CN112938968A - Method for producing activated carbon by using furfural residues - Google Patents

Method for producing activated carbon by using furfural residues Download PDF

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Publication number
CN112938968A
CN112938968A CN202110231707.3A CN202110231707A CN112938968A CN 112938968 A CN112938968 A CN 112938968A CN 202110231707 A CN202110231707 A CN 202110231707A CN 112938968 A CN112938968 A CN 112938968A
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CN
China
Prior art keywords
activated carbon
furfural
phosphoric acid
acid solution
furfural residue
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110231707.3A
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Chinese (zh)
Inventor
仇兆山
施以军
刘支佩
李小双
郭畅
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Anhui Jinxuan Technology Co ltd
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Anhui Jinxuan Technology Co ltd
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Priority to CN202110231707.3A priority Critical patent/CN112938968A/en
Publication of CN112938968A publication Critical patent/CN112938968A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • C01B32/324Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/336Preparation characterised by gaseous activating agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents

Abstract

The invention discloses a method for producing activated carbon by furfural residues, which comprises the following steps of S1: pretreatment: washing and filtering the furfural residues to obtain filter cakes, and drying the filter cakes to obtain the furfural residues; s2: soaking: adding weak alkali phosphate and phosphoric acid solution for soaking, and performing S3: carbonizing: then high temperature carbonization is carried out; s4: and (3) activation: continuously heating, introducing CO2Activating; s5: and drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The invention provides a method for producing active carbon by furfural residue, which comprises the steps of preparing weak alkali phosphate, phosphoric acid solution and CO2The combined activation method is used for preparing the activated carbon with high specific surface area, so that the environmental pollution can be avoided, and the waste can be recycled.

