CN102583366A - Method for washing active carbon with low water consumption - Google Patents
Method for washing active carbon with low water consumption Download PDFInfo
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- CN102583366A CN102583366A CN2012100261869A CN201210026186A CN102583366A CN 102583366 A CN102583366 A CN 102583366A CN 2012100261869 A CN2012100261869 A CN 2012100261869A CN 201210026186 A CN201210026186 A CN 201210026186A CN 102583366 A CN102583366 A CN 102583366A
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Abstract
The invention discloses a method for washing active carbon with low water consumption. The method comprises the following steps of: mixing carbon-containing precursor and KOH or NaOH uniformly in a weight ratio of 1: (1-10), heating from room temperature to the temperature of between 700 and 1,000 DEG C in the present of inert atmosphere, keeping at a constant temperature for 1 to 3 hours, naturally cooling, taking out the activated product when the temperature is reduced to room temperature, adding water in a weight ratio of the activated product to the water of 1: (1-3) to form pulp, performing first solid-liquid separation on the active carbon and the alkali-containing waste water by a reduced pressure filtration or centrifuging method, mixing the separated first solid and an aqueous solution of formic acid in a ratio of the first solid to the formic acid of 1 kilogram: (1-5) liters, violently stirring for 1 to 3 hours, performing second solid-liquid separation, mixing the separated second solid and water in a ratio of 1 kilogram: (5-50) liters, violently stirring for 1 to 3 hours, performing third solid-liquid separation, drying the third solid for 3 to 10 hours at the temperature of between 180 and 250 DEG C under normal pressure or reduced pressure, and thus obtaining a product. The method has the advantages of low water consumption and elimination of chlorine ion residue.
Description
Technical field
The invention belongs to the method for the thick product of a kind of detergent active charcoal, provide the washing methods that a kind of low water consumes and do not have the residual gac of cl ions specifically.
Technical background
The preparation of super-activated carbon generally adopts highly basic such as KOH or NaOH to carry out activation to containing the charcoal precursor, and gained contained the alkaline gac after activation finished, and this gac need wash just with a large amount of water or acid can make super-activated carbon.At present, in document or relevant patent, all the washing methods of activation products not being offered some clarification on, only is to adopt the conventional filtration under diminished pressure or the method for spinning to make with extra care.In this treating process; Generally need a large amount of water that activation products are washed; Through filtration under diminished pressure or centrifugal method gac is separated with alkaliferous waste water then, the solid after the separation once more water or acid wash fully or soak after carry out solid-liquid separation, several times so repeatedly again; Till the pH of washings value is near neutrality, be drying to obtain super-activated carbon afterwards.Can find out that this washing process is wasted time and energy, water loss is very big, and efficient is also very low, is unfavorable for the large-scale production of super-activated carbon.
Patent CN97123209.1 " preparation method of active carbon with high specific surface area ", CN98114553.1 " preparation of activated carbon with high specific surface area ", CN200910219704.7 " a kind of preparation method of active carbon with high specific surface area ", CN200610046177.0 " a kind of method that is prepared active carbon with high specific surface area by refinery coke " etc. adopt big water gaging that gac is washed neutrality, and water loss is obviously very high.
Patent CN200510010670.2 " a kind of method of producing active carbon with high specific surface area ", CN200610038065.0 " a kind of preparation method of high specific surface area active charcoal based on formaldehyde-phenol resin ", CN200810177135.X " preparation method of coir fiber based activated carbon with high specific surface area ", CN201110210608.3 " a kind of high-specific surface area and be rich in the mangosteen shell preparation method of active carbon of mesopore ", CN201010521615.0 " a kind of preparation method of hierarchical porous structure activated carbon " etc. have adopted acid-treated method in washing process; Though reduced the consumption of bath water to a certain extent; But residual cl ions is difficult to remove on the gac, causes in some field such as gac can't meet the demands when using as the electrode of double layer capacitor.
