CN102553555B - Regeneration method of powdered activated carbon - Google Patents
Regeneration method of powdered activated carbon Download PDFInfo
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- CN102553555B CN102553555B CN201210006255.XA CN201210006255A CN102553555B CN 102553555 B CN102553555 B CN 102553555B CN 201210006255 A CN201210006255 A CN 201210006255A CN 102553555 B CN102553555 B CN 102553555B
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- caffeine
- active carbon
- regenerating furnace
- regeneration
- regenerating
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000011069 regeneration method Methods 0.000 title claims abstract description 18
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 claims abstract description 121
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229960001948 caffeine Drugs 0.000 claims abstract description 60
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002699 waste material Substances 0.000 claims abstract description 17
- 230000008929 regeneration Effects 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 230000001172 regenerating effect Effects 0.000 claims description 53
- 229910052799 carbon Inorganic materials 0.000 claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 239000000049 pigment Substances 0.000 claims description 8
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 238000002485 combustion reaction Methods 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000009418 renovation Methods 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical compound CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 1
- 208000007443 Neurasthenia Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
- -1 xanthine alkaloid compound Chemical class 0.000 description 1
Classifications
-
- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention relates to a regeneration method of powdered activated carbon. The method utilizes the technology of continuous recovery of caffeine by two-gradient heating, and the regeneration and comprehensive resource technology of activated carbon, and has the characteristics of continuous production process, high caffeine capture efficiency, and high activated carbon regeneration rate. The caffeine is effectively recovered, and meanwhile the regeneration and resource of waste activated carbon are also realized, and the emission of carbon dioxide formed by the combustion of the waste activated carbon is avoided.
Description
Technical field
The present invention relates to a kind of Regenevating Waste Activated Carbon technology, be specifically related to a kind of renovation process of powdered activated carbon.
Background technology
Caffeine belongs to xanthine alkaloid compound, is a kind of central nervous excitation agent, because the medicine of main component is used for the treatment of the symptom such as neurasthenia and spirit inhibition, headache, respond well with coffee, on market, is widely used now.In caffeine production process, adopt the dimethyl urea synthetic route that urea, monomethyl amine and monoxone are base stock.In production process, adopt active carbon to carry out decolorizing and refining to the synthetic crude product caffeine aqueous solution, in removing pigment and other impurity, also adsorbed a large amount of caffeines, produced thus the waste active carbon of year caffeine.The every annual emissions of this waste active carbon reaches 2000 tons, wherein contains 20% caffeine.
Because it dissolves in chloroform, former process using be chloroform extraction reclaim caffeine, in processing procedure, there is the problems such as medicament loss is large, and reagent toxicity is strong; And the active carbon that removes caffeine adopts burning method to process at present, not only cause the wasting of resources of high added value caffeine and active carbon, and burn toxic and harmfuls such as producing a large amount of CO2 and nitrogen oxide, oxysulfide, pollute environment.Therefore, develop and a kind ofly reclaim caffeine and make the method and technology of regenerating active carbon significant from carrying caffeine active carbon.
At present, the regenerating active carbon technique of industrial use mainly contains following several: chemical method, bio-regeneration method, wet oxidation process, electrolytic oxidation and the thermal regeneration method of medicament wash-out.In heating process, decompose the temperature difference of desorption according to the organic matter adsorbing in active carbon, thermal regeneration method can be divided into low-temperature heat regeneration and high-temperature heating regeneration, but effect is not very good.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, a kind of method of utilizing method of reproduction to process effective decolorizer regeneration of load caffeine in the exquisite process of caffeine has been proposed, two sections of gradient-heated of described method exploitation reclaim caffeine and regenerating active carbon comprehensive resource technology continuously, have the advantages that production process is continuous, caffeine capturing efficiency is high, regenerating active carbon rate is high, regeneration and the resource of waste active carbon in effectively reclaiming caffeine, are also realized, the CO2 emission of having avoided waste active carbon burning to form.
Technical scheme of the present invention is: a kind of renovation process of powdered activated carbon, and described method continuously by one-level regenerating furnace, secondary regenerating furnace, spray column and condenser, through strict temperature control, realizes the regeneration of active carbon by waste active carbon, and concrete steps are:
1) in one-level regenerating furnace, temperature rises to more than 100 DEG C, when secondary regenerating furnace temperature rises to more than 400 DEG C, waste active carbon is added in one-level regenerating furnace continuously.
2) one-level regenerating furnace makes the water evaporation of absorption in carbon granule, and the lower boiling organic matter of part also evaporates thereupon simultaneously, and temperature maintains 100～130 DEG C, and this part water vapour reclaims after condenser.
3) active carbon after dehydration enters in secondary regenerating furnace, and secondary regenerating furnace passes into the nitrogen that linear velocity is 0.005～0.007m/s, and temperature maintains within the scope of 420～450 DEG C, after now caffeine distillation, taken out of by nitrogen, pigment decomposes simultaneously, and active carbon is regenerated.
