CN101274758B - Preparation for water chestnut leather activated char - Google Patents

Preparation for water chestnut leather activated char Download PDF

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Publication number
CN101274758B
CN101274758B CN200810016234XA CN200810016234A CN101274758B CN 101274758 B CN101274758 B CN 101274758B CN 200810016234X A CN200810016234X A CN 200810016234XA CN 200810016234 A CN200810016234 A CN 200810016234A CN 101274758 B CN101274758 B CN 101274758B
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China
Prior art keywords
water
preparation
activated char
water caltrop
water chestnut
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Expired - Fee Related
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CN200810016234XA
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CN101274758A (en
Inventor
张成禄
张建
韩福眷
史倩倩
王丽
李超
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Shandong University
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Shandong University
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Abstract

The invention relates to a method for preparing the activated charcoal of water caltrop peels which comprises the preparation of the powdered activated charcoal of water caltrop peels and the lumpish activated charcoal of water caltrop peels. The preparation method of the invention comprises the steps of drying, pre-oxidation, washing, baking and carbonization. Since the method does not adopt methods such as a potassium hydroxide process and a zinc chloride process, etc., during the preparation process, not only environmental pollution can be avoided, but also the operation becomes simple. The activated charcoal of water caltrop peels prepared by the method of the invention can be applied to a plurality of fields. The powdered activated charcoal can be used as an adsorbent to absorb a plurality of common substances as well as toxic and harmful substances such as dyes and phenol, etc., while the lumpish activated charcoal can be taken as fillers used in fluidized beds, moving beds and certain fixed beds and the fillers have better bio-affinity and hydrophilicity, are beneficial to biofilm culturing and cause no secondary pollution to environment after being disused.

