CN110562975A - Activated carbon-molecular sieve prepared from cow dung and coal fly ash, preparation method and application thereof - Google Patents
Activated carbon-molecular sieve prepared from cow dung and coal fly ash, preparation method and application thereof Download PDFInfo
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- CN110562975A CN110562975A CN201910949659.4A CN201910949659A CN110562975A CN 110562975 A CN110562975 A CN 110562975A CN 201910949659 A CN201910949659 A CN 201910949659A CN 110562975 A CN110562975 A CN 110562975A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
Abstract
the invention discloses an activated carbon-molecular sieve prepared from cow dung and coal fly ash, a preparation method and application thereof, wherein the activated carbon-molecular sieve prepared from cow dung and coal fly ash comprises two components of activated carbon and molecular sieve, is microporous powder, has a particle size of 100-180 mu m and a specific surface area of 400-600 m2(ii) in terms of/g. The activated carbon prepared from the cow dung and the coal fly ash is divided intothe sub-sieve can be used for adsorbing heavy metal ions in wastewater. The invention takes the cow dung and the coal fly ash as the raw materials for preparing the carbon-molecular sieve, realizes the high-value resource utilization of the cow dung and the coal fly ash, and has the specific surface area of 600m2more than g, 2.6-5.0 times of that of the active carbon-molecular sieve prepared by directly adopting coal fly ash. The composite adsorbent is used for adsorbing heavy metal ions in wastewater, and the adsorption capacity can reach more than 4.5mmol/g, which is 2.2-3.2 times of that of the activated carbon-molecular sieve prepared without adding cow dung.
Description
Technical Field
the invention relates to a method for comprehensively utilizing cow dung wastes and coal fly ash.
background
Coal fly ash is low-value waste generated in the coal industrial utilization process, particularly the coal gasification process, and each coal chemical industry enterprise generates a large amount of low-value coal fly ash which cannot be utilized every year, and the coal fly ash is often buried, so that serious resource waste and environmental pollution are caused. Therefore, how to utilize the coal fly ash has important significance for solving the problems of resource utilization of solid wastes of coal chemical enterprises, reduction of treatment cost and environmental pollution. The method for directly preparing the molecular sieve-activated carbon composite material from the coal fly ash is an effective means, the process does not need to separate silicon from aluminum and residual carbon, and can fully utilize the advantages of the silicon and the residual carbon, namely the high specific surface area of the activated carbon and the strong ion exchange capacity and the acidity and alkalinity of the molecular sieve. However, due to the lower carbon content and extremely low volatile content of coal fly ash, the specific surface area of the composite materials tends to be low, limiting their further utilization and development. Generally, the process of preparing the activated carbon-molecular sieve composite material from the coal fly ash comprises the steps of mixing the coal fly ash with NaOH, carrying out high-temperature melting to activate carbon and melt silicon and aluminum in ash, crushing the mixture, adding a silicon source or an aluminum source to regulate the silicon-aluminum ratio, then aging in distilled water, carrying out hydrothermal treatment on the aged mixture, filtering and washing to be neutral to obtain the activated carbon-molecular sieve composite material, wherein the prepared composite material usually has a lower specific surface area due to lower residual carbon content and volatile components of the coal fly ash, and the utilization value of the composite material is reduced.
cow dung is biomass waste generated in the breeding process, and resource utilization of cow dung is also a difficult problem in a cow and sheep breeding area. However, the fly ash contains relatively high volatile components, carbon content and alkali metal and alkaline earth metal content, so that the carbon content in the fly ash can be supplemented and regulated, the silica-alumina ratio in the fly ash can be changed, and the use amount of alkali in the preparation of the molecular sieve-activated carbon material can be reduced due to the high alkali metal content.
Therefore, whether the two materials can be used as raw materials for preparing the carbon-molecular sieve composite material or not has very important social and economic significance.
Disclosure of Invention
the invention aims to disclose an activated carbon-molecular sieve prepared from cow dung and coal fly ash, a preparation method and application thereof, so as to meet the requirements of people.
the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash comprises two components of activated carbon and molecular sieve, is microporous powder, has the particle size of 100-180 mu m and the specific surface area of 400-600 m2/g；
The activated carbon-molecular sieve prepared from the cow dung and the coal fly ash comprises the following components in percentage by weight:
and unavoidable impurities, e.g. K2O and TiO2etc.;
The coal fly ash refers to gasification fly ash, is derived from the coal chemical industry gasification process, and comprises the following components:
Said other impurities being e.g. K2O and TiO2etc.;
the preparation method of the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash comprises the following steps:
(1) Mixing coal fly ash, cow dung and NaOH, and activating for 1-4 hours at 700-900 ℃ in an inert atmosphere;
The mass ratio of the total mass of the coal fly ash and the cow dung to the NaOH is as follows: 1: 1-1: 3;
Coal fly ash, dry cow dung and NaOH are 1: 1-1: 3;
the term "dry-based cow dung" refers to cow dung containing no moisture
(2) and (2) mixing the product obtained in the step (1) with water, carrying out hydrothermal treatment at 80-120 ℃ for 8-24 hours, and then collecting the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash from the system.
the activated carbon-molecular sieve can be used for adsorbing heavy metal ions in wastewater, and the metal ions comprise Ni2+、Cu2+、Pb2+or Cd2+Etc.; the methods of application are conventional, as reported in the literature (Journal of Hazardous Materials 160(2008) 148-153).
