CN1927710A - Method of preparing activated carbon from corn straw - Google Patents
Method of preparing activated carbon from corn straw Download PDFInfo
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- CN1927710A CN1927710A CN 200610096499 CN200610096499A CN1927710A CN 1927710 A CN1927710 A CN 1927710A CN 200610096499 CN200610096499 CN 200610096499 CN 200610096499 A CN200610096499 A CN 200610096499A CN 1927710 A CN1927710 A CN 1927710A
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Abstract
The present invention aims at providing efficient and fast process of preparing corn stalk active carbon with high adsorption performance. The process includes the steps of crushing corn stalk, soaking with composite activating agent at 25-60 deg.c for 20-60 min under ultrasonic action, microwave activation, and final ultrasonic washing for 3-10 min. The composite activating agent consists of phosphoric acid solution, sulfuric acid solution and NaCl. The active carbon of the present invention has a methylene blue adsorbing amount of 19-21 ml/0.1g.
Description
One, technical field
The present invention relates to prepare process of active carbon, belong to ultrasonic and make the field with microwave chemical.
Two, background technology
The technology and the production process of preparation gac mainly are to adopt activator to soak for a long time at a certain temperature with containing carbon feedstock both at home and abroad at present, activate in activation furnace or in the microwave oven then, repeatedly wash with acid, water again.But existing method exists all that soak time is long, consumed energy is big and water consumption is many and problem such as contaminated wastewater.As application number be 200510010672.1 Chinese patent application disclosed " a kind of method of producing mesopore activated carbon " just need with raw material in phosphoric acid solution 40-60 ℃ soaked 4-8 hour down; Application number is that 200410061119.6 Chinese patent application disclosed " produce residue with turmeric saponin and prepare process of active carbon " need be soaked 12-24 hour in liquor zinci chloridi after the raw material carbonization again; The patent No. is that the Chinese patent of ZL02113270.4 disclosed a kind of " microwave radiation tobacco rod solid waste is made process of active carbon " also needs raw material is soaked more than 8 hours in liquor zinci chloridi.In addition, go up the clear described a kind of preparation process of active carbon of delivering of " being equipped with the research of corn stalk active carbon with the phosphoric acid legal system " article that waits of Wang Quan in 2003 the 4th phases " Chinese comprehensive utilization of resources ", also need raw material soaking 24 hours, drying is 2 hours under 67-70 ℃, 450 ℃ activate 2 hours, and activated material needs through the hot water repetitive scrubbing; " chemistry of forest product and industry " last Jiang Hui etc. delivered " microwave method is made corn stalk active carbon processing condition and performance study " article 2005 the 4th phases, with the zinc chloride is activator, soaked 30 hours, microwave activation 570 seconds is after technologies such as pickling, rinsing obtain the gac that the methylene blue decolorizing ability is 13.1mL/0.1g.Though more than disclosed preparation process of active carbon do not report the washing time of activated material, yet find that under study for action the washing of activated material will repeatedly wash that just to reach the pH value be 6.5-7 with a large amount of water in the aforesaid method.
All there are the problems such as pollution that soak time is long, consumed energy is big, have waste water in the single activator of the most employings of the method that foregoing invention patent and document relate to.
Three, summary of the invention
The purpose of this invention is to provide a kind of with maize straw as raw materials for production, the preparation process of active carbon of carrying out rapid soaking and washing activated material with ultrasonic technique fast with composite activating agent and ultrasonic technique.
Provided by the present inventionly a kind ofly prepare process of active carbon with maize straw, comprise to the agricultural wastes maize straw being pulverizing, immersion, microwave activation and the washing step of raw material, it is characterized in that: in immersion and washing step, use ultrasonic generating unit, immersion and washing process are carried out under ultrasonic cavitation.
