CN112371095A - Porous adsorption material and preparation method and application thereof - Google Patents

Porous adsorption material and preparation method and application thereof Download PDF

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Publication number
CN112371095A
CN112371095A CN202011215530.XA CN202011215530A CN112371095A CN 112371095 A CN112371095 A CN 112371095A CN 202011215530 A CN202011215530 A CN 202011215530A CN 112371095 A CN112371095 A CN 112371095A
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cellulose
solution
hydrogel
parts
porous adsorption
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王雪娇
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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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • 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
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
    • B01J20/267—Cross-linked polymers
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047—Gels
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20—Organic adsorbents
    • B01D2253/202—Polymeric adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B01D2257/7027—Aromatic hydrocarbons
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/32—Hydrocarbons, e.g. oil
    • C02F2101/322—Volatile compounds, e.g. benzene

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a porous adsorption material and a preparation method and application thereof, belonging to the field of environmental protection and comprising the following raw materials in parts by weight: 10-20 parts of cellulose, 30-60 parts of activated carbon and a pretreatment solution. The preparation method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 3-12%; adding diglycidyl ether into the cellulose solution, and reacting at the reaction temperature of 0-70 ℃ for 0.1-10h to obtain a cellulose cross-linked product; regenerating the cellulose crosslinking product in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel; the cellulose hydrogel is washed and purified by deionized water, is adjusted into hydrogel with the mass concentration of 0.5-3.5%, and is dried to obtain the porous adsorption material, and the material has the advantages of excellent performance, convenient use, no toxicity, no pollution, safety, environmental protection and environmental protection, so that the material can be widely applied.

Description

Porous adsorption material and preparation method and application thereof
Technical Field
The invention relates to the field of environmental protection, and particularly relates to a porous adsorption material and a preparation method and application thereof.
Background
Cellulose is one of the most abundant biomass resources in the world, has good physical and chemical properties, can be degraded after being discarded, and is valued for producing novel materials by replacing traditional petrochemical products with cellulose. However, cellulose has crystalline regions, which makes cellulose difficult to dissolve in general organic solvents, and thus, potential application studies are hindered. The cellulose is dissolved in a specific solvent, so that the original aggregation form of cellulose molecules can be changed, the accessibility of cellulose reaction is improved, the cellulose is easy to be chemically modified, and the novel cellulose material is prepared.
Common solvents for cellulose include cuprammonium solutions, N-methylmorpholine-N-oxide, lithium chloride/dimethylacetamide systems, ionic liquids, etc., which have their own advantages and disadvantages. The sodium hydroxide/urea/water solvent system is a new method (patent CN101037479B) developed in recent years for dissolving cellulose in a greener way, in which sodium hydroxide reacts with cellulose to form alkali cellulose, so as to further dissolve in the sodium hydroxide/urea/water solvent system. Adopting a sodium hydroxide/urea/water solvent system, and a patent CN102875836B discloses a preparation method of cellulose foam, the method comprises the steps of dissolving cellulose in the sodium hydroxide/urea/water solvent system, placing the prepared cellulose solution in a mould, and carrying out regeneration and freeze-drying treatment to obtain a series of cellulose foam materials with the density of 0.129-0.387 g/cm3 and the average pore diameter of 78-3600 nm; patent CN102504327B discloses a method for preparing cellulose sponge by using sisal hemp waste hemp bran and hemp head waste as raw materials, which comprises dissolving cellulose raw materials in a sodium hydroxide/urea/water solvent system, and regenerating in a mixed bath of sulfuric acid and sodium sulfate by using sodium sulfate as a pore-forming agent to prepare cellulose sponge. The cellulose foam material is a cellulose porous material formed by secondarily stacking cellulose molecules by destroying an inclusion compound formed by cellulose, sodium hydroxide and urea, and intermolecular hydrogen bonds and intermolecular forces, so that the cellulose foam material has the defects of poor stability, hardness and the like, and auxiliary agents such as pore-forming agents and the like are also needed in the preparation process.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provides a porous adsorption material and a preparation method and application thereof.
The technical solution of the invention is as follows:
a porous adsorption material comprises the following raw materials in parts by weight: 10-20 parts of cellulose, 30-60 parts of activated carbon and a pretreatment solution, wherein the pretreatment solution comprises an alkali solution.
The invention also discloses a preparation method of the porous adsorption material, which comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 3-12%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting at the reaction temperature of 0-70 ℃ for 0.1-10h to obtain a cellulose cross-linked product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 0.5-3.5%, and drying to obtain the porous adsorption material.
Preferably, the pre-treatment solution is an alkaline solution, in particular a sodium hydroxide solution.
The invention also discloses application of the porous adsorption material in wastewater and waste gas, wherein the benzene adsorption amount is 611-799 mg/g.
The invention has at least one of the following beneficial effects: the porous adsorption material has good adsorption performance, large specific surface area and high adsorption performance; the obtained porous cellulose adsorbing material has the advantages of excellent performance, convenient use, no toxicity, no pollution, safety, environmental protection and environmental protection, thereby being widely applied.
Detailed Description
This section will describe in detail specific embodiments of the invention. A
Example 1
A porous adsorption material comprises the following raw materials in parts by weight: 10 parts of cellulose, 30 parts of activated carbon and 10 parts of pretreatment solution.
A preparation method of a porous adsorption material comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 4%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting for 10 hours at the reaction temperature of 50 ℃ to obtain a cellulose crosslinking product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and (4) washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 3.5%, and drying to obtain the porous adsorption material.
The pretreatment solution is an alkaline solution, in particular a sodium hydroxide solution.
The specific surface area of the material is 471m2The benzene adsorption capacity is 682 mg/g.
Example 2
A porous adsorption material comprises the following raw materials in parts by weight: 15 parts of cellulose, 35 parts of activated carbon and 8 parts of pretreatment solution.
The invention also discloses a preparation method of the porous adsorption material, which comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 8%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting for 3 hours at the reaction temperature of 60 ℃ to obtain a cellulose cross-linked product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 3%, and drying to obtain the porous adsorption material.
The pretreatment solution is an alkaline solution, in particular a sodium hydroxide solution.
The specific surface area of the material is 456m2G, benzene adsorption capacity 632 mg/g.
Example 3
A porous adsorption material comprises the following raw materials in parts by weight: 20 parts of cellulose, 60 parts of activated carbon and 7 parts of pretreatment solution.
The invention also discloses a preparation method of the porous adsorption material, which comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 12%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting for 10 hours at the reaction temperature of 70 ℃ to obtain a cellulose crosslinking product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and (4) washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 3.5%, and drying to obtain the porous adsorption material.
The specific surface area of the material is 451m2The benzene adsorption capacity is 612 mg/g.
Example 4
A porous adsorption material comprises the following raw materials in parts by weight: 17 parts of cellulose, 58 parts of activated carbon and 8 parts of pretreatment solution.
The invention also discloses a preparation method of the porous adsorption material, which comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 13%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting for 12 hours at the reaction temperature of 75 ℃ to obtain a cellulose crosslinking product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and (4) washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 3.5%, and drying to obtain the porous adsorption material.
Specific surface area of the materialProduct of 461m2The benzene adsorption capacity is 614 mg/g.
Example 5
A porous adsorption material comprises the following raw materials in parts by weight: 15 parts of cellulose, 55 parts of activated carbon and 3 parts of pretreatment solution.
The invention also discloses a preparation method of the porous adsorption material, which comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 10%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting for 8 hours at the reaction temperature of 65 ℃ to obtain a cellulose cross-linked product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and (4) washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 3.5%, and drying to obtain the porous adsorption material.
The specific surface area of the material is 483m2The benzene adsorption amount is 602 mg/g.
The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.
In the description of the embodiments of the present invention, it should be understood that "-" and "-" indicate the same range of two numerical values, and the range includes the endpoints. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by basically the same means are all within the protection scope of the present invention.