4) for preventing that caffeine gas from condensing, caffeine pipeline is auxiliary has companion hot, enters after spray column, with the trapping of aqueous solution caffeine spray.
In above-mentioned steps 1, waste active carbon content of caffeine is 10～25%
In above-mentioned steps 2, the active carbon water content after dehydration is 5～8%.
In above-mentioned steps 3, regenerating active carbon rate is 90～93%.
In above-mentioned steps 4, aqueous solution caffeine concentration is 0～0.25g/mL, and temperature is 20～80 DEG C, and caffeine capture rate is 96～100%.
The present invention has following beneficial effect
Two sections of gradient-heated that the present invention relates to reclaim caffeine and regenerating active carbon comprehensive resource technology continuously, have the advantages that production process is continuous, caffeine capturing efficiency is high, regenerating active carbon rate is high, regeneration and the resource of waste active carbon in effectively reclaiming caffeine, are also realized, the CO2 emission of having avoided waste active carbon burning to form.
Brief description of the drawings
Accompanying drawing is schematic flow sheet of the present invention.
In figure, 1, one-level regenerating furnace; 2, secondary regenerating furnace; 3, condenser; 4, spray column.
Detailed description of the invention
Described in accompanying drawing, the present invention continuously by one-level regenerating furnace 1, secondary regenerating furnace 2, spray column 4 and condenser 3, through strict temperature control, realizes the regeneration of active carbon by waste active carbon.
Embodiment 1
Treat that in one-level regenerating furnace, temperature rises to 100 DEG C, secondary regenerating furnace temperature rises to 400 DEG C, will carry caffeine active carbon by adding speed 0.9t/h to add in one-level regenerating furnace.Treat that active carbon water content is down to 8%, the active carbon after dehydration is advanced in secondary regenerating furnace, and nitrogen gas speed is 0.007m/s, this stage caffeine distillation, and pigment decomposes.Caffeine after distillation enters spray column trapping and reclaims, and the caffeine rate of recovery is 98%, and regenerating active carbon rate is 88%.
Embodiment 2
Treat that in one-level regenerating furnace, temperature rises to 100 DEG C, secondary regenerating furnace temperature rises to 400 DEG C, will carry caffeine active carbon by adding speed 0.6t/h to add in one-level regenerating furnace.Treat that active carbon water content is down to 6%, the active carbon after dehydration is advanced in secondary regenerating furnace, and nitrogen gas speed is 0.006m/s, this stage caffeine distillation, and pigment decomposes.Caffeine after distillation enters spray column trapping and reclaims, and the caffeine rate of recovery is 98.5%, and regenerating active carbon rate is 89%.
Embodiment 3
Treat that in one-level regenerating furnace, temperature rises to 105 DEG C, secondary regenerating furnace temperature rises to 420 DEG C, will carry caffeine active carbon by adding speed 0.5t/h to add in one-level regenerating furnace.Treat that active carbon water content is down to 5%, the active carbon after dehydration is advanced in secondary regenerating furnace, and nitrogen gas speed is 0.005m/s, this stage caffeine distillation, and pigment decomposes.Caffeine after distillation enters spray column trapping and reclaims, and the caffeine rate of recovery is 98%, and regenerating active carbon rate is 90%.
Embodiment 4
Treat that in one-level regenerating furnace, temperature rises to 100 DEG C, secondary regenerating furnace temperature rises to 400 DEG C, will carry caffeine active carbon by adding speed 0.5t/h to add in one-level regenerating furnace.Treat that active carbon water content is down to 6%, the active carbon after dehydration is advanced in secondary regenerating furnace, and nitrogen gas speed is 0.007m/s, this stage caffeine distillation, and pigment decomposes.Caffeine after distillation enters spray column trapping and reclaims, and the caffeine rate of recovery is 97%, and regenerating active carbon rate is 90%.
Embodiment 5
Treat that in one-level regenerating furnace, temperature rises to 100 DEG C, secondary regenerating furnace temperature rises to 410 DEG C, will carry caffeine active carbon by adding speed 0.6t/h to add in one-level regenerating furnace.Treat that active carbon water content is down to 8%, the active carbon after dehydration is advanced in secondary regenerating furnace, and nitrogen gas speed is 0.006m/s, this stage caffeine distillation, and pigment decomposes.Caffeine after distillation enters spray column trapping and reclaims, and the caffeine rate of recovery is 97.5%, and regenerating active carbon rate is 89%.
