CN102923701A - Method for preparing high-quality active carbon through hickory hulls - Google Patents
Method for preparing high-quality active carbon through hickory hulls Download PDFInfo
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- CN102923701A CN102923701A CN2012104640099A CN201210464009A CN102923701A CN 102923701 A CN102923701 A CN 102923701A CN 2012104640099 A CN2012104640099 A CN 2012104640099A CN 201210464009 A CN201210464009 A CN 201210464009A CN 102923701 A CN102923701 A CN 102923701A
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Abstract
The invention relates to a method for preparing high-quality active carbon through hickory hulls. By adopting the method, agricultural solid wastes with pollution is processed and recycled, and the 'waste' is turned into 'treasure', so that the problem that lots of hickory hulls are disorderly piled to result in the serious pollution to the environment is solved. The method comprises steps as follows: crushing the waste hickory hulls through a crusher to reach a certain granularity; carbonizing for 0.5 to 2h at the temperature of 500 to 800 DEG C; mixing the carbonized material and sodium carbonate based on weight ratio of 1: 1 to 1: 10; activating for 0.5 to 2 hours at 800 to 1000 DEG C; cooling the activated material; repeatedly washing by diluted hydrochloric acid and acetic acid; washing by distilled water until the pH (Potential Of Hydrogen) of the washing solution is of 6 to 7; and drying at the temperature of 130 DEG C to obtain the high-quality active carbon product, wherein the specific surface area of the high-quality active carbon product is 1500 to 2500m<2>/g, the ash content of the high-quality active carbon product is 0.3 to 2%, the content of iron is 0.003 to 0.02%, and the content of heavy metal is less than 0.002%.
Description
Technical field
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, belong to field of material preparation.
Background technology
Semen Caryae Cathayensis is less in national distribution range, mainly is distributed in Northwest Mountain Area of Zhejiang and Southeastern Anhui mountain area, and wherein 60% to be distributed in Linan City, Zhejiang Province domestic.According to the preliminary statistics, Linan City produces per year about Semen Caryae Cathayensis 15000-30000 ton within the border, and consequent Hickory Hull is about the 45000-90000 ton.Contain a kind of alkaloid in the Hickory Hull, have than strong basicity, and not perishable, the Hickory Hull that annual Semen Caryae Cathayensis is abandoned after plucking all causes severe contamination to local environment.At present no matter be to stack on the mountain or concentrating special-purpose place to stack all can't to solve the Hickory Hull solid waste that day by day increases processes, annual Linan City all drops into a large amount of manpower and materials and fund does not all obtain good effect.The present invention utilizes Hickory Hull as raw material just, produces active carbon with high specific surface area, has solved to a certain extent the difficult problem of long-term puzzlement Hickory Hull environmental pollution.
The raw material of preparation gac is very extensive, mainly is divided into ature of coal and wood material.Coal raw materials mainly contains hard coal, bituminous coal, brown coal and petroleum pitch, refinery coke etc.; Wood material mainly refers to shell, agricultural crop straw, Exocarpium cocois (Cocos nucifera L), nut-shell, oil palm shell, reaches spent pulping liquor etc.The preparation method mainly is chemical activation method and physical activation method.Physical activation method is raw material to be carried out first charing then under 600-1200 ℃ carbide is activated, and this method reactivity gas commonly used is water vapour and carbonic acid gas.The physical activation method process characteristic is activation temperature high (generally about 1000 ℃), soak time long (more than tens hours), facility investment is large, energy consumption is high.And the yield of gac is low, but environmental pollution is less, so generally at industrial the method composite reactive charcoal that seldom adopts.
Chemical activation method is after raw material and pharmaceutical chemicals are mixed, flood for some time with certain proportion; with charing and a kind of preparation method of carrying out simultaneously of activation, essence is that chemical reagent is inlaid in the charcoal granule interior structure effect and starts out abundant micropore under protection of inert gas.Activator commonly used has oxyhydroxide and the number acid of basic metal, alkaline-earth metal.Compare with physical activation method, the process characteristic of chemical activation method is: operation is simplified greatly, and activation temperature reduces, time shorten, and Energy Intensity Reduction, and can have by selecting different activators to make the gac of special hole gauge structure.The advantage of the method is: different activators and consumption thereof can make pore size distribution and the different gac of surface chemical property, can obtain high quality active carbon, and yield is high.
The patent of Chinese invention patent 200710069706 " a kind of coal mixes the super active carbon based preparation method of Semen Caryae Cathayensis ", the patent of patent CN200610049742.9 " pecan shell becomes charcoal method and charcoal device ", all be to be confined to take pecan shell as raw material, the Semen Caryae Cathayensis Pu shell of Duoing than its several times is still huddled puts serious environment pollution; The patent " a kind of method of utilizing waste walnut outer peel to prepare gac " of China invention CN200810121864.3 is to be raw material with hickory nut epicarp, the method of burnettize prepares gac, and its performance not yet can satisfy the demand of high quality active carbon.
