CN105170089A - Method for preparing chemical leakage accident adsorbents from excess activated sludge - Google Patents

Method for preparing chemical leakage accident adsorbents from excess activated sludge Download PDF

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Publication number
CN105170089A
CN105170089A CN201510670123.0A CN201510670123A CN105170089A CN 105170089 A CN105170089 A CN 105170089A CN 201510670123 A CN201510670123 A CN 201510670123A CN 105170089 A CN105170089 A CN 105170089A
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CN
China
Prior art keywords
residual
leakage accident
sludge
chemical leakage
adsorbent
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Pending
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CN201510670123.0A
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Chinese (zh)
Inventor
张宏哲
牟桂琴
郭亚逢
唐晓丽
张志远
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Priority to CN201510670123.0A priority Critical patent/CN105170089A/en
Publication of CN105170089A publication Critical patent/CN105170089A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for preparing chemical leakage accident adsorbents from excess activated sludge, and mainly solves the problems of higher cost and environment pollution in the prior art. According to the method for preparing the chemical leakage accident adsorbents from the excess activated sludge, crushed excess activated sludge with the moisture content being lower than 60 percent and alkali liquor are subjected to sealing steeping after being mixed and are then put into an electric heating box for constant temperature heating; the mixture is taken out and is then washed until the pH is 6 to 8; then, drying is carried out; the dried excess activated sludge is ground; the ground excess activated sludge and a phosphoric acid solution are mixed; the mixed solution is put into a drying box to be subjected to air pre-oxidation; the excess activated sludge subjected to pre-oxidation is subjected to temperature rise under the nitrogen gas atmosphere for carbonization and activation; the excess activated sludge subjected to carbonization and activation is taken out after the temperature is lowered; after washing, the chemical leakage accident adsorbents are obtained. Through the technical scheme, the problems are better solved, and the method can be used for preparing the chemical leakage accident adsorbents.

