heated in the initial pyrolysis stage, and the pyrolysis process is optimized;
stirring is carried out in the process of mixing the proppant powder, so that the uniform mixing of the proppant powder and the swelling rubber is accelerated, wherein the stirring can be carried out by adopting a stirrer for stirring or ultrasonic stirring or the combination of the stirring and the ultrasonic stirring, and the flow is further accelerated;
by filtering the mixture of the swollen rubber particles, the carbon black and the residual proppant obtained by filtering can be utilized, and resources are saved.
Description of the drawings:
FIG. 1 is a flow chart of the present invention.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict.
As shown in fig. 1, a method for processing waste tires based on pyrolysis includes the following steps:
step 1: feeding the swelling solvent and the rubber particles of the waste tire into a swelling tank for swelling treatment;
step 2: after the swelling treatment is finished, pouring the proppant powder into the mixture of the swelling rubber and the swelling solvent, and stirring and mixing to enable the proppant to enter the pore channels of the swelling rubber;
and step 3: carrying out treatment of evaporating swelling solvent on the mixture obtained in the step 2;
and 4, step 4: after the evaporation treatment is finished, obtaining a mixture of the swollen rubber particles, the carbon black and the residual propping agent, and filtering the mixture to separate the swollen rubber particles;
and 5: and taking the filtered swollen rubber particles as a pyrolysis raw material, and carrying out pyrolysis operation to finish the harmless treatment of the swollen rubber.
The swelling treatment in the step 1 is conventional rubber swelling, the swelling treatment is carried out at normal temperature or in a heating environment, wherein the swelling treatment process in the step 1 can be completed more quickly in the heating environment, and if the heating environment is selected for swelling treatment, the temperature is gradually increased, and the highest temperature is not more than 300 ℃. The swelling solvent comprises one or any combination of toluene, benzene, xylene, chloroform, carbon tetrachloride, cyclohexane, heptane, methanol, ethanol, n-butanol, acetone, cyclohexanone, methyl ethyl ketone, ethyl acetate, amyl acetate, kerosene, gasoline and diesel oil. Stirring is needed in the swelling treatment process, the swelling solvent and the rubber particles of the waste tire can be fully mixed firstly, the swelling process of the rubber can be further accelerated, and the carbon black in the swollen rubber can be discharged conveniently. Wherein the time range of stirring after adding the swelling solvent is 30min-540min, preferably 60min-120 min. It should be noted that impurities in the waste tire, including steel wires, mesh cloth, etc., need to be extracted in advance in the process of preparing the waste tire rubber particles. The particle size range of the waste tire rubber particles is 10mm-20 mm.
In the step 2, the proppant powder is added and stirred for mixing, and the stirring is completed through ultrasonic treatment. Because the swelling of the waste tire rubber particles is finished, the damage to the structure of the swollen rubber caused by too fast stirring needs to be avoided, so the stirring speed is in the range of 10r/min-10000r/min, and the preferred stirring speed is in the range of 500 r/min-700 r/min. The proppant powder comprises one or any combination of lithium chloride, potassium chloride, silicon dioxide, calcium dioxide, aluminum oxide, iron oxide, titanium oxide, copper oxide, carbon nano tubes, artificial ceramic particles and resin coated sand. The particle size of the proppant powder ranges from 500nm to 500 μm, preferably from 50 μm to 100 μm. The addition mass of the supporting agent powder is in the range of 0.1-150% of the mass of the used tire rubber particles in the step 1, wherein the preferable range is 8-15%.
The evaporation treatment in the step 3 can be heating evaporation or vacuum drying evaporation or a combination of the two. When heating and evaporation are selected, the main material of the waste tire is natural rubber, and when the heating temperature of the natural rubber exceeds 200 ℃, the natural rubber is decomposed, so that the temperature of heating treatment cannot be higher than the decomposition temperature of the rubber. If the solvent evaporation temperature is higher than 200 ℃, reduced pressure evaporation can be adopted. Wherein the evaporated swelling solvent can be recycled.