Description

The preparation method of water chestnut leather activated char
Technical field
The present invention relates to a kind of preparation method of active carbon, especially a kind of preparation method of water chestnut leather activated char.
Background technology
The raw material of preparation gac mainly contains timber, wood chip, shell etc. at present, wherein based on timber, but forest coverage falls sharply in recent years, the wood supply amount reduces, make the raw material supply of gac present nervous trend, price also is rise trend, causes the preparation of gac and utilization to be subjected to great restriction.In addition, what also have is the feedstock production gac with coal, mud, plastics, but these raw materials can cause environmental pollution, therefore can not be widely used at present.Recently, make the favor that gac has been subjected to the investigator, disperse, be difficult to centralized collection, and expense is higher, also be difficult to promote the use of but most of shell produces ground with shell.In addition, the preparation technology of existing gac mainly is potassium hydroxide method, zinc chloride process, and the waste liquid that these two kinds of methods produce is difficult to reuse again, more easily produces environmental pollution, and danger is bigger when operation.
Summary of the invention
The present invention is for overcoming above-mentioned the deficiencies in the prior art, and a kind of preparation method of simple for production, cheap, water chestnut leather activated char that environmental pollution is little is provided.
The objective of the invention is to adopt following technical proposals to realize: a kind of preparation method of water chestnut leather activated char, water chestnut leather activated char comprises Powdered and block, the preparation method of Powdered water chestnut leather activated char may further comprise the steps:
1) with water caltrop skin drying, is crushed to 80~100 orders then;
2) pre-oxidation treatment is soaked the water caltrop skin after the drying and crushing 5~9 hours with Peracetic Acid;
3) washing, with the water caltrop skin of preoxidation with distilled water immersion 10~12 hours, wash to pH be 6.0~6.5,105 ℃~120 ℃ oven dry;
4) dipping is used phosphate impregnation 10~16 hours with the water caltrop skin of oven dry;
5) charing, activation are put into retort furnace to the good water caltrop skin of dipping and are carried out charing, activation, and temperature is 390 ℃~430 ℃, and the time is 70~90 minutes, take out after being cooled to normal temperature;
6) washing, oven dry, charing, water caltrop skin that activation is good wash to pH be 6.5~7.0, at last 105 ℃~120 ℃ oven dry, get final product Powdered water chestnut leather activated char.
Drying in the step 1) is meant in baking oven and dries or dry naturally in 105 ℃~120 ℃.
The volume fraction of the Peracetic Acid step 2) is 30%~60%.
Distilled water is adopted in washing in the step 3).
Phosphoric acid volume fraction in the step 4) is 35%~45%, and phosphoric acid is 1.8: 1~2.0: 1 with the ratio of water caltrop powder quality.
Distilled water is adopted in washing in the step 6).
A kind of preparation method of water chestnut leather activated char, water chestnut leather activated char comprises Powdered and block, the preparation method of block water chestnut leather activated char may further comprise the steps:
1) the water caltrop skin drying of will not pulverizing;
2) pre-oxidation treatment is soaked dried water caltrop skin 5~9 hours with Peracetic Acid.
3) washing is used distilled water immersion 10~12 hours with the water caltrop skin after the pre-oxidation treatment, washs to pH to 6.0~6.5 again, takes out the water caltrop skin then;
4) charing is put into the water caltrop skin after the washing charring furnace and is carried out charing, and carbonization temperature is 250 ℃~310 ℃, and carbonization time is 40~70 minutes, places in stove then after 1.5~2 hours and takes out, get final product block water chestnut leather activated char.
Drying in the step 1) is meant in baking oven and dries or dry naturally in 105 ℃~120 ℃.
The volume fraction of the Peracetic Acid step 2) is 30%~60%.
What the washing in the step 3) was adopted is distilled water.
The water caltrop skin is as a kind of shell skin of waterplant fruit, and quality is hard, not perishable, and produces in a large number in wetland, as inappropriate processing, can pollute environment.Therefore, manage to utilize the raw material of this shell, it is turned waste into wealth, have great importance as gac.The charcoal that water caltrop skin powder is fired into has the advantage of other gacs, also has certain intensity, and does not use methods such as potassium hydroxide method, zinc chloride process in preparation process, has both avoided the pollution to environment, and is easy and simple to handle again.
The prepared water chestnut leather activated char of the present invention can be used for a lot of fields, and pulverous gac both can adsorb some conventional substances as sorbent material, again can absorbing dye, hazardous and noxious substances such as phenol; Blocky gac can be used as the filler of fluidized-bed, moving-bed and some fixed bed, and this filler has bioaffinity and hydrophilicity preferably, is beneficial to biofilm, and can not produce secondary pollution to environment after it is discarded
