CN101164876A - Method for preparing carbon black and active carbon from waste tyre pyrolytic carbon - Google Patents
Method for preparing carbon black and active carbon from waste tyre pyrolytic carbon Download PDFInfo
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- CN101164876A CN101164876A CNA2007100613208A CN200710061320A CN101164876A CN 101164876 A CN101164876 A CN 101164876A CN A2007100613208 A CNA2007100613208 A CN A2007100613208A CN 200710061320 A CN200710061320 A CN 200710061320A CN 101164876 A CN101164876 A CN 101164876A
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Abstract
This invention relates to a method for preparing carbon-black and activated-carbon, by using waste-tyre as raw material after thermal decomposition and modification. The procedures are as follows: the carbon black from waste tyre is fed into a bag made from filter paper, extracted in flask with organic solvent; the solid is air-dried, weighing, the liquid is proceeded distillation for removing solvent, collecting the residul oil from the carbon black. The carbon black thus treated is put into a flask together with dilute acid, proceeded by agitation, vacuum filtering. The carbon black is then placed in quartz ship, and they are put in quartz tube, connected with flask with distilled water in it; heating the distilled water at 150-1000deg.C for treating the carbon black, drying, obtaining the final carbon black and activated carbon. Advantages are: reutilization of solvent and residual oil, utilization of dilute acid (less corrosion), high purity and high specific superficial area of final products.
Description
Technical field
The present invention relates to by carbon black modified Processing of Preparation carbon black and process of active carbon, particularly the modification Processing of Preparation carbon black and the gac of waste tyre pyrolytic charcoal.
Background technology
Along with developing of automobile industry and automobile constantly update, junked tire be treated as serious environmental problem day by day, not only cause the huge waste of resource, and become a kind of endanger increasing " black pollution ".At present, it is one of the most desirable recoverying and utilizing method that junked tire is carried out pyrolysis, and its reclaims pyrolytic carbon, oil product, high heating value combustion gas and the steel wire etc. of high added value, thereby has fully reclaimed the precious resources of damaged tire.The productive rate of waste tyre pyrolytic charcoal is about 39%～44%, and how utilizing this part pyrolytic carbon is the key factor that is related to waste tyre pyrolytic process economics practicality.The carbon black demand in the whole world constantly increases at present, and according to the prediction of U.S. Notch consulting group, global carbon black demand annual growth is expected to be 3.6% in 5 years from now on.And the rising of carbon black price is not consistent with the quick rise of its stock oil and gas cost, and this has been brought unprecedented in history impact to the carbon black industry.
Commercial carbon blacks and waste tyre pyrolytic charcoal have essentially identical agent structure, as seen, replace expensive stock oil to produce carbon black with the waste tyre pyrolytic charcoal, not only can solve the environmental issue that damaged tire produces, and also can alleviate the situation that is critical in carbon black market simultaneously.But deposited the carbonaceous coking material on the pyrolytic carbon surface, covered the surfactivity position of some amount, influenced the use properties of pyrolytic carbon, therefore, Research on Surface Modification by pyrolytic carbon, the carbon black materials of preparation high added value just can make renewable resource make the best use of everything, and the maximum regeneration of performance is worth, and has very important significance.
The carbon black demand in the whole world constantly increases at present, wherein 70% is used for tyre industry, and still, the waste tyre pyrolytic carbon black is owing to be subjected to the restriction of surface tissue, can only be used for the production of low-grade bias tyre, and tire uses sooty demand major part from high performance radial at present; And, automobile industry development has the trend of postponement, the tire reinforcement increases (2.6%) with the sooty demand and has been lower than the mean level (ML) (3.5%) that the carbon black demand increases, therefore prepare high structure, high performance carbon black by the modification of waste tyre pyrolytic charcoal, be used to produce high-grade tire and other rubber items, perhaps be used for industries such as manufacture of ink, sorbent material, caused domestic and international colleague's very big concern, and correspondingly various research work have been carried out, but up to now, also there is not the investigator to propose to carry out industrialized effective pyrolytic carbon method of modifying.