The invention has the beneficial effects that:
cow dung and coal fly ash are jointly used as raw materials for preparing the carbon-molecular sieve composite material, and the structural property and the adsorption catalysis performance of the activated carbon-molecular sieve are regulated and controlled by adjusting the proportion of the cow dung and the coal fly ash so as to realize high-value resource utilization of the cow dung and the coal fly ash. The activated carbon-molecular sieve obtained by the method has the specific surface area of 600m2More than g, 2.6-5.0 times of that of the active carbon-molecular sieve composite material prepared by directly adopting coal fly ash. The activated carbon-molecular sieve composite material can be used for adsorbing heavy metal ions in wastewater, the adsorption capacity can reach more than 4.5mmol/g, and the adsorption capacity is 2.2-3.2 times that of an activated carbon-molecular sieve prepared before cow dung is added.
Detailed Description
Comparative example 1
the formula is as follows: (weight)
100% of coal fly ash;
The coal fly ash is produced by selecting Texaco gasification fly ash, and comprises the following components:
5.3 percent of other impurities; s, O13.0.0% in the residual carbon, which refers to the incomplete coal powder carried in the coal fly ash;
the preparation method comprises the following steps:
(1) Mixing coal fly ash and NaOH according to a weight ratio of 1:1, and then activating for 2 hours at 750 ℃ under nitrogen;
(2) Mixing the product obtained in the step (1) with water, wherein the mass ratio of the product obtained in the step (1) to the water is as follows:
performing hydrothermal treatment on the product obtained in the step (1) and water at the temperature of 100 ℃ for 16 hours, and then performing washing, suction filtration, drying, crushing and screening to obtain the activated carbon-molecular sieve which is prepared by taking coal fly ash as a raw material, wherein the activated carbon-molecular sieve is microporous powder and has the particle size of 100-180 mu m;
The XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
The specific surface area was 120m as measured by a method reported in the literature (International Journal of Hydrogen Energy 41(2016)10661-10669)2/g；
The following method was used for evaluation;
0.5g of the activated carbon-molecular sieve was put into 1L of Ni with a concentration of 400ppm2+Standing in water solution at 25 deg.C for 24 hr, taking out activated carbon-molecular sieve, and measuring Ni in the solution before and after adsorption by atomic absorption spectrophotometer2+the concentration can be as follows:
Ni2+the adsorption amount was 1.4 mmol/g.
Example 1
The formula is as follows: (weight)
80% of coal fly ash and 20% of dry-base cow dung, wherein the coal fly ash is Texaco gasification fly ash. The coal fly ash composition was the same as comparative example 1;
The preparation method comprises the following steps:
(1) mixing coal fly ash, cow dung and NaOH, and then activating for 2 hours at 750 ℃ under nitrogen;
The mass ratio of the total mass of the coal fly ash and the cow dung to the NaOH is as follows:
Coal fly ash, dry cow dung and NaOH are 1: 1;
(2) Mixing the product of the step (1) with water, carrying out hydrothermal treatment at 100 ℃ for 16 hours, and then collecting the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash from the system.
Then washing, filtering, drying, crushing and screening to obtain an activated carbon-molecular sieve which takes coal fly ash as a raw material and is microporous powder with the particle size of 100-180 mu m;
The XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
The specific surface area was 310m as measured by a method reported in the literature (International Journal of Hydrogen Energy 41(2016)10661-10669)2/g；
The following method was used for evaluation;
0.5g of the activated carbon-molecular sieve was put into 1L of Ni with a concentration of 400ppm2+standing in water solution at 25 deg.C for 24 hr, taking out activated carbon-molecular sieve, and measuring Ni in the solution before and after adsorption by atomic absorption spectrophotometer2+the concentration can be as follows:
Ni2+the adsorption amount was 3.1 mmol/g.
example 2
60% of coal fly ash and 40% of dry-base cow dung, wherein the coal fly ash is GSP gasification fly ash and comprises the following components: (weight)
4.3 of other impurities; and S, O2.7.7% in carbon residue;
The preparation method comprises the following steps:
(1) Mixing coal fly ash, cow dung and NaOH, and then activating for 2 hours at 800 ℃ under nitrogen;
The mass ratio of the total mass of the coal fly ash and the cow dung to the NaOH is as follows:
coal fly ash, dry cow dung and NaOH are 1: 1;
(2) mixing the product obtained in the step (1) with water, carrying out hydrothermal treatment at 80 ℃ for 8 hours, and collecting the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash from the system.