Summary of the invention
The objective of the invention is to solve Hickory Hull ecotope is caused the problem of severe contamination, and for the deficiency that has activated carbon technology now, provide a kind of method of utilizing Semen Caryae Cathayensis Pu shell to prepare high quality active carbon.
A kind of method of utilizing Hickory Hull to prepare high quality active carbon of the present invention is characterized in that comprising following concrete steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 200～600 orders.
2) with step 1) charing under nitrogen protection of Semen Caryae Cathayensis Pu shell powder, the temperature of charing is 500～800 ℃, carbonization time is 0.5～2 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and potassium hydroxide is 1: 1～1: 10, and activation temperature is 800～1000 ℃, and soak time is 0.5～2 hour.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the active carbon with high specific surface area product 130 ℃ of lower oven dry.
Be 400 orders as preferred described Semen Caryae Cathayensis Pu shell powder optimum size.
As preferred steps 2) best carbonization temperature is 650 ℃.
As preferred steps 2) best carbonization time is 1.0 hours.
As preferred steps 3) optimum weight ratio of carbonized material and potassium hydroxide is 1: 6.
As preferred steps 3) the optimal activation temperature is 900 ℃.
As preferred steps 3) optimum activating time is 1.5 hours.
As preferred steps 2), 3) temperature rise rate be 10 ℃/min.
As preferred steps 4) the concentration of dilute hydrochloric acid be 0.2mol/L.
As preferred steps 4) the concentration of acetic acid be 1.0mol/L.
The present invention will solve Hickory Hull local environment will be polluted, and save treatment cost, make huge contribution for safeguarding ecotope.Along with the increasing of national economy every profession and trade to the active carbon with high specific surface area product demand, will produce good economic benefit and social benefit.
Embodiment
Describe the present invention below in conjunction with embodiment, better understand purpose of the present invention, characteristics and advantage.Although the present invention is described in conjunction with this specific embodiment, is not intended that the invention be limited to described specific embodiment.On the contrary, the embodiment that substitutes, improves and be equal to the embodiment that can be included in the protection domain defined in the claim of the present invention carries out all belongs to protection scope of the present invention.
Embodiment 1:
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, the method may further comprise the steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 200 orders.
2) with step 1) charing under nitrogen protection of Semen Caryae Cathayensis Pu shell powder, the temperature of charing is 500 ℃, carbonization time is 0.5 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 2, and activation temperature is 800 ℃, and soak time is 0.5 hour.
4) until step 3) clean with dilute hydrochloric acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Semen Caryae Cathayensis Pu shell gac for preparing is 1436m
2/ g, yield is 42.4%, and ash content is 1.87%, and iron level is 0.017%, and heavy metal content is 0.0016%.
Embodiment 2:
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, the method may further comprise the steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 300 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 700 ℃, carbonization time is 1.5 hours.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 3, and activation temperature is 900 ℃, and soak time is 1 hour.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Semen Caryae Cathayensis Pu shell gac for preparing is 1692m
2/ g, yield is 45.5%, and ash content is 1.43%, and iron level is 0.012%, and heavy metal content is 0.0012%.
Embodiment 3:
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, the method may further comprise the steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 400 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 4, and activation temperature is 900 ℃, and soak time is 1 hour.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Semen Caryae Cathayensis Pu shell gac for preparing is 1830m
2/ g, yield is 43.5%, and ash content is 0.93%, and iron level is 0.007%, and heavy metal content is 0.0015%.
Embodiment 4:
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, the method may further comprise the steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 500 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 5, and activation temperature is 1000 ℃, and soak time is 2 hours.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Semen Caryae Cathayensis Pu shell gac for preparing is 1676m
2/ g, yield is 39.8%, and ash content is 0.73%, and iron level is 0.008%, and heavy metal content is 0.0018%.
Embodiment 5:
The present invention relates to a kind of method of utilizing Hickory Hull to prepare high quality active carbon, the method may further comprise the steps:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 600 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 6, and activation temperature is 800 ℃, and soak time is 1.5 hours.
4) until step 3) repeatedly clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Semen Caryae Cathayensis Pu shell gac for preparing is 1742m
2/ g, yield is 42.2%, and ash content is 1.56%, and iron level is 0.016%, and heavy metal content is 0.0017%.
Embodiment 6:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 400 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 6, and activation temperature is 900 ℃, and soak time is 1 hour.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Hickory Hull gac for preparing is 2030m
2/ g, yield is 43.1%, and ash content is 0.53%, and iron level is 0.006%, and heavy metal content is 0.0012%.