The present invention is a raw material with wide material sources, water caltrop skin cheap and easy to get, belongs to utilization of waste material, has the following advantages:
1. the water caltrop skin is easy to a large amount of collections, can reduce preparation cost;
2, compare with other raw material making methods, the phosphoric acid method is adopted in the preparation of water chestnut leather activated char, and preparation is easy, and easy and simple to handle, preparation process is less to the pollution of environment;
3, the gac that makes of this method has abundant pore texture and bigger specific surface area;
4, utilize hard, the not perishable water caltrop skin of quality, can reduce its pollution surrounding environment.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1
With the water caltrop skin in baking oven in 105 ℃ of oven dry or dry naturally, pulverize then, make it pass through 80 purpose sieves, be that preoxidation is carried out in 30% Peracetic Acid immersion with volume fraction again, soak time is 9 hours; The exhausted Peracetic Acid is poured in the specified container, uses distilled water immersion water caltrop skin 10 hours again, and being washed with distilled water to pH again is 6.0,105 ℃ of oven dry; 's 1.8: 1 impregnating ratio dipping 16 hours with the particle after the preoxidation with 35% phosphoric acid, then the good water caltrop skin of dipping is put into retort furnace, 390 ℃ of charings, activation 90 minutes, take out after being cooled to normal temperature, being washed with distilled water to pH is 6.5, again 105 ℃ of oven dry, get final product Powdered water chestnut leather activated char.
Embodiment 2
With the water caltrop skin in baking oven in 120 ℃ of oven dry or dry naturally, pulverize then, make it pass through 100 purpose sieves, be that preoxidation is carried out in 60% Peracetic Acid immersion with volume fraction again, soak time is 5 hours; The exhausted Peracetic Acid is poured in the specified container, uses distilled water immersion water caltrop skin 12 hours again, and being washed with distilled water to pH then is 6.5,120 ℃ of oven dry; 's 2.0: 1 impregnating ratio dipping 10 hours with the particle after the preoxidation with 45% phosphoric acid, then the good water caltrop skin of dipping is put into retort furnace, 430 ℃ of charings, activation 70 minutes, take out after being cooled to normal temperature, being washed with distilled water to pH is 7.0, again 120 ℃ of oven dry, get final product Powdered water chestnut leather activated char.
Embodiment 3
With the water caltrop skin in baking oven in 110 ℃ of oven dry or dry naturally, pulverize then, make it pass through 90 purpose sieves, be that preoxidation is carried out in 45% Peracetic Acid immersion with volume fraction again, soak time is 7 hours; The exhausted Peracetic Acid is poured in the specified container, uses distilled water immersion water caltrop skin 11 hours again, and being washed with distilled water to pH then is 6.3,115 ℃ of oven dry; 's 1.9: 1 impregnating ratio dipping 13 hours with the particle after the preoxidation with 40% phosphoric acid, then the good water caltrop skin of dipping is put into retort furnace, 410 ℃ of charings, activation 80 minutes, take out after being cooled to normal temperature, being washed with distilled water to pH is 6.7, again 115 ℃ of oven dry, get final product Powdered water chestnut leather activated char.
Embodiment 4
With the water caltrop skin in baking oven in 105 ℃ of oven dry or dry naturally, be that preoxidation is carried out in the immersion of 30% Peracetic Acid with volume fraction then, soak time is 9 hours; The Peracetic Acid of exhausted is poured in the specified containers, used distilled water immersion then 10 hours, being washed with distilled water to pH again is 6.5; Take out the water caltrop skin then, put it in the charring furnace and carry out charing at 310 ℃, the time is 40 minutes, places in stove after 2 hours then and takes out, get final product block water chestnut leather activated char.
Embodiment 5
With the water caltrop skin in baking oven in 120 ℃ of oven dry or dry naturally, be that preoxidation is carried out in the immersion of 60% Peracetic Acid with volume fraction then, soak time is 5 hours; The exhausted Peracetic Acid is poured in the specified containers, and the exhausted Peracetic Acid is poured in the specified container, uses distilled water immersion water caltrop skin 12 hours again, and being washed with distilled water to pH again is 6.0; Take out the water caltrop skin then, put it in the charring furnace and carry out charing at 250 ℃, the time is 70 minutes, places in stove after 1.5 hours then and takes out, get final product block water chestnut leather activated char.
Embodiment 6:
With the water caltrop skin in baking oven in 110 ℃ of oven dry or dry naturally, be that preoxidation is carried out in the immersion of 50% Peracetic Acid with volume fraction then, soak time is 6 hours; The exhausted Peracetic Acid is poured in the specified container, uses distilled water immersion water caltrop skin 11 hours again,, being washed with distilled water to pH again is 6.3; Take out the water caltrop skin then, put it in the charring furnace and carry out charing at 270 ℃, the time is 60 minutes, places in stove after 1.7 hours then and takes out, get final product block water chestnut leather activated char.