Description

Residual actived sludge is for the method for chemical leakage accident adsorbent
Technical field
The present invention relates to the method for a kind of residual actived sludge for chemical leakage accident adsorbent.
Background technology
Since the sixties in 20th century, in world wide, there occurs the environmental pollution accident of a lot of burst chemicals, as Rhine contamination accident in 1986, Danube contamination accident in 2000 and Songhua River Pollution events in 2005 etc.These environmental pollution sudden accidents not only cause huge economic loss, and bring huge disaster to environment, human health, society and expanding economy.Therefore, the emergency disposal technology of burst chemicals environmental pollution accident is caused to the great attention of countries in the world government.How people prevent and except the sudden environmental disaster event of prediction and warning occurs, also carried out the emergency disposal technical research to the chemicals leaked and waste water, the enforcement for government decision, technical measures provides technical support and guarantee except actively developing.
Carbon Materials, as sorbing material, has very large application potential in the adsorption treatment of the leakage accident such as oils and toxic chemical, has the irreplaceable effect of other materials.But traditional Carbon Materials exist in chemical accident disposal process aperture easily block, adsorb leakage while also absorb water, and the shortcoming such as buoyant properties difference, is difficult to meet the demand that chemical accident is emergent.Therefore the controlled functional porous Carbon Materials of lightweight of design, synthetic aperture, surface functional group is very important.The porous carbon material of lightweight is used for chemical accident to meet an urgent need and cause the concern of people.
CN201110180023.1 relates to nicotine absorbent, quinoline adsorbent, BaP adsorbent, toluidines adsorbent and carcinogen absorbent.More specifically, the present invention relates to a kind of nicotine absorbent, it comprises and is more than 10m2/g according to the specific area of nitrogen BET method and is the porous carbon material of more than 0.2cm3/g according to the pore volume of BJH method.
The main component of residual active sludge is biosolids, the mixture be namely made up of xenogeneic subject groups such as bacterium class, Mycophyta, protozoans.In excess sludge, most of material is organic matter, the thick protein wherein approximately containing 60%-70%, the carbohydrate of about 25%, and inorganic ash content only accounts for about 5%.Owing to containing more carbon in residual active sludge, possesses the objective condition preparing active carbon.Although the Properties of Activated Carbon obtained by residual actived sludge is not high, practical application is also less, and because it is cheap, carbon content rate is high, material is easy to get, raw material is sufficient and green non-poisonous and day by day favored.Active carbon with residual active sludge obtained by raw material all has flourishing microcellular structure and larger specific area, and this active carbon all has good treatment effect to dyeing waste water, heavy metal-containing waste water.Therefore, the standby active carbon of residual actived sludge is a kind of high porosity materials, with the Carbon Materials that it is prepared for raw material, have quite high adsorption effect to chemicals, these features impel us to go the functional porous Carbon Materials of research residual active sludge base as a kind of sorbing material place to go Physicochemical accident.
Summary of the invention
Technical problem to be solved by this invention is the problem of higher, the contaminated environment of cost in prior art, provides a kind of new residual actived sludge for the method for chemical leakage accident adsorbent.The method, for the preparation of in chemical leakage accident adsorbent, has the advantage that cost is lower, free from environmental pollution.
For solving the problem, the technical solution used in the present invention is as follows: a kind of residual actived sludge is for the method for chemical leakage accident adsorbent, by the moisture content pulverized lower than 60% residual active sludge mix with alkali lye after seal dipping, then electrocaloric effect heated at constant temperature is placed in, after taking out, washing is to pH=6-8, then drying is carried out, dried residual active sludge is ground, residual active sludge after grinding mixes with phosphoric acid solution, mixed solution is positioned over air pre-oxidation in 120 ~ 240 DEG C of drying boxes, residual active sludge after pre-oxidation is warming up to 600 ~ 1000 DEG C with 2 ~ 10 DEG C/min in a nitrogen atmosphere, constant temperature carries out carbonization-activation in 2 ~ 6 hours, take out after cooling, chemical leakage accident adsorbent is obtained after washing.
In technique scheme, preferably, described 20 ~ 100 orders are ground to dried residual active sludge.
In technique scheme, preferably, described concentration of lye is 2 ~ 4, and the mass ratio of residual active sludge and alkali lye is 0.2:1 ~ 3:1.
In technique scheme, preferably, dipping is sealed 12 ~ 24 hours after being mixed with alkali lye by residual active sludge.
In technique scheme, preferably, heated at constant temperature 12 ~ 24 hours in electrocaloric effect.
In technique scheme, preferably, described air preoxidation time is 4 ~ 12 hours.
In technique scheme, preferably, described cooling is Temperature fall.
In technique scheme, preferably, the concentration of described phosphoric acid solution is 30 ~ 50%, and the residual active sludge after grinding and the mass ratio of phosphoric acid solution are 0.1:1 ~ 1:1.