CN200910073682.8 " a kind of method that gac is washed " innovates the washing of gac first; But be to adopt water to wash after all; And being difficult for water, removes in the alkali on the gac; Finally cause the bath water amount still bigger, and, then produce the residual of cl ions again inevitably if adopt hydrochloric acid.
Summary of the invention
The purpose of this invention is to provide the washing methods that a kind of low water consumes and do not have the residual gac of cl ions.
Method of the present invention is following:
With weight ratio is 1: (1-10) contain carbon precursor and KOH or NaOH mix, and in the presence of inert atmosphere, are raised to 700-1000 ℃ from room temperature; Naturally cooling after constant temperature 1-3 hour; When treating that temperature drops to room temperature, take out activation products, according to the weight ratio 1 of activation products and water: (1-3) add water pulp thing after; Through filtration under diminished pressure or centrifugal method gac and alkaliferous waste water are carried out the solid-liquid separation first time; With after separating the first time solid according to the solid first time: formic acid=1 kilogram: 1-5 rises and adds aqueous formic acid and mix, and carries out solid-liquid separation second time after vigorous stirring 1-3 hour, with after separating the second time solid again by the solid second time: water=1 kilogram: 5-50 liter; Solid mixes with water for the second time; Carry out solid-liquid separation for the third time after vigorous stirring 1-3 hour, will be for the third time solid in 180-250 ℃ of following normal pressure or drying under reduced pressure 3-10 hour, obtain product.
The aforesaid carbon precursor that contains is refinery coke, coal, resol, corn straw, shell carbonized material, bamboo charcoal, coconut husk carbonized material, charred rice husk material.
Aforesaid inert atmosphere is N
2
The concentration of aforesaid aqueous formic acid is 5-50wt%..
Advantage of the present invention:
The sub product that 1 the present invention produces is potassium formiate or sodium formiate, and this product can be used for petroleum drilling, leather and dyeing, when reducing pollution, has realized waste and old utilization, and can reduce the cost of Preparation of Activated Carbon;
The significantly minimizing of 2 bath wateies can alleviate the pressure recovery of follow-up waste lye greatly, reduces cost recovery.
Embodiment;
3 since washing process in do not use hydrochloric acid, so there is not cl ions in the product.
Embodiment
Embodiment 1
With weight ratio is that 1: 1 refinery coke and KOH mixes, and in the presence of N2, is raised to 1000 ℃ from room temperature; Constant temperature is cooling naturally after 1 hour, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 1 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through centrifugal method, the solid after the separation according to the mixed of 1 kilogram of its weight and 1 liter of 5% aqueous formic acid after vigorous stirring 3 hours; Press 1 kilogram of water with 5 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 3 hours, solid-liquid separation; Solid obtains product in 180 ℃ of following constant pressure and dries 10 hours.Water loss is merely 5 liters of/kilogram gacs.Through check, the K ion content in the gac is 85ppm, no cl ions.
Embodiment 2
With weight ratio is that 1: 10 hard coal and NaOH mixes, and in the presence of N2, is raised to 700 ℃ from room temperature; Constant temperature is cooling naturally after 3 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through the filtration under diminished pressure method, the solid after the separation according to the mixed of 1 kilogram of its weight and 5 liter of 50% aqueous formic acid after vigorous stirring 1 hour; Press 1 kilogram of water with 50 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 1 hour, solid-liquid separation; Solid obtains product in 250 ℃ of following drying under reduced pressure 3 hours.Water loss is merely 50 liters of/kilogram gacs.Through check, the Na ion content in the gac is 15ppm, no cl ions.
Comparative Examples: with weight ratio is that 1: 10 hard coal and NaOH mixes, and in the presence of N2, is raised to 700 ℃ from room temperature; Constant temperature is cooling naturally after 3 hours, when treating that temperature drops near room temperature, takes out the activatory product; Use the water washing activation products, washing to middle sexual needs 500 premium on currency, solid-liquid separation afterwards; Solid obtains product in 250 ℃ of following drying under reduced pressure 3 hours.Water loss is merely 500 liters of/kilogram gacs.Through check, the Na ion content in the gac is 1205ppm, no cl ions.