The United States Patent (USP) Nr.5894012 of Dension has described the whole bag of tricks and the equipment configuration that the waste rubber pyrolysis in the doughnut becomes carbon black solid, low density appropriate hydrocarbon gas and liquid hydrocarbon ils, though its refining sooty production system can remove metal and the glass fibre fragment is produced the quite high carbon black of grade, but it has still comprised the impurity atom that is difficult to remove (metal oxide particle of about 2.5wt% and sulphur particle and silicon-dioxide) that remains from basic pyrolytic process.Such impurity makes this kind carbon black all can not use the higher part of carbon black refining grade at toning agent of Xerographic printer and laser printer etc., this high-grade carbon black still mainly obtains from petroleum products at present, perhaps the hydrocarbon production that can go out from the pyrolysis that contains few magazine (Chinese patent publication number CN 1696210A).Therefore, if can make more high-grade carbon black products from the directly further refining of pyrolytic carbon black product with more economical mode, the value of so whole pyrolytic process also can obtain better marketability thus.Fed Recycling Technologies Inc of the U.S. has designed a metal oxide of applying mechanically in the sour dissolution extraction carbon black, and with the method (Chinese patent publication number CN 1481335A) of the sulphur in the organic aromatic solvent extraction acid treatment carbon black later, but this kind method has been used concentrated hydrochloric acid and organic solvent, for having relatively high expectations of equipment, running cost is also higher, still fails to be accepted by the industrial production of China.The equipment of the recovery charcoal blacks that Britain Lei Ma company makes comprises magnetic separation sieve, Vibrationsifter, regurgitates and penetrate branch selective grinding and cyclonic separator etc., they adopt physical method to extract ink pigment from the waste tyre pyrolytic carbon black, plant issue and the pollution problem of having avoided acid, alkali reaction to bring, but, their production process need be through the carbon black of the broken processing of micro mist, to having relatively high expectations of raw material, need specific preprocessing process and equipment (carbon black is translated from 2006 Vol.272 p1～5).
Gac is a kind of gas and isolating nano material of liquid adsorption of being widely used in, and very big demand is being arranged aspect the environmental improvement waste water and gas.Gac is mainly by preparations such as timber, coal and husks at present, and cost is high; If can prepare gac with junked tire with low cost, damaged tire can not only be turned waste into wealth, also can reduce the cost that gac is administered waste water and gas simultaneously greatly.Helleur (Journal of Analytical and Applied Pyrolysis 2001 (58-59), 813-824), San Miguel (Carbon 2003 (41), 1009-1016) and Harris people such as (CHEMECA 2004) adopt earlier in 450～900 ℃ of nitrogen atmosphere physically activated again in 850～1100 ℃ with water vapor, carbonic acid gas or the mixture gas treatment of the two.This method energy consumption height, and to the equipment requirements height.
This shows that the route of seeking an industrial refining waste tyre pyrolytic charcoal of suitable China as early as possible has considerable meaning for damaged tire after-treatment products high-valued.
Summary of the invention
The invention provides a kind of by waste tyre pyrolytic sooty modification Processing of Preparation carbon black and process of active carbon
The inventive method modification processing waste tyre pyrolytic charcoal prepares carbon black materials and comprises the steps:
(1) the waste tyre pyrolytic carbon black powder is packed in the paper bag that filter paper is seamed into, organic solvent is put into round-bottomed flask, Soxhlet was extracted 8 hours, to separate carbon black feed stock in the waste tyre pyrolytic charcoal and residual oil content.Then solid dries, weighs, and liquid removes out organic solvent by rotary distillation, collects residual oil product in the waste tyre pyrolytic carbon black;
(2) will remove oil content the waste tyre pyrolytic carbon black powder and diluted acid put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, suction filtration repeats above-mentioned steps twice again, gained carbon black pressed powder dries standby;
(3) carbon black powder that will remove oil content and metal oxide impurities is put into quartz boat, pack in the silica tube of electric tube furnace, the round-bottomed flask and the heated and boiled distilled water that connect the distilled water of packing at silica tube one end, use steam treatment 1～10 hour down at 150 ℃～1000 ℃ respectively, dry, obtain carbon black or gac;
Described diluted acid is selected from dilute sulphuric acid, dilute hydrochloric acid or rare nitric acid.