Described immersion process uses soak solution to be composite activating agent.Composite activating agent be by the phosphoric acid solution of technical grade purity weight concentration 18%-40% by solid-to-liquid ratio (grams per milliliter) than being 1: 1.5-10, the vitriol oil [add-on (unit milliliter)=amount of solid (unit gram)/(80-100 concentration of phosphoric acid)] and sodium-chlor (add-on gram=amount of solid gram/10) are formed;
Ultrasonic power is 100-500 watt in the described immersion process, and power is adjustable continuously, and frequency 28KHz, 45Hz and 100Hz three are frequently adjustable, and 600 watts of heating powers, ultrasonic soaking temperature are 25-60 ℃, and ultrasonic soak time is 20-60 minute;
Described washing process ultrasonic power is 100-500 watt, and power is adjustable continuously, and frequency 28KHz, 45Hz and 100Hz three are frequently adjustable, 600 watts of heating powers, and supersound washing 3 times each time 3-10 minute, makes the pH value of solution reach 6.5-7;
The present invention compares with existing preparation corn stalk active carbon technology has following advantage:
(1) adopt composite activating agent to improve than the quality product of the corn stalk active carbon that adopts phosphoric acid or zinc chloride activation agent to prepare, decolorizing ability strengthens, and the methylene blue decolorizing ability surpasses 19mL/0.1g;
(2) adopt the ultrasonic-microwave coupling technique to support composite activating agent, make the production cycle of preparation corn stalk active carbon shorten, enhance productivity;
(3) adopt ultrasonic technique washing activated material, make washing time shorten, washings can use repeatedly, has reduced the discharging of waste water, has saved resource, has protected environment.
Four, specific implementation method
The present invention is further illustrated below by example.
Embodiment 1
After will taking from the geographic maize straw in Huaian, Jiangsu and being crushed to about 10mm, getting concentration at 1: 10 according to solid-to-liquid ratio is 18% phosphoric acid, with add-on ((milliliter)=amount of solid (unit gram)/(80 concentration of phosphoric acid) according to the vitriol oil, the vitriol oil that NaCl add-on gram=amount of solid gram/10 calculation formula are calculated, NaCl mixes, 25 ℃ of controlled temperature are ultrasonic 60 minutes in 100 watts of ultra-sonic generators, after the power of packing into be activation 8 minutes in 700 watts the microwave oven, the water that adds 5 times of activated materials, fully stir and be placed in the ultra-sonic generator ultrasonic 3 minutes, repeat 2 times according to identical method again behind the suction filtration and become the aqueous solution that pH is 6.5-7, drying promptly gets activated carbon product again, and the yield of gac is 30.56%.According to national standard (GB12496.1-22-1999) test, leading indicator---methylene blue adsorption value is 19mL/0.1g.And the methylene blue adsorption value of gac first grade is 9mL/0.1g in the national standard (GB13803.3-1999), and the activated carbon product methylene blue adsorption value of present embodiment production is 2.11 times of country-level standard.
Embodiment 2
After will taking from the geographic maize straw in Huaian, Jiangsu and being crushed to about 15mm, getting concentration at 1: 6 according to solid-to-liquid ratio is 30% phosphoric acid, with add-on=amount of solid (unit gram)/(90 concentration of phosphoric acid) according to the vitriol oil, the vitriol oil that NaCl add-on gram=amount of solid gram/10 calculation formula are calculated, NaCl mixes, 45 ℃ of controlled temperature are ultrasonic 50 minutes in 300 watts of ultra-sonic generators, after the power of packing into be activation 8 minutes in 700 watts the microwave oven, the water that adds 5 times of activated materials, fully stir and be placed in the ultra-sonic generator ultrasonic 3 minutes, repeating 2 times according to identical method again behind the suction filtration becomes the aqueous solution that pH is 6.5-7, and drying promptly gets activated carbon product again.The yield of gac is 31.36%, and according to national standard (GB12496.1-22-1999) test, leading indicator---methylene blue adsorption value is 21mL/0.1g.And the methylene blue adsorption value of gac first grade is 9mL/0.1g in the national standard (GB13803.3-1999), and the activated carbon product methylene blue adsorption value of present embodiment production is 2.33 times of international primary standard.