Claims (2)
1. the method for the regeneration of a powdered activated carbon and recovery caffeine, it is characterized in that: waste active carbon is passed through continuously one-level regenerating furnace, secondary regenerating furnace, spray column and condenser by described method, through strict temperature control, realize the regeneration of active carbon, concrete steps are:
1) in one-level regenerating furnace, temperature rises to 100-105 DEG C, when secondary regenerating furnace temperature rises to 400-420 DEG C, waste active carbon is added in one-level regenerating furnace continuously;
2) one-level regenerating furnace makes the water evaporation of absorption in carbon granule, and the lower boiling organic matter of part also evaporates thereupon simultaneously, and temperature maintains 100～130 DEG C, and this part water vapour reclaims after condenser;
3) active carbon after dehydration enters in secondary regenerating furnace, and secondary regenerating furnace passes into the nitrogen that linear velocity is 0.005～0.007m/s, and temperature maintains within the scope of 420～450 DEG C, after now caffeine distillation, taken out of by nitrogen, pigment decomposes simultaneously, and active carbon is regenerated;
4) for preventing that caffeine gas from condensing, caffeine pipeline is auxiliary has companion hot, enters after spray column, with the trapping of aqueous solution caffeine spray; Wherein, described waste active carbon is at the decolorizer of processing load caffeine in caffeine subtractive process,
Step 4) in, the temperature of aqueous solution caffeine is 20～80 DEG C, and caffeine capture rate is 97～98.5%, and aqueous solution caffeine concentration is 0-0.25g/mL, does not wherein comprise 0.
2. the method for the regeneration of powdered activated carbon according to claim 1 and recovery caffeine, is characterized in that: in step 1, and waste active carbon content of caffeine 10～25%, in step 2, active carbon water content after dehydration is 5～8%, and in step 3, regenerating active carbon rate is 90～93%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210006255.XA CN102553555B (en) | 2012-01-09 | 2012-01-09 | Regeneration method of powdered activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210006255.XA CN102553555B (en) | 2012-01-09 | 2012-01-09 | Regeneration method of powdered activated carbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102553555A CN102553555A (en) | 2012-07-11 |
| CN102553555B true CN102553555B (en) | 2014-11-05 |
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| CN201210006255.XA Active CN102553555B (en) | 2012-01-09 | 2012-01-09 | Regeneration method of powdered activated carbon |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044425B (en) * | 2013-01-23 | 2015-04-22 | 蒋仕军 | Active carbon and caffeine separation pyrolysis apparatus |
| CN103706344A (en) * | 2013-12-18 | 2014-04-09 | 江苏江山制药有限公司 | Active carbon recovery process |
| CN108212135A (en) * | 2017-12-29 | 2018-06-29 | 南通泰禾化工股份有限公司 | The recycling and processing device and method of dead catalyst in a kind of Bravo synthesis technology |
| CN111644167A (en) * | 2020-06-10 | 2020-09-11 | 湖北君集水处理有限公司 | Device and method for efficient regeneration and waste gas treatment of powdered activated carbon |
| CN112090417B (en) * | 2020-08-27 | 2023-06-13 | 杭州电子科技大学 | Powder activated carbon regeneration device based on air flow heating and regeneration method thereof |
| JPWO2022163690A1 (en) * | 2021-01-28 | 2022-08-04 | ||
| CN113976603A (en) * | 2021-11-08 | 2022-01-28 | 北京艾孚润德环境科技有限责任公司 | In-situ soil remediation process for treating underground water based on multilayer reaction wall technology |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007145052A1 (en) * | 2006-06-14 | 2007-12-21 | Calgon Mitsubishi Chemical Corporation | Phosphorus compound-complexed activated carbon for electric double layer capacitor and method for producing the same |
| CN101704818A (en) * | 2009-12-22 | 2010-05-12 | 陈学玺 | Method for extracting caffeine from methylated mother through adsorption separation |
-
2012
- 2012-01-09 CN CN201210006255.XA patent/CN102553555B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007145052A1 (en) * | 2006-06-14 | 2007-12-21 | Calgon Mitsubishi Chemical Corporation | Phosphorus compound-complexed activated carbon for electric double layer capacitor and method for producing the same |
| CN101704818A (en) * | 2009-12-22 | 2010-05-12 | 陈学玺 | Method for extracting caffeine from methylated mother through adsorption separation |
Non-Patent Citations (2)
| Title |
|---|
| "A NEW METHOD FOR REGENERATING ACTIVATED CARBON BY THERMAL DESORPTION WITH LIQUID WATER UNDER SUBCRITICAL CONDITIONS";F.SALVADOR et al;《Carbon》;19961231;第34卷(第4期);第511-516页 * |
| F.SALVADOR et al."A NEW METHOD FOR REGENERATING ACTIVATED CARBON BY THERMAL DESORPTION WITH LIQUID WATER UNDER SUBCRITICAL CONDITIONS".《Carbon》.1996,第34卷(第4期),第511-516页. * |
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| CN102553555A (en) | 2012-07-11 |
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| ASS | Succession or assignment of patent right |
Owner name: SHANDONG XINHUA PHARMACEUTICAL CO., LTD. Effective date: 20130502 |
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| TA01 | Transfer of patent application right |
Effective date of registration: 20130502 Address after: 266061 Shandong Province, Qingdao city Laoshan District Songling Road No. 99 Applicant after: Qingdao University of Science & Technology Applicant after: Shandong Xinhua Pharmaceutical Co., Ltd. Address before: 266061 Shandong Province, Qingdao city Laoshan District Songling Road No. 99 Applicant before: Qingdao University of Science & Technology |
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