Embodiment 3
With weight ratio is that 1: 5 resol and KOH mixes, and in the presence of N2, is raised to 800 ℃ from room temperature; Constant temperature is cooling naturally after 2 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through the filtration under diminished pressure method, the solid after the separation according to the mixed of 1 kilogram of its weight and 3 liter of 10% aqueous formic acid after vigorous stirring 2 hours; Press 1 kilogram of water with 10 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 2 hours, solid-liquid separation; Solid obtains product in 200 ℃ of following constant pressure and dries 8 hours.Water loss is merely 10 liters of/kilogram gacs.Through check, the K ion content in the gac is 65ppm, no cl ions.
Embodiment 4
With weight ratio is that 1: 6 coconut husk carbonized material and KOH mixes, and in the presence of N2, is raised to 900 ℃ from room temperature; Constant temperature is cooling naturally after 2 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through filter method, the solid after the separation according to the mixed of 1 kilogram of its weight and 2 liter of 5% aqueous formic acid after vigorous stirring 2 hours; Press 1 kilogram of water with 20 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 2 hours, solid-liquid separation; Solid obtains product in 230 ℃ of following constant pressure and dries 5 hours.Water loss is merely 20 liters of/kilogram gacs.Through check, the K ion content in the gac is 43ppm, no cl ions.
Embodiment 5
With weight ratio is that 1: 4 rice husk carbide and NaOH mixes, and in the presence of N2, is raised to 1000 ℃ from room temperature; Constant temperature is cooling naturally after 3 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through filter method, the solid after the separation according to the mixed of 1 kilogram of its weight and 3 liter of 50% aqueous formic acid after vigorous stirring 3 hours; Press 1 kilogram of water with 50 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 2 hours, solid-liquid separation; Solid obtains product in 150 ℃ of following drying under reduced pressure 10 hours.Water loss is merely 50 liters of/kilogram gacs.Through check, the Na ion content in the gac is 38ppm, no cl ions.
Embodiment 6
With weight ratio is that 1: 7 shell carbonized material and KOH mixes, and in the presence of N2, is raised to 700 ℃ from room temperature; Constant temperature is cooling naturally after 3 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through centrifugal method, the solid after the separation according to the mixed of 1 kilogram of its weight and 3 liter of 50% aqueous formic acid after vigorous stirring 2 hours; Press 1 kilogram of water with 50 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 3 hours, solid-liquid separation; Solid obtains product in 100 ℃ of following drying under reduced pressure 5 hours.Water loss is merely 50 liters of/kilogram gacs.Through check, the K ion content in the gac is 62ppm, no cl ions.
Embodiment 7
With weight ratio is that 1: 10 bamboo charcoal and NaOH mixes, and in the presence of N2, is raised to 800 ℃ from room temperature; Constant temperature is cooling naturally after 3 hours, when treating that temperature drops near room temperature, takes out the activatory product; After adding water pulp thing at 1: 3 according to the weight ratio of activation products and water, gac is separated with alkaliferous waste water through filter method, the solid after the separation according to the mixed of 1 kilogram of its weight and 3 liter of 30% aqueous formic acid after vigorous stirring 3 hours; Press 1 kilogram of water with 40 liters of solid after the solid-liquid separation again and mix, vigorous stirring is after 2 hours, solid-liquid separation; Solid obtains product in 200 ℃ of following constant pressure and dries 8 hours.Water loss is merely 40 liters of/kilogram gacs.Through check, the Na ion content in the gac is 20ppm, no cl ions.