Description

Method for producing activated carbon by using furfural residues
Technical Field
The invention relates to the technical field of chemical production, in particular to a method for producing activated carbon by furfural residues.
Background
In the process of producing furfural by using corncobs as raw materials, the residual furfural residues after hydrolysis are sent to a biomass boiler for combustion and power generation, so that the utilization rate of the furfural residues is low, the main components of the furfural residues are pentosan, cellulose and lignin, the carbon content of the furfural residues is more than 40 percent, and the furfural residues are excellent raw materials for preparing activated carbon, so that the high-adsorbability powdery activated carbon is prepared by using the furfural residues, the pollution to the environment can be avoided, and the waste recycling can be realized.
The invention patent CN 109748277A provides a method for preparing high-adsorptivity activated carbon from furfural waste residues, which comprises the steps of soaking with phosphoric acid, performing high-temperature carbonization, and then performing activation, but does not propose substances required by activation.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for producing activated carbon by furfural residues, which comprises the steps of washing the furfural residues with water, screening, drying, adding the furfural residues into a phosphoric acid solution for soaking, then carrying out high-temperature carbonization, continuing to heat, and introducing CO2Activating, drying, grinding and sieving to obtain the high-adsorbability activated carbon.
A method for producing activated carbon by furfural residue comprises the following steps:
s1: pretreatment: washing and filtering the furfural residues to obtain filter cakes, and drying the filter cakes to obtain the furfural residues;
s2: soaking: adding into weak base phosphate and phosphoric acid solution, soaking,
s3: carbonizing: then high temperature carbonization is carried out;
s4: and (3) activation: continuously heating, introducing CO2Activating;
s5: and drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon.
Preferably, the furfural residue in S2 is mixed with weak alkali phosphate and phosphoric acid solution according to a solid-to-liquid ratio of 1: 0.8-1.2.
Preferably, the volume ratio of the weak base phosphate solution to the phosphoric acid solution in the weak base phosphate and the phosphoric acid solution is (0.5-1): 1-3), the mass concentration of the weak base phosphate solution is 30-50%, and the mass concentration of the phosphoric acid solution is 30-50%.
Preferably, the soaking time in the S2 is 1-2h, and the soaking temperature is 60-90 ℃.
Preferably, the carbonization temperature in the S3 is 430-470 ℃, and the carbonization time is 3.5-5 h.
Preferably, the CO flow rate of 600L/min to 1000L/min in the S4 is2Introducing the activated furfural residue into carbonized furfural residue for activation, wherein the temperature is controlled to be 440 ℃ and 460 ℃ in the activation process.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for producing active carbon by furfural residue, which comprises the steps of preparing weak alkali phosphate, phosphoric acid solution and CO2The combined activation method is used for preparing the activated carbon with high specific surface area, the physical method and the chemical method are combined, the carbonization tail gas of the physical method is used for supplying heat for the chemical method, no coal consumption is caused in the production process, the physical activated carbon and the chemical activated carbon are obtained at the same time, and the furfural waste residue is used for preparing the high-adsorbability powdery activated carbon, so that the environmental pollution can be avoided, and the waste recycling can be realized.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example 1
Washing and filtering the furfural residue to obtain a filter cake, and drying the filter cake to obtain the treated furfural residue; mixing the treated furfural residue with weak base phosphate and phosphoric acid solution according to the solid-to-liquid ratio of 1:0.8, heating to 90 ℃, and soaking for 1 h; the volume ratio of the weak alkali phosphate to the phosphoric acid solution in the weak alkali phosphate and phosphoric acid solution is 0.5:1, the mass concentration of the weak alkali phosphate solution is 30%, and the mass concentration of the phosphoric acid solution is 30%.
Carbonizing the soaked mixed solution at 430 ℃ for 3.5h to obtain carbonized furfural residue; mixing CO at a flow rate of 600L/min2Introducing the activated furfural residue into carbonized furfural residue, and activating, wherein the temperature is controlled at 450 ℃ in the activation process; drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The specific surface area is up to 2510m2/g。
Example 2
Washing and filtering the furfural residue to obtain a filter cake, and drying the filter cake to obtain the treated furfural residue; mixing the treated furfural residue with weak base phosphate and phosphoric acid solution according to the solid-to-liquid ratio of 1:0.9, heating to 60 ℃, and soaking for 2 hours; the volume ratio of the weak base phosphate to the phosphoric acid solution in the weak base phosphate and the phosphoric acid solution is 1:3, the mass concentration of the weak base phosphate solution is 50%, and the mass concentration of the phosphoric acid solution is 50%.
Carbonizing the soaked mixed solution at 470 ℃ for 5.5h to obtain carbonized furfural residue; CO at a flow rate of 700L/min2Introducing the activated furfural residue into carbonized furfural residue, and activating, wherein the temperature is controlled to 440 ℃ in the activation process; drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The specific surface area is up to 2750m2/g。
Example 3
Washing and filtering the furfural residue to obtain a filter cake, and drying the filter cake to obtain the treated furfural residue; mixing the treated furfural residue with weak base phosphate and phosphoric acid solution according to the solid-to-liquid ratio of 1:1.0, heating to 70 ℃, and soaking for 1.5 h; the volume ratio of the weak alkali phosphate to the phosphoric acid solution in the weak alkali phosphate and phosphoric acid solution is 0.5:2, the mass concentration of the weak alkali phosphate solution is 35%, and the mass concentration of the phosphoric acid solution is 45%.
Carbonizing the soaked mixed solution at 450 ℃ for 4h to obtain carbonized furfural residue; mixing CO at a flow rate of 800L/min2Introducing the activated furfural residue into carbonized furfural residue, and activating, wherein the temperature in the activating process is controlled to be 460 ℃; drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The specific surface area is measured to reach 2940m2/g。
Example 4
Washing and filtering the furfural residue to obtain a filter cake, and drying the filter cake to obtain the treated furfural residue; mixing the treated furfural residue with weak base phosphate and phosphoric acid solution according to the solid-to-liquid ratio of 1:1.1, heating to 80 ℃, and soaking for 1.5 h; the volume ratio of the weak base phosphate to the phosphoric acid solution in the weak base phosphate and the phosphoric acid solution is 0.8:2.5, the mass concentration of the weak base phosphate solution is 45%, and the mass concentration of the phosphoric acid solution is 35%.
Carbonizing the soaked mixed solution at 440 ℃ for 4.5h to obtain carbonized furfural residue; will 900L/min flow rate of CO2Introducing into carbonized furfural residue, activating, and controlling the temperature at 445 deg.C during activation; drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The specific surface area is up to 3010m2/g。
Example 5
Washing and filtering the furfural residue to obtain a filter cake, and drying the filter cake to obtain the treated furfural residue; mixing the treated furfural residue with weak base phosphate and phosphoric acid solution according to the solid-to-liquid ratio of 1:1.1, heating to 75 ℃, and soaking for 1.5 h; the volume ratio of the weak alkali phosphate to the phosphoric acid solution in the weak alkali phosphate and phosphoric acid solution is 0.5:3, the mass concentration of the weak alkali phosphate solution is 40%, and the mass concentration of the phosphoric acid solution is 40%.
Carbonizing the soaked mixed solution at 460 ℃ for 5.5h to obtain carbonized furfural residue; CO at a flow rate of 1000L/min2Introducing the activated furfural residue into carbonized furfural residue, and activating, wherein the temperature is controlled at 455 ℃ in the activation process; drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon. The specific surface area is measured to reach 2980m2/g。
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (6)

