CN101045535A - Active carbon of produced by concentration carbonization papermaking pulping black liquor - Google Patents
Active carbon of produced by concentration carbonization papermaking pulping black liquor Download PDFInfo
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- CN101045535A CN101045535A CN 200610020645 CN200610020645A CN101045535A CN 101045535 A CN101045535 A CN 101045535A CN 200610020645 CN200610020645 CN 200610020645 CN 200610020645 A CN200610020645 A CN 200610020645A CN 101045535 A CN101045535 A CN 101045535A
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- gac
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Abstract
A process for preparing activated carbon from block paper-making liquid by concentrating and charring includes such steps as evaporating for concentrating, charring at 500-800 deg.C for 10-90 min to obtain alkali contained coke, immersing in hot water, eluting, filtering and drying.
Description
(1) technical field:
Patent of the present invention relates to a kind of production method of gac, particularly is raw material with the paper-making pulping black liquor, comes the production process of active carbon through concentrating with charing.
(2) background technology:
Gac is the black porous particle of making through charing and reactivation process with plurality of raw materials such as timber, wood chip, shell, coals, is to be made of crystallite charcoal and unformed charcoal.Gac is one of the most ancient most important industrial adsorbents, and its maximum characteristics are to have flourishing pore texture and huge specific surface area (500-3000m
2/ g), because it has unique pore texture and surface functional group (as carboxyl, carbonyl, hydroxyl, lactone etc.), organic or inorganic material in gas, the solution and colloidal solid etc. there are very strong adsorptive power. gac has enough chemical stabilities, characteristic with physical strength and acidproof, alkaline-resisting, heat-resisting, water insoluble and organic solvent, have and use the back regenerated characteristic easily that lost efficacy, make it extensive and important purposes be arranged, be widely used in every field such as pharmacy, chemical industry, food, processing, metallurgical industry, agricultural in all trades and professions.Before the seventies in 20th century, gac application at home mainly concentrates on sugaring, pharmacy and monosodium glutamate industry; Expanded to industries such as water treatment and environmental protection afterwards again; The nineties in 20th century, except that above field, expand fields such as solvent recuperation, food-drink purification, purifying air, desulfurization, carrier, medicine, gold extraction, semiconductor application, electric energy storage, hydrogen storage to, at present, American-European countries is launching the research of medicinal carbon.
Method for preparation of active carbon mainly contains physical activation method and chemical activation method.(1) physical activation method: carbonated material is at high temperature reacted with oxidizing gas such as water vapour, carbonic acid gas or air and raw material of wood-charcoal material, make unordered charcoal partial oxidation etching pore-forming in the raw material of wood-charcoal material, form flourishing microvoid structure at material internal.Carbonization temperature is generally at 600 ℃, and generally between 800～900 ℃, the carbonoxide atom forms pore texture to activation temperature so the activation yield is not high because rely on, and activation temperature is higher, needs first charing reactivate.(2) chemical activation method: chemical activation is by selecting suitable activator, activator is mixed one step of back direct activation can make gac with raw material.Press the different ZnCl of branch of activator
2Method, KOH method, H
3PO
4Method.ZnCl
2Activation method is the chemical process of topmost production gac in China, mainly is that raw material adopts rotary kiln or flat band method preparation with the wood chip.Be that activator is produced gac and started from the seventies in 20th century with KOH, domestic in this respect report in recent years is more, adopting refinery coke, coal-tar pitch, nut-shell is raw material, and making specific surface area with basic metal such as NaOH, KOH or alkali metal compound as activator is 3000～3600m
2The gac of/g.H
3PO
4The required temperature of method activation is hanged down generally at 300～350 ℃, and production cost is low, and U.S.'s production of active carbon adopts H more
3PO
4Method.
China is one of world Activated Carbon Production big country, and the annual production in 2002 of China's gac has broken through 210,000 t, and replacing the U.S. (15-17 ten thousand t) becomes the first in the world Activated Carbon Production big country; The gac export volume also rises year by year, and outlet 150,000 t in 2002 have been sure to occupy first place, the world.But owing to adopt coal and pitch to produce the technical requirements height of gac, the production of the gac of China is still based on timber, wood chip and timber rim charge, and the gac development to a certain degree is subjected to the restriction of timber resources.For this reason, seek the new raw material of producing gac, explore the novel method of producing gac, significant to further developing activated carbon in China.