And 4, after the evaporation treatment in the step 4, solid granular swelling rubber particles and a solid powdery mixture formed by part of the propping agent and the carbon black can be obtained, the solid granular swelling rubber particles can be separated through filtering operation, and the mixture of the separated carbon black and the residual propping agent can be reused, so that resources are saved.
In the step 5, after the rubber pyrolysis is completed, the propping agent is left in the solid pyrolysis ash as a part of the pyrolysis ash, and the pyrolysis ash can be separated through simple filtration treatment.
The first embodiment is as follows:
a pyrolysis-based waste tire treatment method comprises the following steps:
firstly, crushing the waste tires to obtain waste tire rubber particles with the average particle size of 13 mm; stirring and mixing the waste tire rubber particles and a toluene swelling solvent according to the mass ratio of 1:3 for 1 hour, and standing for 3 hours to complete swelling treatment; adding SiO2 which accounts for 10 percent of the dry weight of the waste tire rubber particles into the rubber swelling solution, wherein SiO2 is used as propping agent powder, and the particle size range of SiO2 is 50-150 mu m; stirring the rubber swelling solution added with the proppant powder at the stirring speed of 120r/min for 100 min; then heating to 120 ℃, and carrying out evaporation treatment under the environment of 120 ℃ to evaporate the solvent swelling with toluene; and finally, filtering, separating out the swollen rubber particles, and performing pyrolysis operation by using the swollen rubber particles as a pyrolysis raw material to finish the harmless treatment of the waste tires.
Example two:
a pyrolysis-based waste tire treatment method comprises the following steps:
firstly, crushing the waste tires to obtain waste tire rubber particles with the average particle size of 16 mm; stirring and mixing the waste tire colloidal particles and the carbon tetrachloride swelling solvent according to the mass ratio of 1:5 for 1 hour, and standing for 1 hour to complete swelling treatment; adding potassium chloride which accounts for 20 percent of the dry weight of the waste tire rubber particles into the rubber swelling solution, wherein the potassium chloride is used as proppant powder; stirring the rubber swelling solution added with the proppant powder at the stirring speed of 120r/min for 60 min; and then heating to 90 ℃, evaporating the carbon tetrachloride swelling solvent at the temperature of 90 ℃ to obtain swollen rubber particles and carbon black, wherein the swollen rubber particles are used as pyrolysis raw materials to carry out pyrolysis operation, and the harmless treatment of the waste tires is completed.
Example three:
a pyrolysis-based waste tire treatment method comprises the following steps:
firstly, crushing the waste tires to obtain waste tire rubber particles with the average particle size of 16 mm; stirring and mixing the waste tire rubber particles and a cyclohexane swelling solvent according to the mass ratio of 1:4 for 1 hour, and standing for 2 hours to complete swelling treatment; adding iron oxide which accounts for 10 percent of the dry weight of the rubber particles of the waste tire into the rubber swelling solution, wherein the iron oxide is used as proppant powder, and the particle size range of the iron oxide is 500nm-20 mu m; stirring the rubber swelling solution added with the proppant powder at the stirring speed of 120r/min, and simultaneously carrying out ultrasonic auxiliary stirring at the power of 20kHz and 400W for 120 min; and then heating to 90 ℃, and evaporating the cyclohexane swelling solvent at the temperature of 90 ℃ to obtain swollen rubber particles and carbon black, wherein the swollen rubber particles are used as pyrolysis raw materials to carry out pyrolysis operation, so that the harmless treatment of the waste tires is completed.
The above description is only a few specific examples of the present invention and should not be construed as limiting the invention in any way. It will be apparent to persons skilled in the relevant art(s) that, having the benefit of this disclosure and its principles, various modifications and changes in form and detail can be made without departing from the principles and structures of the invention, which are, however, encompassed by the appended claims.