The invention provides a kind of residual actived sludge that utilizes for the method for chemical leakage accident adsorbent, traditional Carbon Materials have aperture easily block, adsorb leakage while also absorb water, and the shortcoming such as buoyant properties difference, is difficult to meet the demand that chemical accident is emergent.And residual active sludge have cheap, carbon content rate is high, material is easy to get, raw material is sufficient, take residual active sludge as raw material, by directed regulation activity charcoal pore-size distribution and surface functional group, this difficulty can be solved, reach the object to leakage absorption, separation, harmless treatment, achieve good technique effect.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
The NaOH aqueous solution being 2mol/L by the 150g residual active sludge pulverized and 375mL concentration fully mixes, and sealing dipping 24h, be then placed in the electrocaloric effect heated at constant temperature 24h of 110 DEG C, after taking out, washing is to pH=7, drying for standby.Residual active sludge after dried alkali heat-treatment is ground to 40 orders, get the phosphoric acid solution that the residual active sludge after grinding and 8g and 30mL quality solubility are 38% fully to mix, abundant mixed material is placed in 200 DEG C of drying box air pre-oxidation 6h, Temperature fall.Material after pre-oxidation is warming up to 800 DEG C with 5 DEG C/min in a nitrogen atmosphere, and constant temperature 2h carries out carbonization-activation, takes out after Temperature fall.Wash to pH=7 through 100 DEG C of distilled water again, the acticarbon that the aperture that can make is flourishing, mesoporous is high.Be used for by acticarbon adsorbing the aniline in 200ml aniline solution, the concentration of aniline in aniline solution is 500mg/L, and adsorptive value is 175mg/g, and specific area is 524m 2/ g, mesoporous is 81.2%.
[embodiment 2]
The NaOH aqueous solution being 2mol/L by the 150g residual active sludge pulverized and 375mL concentration fully mixes, and sealing dipping 24h, be then placed in the electrocaloric effect heated at constant temperature 24h of 110 DEG C, after taking out, washing is to pH=7, drying for standby.Residual active sludge after dried alkali heat-treatment is ground to 40 orders, get the phosphoric acid solution that the residual active sludge after grinding and 8g and 30mL quality solubility are 25% fully to mix, abundant mixed material is placed in 160 DEG C of drying box air pre-oxidation 6h, Temperature fall.Material after pre-oxidation is warming up to 800 DEG C with 5 DEG C/min in a nitrogen atmosphere, and constant temperature 2h carries out carbonization-activation, takes out after Temperature fall.Wash to pH=7 through 100 DEG C of distilled water again, the active carbon that the aperture that can make is flourishing, mesoporous is high.Be used for by acticarbon adsorbing the aniline in 200ml aniline solution, the concentration of aniline in aniline solution is 500mg/L, and adsorptive value is 181mg/g, and specific area is 624m 2/ g, mesoporous is 70.2%.
[embodiment 3]
The NaOH aqueous solution being 2mol/L by the 150g residual active sludge pulverized and 375mL concentration fully mixes, and sealing dipping 24h, be then placed in the electrocaloric effect heated at constant temperature 24h of 110 DEG C, after taking out, washing is to pH=7, drying for standby.Residual active sludge after dried alkali heat-treatment is ground to 40 orders, get the phosphoric acid solution that the residual active sludge after grinding and 8g and 30mL quality solubility are 25% fully to mix, abundant mixed material is placed in 160 DEG C of drying box air pre-oxidation 6h, Temperature fall.Material after pre-oxidation is warming up to 900 DEG C with 5 DEG C/min in a nitrogen atmosphere, and constant temperature 2h carries out carbonization-activation, takes out after Temperature fall.Wash to pH=7 through 100 DEG C of distilled water again, the active carbon that the aperture that can make is flourishing, mesoporous is high.Be used for by acticarbon adsorbing the aniline in 200ml aniline solution, the concentration of aniline in aniline solution is 500mg/L, and adsorptive value is 168mg/g, and specific area is 564m 2/ g, mesoporous is 68.2%.
[embodiment 4]
The NaOH aqueous solution being 4mol/L by the 150g residual active sludge pulverized and 375mL concentration fully mixes, and sealing dipping 12h, be then placed in the electrocaloric effect heated at constant temperature 12h of 110 DEG C, after taking out, washing is to pH=6, drying for standby.Residual active sludge after dried alkali heat-treatment is ground to 100 orders, get the phosphoric acid solution that the residual active sludge after grinding and 30g and 30mL quality solubility are 50% fully to mix, abundant mixed material is placed in 240 DEG C of drying box air pre-oxidation 4h, Temperature fall.Material after pre-oxidation is warming up to 1000 DEG C with 10 DEG C/min in a nitrogen atmosphere, and constant temperature 4h carries out carbonization-activation, takes out after Temperature fall.Wash to pH=7 through 100 DEG C of distilled water again, the acticarbon that the aperture that can make is flourishing, mesoporous is high.Be used for by acticarbon adsorbing the aniline in 200ml aniline solution, the concentration of aniline in aniline solution is 500mg/L, and adsorptive value is mg/g, and specific area is m 2/ g, mesoporous is 83.2%.
[comparative example]
Adopt the aniline in 0.2g acticarbon of the prior art absorption 200ml aniline solution, the concentration of aniline in aniline solution is 500mg/L, and active carbon physical property is: particle diameter 200 order, and adsorptive value is 191mg/g, and specific area is 962m 2/ g, mesoporous is 90.6%.