1. A method for producing activated carbon by using furfural residues is characterized by comprising the following steps:
s1: pretreatment: washing and filtering the furfural residues to obtain filter cakes, and drying the filter cakes to obtain the furfural residues;
s2: soaking: adding into weak base phosphate and phosphoric acid solution, soaking,
s3: carbonizing: then high temperature carbonization is carried out;
s4: and (3) activation: continuously heating, introducing CO2Activating;
s5: and drying, grinding and sieving the activated carbon to obtain the high-adsorbability activated carbon.
2. The method for producing activated carbon from furfural residue as claimed in claim 1, wherein the furfural residue in S2 is mixed with weak alkali phosphate and phosphoric acid solution according to a solid-to-liquid ratio of 1: 0.8-1.2.
3. The method for producing activated carbon from furfural residue as claimed in claim 2, wherein the volume ratio of the weak alkali phosphate solution to the phosphoric acid solution in the weak alkali phosphate and phosphoric acid solution is (0.5-1): 1-3), the mass concentration of the weak alkali phosphate solution is 30-50%, and the mass concentration of the phosphoric acid solution is 30-50%.
4. The method for producing activated carbon from furfural residue as claimed in claim 1, wherein the soaking time in S2 is 1-2h and the soaking temperature is 60-90 ℃.
5. The method for producing activated carbon from furfural residue as claimed in claim 1, wherein the carbonization temperature in S3 is 430-470 ℃ and the carbonization time is 3.5-5 h.
6. The method for producing activated carbon from furfural residue as claimed in claim 1, wherein CO at a flow rate of 600L/min to 1000L/min is added in S42Introducing the activated furfural residue into carbonized furfural residue for activation, wherein the temperature is controlled to be 440 ℃ and 460 ℃ in the activation process.
CN202110231707.3A 2021-03-02 2021-03-02 Method for producing activated carbon by using furfural residues Pending CN112938968A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115124024A (en) * 2022-08-04 2022-09-30 安徽固瑞特新材料科技有限公司 Porous carbon material, composite rubber filler, preparation method of composite rubber filler and rubber material

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Publication number Priority date Publication date Assignee Title
CN101391767A (en) * 2008-11-03 2009-03-25 浙江大学城市学院 Method for preparing active carbon by using waste walnut outer peel
CN101885486A (en) * 2010-07-05 2010-11-17 南京林业大学 Technology for producing acid granular activated carbon by air activation method
US20140208945A1 (en) * 2013-01-25 2014-07-31 Cabot Corporation Phosphoric acid treatment of carbonaceous material prior to activation
CN106379897A (en) * 2016-08-27 2017-02-08 荥经县极星生物科技有限公司 Method for preparing bamboo-based activated carbon based on phosphoric acid method and physical and chemical combination method
CN109534342A (en) * 2019-01-18 2019-03-29 中国石油大学(华东) The preparation method of biomass super-activated carbon

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101391767A (en) * 2008-11-03 2009-03-25 浙江大学城市学院 Method for preparing active carbon by using waste walnut outer peel
CN101885486A (en) * 2010-07-05 2010-11-17 南京林业大学 Technology for producing acid granular activated carbon by air activation method
US20140208945A1 (en) * 2013-01-25 2014-07-31 Cabot Corporation Phosphoric acid treatment of carbonaceous material prior to activation
CN106379897A (en) * 2016-08-27 2017-02-08 荥经县极星生物科技有限公司 Method for preparing bamboo-based activated carbon based on phosphoric acid method and physical and chemical combination method
CN109534342A (en) * 2019-01-18 2019-03-29 中国石油大学(华东) The preparation method of biomass super-activated carbon

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115124024A (en) * 2022-08-04 2022-09-30 安徽固瑞特新材料科技有限公司 Porous carbon material, composite rubber filler, preparation method of composite rubber filler and rubber material
CN115124024B (en) * 2022-08-04 2024-04-12 安徽固瑞特新材料科技有限公司 Porous carbon material, composite rubber filler, preparation method of porous carbon material and composite rubber filler, and rubber material

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Application publication date: 20210611