Claims (10)

1. the preparation method of a Powdered water chestnut leather activated char is characterized in that, may further comprise the steps:
1) with water caltrop skin drying, is crushed to 80~100 orders then;
2) pre-oxidation treatment is soaked the water caltrop skin after the drying and crushing 5~9 hours with Peracetic Acid;
3) washing, with the water caltrop skin of preoxidation with distilled water immersion 10~12 hours, wash to pH be 6.0~6.5,105~120 ℃ of oven dry;
4) dipping is used phosphate impregnation 10~16 hours with the water caltrop skin of oven dry;
5) charing, activation are put into retort furnace to the good water caltrop skin of dipping and are carried out charing, activation, and temperature is 390 ℃~430 ℃, and the time is 70~90 minutes, take out after being cooled to normal temperature;
6) washing, oven dry, charing, water caltrop skin that activation is good wash to pH be 6.5~7.0, at last 105 ℃~120 ℃ oven dry, get final product Powdered water chestnut leather activated char.
2. the preparation method of Powdered water chestnut leather activated char according to claim 1 is characterized in that, the drying in the step 1) is meant in baking oven and dries or dry naturally in 105 ℃~120 ℃.
3. the preparation method of Powdered water chestnut leather activated char according to claim 1 is characterized in that step 2) in the volume fraction of Peracetic Acid be 30%~60%.
4. the preparation method of Powdered water chestnut leather activated char according to claim 1 is characterized in that, distilled water is adopted in the washing in the step 3).
5. the preparation method of Powdered water chestnut leather activated char according to claim 1 is characterized in that, the volume fraction of the phosphoric acid in the step 4) is 35%~45%, and phosphoric acid is 1.8: 1~2.0: 1 with the ratio of water caltrop powder quality.
6. the preparation method of Powdered water chestnut leather activated char according to claim 1 is characterized in that, distilled water is adopted in the washing in the step 6).
7. the preparation method of a block water chestnut leather activated char is characterized in that, may further comprise the steps:
1) the water caltrop skin drying of will not pulverizing;
2) pre-oxidation treatment is soaked dried water caltrop skin 5~9 hours with Peracetic Acid;
3) washing is used distilled water immersion 10~12 hours with the water caltrop skin after the pre-oxidation treatment, washs to pH to 6.0~6.5 again, takes out the water caltrop skin then;
4) charing is put into the water caltrop skin after the washing charring furnace and is carried out charing, and carbonization temperature is 250 ℃~310 ℃, and carbonization time is 40~70 minutes, places in stove then after 1.5~2.0 hours and takes out, get final product block water chestnut leather activated char.
8. the preparation method of block water chestnut leather activated char according to claim 7 is characterized in that, the drying in the step 1) is meant in baking oven and dries or dry naturally in 105 ℃~120 ℃.
9. the preparation method of block water chestnut leather activated char according to claim 7 is characterized in that step 2) in the volume fraction of Peracetic Acid be 30%~60%.
10. the preparation method of block water chestnut leather activated char according to claim 7 is characterized in that, what the washing in the step 3) was adopted is distilled water.
CN200810016234XA 2008-05-19 2008-05-19 Preparation for water chestnut leather activated char Expired - Fee Related CN101274758B (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942284B (en) * 2012-10-23 2014-06-04 浙江工业大学 Method for preparing biological fluidized bed carrier and treating waste water
CN104445191A (en) * 2013-09-13 2015-03-25 中国科学院兰州化学物理研究所 Method for preparation of activated carbon with high specific surface area by using potato as carbon source
CN103466619A (en) * 2013-09-26 2013-12-25 山东大学 Method for preparing active carbon by organic alcohol or organic acid doping modification
CN108793157B (en) * 2018-08-24 2020-04-24 山东大学 Method for preparing activated carbon from wetland fruit shells and hydrolyzed feather meal mixed base carbon precursor
CN116099509B (en) * 2023-01-13 2023-08-01 安徽工业大学 Sodium alginate/gelatin biochar multi-element composite material, preparation method and method for treating cadmium in water body

Citations (4)

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Publication number Priority date Publication date Assignee Title
GB1467496A (en) * 1974-10-28 1977-03-16 North American Carbon Method of manufacturing activated carbon
CA1024972A (en) * 1974-10-21 1978-01-24 Julius L. Kovach Method to manufacturing activated carbon
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CN101070156A (en) * 2007-06-08 2007-11-14 山东大学 Method for preparing active charcoal of poly gonum orientale straw stem

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CA1024972A (en) * 1974-10-21 1978-01-24 Julius L. Kovach Method to manufacturing activated carbon
GB1467496A (en) * 1974-10-28 1977-03-16 North American Carbon Method of manufacturing activated carbon
CN101070155A (en) * 2007-06-08 2007-11-14 山东大学 Method for preparing active charcoal of scripus tubernaemontani stem
CN101070156A (en) * 2007-06-08 2007-11-14 山东大学 Method for preparing active charcoal of poly gonum orientale straw stem

Non-Patent Citations (4)

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Title
XING Wei et al..EFFECTS OF PREOXIDATION ON THESURFACEPROPERTIES OF SUPER ACTIVE CARBON.新型炭材料17 3.2002,17(3),25-30.
XING Wei et al..EFFECTS OF PREOXIDATION ON THESURFACEPROPERTIES OF SUPER ACTIVE CARBON.新型炭材料17 3.2002,17(3),25-30. *
王晓瑞等.煤沥青预处理工艺对活性炭孔结构的影响.煤炭转化27 4.2004,27(4),59-63.
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