Claims (4)

1. A porous adsorbent material, characterized by: comprises the following raw materials in parts by weight: 10-20 parts of cellulose, 30-60 parts of activated carbon and a pretreatment solution, wherein the pretreatment solution comprises an alkali solution.
2. A preparation method of a porous adsorption material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: dissolving a cellulose raw material in a pretreatment solution to prepare a cellulose solution with the mass percentage concentration of 3-12%;
step two: adding diglycidyl ether into the cellulose solution obtained in the step one, and reacting at the reaction temperature of 0-70 ℃ for 0.1-10h to obtain a cellulose cross-linked product;
step three: regenerating the cellulose cross-linking product obtained in the step two in a dilute acid solution, adding activated carbon, and uniformly stirring to obtain cellulose hydrogel;
step four: and washing and purifying the cellulose hydrogel obtained in the step three by using deionized water, adjusting the cellulose hydrogel into hydrogel with the mass concentration of 0.5-3.5%, and drying to obtain the porous adsorption material.
3. The method for preparing a porous adsorbent material according to claim 2, wherein: the pretreatment solution is an alkaline solution, in particular a sodium hydroxide solution.
4. The application of the porous adsorption material in waste water and waste gas is characterized in that the benzene adsorption amount is 611-799 mg/g.
CN202011215530.XA 2020-11-04 2020-11-04 Porous adsorption material and preparation method and application thereof Withdrawn CN112371095A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115490392A (en) * 2022-08-19 2022-12-20 净化控股集团股份有限公司 Zero carbon source is thrown and is thrown municipal sewage and carry mark system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115490392A (en) * 2022-08-19 2022-12-20 净化控股集团股份有限公司 Zero carbon source is thrown and is thrown municipal sewage and carry mark system
CN115490392B (en) * 2022-08-19 2024-01-02 净化控股集团股份有限公司 Zero carbon source adds municipal sewage and carries mark system

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