Organic solvent is selected from toluene, sherwood oil, methylene dichloride or ethanol, and the ratio between the raw material is: the carbon black powder of every 1g adds organic solvent 50～300ml.
The temperature of having extracted oil content and having handled in water vapour with the sour pyrolytic carbon of having removed behind the inorganic ash is 150 ℃～1000 ℃, wherein 150 ℃～700 ℃ carbon black powders that processing obtains, and 700 ℃～1000 ℃ processing obtain gac.
In the treating processes of waste tyre pyrolytic charcoal, residual oil content and inorganic ash are very big to the influence of treatment effect, the present invention adopts organic solvent and sour pretreated method first, carry out steam treatment again, has obtained the carbon black materials and the absorbent charcoal material of high purity, high-ratio surface.
The contriver has carried out XRD, XPS, nitrogen adsorption-desorption and laser particle size mensuration to carbon black materials and the absorbent charcoal material that obtains with this law, with chemical constitution, textural property and the surface properties of gained material after definite waste tyre pyrolytic charcoal modification, measurement result is seen accompanying drawing 1 ~ accompanying drawing 3.The result shows that the gained carbon black materials does not contain Zn and sulfur-bearing not substantially; Epigranular, specific surface area carbon black materials can reach 632m
2/ g, gac can reach 1240m
2/ g; Further oxidized through the carbon black materials surface that the modification processing obtains, carboxyl and carbonyl functional group's ratio increases.The contriver also is used for the gained carbon black materials absorption of methylene blue, obtains the adsorptive capacity (176mmol/g) suitable with commercial carbon black.
Compare the present invention with technology in the past following advantage arranged:
With the recyclable utilization of the residual oil content of the pyrolytic carbon of organic solvent extraction, solvent also can reuse.
Dilute sulphuric acid can be removed inorganic ash residual in the waste tyre pyrolytic charcoal effectively, the equipment corrosion problem of avoiding concentrated acid to bring simultaneously.The pretreated waste tyre pyrolytic charcoal of process can obtain the carbon black materials and the gac of high purity, high-specific surface area by simple steam treatment, and the gained material is used for the absorption of methylene blue, obtains the adsorptive capacity suitable with commercial gac.
Description of drawings
The XRD spectra of accompanying drawing 1 carbon black and gac (A carbon black, B gac)
The XPS spectrum figure of accompanying drawing 2 materials
Embodiment
The feature that the invention is further illustrated by the following examples, but the present invention is not limited to following example.
Embodiment 1,
Getting 1g waste tyre pyrolytic sooty powder packs in the paper bag that filter paper is seamed into, place the return line of apparatus,Soxhlet's, get 100ml toluene and put into round-bottomed flask, carry out Soxhlet and extracted 8 hours, liquid is removed out organic solvent by rotary distillation, collect the oil product in the waste tyre pyrolytic carbon black.The paper bag that sample is equipped with in taking-up dries, and collects the exsiccant solid.Get this solid of 1g and 30ml concentration and be the dilute sulphuric acid of 0.1mol/L and put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, and suction filtration repeats above-mentioned steps twice again, and final suction filtration gained solid dries.Get dried this solid and put into quartz boat, pack in the silica tube of electric tube furnace, connect the round-bottomed flask and the heated and boiled distilled water of the distilled water of packing at silica tube one end, respectively at 150 ℃ down with steam treatment 4 hours, the solid that finally obtains is dried, and can obtain specific surface is 97m
2/ g carbon black materials.