Embodiment 3
After will taking from the geographic maize straw in Huaian, Jiangsu and being crushed to about 5mm, getting concentration at 1: 1.5 according to solid-to-liquid ratio is 40% phosphoric acid, with add-on=amount of solid (unit gram)/(100 concentration of phosphoric acid) according to the vitriol oil, the vitriol oil that NaCl add-on gram=amount of solid gram/10 calculation formula are calculated, NaCl mixes, 60 ℃ of controlled temperature are ultrasonic 20 minutes in 100 watts of ultra-sonic generators, after the power of packing into be activation 8 minutes in 700 watts the microwave oven, the water that adds 5 times of activated materials, fully stir and be placed in the ultra-sonic generator ultrasonic 3 minutes, repeating 2 times according to identical method again behind the suction filtration becomes the aqueous solution that pH is 6.5-7, and drying promptly gets activated carbon product again.The yield of gac is 30.25%, and according to national standard (GB12496.1-22-1999) test, leading indicator---methylene blue adsorption value is 20.6mL/0.1g.And the methylene blue adsorption value of gac first grade is 9mL/0.1g in the national standard (GB13803.3-1999), and the activated carbon product methylene blue adsorption value of present embodiment production is 2.3 times of international primary standard.
Claims (4)
1, a kind ofly prepares process of active carbon with maize straw, comprise to the agricultural wastes maize straw being pulverizing, immersion, microwave activation and the washing step of raw material, it is characterized in that: in immersion and washing step, use ultrasonic generating unit, immersion and washing process are carried out under ultrasonic cavitation.
2, a kind ofly prepare process of active carbon according to claim 1 is described with maize straw, it is characterized in that: the soak solution that described immersion process uses is composite activating agent, this composite activating agent be by the phosphoric acid solution of technical grade purity weight concentration 18%-40% by solid-to-liquid ratio (grams per milliliter) than being 1: 1.5～10, the vitriol oil [add-on (unit milliliter)=amount of solid (unit gram)/(80～100 concentration of phosphoric acid)] and sodium-chlor (add-on gram=amount of solid gram/10) are formed.
3, describedly a kind ofly prepare process of active carbon according to claim 1 or 2 with maize straw, it is characterized in that: ultrasonic power is 100～500 watts in the described immersion process, power is adjustable continuously, frequency 28KHz, 45Hz and 100Hz three are frequently adjustable, 600 watts of heating powers, ultrasonic soaking temperature is 25～60 ℃, and ultrasonic soak time is 20～60 minutes.
4, according to claim 3 described a kind of methods that prepare process of active carbon with maize straw, it is characterized in that: ultrasonic power is 100～500 watts in the described washing step, power is adjustable continuously, frequency 28KHz, 45Hz and 100Hz three are frequently adjustable, 600 watts of heating powers, carry out 3 supersound washings, each time carried out 3～10 minutes, made the pH value of solution reach 6.5～7.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100964996A CN100482587C (en) | 2006-09-28 | 2006-09-28 | Method of preparing activated carbon from corn straw |
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| CNB2006100964996A CN100482587C (en) | 2006-09-28 | 2006-09-28 | Method of preparing activated carbon from corn straw |
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| CN1927710A true CN1927710A (en) | 2007-03-14 |
| CN100482587C CN100482587C (en) | 2009-04-29 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134069A (en) * | 2010-11-18 | 2011-07-27 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of activated carbon |
| CN102292289A (en) * | 2008-10-06 | 2011-12-21 | 卡波恩科斯集团有限公司 | System and method for activating carbonaceous material |