Claims (4)
1. the method for one kind low water consumption gac washing is characterized in that comprising the steps:
With weight ratio is 1: the contain carbon precursor and KOH or NaOH of 1-10 mix, and in the presence of inert atmosphere, are raised to 700-1000 ℃ from room temperature; Naturally cooling after constant temperature 1-3 hour; When treating that temperature drops to room temperature, take out activation products, add water pulp thing according to the weight ratio 1 of activation products and water: 1-3 after; Through filtration under diminished pressure or centrifugal method gac and alkaliferous waste water are carried out the solid-liquid separation first time; With after separating the first time solid according to the solid first time: formic acid=1 kilogram: 1-5 rises and adds aqueous formic acid and mix, and carries out solid-liquid separation second time after vigorous stirring 1-3 hour, with after separating the second time solid again by the solid second time: water=1 kilogram: 5-50 liter; Solid mixes with water for the second time; Carry out solid-liquid separation for the third time after vigorous stirring 1-3 hour, will be for the third time solid in 180-250 ℃ of following normal pressure or drying under reduced pressure 3-10 hour, obtain product.
2. the method for a kind of low water consumption gac as claimed in claim 1 washing is characterized in that the described carbon precursor that contains is refinery coke, coal, resol, corn straw, shell carbonized material, bamboo charcoal, coconut husk carbonized material or charred rice husk material.
3. the method for a kind of low water consumption gac as claimed in claim 1 washing is characterized in that described inert atmosphere is N
2
4. the method for a kind of low water consumption gac as claimed in claim 1 washing, the concentration that it is characterized in that described aqueous formic acid is 5-50wt%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274403A (en) * | 2013-06-08 | 2013-09-04 | 中国科学院山西煤炭化学研究所 | Method for recycling strong alkali in preparation process of active carbon having high specific surface area |
| WO2017092077A1 (en) * | 2015-12-01 | 2017-06-08 | 浙江大学 | Method for preparing and forming koh solid-activated charcoal |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
| CN109455717A (en) * | 2018-10-23 | 2019-03-12 | 中国科学院山西煤炭化学研究所 | A kind of method of free state chloride ion in removal super capacitor active carbon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1669918A (en) * | 2005-02-28 | 2005-09-21 | 昆明理工大学 | Method for producing active carbon with high specific surface area |
| CN101209839A (en) * | 2007-12-24 | 2008-07-02 | 中国科学院山西煤炭化学研究所 | Preparation method of high performance active carbon |
| CN101269810A (en) * | 2008-05-06 | 2008-09-24 | 同方炭素科技有限公司 | Absorbent charcoal fine purification technique |
| CN101428794A (en) * | 2008-12-01 | 2009-05-13 | 海南大学 | Preparation of coir fiber based activated carbon with high specific surface area |
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2012
- 2012-01-19 CN CN2012100261869A patent/CN102583366A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1669918A (en) * | 2005-02-28 | 2005-09-21 | 昆明理工大学 | Method for producing active carbon with high specific surface area |
| CN101209839A (en) * | 2007-12-24 | 2008-07-02 | 中国科学院山西煤炭化学研究所 | Preparation method of high performance active carbon |
| CN101269810A (en) * | 2008-05-06 | 2008-09-24 | 同方炭素科技有限公司 | Absorbent charcoal fine purification technique |
| CN101428794A (en) * | 2008-12-01 | 2009-05-13 | 海南大学 | Preparation of coir fiber based activated carbon with high specific surface area |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274403A (en) * | 2013-06-08 | 2013-09-04 | 中国科学院山西煤炭化学研究所 | Method for recycling strong alkali in preparation process of active carbon having high specific surface area |
| WO2017092077A1 (en) * | 2015-12-01 | 2017-06-08 | 浙江大学 | Method for preparing and forming koh solid-activated charcoal |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
| CN108083276B (en) * | 2017-12-29 | 2020-12-01 | 北海星石碳材料科技有限责任公司 | Preparation method of super capacitor activated carbon |
| CN109455717A (en) * | 2018-10-23 | 2019-03-12 | 中国科学院山西煤炭化学研究所 | A kind of method of free state chloride ion in removal super capacitor active carbon |
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Application publication date: 20120718 |