Black liquor is in the chemical pulping process, and wood chip is through (alkali) boiling and filtration, obtains remaining black liquor behind the fibrous matter.The color of black liquor is pitch black, and COD reaches several ten thousand mg/l, is the main source of papermaking sewage.Contain organic substances such as xylogen, Mierocrystalline cellulose, hemicellulose in the black liquor, contain NaOH, Na simultaneously
2CO
3Etc. alkaline chemical.Document [1,2,3] utilize black liquor to prepare gac research as carbon source, their preparation method takes to add acidic substance the xylogen in the black liquor is precipitated, filtering separation obtains xylogen, again xylogen is carried out charing and handle, obtain wood charcoal powder, wood charcoal powder obtains gac through chemical activation.Fig. 1 is its process flow sheet.
(3) summary of the invention:
Active carbon of produced by concentration carbonization papermaking pulping black liquor is a kind of production process of active carbon.This method is utilized and is contained the organic substance that xylogen, Mierocrystalline cellulose, hemicellulose etc. can prepare charcoal in the paper-making pulping black liquor, contains NaOH, Na simultaneously
2CO
3Deng making charcoal form the characteristics of the alkaline chemical of vesicular structure, take the thermolysis means, make black-liquid carbonizedly, and form the gac of porous loose structure.The sequential process of this treatment process is: rare black liquor obtains concentrated black liquid through pervaporation; Concentrated black liquid is transferred to and is carried out charing in the charring furnace, and carbonization temperature is at 500～800 ℃, and the residence time of black liquor in charring furnace is 10-90 minute, after the charing, obtains alkaliferous solid coke; Contain the alkali solid coke and contain energy water-soluble NaOH, Na
2CO
3, Na
2Alkaline matters such as S through hot-water soak, wash-out, filtration, obtain wet wood charcoal powder and basic solution; Wet wood charcoal powder obtains gac after super-dry.Its technical process such as Fig. 2.
The essential characteristic that paper-making pulping black liquor concentration carbonization method is produced gac is: be raw material with the black liquor, after rare black liquor is carried out evaporation concentration, concentrated black liquid carried out charing handle, pass through wash-out, filtration and drying again, obtain activated carbon product.Carbonization temperature is at 500～800 ℃.Process order is through concentrated, charing, wash-out, filtration, dry five master operations.
Compare with current black liquor acid-precipitation method (both xylogen precipitator method), it is significantly distinguished and is: (1) black liquor acid-precipitation method takes to add acid, reduces the alkalescence of black liquor, makes the sedimentary means of xylogen; And black liquor concentration carbonization method takes rare black liquor is carried out the means of evaporation concentration, does not need to add acidic substance, does not need to isolate xylogen; (2) in the carbonization-activation process, the black liquor acid-precipitation method need add certain chemical reagent, so that obtain high specific surface area; And black liquor concentration carbonization method relies on the black liquor self EMS memory that NaOH, Na are being arranged
2CO
3, Na
2Alkaline matters such as S do not need to add the product that chemical reagent also obtains high-specific surface area.Take paper-making pulping black liquor concentration carbonization method to produce gac, the gac yield is 8～15% of a drying solid black liquor quality, specific surface area 500-1200m
2/ g.
(4) embodiment:
The sequential process of this treatment process is: rare black liquor obtains concentrated black liquid through pervaporation; Concentrated black liquid is transferred to and is carried out charing in the charring furnace, and carbonization temperature is at 500～800 ℃, and the residence time of black liquor in charring furnace is 10-90 minute, after the charing, obtains alkaliferous solid coke; Contain the alkali solid coke and contain energy water-soluble NaOH, Na
2CO
3, Na
2Alkaline matters such as S through hot-water soak, wash-out, filtration, obtain wet wood charcoal powder and basic solution; Wet wood charcoal powder obtains gac after super-dry.Its technical process such as Fig. 2.
Reference
1. the auspicious Li Haichao in road is in steel, and softwood papermaking digesting black liquor xylogen prepares gac, forest chemical engineering communication, 2005.3.1-4.
Summary: with xylogen in the softwood papermaking digesting black liquor is that raw material has carried out charcoal preparation experiment alive.Inquired into the influence of different soak times, activation temperature, phosphorus material comparison preparation Properties of Activated Carbon.The result shows: xylogen can be used as a kind of good raw material for preparing gac in the softwood papermaking digesting black liquor, optimal conditions is: activation temperature is 550 ~ C, phosphorus material ratio is 4.5: 1, soak time is 40min, the gac methylene blue adsorption value that makes can reach 195mL/g, iodine sorption value is 656mL/g, and yield is 40.75%.Factor affecting is followed successively by in proper order: activation temperature＞phosphorus material ratio＞soak time.