| CN103058462A (en) * | 2013-01-14 | 2013-04-24 | 江苏省农业科学院 | Method for purifying dye wastewater by series connection of double systems |
| CN101723359B (en) * | 2008-10-23 | 2013-09-25 | 浙江富来森能源科技有限公司 | Method for washing electrode active carbon |
| CN104071787A (en) * | 2014-06-20 | 2014-10-01 | 西北师范大学 | Preparation method of biomass-based active carbon |
| CN104229794A (en) * | 2014-09-18 | 2014-12-24 | 苏州新协力环保科技有限公司 | Method for preparing activated carbon with corn stalks |
| CN104821396A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | Porous active carbon/aluminum oxide composite electrode material and preparation method |
| CN109231202A (en) * | 2018-12-05 | 2019-01-18 | 重庆文理学院 | A kind of ginger straw base nanometer porous carbon and preparation method thereof |
| CN110755991A (en) * | 2018-07-27 | 2020-02-07 | 中国石油化工股份有限公司 | Styrene waste gas treatment method |
| CN112973627A (en) * | 2021-02-08 | 2021-06-18 | 北京工业大学 | Active carbon composite modification method for removing LAS in building grey water |
| CN115178235A (en) * | 2022-06-16 | 2022-10-14 | 昆明理工大学 | Method for removing Cr (VI) in water body by high-efficiency adsorption of modified biochar |
-
2006
- 2006-09-28 CN CNB2006100964996A patent/CN100482587C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102292289A (en) * | 2008-10-06 | 2011-12-21 | 卡波恩科斯集团有限公司 | System and method for activating carbonaceous material |
| CN101723359B (en) * | 2008-10-23 | 2013-09-25 | 浙江富来森能源科技有限公司 | Method for washing electrode active carbon |
| CN102134069B (en) * | 2010-11-18 | 2012-11-21 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of activated carbon |
| CN102134069A (en) * | 2010-11-18 | 2011-07-27 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of activated carbon |
| CN103058462A (en) * | 2013-01-14 | 2013-04-24 | 江苏省农业科学院 | Method for purifying dye wastewater by series connection of double systems |
| CN103058462B (en) * | 2013-01-14 | 2013-12-18 | 江苏省农业科学院 | Method for purifying dye wastewater by series connection of double systems |
| CN104071787B (en) * | 2014-06-20 | 2016-01-27 | 西北师范大学 | A kind of preparation method of biomass-based gac |
| CN104071787A (en) * | 2014-06-20 | 2014-10-01 | 西北师范大学 | Preparation method of biomass-based active carbon |
| CN104229794A (en) * | 2014-09-18 | 2014-12-24 | 苏州新协力环保科技有限公司 | Method for preparing activated carbon with corn stalks |
| CN104821396A (en) * | 2015-04-03 | 2015-08-05 | 安徽江威精密制造有限公司 | Porous active carbon/aluminum oxide composite electrode material and preparation method |
| CN110755991A (en) * | 2018-07-27 | 2020-02-07 | 中国石油化工股份有限公司 | Styrene waste gas treatment method |
| CN110755991B (en) * | 2018-07-27 | 2021-12-24 | 中国石油化工股份有限公司 | Styrene waste gas treatment method |
| CN109231202A (en) * | 2018-12-05 | 2019-01-18 | 重庆文理学院 | A kind of ginger straw base nanometer porous carbon and preparation method thereof |
| CN112973627A (en) * | 2021-02-08 | 2021-06-18 | 北京工业大学 | Active carbon composite modification method for removing LAS in building grey water |
| CN112973627B (en) * | 2021-02-08 | 2023-07-28 | 北京工业大学 | Active carbon composite modification method for LAS removal in building grey water |
| CN115178235A (en) * | 2022-06-16 | 2022-10-14 | 昆明理工大学 | Method for removing Cr (VI) in water body by high-efficiency adsorption of modified biochar |
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| CN100482587C (en) | 2009-04-29 |
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Assignee: Huaian MDC Chemical Co., Ltd. Assignor: Huaiyin Normal College Contract fulfillment period: 2009.5.10 to 2015.5.9 contract change Contract record no.: 2009320001357 Denomination of invention: Method of preparing activated carbon from corn straw Granted publication date: 20090429 License type: Exclusive license Record date: 2009.8.4 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.5.10 TO 2015.5.9; CHANGE OF CONTRACT Name of requester: HUAIAN MDC-CHEM CO., LTD. Effective date: 20090804 |
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