Claims (4)
1. A method for processing waste tires based on pyrolysis is characterized by comprising the following steps:
step 1: feeding the swelling solvent and the rubber particles of the waste tire into a swelling tank for swelling treatment;
step 2: after the swelling treatment is finished, pouring the proppant powder into the mixture of the swelling rubber and the swelling solvent, and stirring and mixing;
and step 3: carrying out treatment of evaporating swelling solvent on the mixture obtained in the step 2;
and 4, step 4: after the evaporation treatment is finished, obtaining a mixture of the swollen rubber particles, the carbon black and the residual propping agent, filtering the mixture, and separating the swollen rubber particles;
and 5: taking the swollen rubber particles obtained by filtering as a pyrolysis raw material, and carrying out pyrolysis operation to finish the harmless treatment of the swollen rubber;
the swelling treatment in the step 1 comprises a stirring step, wherein the stirring time is 30-540 min; the waste tire particles need to be pretreated before swelling treatment, impurities in the waste tire particles are removed, the impurities comprise steel wires and screen cloth, and the particle size range of the pretreated waste tire particles is 10-20 mm;
in the step 2, the proppant powder comprises one or any combination of lithium chloride, potassium chloride and carbon nanotubes;
the particle size range of the propping agent powder in the step 2 is 50-100 mu m, and the mass ratio of the added propping agent powder to the mass of the waste tire rubber particles in the step 1 is 8-15%;
the stirring in the step 2 is ultrasonic stirring, and the stirring speed range is 500 r/min-700 r/min;
the swelling solvent comprises one or any combination of toluene, benzene, xylene, chloroform, carbon tetrachloride, cyclohexane, heptane, methanol, ethanol, n-butanol, acetone, cyclohexanone, methyl ethyl ketone, ethyl acetate, amyl acetate, kerosene, gasoline and diesel oil.
2. The method for processing waste and old tires based on pyrolysis as claimed in claim 1, wherein the swelling process in step 1 is performed under normal temperature or elevated temperature environment.
3. A method for the treatment of scrap tyres based on pyrolysis according to claim 1, characterized in that said swelling treatment is carried out in an environment with an elevated temperature, the maximum temperature not exceeding 300 ℃.
4. The method for processing waste and old tires based on pyrolysis according to claim 1, wherein the evaporation treatment in step 3 is heating evaporation or vacuum drying evaporation or a combination of the two, wherein the temperature of the heating evaporation does not exceed 200 ℃.
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Citations (5)
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| BR9504429A (en) * | 1995-10-17 | 1997-05-27 | Da Cunha Lima Luiz Ca Oliveira | Improved process for the regeneration of vulcanized or semi-vulcanized rubber |
| CN106397652A (en) * | 2016-09-14 | 2017-02-15 | 济南大学 | Method for preparing super-macroporous high-specific-area polymer |
| CN106995542A (en) * | 2017-05-18 | 2017-08-01 | 贵州理工学院 | A kind of high swelling ratio butadiene-styrene rubber and preparation method thereof |
| CN110475824A (en) * | 2017-04-18 | 2019-11-19 | 善路设备有限公司 | Rubber composite material and technique for obtaining the rubber composite material |
| CN110577665A (en) * | 2018-06-09 | 2019-12-17 | 益科达回收有限公司 | reprocessed rubber and process for producing the same |
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2020
- 2020-09-14 CN CN202010961146.8A patent/CN112063405B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BR9504429A (en) * | 1995-10-17 | 1997-05-27 | Da Cunha Lima Luiz Ca Oliveira | Improved process for the regeneration of vulcanized or semi-vulcanized rubber |
| CN106397652A (en) * | 2016-09-14 | 2017-02-15 | 济南大学 | Method for preparing super-macroporous high-specific-area polymer |
| CN110475824A (en) * | 2017-04-18 | 2019-11-19 | 善路设备有限公司 | Rubber composite material and technique for obtaining the rubber composite material |
| CN106995542A (en) * | 2017-05-18 | 2017-08-01 | 贵州理工学院 | A kind of high swelling ratio butadiene-styrene rubber and preparation method thereof |
| CN110577665A (en) * | 2018-06-09 | 2019-12-17 | 益科达回收有限公司 | reprocessed rubber and process for producing the same |
Non-Patent Citations (1)
| Title |
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| 废旧轮胎溶胀特性将其半焦热重分析实验;程文飞等;《有色金属科学与工程》;20181231;正文第2节 * |
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