Claims (8)

1. a residual actived sludge is for the method for chemical leakage accident adsorbent, by the moisture content pulverized lower than 60% residual active sludge mix with alkali lye after seal dipping, then electrocaloric effect heated at constant temperature is placed in, after taking out, washing is to pH=6-8, then drying is carried out, dried residual active sludge is ground, residual active sludge after grinding mixes with phosphoric acid solution, mixed solution is positioned over air pre-oxidation in 120 ~ 240 DEG C of drying boxes, residual active sludge after pre-oxidation is warming up to 600 ~ 1000 DEG C with 2 ~ 10 DEG C/min in a nitrogen atmosphere, constant temperature carries out carbonization-activation in 2 ~ 6 hours, take out after cooling, chemical leakage accident adsorbent is obtained after washing.
2. residual actived sludge, for the method for chemical leakage accident adsorbent, is characterized in that describedly being ground to 20 ~ 100 orders to dried residual active sludge according to claim 1.
3. residual actived sludge, for the method for chemical leakage accident adsorbent, is characterized in that described concentration of lye is 2 ~ 4 according to claim 1, and the mass ratio of residual active sludge and alkali lye is 0.2:1 ~ 3:1.
4. residual actived sludge, for the method for chemical leakage accident adsorbent, seals dipping 12 ~ 24 hours after it is characterized in that residual active sludge to mix with alkali lye according to claim 1.
5. residual actived sludge, for the method for chemical leakage accident adsorbent, to is characterized in that in electrocaloric effect heated at constant temperature 12 ~ 24 hours according to claim 1.
6. residual actived sludge, for the method for chemical leakage accident adsorbent, is characterized in that described air preoxidation time is 4 ~ 12 hours according to claim 1.
7. residual actived sludge, for the method for chemical leakage accident adsorbent, is characterized in that described cooling is Temperature fall according to claim 1.
8. residual actived sludge is for the method for chemical leakage accident adsorbent according to claim 1, and it is characterized in that the concentration of described phosphoric acid solution is 30 ~ 50%, the residual active sludge after grinding and the mass ratio of phosphoric acid solution are 0.1:1 ~ 1:1.
CN201510670123.0A 2015-10-13 2015-10-13 Method for preparing chemical leakage accident adsorbents from excess activated sludge Pending CN105170089A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106622105A (en) * 2016-11-22 2017-05-10 环境保护部南京环境科学研究所 Method for preparing phosphorus and heavy metal adsorbent from alkaline leaching excess sludge and application method of phosphorus and heavy metal adsorbent

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59109299A (en) * 1982-12-14 1984-06-23 Chisso Corp Treatment of excess sludge and material to be treated
CN102432007A (en) * 2011-09-23 2012-05-02 南京工业大学 Method for preparing activated carbon by physical activation of excess sludge
CN102626607A (en) * 2012-05-04 2012-08-08 江苏省交通规划设计院股份有限公司 Preparation method and application of residual activated sludge adsorbent
CN103288080A (en) * 2013-06-14 2013-09-11 中国石油大学(华东) Method for preparing high-mesopore-ratio high-adsorptivity ecological carbon

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59109299A (en) * 1982-12-14 1984-06-23 Chisso Corp Treatment of excess sludge and material to be treated
CN102432007A (en) * 2011-09-23 2012-05-02 南京工业大学 Method for preparing activated carbon by physical activation of excess sludge
CN102626607A (en) * 2012-05-04 2012-08-08 江苏省交通规划设计院股份有限公司 Preparation method and application of residual activated sludge adsorbent
CN103288080A (en) * 2013-06-14 2013-09-11 中国石油大学(华东) Method for preparing high-mesopore-ratio high-adsorptivity ecological carbon

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106622105A (en) * 2016-11-22 2017-05-10 环境保护部南京环境科学研究所 Method for preparing phosphorus and heavy metal adsorbent from alkaline leaching excess sludge and application method of phosphorus and heavy metal adsorbent

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Application publication date: 20151223