2. the auspicious money in road is learned benevolence Yu Gang etc., and papermaking black liquor lignin prepares gac, paper and papermaking, 2005.2.61-63
Summary: this paper is at the extraction of lignin in the softwood black digestion liquid, and the preparation that is used for gac studies, and the performance of experiment gained gac is analyzed.Inquired into soak time, activation temperature emphatically, to the charcoal absorption performance impact, it is followed successively by material in proper order than factors: activation temperature＞material ratio＞soak time.The result shows that the lignin in the black liquid can be used as the good raw material of preparation gac.
3. Tian Yongshu, straw pulp xylogen preparing active carbon, Chinese comprehensive utilization of resources, 2000.10.8-9.
Summary: this paper has set forth the optimum process condition of the technological process of utilizing this quality of leather slurry black liquid acid out preparing active carbon.
Claims (1)
1. the production method of a gac particularly is raw material with the black liquor, comes the production process of active carbon through concentrating with charing.Its essential characteristic is: be raw material with the black liquor, after rare black liquor is carried out evaporation concentration, concentrated black liquid carried out charing handle, pass through wash-out, filtration and drying again, obtain activated carbon product; Carbonization temperature is at 500～800 ℃, carbonization time 10-90 minute; Process order is through concentrated, charing, wash-out, filtration, dry five master operations.
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Cited By (17)
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|---|---|---|---|---|
| CN102344136A (en) * | 2011-04-15 | 2012-02-08 | 山东轻工业学院 | Method for preparing active carbon by waste water sludge from chemical pulping and paper mill |
| CN102363930A (en) * | 2011-06-07 | 2012-02-29 | 山东轻工业学院 | Method for preparing active carbon during alkali recovery of papermaking black liquor |
| CN102587187A (en) * | 2012-02-10 | 2012-07-18 | 中国科学院过程工程研究所 | Alkali recovery method for by-producing activated carbon and white carbon black by using paper making black liquid |
| CN102757045A (en) * | 2011-12-23 | 2012-10-31 | 山东轻工业学院 | Method for preparing active carbon by using alkali in aluminum-making industry red mud and recovering alkali |
| CN102942180A (en) * | 2012-11-23 | 2013-02-27 | 浙江建中竹业科技有限公司 | Air circulation carbon granule for air conditioner |
| CN103964432A (en) * | 2013-02-04 | 2014-08-06 | 济南圣泉集团股份有限公司 | Method for preparing granular activated carbon from lignin |
| CN104599861A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method of graphene/xylogen-based active carbon |
| CN105531303A (en) * | 2013-08-09 | 2016-04-27 | 森高工业有限公司 | Method for extracting lignin from black liquor and products produced thereby |
| CN106185920A (en) * | 2016-06-27 | 2016-12-07 | 农业部环境保护科研监测所 | A kind of porous carbon materials and its preparation method and application |
| CN106622137A (en) * | 2017-01-03 | 2017-05-10 | 南京林业大学 | Production method of adsorbent for removing mercury from flue gas |
| CN107142765A (en) * | 2017-07-05 | 2017-09-08 | 陈翀航 | A kind of extraction rice straw cellulose and its residue prepare the complete utilization method of activated carbon |
| CN108715446A (en) * | 2018-07-04 | 2018-10-30 | 北京林业大学 | A kind of preparation method of more mesoporous Lignin-Based Activated Carbons |
| CN111450799A (en) * | 2020-03-24 | 2020-07-28 | 天津科技大学 | Preparation method of magnetic activated carbon based on black liquor lignin and Fenton sludge |
| CN111977647A (en) * | 2020-03-12 | 2020-11-24 | 齐鲁工业大学 | Method for preparing sulfur-doped porous carbon from sulfur-doped porous carbon and eucalyptus black liquid and application of sulfur-doped porous carbon |
| CN113247894A (en) * | 2021-05-31 | 2021-08-13 | 广西科学院 | Paper pulp-capacitance carbon joint production method |
| CN115430439A (en) * | 2022-08-29 | 2022-12-06 | 齐鲁工业大学 | Black liquor-based solid acid catalyst, preparation method thereof and application thereof in furfural production |