Embodiment 7:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 400 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 6, and activation temperature is 900 ℃, and soak time is 1.5 hours.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Hickory Hull gac for preparing is 2370m
2/ g, yield is 41.7%, and ash content is 0.23%, and iron level is 0.003%, and heavy metal content is 0.001%.
Embodiment 8:
1) with the outdoor natural air drying of Hickory Hull, dry, in pulverizer, pulverize, powder is crossed 400 orders.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 600 ℃, carbonization time is 1.2 hours.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 6, and activation temperature is 900 ℃, and soak time is 2.0 hours.
4) until step 3) clean with dilute hydrochloric acid and acetic acid after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
The specific surface area of the Hickory Hull gac for preparing is 2010m
2/ g, yield is 42.1%, and ash content is 0.38%, and iron level is 0.005%, and heavy metal content is 0.0016%.
Claims (9)
1. method of utilizing Hickory Hull to prepare high quality active carbon is characterized in that the method may further comprise the steps:
1) Hickory Hull is positioned over outdoor naturally dry, air-dry, in pulverizer, pulverize, powder is crossed the 200-600 order.
2) with step 1) charing under nitrogen protection of Hickory Hull powder, the temperature of charing is 500～800 ℃, carbonization time is 0.5～2 hour.
3) with step 2) carbonized material and yellow soda ash activates under nitrogen protection after mixing, and the weight ratio of carbonized material and yellow soda ash is 1: 1～1: 10, and activation temperature is 800～1000 ℃, and soak time is 0.5～2 hour.
4) until step 3) clean with dilute hydrochloric acid and acetic acid respectively after the products therefrom cooling, again with distilled water clean to washing lotion pH value be 6～7, namely obtain the high quality active carbon product 130 ℃ of lower oven dry.
2. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1, it is characterized in that: described Hickory Hull powder optimum size was 400 orders.
3. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 2 wherein) best carbonization temperature is 650 ℃.
4. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 2 wherein) best carbonization time is 1.0 hours.
5. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 3 wherein) optimum weight ratio of carbonized material and yellow soda ash is 1: 6.
6. a kind of method of utilizing Hickory Hull to prepare active carbon with high specific surface area as claimed in claim 1 is characterized in that: step 3 wherein) the optimal activation temperature is 900 ℃.
7. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 3 wherein) optimum activating time is 1.5 hours.
8. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 2 wherein), 3) temperature rise rate be 10 ℃/min.
9. a kind of method of utilizing Hickory Hull to prepare high quality active carbon as claimed in claim 1 is characterized in that: step 4 wherein) the concentration of dilute hydrochloric acid be 0.2mol/L, acetate concentration is 1.0mol/L.
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| CN2012104640099A CN102923701A (en) | 2012-11-12 | 2012-11-12 | Method for preparing high-quality active carbon through hickory hulls |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104192841A (en) * | 2014-09-27 | 2014-12-10 | 管天球 | Preparation method for old oil tea tree branch active carbon |
| CN104192842A (en) * | 2014-09-27 | 2014-12-10 | 管天球 | Method for preparing walnut shell activated carbon |
| CN104925806A (en) * | 2014-03-20 | 2015-09-23 | 吕凤楼 | Preparation method of walnut activated carbon |
| CN113267573A (en) * | 2021-06-21 | 2021-08-17 | 国科大杭州高等研究院 | Preparation method and application of walnut shell activated carbon solid-phase extraction column |
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| CN102050446A (en) * | 2010-12-18 | 2011-05-11 | 江苏技术师范学院 | Method for preparing activated carbon by using corn cob |
| CN102423688A (en) * | 2011-08-26 | 2012-04-25 | 昆明理工大学 | Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine |
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| CN102050446A (en) * | 2010-12-18 | 2011-05-11 | 江苏技术师范学院 | Method for preparing activated carbon by using corn cob |
| CN102423688A (en) * | 2011-08-26 | 2012-04-25 | 昆明理工大学 | Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine |
Non-Patent Citations (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925806A (en) * | 2014-03-20 | 2015-09-23 | 吕凤楼 | Preparation method of walnut activated carbon |
| CN104192841A (en) * | 2014-09-27 | 2014-12-10 | 管天球 | Preparation method for old oil tea tree branch active carbon |
| CN104192842A (en) * | 2014-09-27 | 2014-12-10 | 管天球 | Method for preparing walnut shell activated carbon |
| CN104192842B (en) * | 2014-09-27 | 2015-12-02 | 管天球 | A kind of preparation method of nut-shell gac |
| CN104192841B (en) * | 2014-09-27 | 2015-12-09 | 管天球 | A kind of preparation method of old oil tea branch gac |
| CN113267573A (en) * | 2021-06-21 | 2021-08-17 | 国科大杭州高等研究院 | Preparation method and application of walnut shell activated carbon solid-phase extraction column |
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Application publication date: 20130213 |