Then washing, filtering, drying, crushing and screening to obtain an activated carbon-molecular sieve which takes coal fly ash as a raw material and is microporous powder with the particle size of 100-180 mu m;
the XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
the specific surface area was 410m as measured by a method reported in the literature (International Journal of Hydrogen Energy 41(2016)10661-10669)2/g；
The following method was used for evaluation;
0.5g of the composite was placed in 1L of Ni with a concentration of 400ppm2+Standing in water solution at 25 deg.C for 24 hr, taking out activated carbon-molecular sieve, and measuring Ni in the solution before and after adsorption by atomic absorption spectrophotometer2+The concentration can be as follows:
Ni2+the adsorption amount was 3.5 mmol/g.
Example 3
40% of coal fly ash and 60% of dry-based cow dung, wherein the coal fly ash is Texaco gasification fly ash and has the same components as in example 1.
the preparation method is the same as that of the example 2:
The XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
Specific surface area of 600m2/g；Ni2+The adsorption amount was 4.5 mmol/g.
example 4
The formula is as follows: (weight)
40% of coal fly ash, 60% of dry cow dung and the same coal fly ash as in example 1;
The preparation method comprises the following steps:
(1) mixing coal fly ash, cow dung and NaOH, and then activating for 4 hours at 850 ℃ under nitrogen;
the mass ratio of the total mass of the coal fly ash and the cow dung to the NaOH is as follows:
Coal fly ash and dry cow dung are mixed with NaOH in the ratio of 1 to 2;
(2) Mixing the product of the step (1) with water, carrying out hydrothermal treatment at 120 ℃ for 24 hours, and then collecting the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash from the system.
Then, washing, filtering, drying, crushing and screening to obtain activated carbon-molecular sieve which is microporous powder with the particle size of 100-180 mu m by taking coal fly ash as a raw material;
The XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
The specific surface area is 525m2/g，Cu2+the adsorption capacity was 4.1 mmol/g.
example 5
The formula is as follows: (weight)
20% of coal fly ash and 80% of dry-base cow dung;
The other example is the same as example 4, and the powder is a microporous powder with the particle size of 100-180 μm;
The XRF method is adopted for analysis and detection, and the percentage of each component in the product is as follows:
specific surface area of 505m2/g，Ni2+the adsorption capacity can reach 3.7 mmol/g.
as can be seen from comparative example 1 and examples 1-5, the silica-alumina ratio, the structure, the specific surface area and the adsorption capacity of the prepared activated carbon-molecular sieve can be regulated and controlled by regulating the mixing ratio of the cow dung and the coal fly ash. Specific surface area and Ni adsorption of activated carbon-molecular sieve prepared by taking cow dung and coal fly ash as raw materials2+The capability is obviously increased and is 2.6-5.0 times and 2.2-3.2 times of that of the activated carbon-molecular sieve prepared by independently using the coal fly ash.
Claims (10)
1. the activated carbon-molecular sieve prepared from cow dung and coal fly ash is characterized by comprising two components of activated carbon and molecular sieve, wherein the two components are microporous powder, the particle size is 100-180 mu m, and the specific surface area is 400-600 m2/g。
2. the activated carbon-molecular sieve prepared from cow dung and coal fly ash according to claim 1, which is characterized by comprising the following components in percentage by weight:
and inevitable impurities.
3. The activated carbon-molecular sieve produced from cow dung and coal fly ash according to claim 1 or 2, wherein the coal fly ash is gasified fly ash.
4. The activated carbon-molecular sieve prepared from cow dung and coal fly ash according to claim 3, wherein the coal fly ash comprises the following components:
5. The preparation method of the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash is characterized by comprising the following steps of:
(1) mixing coal fly ash, cow dung and NaOH, and activating in inert atmosphere;
(2) And (2) mixing the product obtained in the step (1) with water for hydrothermal treatment, and then collecting the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash from the system.
6. The method according to claim 5, wherein the step (1) is carried out by activating at 700 to 900 ℃ for 1 to 4 hours in an inert atmosphere.
7. The method of claim 6, wherein the mass ratio of the total mass of coal fly ash and cow dung to NaOH is: 1: 1-1: 3; coal fly ash, dry cow dung and NaOH are 1: 1-1: 3.
8. the method according to claim 5, wherein in the step (2), the product of the step (1) is mixed with water and subjected to hydrothermal treatment at 80-120 ℃ for 8-24 hours.
9. The application of the activated carbon-molecular sieve prepared from the cow dung and the coal fly ash according to any one of claims 1 to 3, which is characterized by being used for adsorbing heavy metal ions in wastewater.
10. The use of claim 9, wherein the heavy metal ions comprise Ni2+、Cu2+、Pb2+Or Cd2+。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054212A (en) * | 2020-03-18 | 2020-04-24 | 山东中航天业科技有限公司 | Heat-storage molecular sieve-regulated catalytic reduction denitration device |
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| CN111054212A (en) * | 2020-03-18 | 2020-04-24 | 山东中航天业科技有限公司 | Heat-storage molecular sieve-regulated catalytic reduction denitration device |
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