| CN115445588A (en) * | 2022-08-15 | 2022-12-09 | 东南大学 | Biomass-based porous carbon composite material, preparation method thereof and application thereof in CO 2 Application in adsorption |
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2006
- 2006-03-30 CN CN 200610020645 patent/CN101045535A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102344136A (en) * | 2011-04-15 | 2012-02-08 | 山东轻工业学院 | Method for preparing active carbon by waste water sludge from chemical pulping and paper mill |
| CN102363930B (en) * | 2011-06-07 | 2014-10-22 | 山东轻工业学院 | Method for preparing active carbon during alkali recovery of papermaking black liquor |
| CN102363930A (en) * | 2011-06-07 | 2012-02-29 | 山东轻工业学院 | Method for preparing active carbon during alkali recovery of papermaking black liquor |
| CN102757045A (en) * | 2011-12-23 | 2012-10-31 | 山东轻工业学院 | Method for preparing active carbon by using alkali in aluminum-making industry red mud and recovering alkali |
| CN102587187B (en) * | 2012-02-10 | 2014-06-04 | 中国科学院过程工程研究所 | Alkali recovery method for by-producing activated carbon and white carbon black by using paper making black liquid |
| CN102587187A (en) * | 2012-02-10 | 2012-07-18 | 中国科学院过程工程研究所 | Alkali recovery method for by-producing activated carbon and white carbon black by using paper making black liquid |
| CN102942180B (en) * | 2012-11-23 | 2014-05-14 | 浙江建中竹业科技有限公司 | Air circulation carbon granule for air conditioner |
| CN102942180A (en) * | 2012-11-23 | 2013-02-27 | 浙江建中竹业科技有限公司 | Air circulation carbon granule for air conditioner |
| CN103964432A (en) * | 2013-02-04 | 2014-08-06 | 济南圣泉集团股份有限公司 | Method for preparing granular activated carbon from lignin |
| US9902816B2 (en) | 2013-08-09 | 2018-02-27 | Suncoal Industries Gmbh | Method for extracting lignin from black liquor and products produced thereby |
| CN105531303A (en) * | 2013-08-09 | 2016-04-27 | 森高工业有限公司 | Method for extracting lignin from black liquor and products produced thereby |
| US10611885B2 (en) | 2013-08-09 | 2020-04-07 | Suncoal Industries Gmbh | Products extracted from black liquor |
| CN104599861A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method of graphene/xylogen-based active carbon |
| CN106185920A (en) * | 2016-06-27 | 2016-12-07 | 农业部环境保护科研监测所 | A kind of porous carbon materials and its preparation method and application |
| CN106622137A (en) * | 2017-01-03 | 2017-05-10 | 南京林业大学 | Production method of adsorbent for removing mercury from flue gas |
| CN107142765A (en) * | 2017-07-05 | 2017-09-08 | 陈翀航 | A kind of extraction rice straw cellulose and its residue prepare the complete utilization method of activated carbon |
| CN108715446A (en) * | 2018-07-04 | 2018-10-30 | 北京林业大学 | A kind of preparation method of more mesoporous Lignin-Based Activated Carbons |
| CN111977647A (en) * | 2020-03-12 | 2020-11-24 | 齐鲁工业大学 | Method for preparing sulfur-doped porous carbon from sulfur-doped porous carbon and eucalyptus black liquid and application of sulfur-doped porous carbon |
| CN111450799A (en) * | 2020-03-24 | 2020-07-28 | 天津科技大学 | Preparation method of magnetic activated carbon based on black liquor lignin and Fenton sludge |
| CN113247894A (en) * | 2021-05-31 | 2021-08-13 | 广西科学院 | Paper pulp-capacitance carbon joint production method |
| CN115445588A (en) * | 2022-08-15 | 2022-12-09 | 东南大学 | Biomass-based porous carbon composite material, preparation method thereof and application thereof in CO 2 Application in adsorption |
| CN115445588B (en) * | 2022-08-15 | 2023-10-17 | 东南大学 | Biomass-based porous carbon composite material, preparation and CO production 2 Application in adsorption |
| US12102977B2 (en) | 2022-08-15 | 2024-10-01 | Southeast University | Biomass-based porous carbon composite materials and preparation thereof and application in CO2 adsorption |
| CN115430439A (en) * | 2022-08-29 | 2022-12-06 | 齐鲁工业大学 | Black liquor-based solid acid catalyst, preparation method thereof and application thereof in furfural production |
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