Embodiment 2,
Getting 1g waste tyre pyrolytic sooty powder packs in the paper bag that filter paper is seamed into, place the return line of apparatus,Soxhlet's, get 100ml toluene and put into round-bottomed flask, carry out Soxhlet and extracted 8 hours, liquid is removed out organic solvent by rotary distillation, collect the oil product in the waste tyre pyrolytic carbon black.The paper bag that sample is equipped with in taking-up dries, and collects the exsiccant solid.Get this solid of 1g and 30ml concentration and be the dilute sulphuric acid of 0.1mol/L and put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, and suction filtration repeats above-mentioned steps twice again, and final suction filtration gained solid dries.Get dried this solid and put into quartz boat, pack in the silica tube of electric tube furnace, connect the round-bottomed flask and the heated and boiled distilled water of the distilled water of packing at silica tube one end, respectively at 400 ℃ down with steam treatment 4 hours, the solid that finally obtains is dried, and can obtain specific surface is 353m
2/ g carbon black materials.
Embodiment 3,
Getting 1g waste tyre pyrolytic sooty powder packs in the paper bag that filter paper is seamed into, place the return line of apparatus,Soxhlet's, get 100ml toluene and put into round-bottomed flask, carry out Soxhlet and extracted 8 hours, liquid is removed out organic solvent by rotary distillation, collect the oil product in the waste tyre pyrolytic carbon black.The paper bag that sample is equipped with in taking-up dries, and collects the exsiccant solid.Get this solid of 1g and 30ml concentration and be the dilute sulphuric acid of 0.1mol/L and put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, and suction filtration repeats above-mentioned steps twice again, and final suction filtration gained solid dries.Get dried this solid and put into quartz boat, pack in the silica tube of electric tube furnace, connect the round-bottomed flask and the heated and boiled distilled water of the distilled water of packing at silica tube one end, respectively at 700 ℃ down with steam treatment 4 hours, the solid that finally obtains is dried, and can obtain specific surface is 632m
2/ g carbon black materials.
Embodiment 4,
Getting 1g waste tyre pyrolytic sooty powder packs in the paper bag that filter paper is seamed into, place the return line of apparatus,Soxhlet's, get 100ml toluene and put into round-bottomed flask, carry out Soxhlet and extracted 8 hours, liquid is removed out organic solvent by rotary distillation, collect the oil product in the waste tyre pyrolytic carbon black.The paper bag that sample is equipped with in taking-up dries, and collects the exsiccant solid.Get this solid of 1g and 30ml concentration and be the dilute sulphuric acid of 0.1mol/L and put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, and suction filtration repeats above-mentioned steps twice again, and final suction filtration gained solid dries.Get dried this solid and put into quartz boat, pack in the silica tube of electric tube furnace, connect the round-bottomed flask and the heated and boiled distilled water of the distilled water of packing at silica tube one end, respectively at 700 ℃ down with steam treatment 8 hours, the solid that finally obtains is dried, and can obtain specific surface is 972m
2/ g absorbent charcoal material.
Embodiment 5,
Getting 1g waste tyre pyrolytic sooty powder packs in the paper bag that filter paper is seamed into, place the return line of apparatus,Soxhlet's, get 100ml toluene and put into round-bottomed flask, carry out Soxhlet and extracted 8 hours, liquid is removed out organic solvent by rotary distillation, collect the oil product in the waste tyre pyrolytic carbon black.The paper bag that sample is equipped with in taking-up dries, and collects the exsiccant solid.Get this solid of 1g and 30ml concentration and be the dilute sulphuric acid of 0.1mol/L and put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, and suction filtration repeats above-mentioned steps twice again, and final suction filtration gained solid dries.Get dried this solid and put into quartz boat, pack in the silica tube of electric tube furnace, connect the round-bottomed flask and the heated and boiled distilled water of the distilled water of packing at silica tube one end, respectively at 900 ℃ down with steam treatment 4 hours, the solid that finally obtains is dried, and can obtain specific surface is 1240m
2/ g absorbent charcoal material.
Claims (3)
1. one kind by waste tyre pyrolytic sooty modification Processing of Preparation high quality carbon black or process of active carbon, it is characterized in that adopting the method for steam treatment that preprocessing process is arranged, and concrete grammar may further comprise the steps:
(1) the waste tyre pyrolytic carbon black powder is packed in the paper bag that filter paper is seamed into, organic solvent is put into round-bottomed flask, Soxhlet was extracted 8 hours, to separate carbon black feed stock in the waste tyre pyrolytic charcoal and residual oil content.Then solid dries, weighs, and liquid removes out organic solvent by rotary distillation, collects residual oil product in the waste tyre pyrolytic carbon black;
(2) will remove oil content the waste tyre pyrolytic carbon black powder and diluted acid put into round-bottomed flask, 30 ℃ were stirred 0.5 hour, suction filtration repeats above-mentioned steps twice again, gained carbon black pressed powder dries standby;
(3) carbon black powder that will remove oil content and metal oxide impurities is put into quartz boat, pack in the silica tube of electric tube furnace, the round-bottomed flask and the heated and boiled distilled water that connect the distilled water of packing at silica tube one end, use steam treatment 1～10 hour down at 150 ℃～1000 ℃ respectively, dry, obtain carbon black or gac;
Described diluted acid is selected from dilute sulphuric acid, dilute hydrochloric acid or rare nitric acid.
2. method according to claim 1 is characterized in that organic solvent is selected from toluene, sherwood oil, methylene dichloride or ethanol, and the ratio between the raw material is: the carbon black powder of every 1g adds organic solvent 50～300ml.
3. method according to claim 1, it is characterized in that, the temperature of having extracted oil content in the step (3) and having handled in water vapour with the sour pyrolytic carbon of having removed behind the inorganic ash is 150 ℃～1000 ℃, wherein 150 ℃～700 ℃ carbon black powders that processing obtains, 700 ℃～1000 ℃ processing obtain gac.
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| CN102214516A (en) * | 2011-03-17 | 2011-10-12 | 南开大学 | Method for preparing capacitor electrode material from waste tire pyrolytic carbon |
| CN102224103A (en) * | 2008-11-20 | 2011-10-19 | R.J.雷诺兹烟草公司 | Carbonaceous material having modified pore structure |
| CN102580674A (en) * | 2012-02-21 | 2012-07-18 | 南开大学 | Method for preparing mercury removal agent by utilizing modified waste tire pyrolysis residue |
| CN103013188A (en) * | 2012-12-11 | 2013-04-03 | 开平市康汇橡胶制品有限公司 | Production process for environment-friendly carbon black powder |
| CN103265828A (en) * | 2013-05-08 | 2013-08-28 | 明溪县宝福再生资源开发中心 | Solid phase grafting modification method of regeneration pyrolysis carbon black |
| CN105331147A (en) * | 2015-10-28 | 2016-02-17 | 贵州安泰再生资源科技有限公司 | Method of preparing carbon black from junked tires |
| CN106276892A (en) * | 2016-08-05 | 2017-01-04 | 北京林业大学 | A kind of method preparing pressed active carbon for raw material with thermal cracking charcoal |
| CN107488455A (en) * | 2017-08-17 | 2017-12-19 | 太原理工大学 | A kind of method that thermal decomposing waste tire residue is upgraded to tire carbon black |
| CN109289773A (en) * | 2018-11-07 | 2019-02-01 | 华侨大学 | A method of it is pyrolyzed using scrap tire powder as raw material and prepares magnetic carbon black adsorbent |
| CN109513423A (en) * | 2018-11-26 | 2019-03-26 | 厦门庚能新材料技术有限公司 | A kind of magnetism carbon black adsorbent, preparation method and application |
| CN110760204A (en) * | 2019-10-25 | 2020-02-07 | 珠海格力绿色再生资源有限公司 | System and method for reducing soot ash content of waste tire cracking carbon and recovering Zn |
| CN110878148A (en) * | 2019-11-19 | 2020-03-13 | 珠海格力绿色再生资源有限公司 | Method for modifying pyrolysis carbon black |
| CN111500092A (en) * | 2020-04-15 | 2020-08-07 | 安徽省克林泰迩再生资源科技有限公司 | Modification treatment method of waste tire cracking carbon black |
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| CN113501519A (en) * | 2021-08-02 | 2021-10-15 | 江苏龙腾城矿环境技术有限公司 | Method for preparing activated carbon and recovering zinc by utilizing waste tire rubber pyrolytic carbon |
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- 2007-09-30 CN CNA2007100613208A patent/CN101164876A/en active Pending
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| CN102214516A (en) * | 2011-03-17 | 2011-10-12 | 南开大学 | Method for preparing capacitor electrode material from waste tire pyrolytic carbon |
| CN102580674A (en) * | 2012-02-21 | 2012-07-18 | 南开大学 | Method for preparing mercury removal agent by utilizing modified waste tire pyrolysis residue |
| CN103013188A (en) * | 2012-12-11 | 2013-04-03 | 开平市康汇橡胶制品有限公司 | Production process for environment-friendly carbon black powder |
| CN103013188B (en) * | 2012-12-11 | 2014-11-26 | 开平市康汇橡胶制品有限公司 | Production process for environment-friendly carbon black powder |
| CN103265828A (en) * | 2013-05-08 | 2013-08-28 | 明溪县宝福再生资源开发中心 | Solid phase grafting modification method of regeneration pyrolysis carbon black |
| CN105331147A (en) * | 2015-10-28 | 2016-02-17 | 贵州安泰再生资源科技有限公司 | Method of preparing carbon black from junked tires |
| CN106276892A (en) * | 2016-08-05 | 2017-01-04 | 北京林业大学 | A kind of method preparing pressed active carbon for raw material with thermal cracking charcoal |
| CN107488455A (en) * | 2017-08-17 | 2017-12-19 | 太原理工大学 | A kind of method that thermal decomposing waste tire residue is upgraded to tire carbon black |
| CN109289773A (en) * | 2018-11-07 | 2019-02-01 | 华侨大学 | A method of it is pyrolyzed using scrap tire powder as raw material and prepares magnetic carbon black adsorbent |
| CN109513423A (en) * | 2018-11-26 | 2019-03-26 | 厦门庚能新材料技术有限公司 | A kind of magnetism carbon black adsorbent, preparation method and application |
| CN110760204A (en) * | 2019-10-25 | 2020-02-07 | 珠海格力绿色再生资源有限公司 | System and method for reducing soot ash content of waste tire cracking carbon and recovering Zn |
| CN110760204B (en) * | 2019-10-25 | 2021-05-11 | 珠海格力绿色再生资源有限公司 | System and method for reducing soot ash content of waste tire cracking carbon and recovering Zn |
| CN110878148A (en) * | 2019-11-19 | 2020-03-13 | 珠海格力绿色再生资源有限公司 | Method for modifying pyrolysis carbon black |
| CN110878148B (en) * | 2019-11-19 | 2021-06-15 | 珠海格力绿色再生资源有限公司 | Method for modifying pyrolysis carbon black |
| CN111500092A (en) * | 2020-04-15 | 2020-08-07 | 安徽省克林泰迩再生资源科技有限公司 | Modification treatment method of waste tire cracking carbon black |
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| CN113501519A (en) * | 2021-08-02 | 2021-10-15 | 江苏龙腾城矿环境技术有限公司 | Method for preparing activated carbon and recovering zinc by utilizing waste tire rubber pyrolytic carbon |
| CN114551885A (en) * | 2022-02-21 | 2022-05-27 | 上海紫江新材料科技股份有限公司 | Black adhesive for lithium battery aluminum plastic film and use method thereof |
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| CN114634722A (en) * | 2022-04-06 | 2022-06-17 | 安徽固瑞特新材料科技有限公司 | Method for improving structure of regenerated carbon black |
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