CN114425307B - Biomass aerogel material based on color response mechanism, preparation method and application - Google Patents
Biomass aerogel material based on color response mechanism, preparation method and application Download PDFInfo
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- CN114425307B CN114425307B CN202111405607.4A CN202111405607A CN114425307B CN 114425307 B CN114425307 B CN 114425307B CN 202111405607 A CN202111405607 A CN 202111405607A CN 114425307 B CN114425307 B CN 114425307B
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- carboxymethyl cellulose
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- nickel chloride
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 239000004964 aerogel Substances 0.000 title claims abstract description 54
- 239000002028 Biomass Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920001661 Chitosan Polymers 0.000 claims abstract description 80
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims abstract description 78
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 66
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 66
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 66
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 66
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000001179 sorption measurement Methods 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims description 73
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000000084 colloidal system Substances 0.000 claims description 32
- 229910021529 ammonia Inorganic materials 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 18
- 238000004108 freeze drying Methods 0.000 claims description 17
- 239000000017 hydrogel Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000003929 acidic solution Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 abstract description 16
- 239000003463 adsorbent Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract description 4
- 229920005615 natural polymer Polymers 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 4
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 206010001052 Acute respiratory distress syndrome Diseases 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010008479 Chest Pain Diseases 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010023644 Lacrimation increased Diseases 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 208000013616 Respiratory Distress Syndrome Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000006221 furniture coating Substances 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000004317 lacrimation Effects 0.000 description 1
- 241000238565 lobster Species 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 208000005333 pulmonary edema Diseases 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
-
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28014—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
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- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
Abstract
The invention discloses a biomass aerogel material based on a color response mechanism, a preparation method and application thereof. The biomass aerogel material comprises carboxymethyl cellulose, chitosan, lithium bromide and nickel chloride; the mass ratio of the carboxymethyl cellulose to the chitosan is 0.2-4:l; the mass ratio of the nickel chloride to the carboxymethyl cellulose is 0.1-4.8:1; the mass ratio of the lithium bromide to the chitosan is 0.1-3:1. According to the invention, two natural polymer biomass materials are used as matrixes, lithium bromide is used as a cross-linking agent, the composite biomass aerogel adsorbent is prepared through a non-toxic and environment-friendly process, the adsorption performance of the aerogel on ammonia gas is improved, and the adsorption condition can be judged through a color response mechanism, so that the ammonia gas adsorption process is visualized.
Description
Technical Field
The invention belongs to the technical field of preparation of visualized ammonia adsorbents, and particularly relates to a biomass aerogel material based on a color response mechanism, a preparation method and application thereof.
Background
Ammonia is a colorless, but toxic gas with a strong irritating odor. The minimum concentration of ammonia which can be sensed by a human body is 5.3ppm, when the concentration is high, a strong pungent odor exists, the skin tissue contacted with the ammonia can be corroded and stimulated, the human tissue can be greatly damaged, symptoms such as lacrimation, pharyngalgia, chest distress, headache, nausea and dyspnea can occur after a large amount of ammonia is inhaled for a short time, and pulmonary edema and respiratory distress syndrome can occur in severe cases.
With the gradual aggravation of ammonia pollution, the production and the living of people are seriously influenced, and the ammonia emission is required to be controlled. The ammonia pollution in indoor air mainly comes from indoor decoration materials, most of additives and whitening agents used in furniture coating contain ammonia water, and meanwhile, high-alkali concrete expansion agents and urea-containing concrete antifreezing agents in building materials slowly release ammonia, and the indoor ammonia content is regulated to be less than 0.2mg/m according to indoor air quality standards 3 (1 hour mean). Therefore, in order to solve the problem of serious ammonia pollution, we need to develop a material with a specific removal effect on ammonia, and judge the adsorption saturation degree of ammonia through color change, so as to be convenient for replacing the adsorbent in time.
The chitosan is natural polymer polysaccharide prepared from chitin in shells of shellfish such as crab and lobster by deacetylation, and has good biocompatibility, biodegradability and biocompatibility. As the molecular chain of the chitosan has rich hydroxyl groups, the chitosan has good adsorption performance on various pollutants, and is a common adsorbent material, so the chitosan has a wide interest in the treatment application of industrial three wastes. Among various types of chitosan-based adsorption materials (powder, gel particles, films, hydrogels and aerogel), aerogel has the highest specific surface area and lighter weight, and can effectively utilize adsorption sites of chitosan, so that a degradable biological adsorbent is prepared. However, chitosan aerogel has poor acid and alkali resistance, poor mechanical properties and low ammonia adsorption efficiency. Cellulose is used as a structural material with better performance and is rich in carboxyl groups, so that chitosan and cellulose are mutually connected to form the composite aerogel for efficiently removing ammonia gas.
Disclosure of Invention
The invention aims to: aiming at the problem of removing ammonia without color in the prior art in a visual way, the invention provides a biomass aerogel material based on a color response mechanism, a preparation method and application thereof. According to the metal-loaded polymer biomass composite adsorbent, natural biological macromolecules are used as base materials, and two polymer biomass materials are mixed and copolymerized to prepare the aerogel material with higher specific surface area and lower density. And the color can be intuitively seen to be changed from yellow to blue-green before and after ammonia adsorption.
The technical scheme is as follows: the biomass aerogel material based on the color response mechanism comprises carboxymethyl cellulose, chitosan, lithium bromide and nickel chloride; the mass ratio of the carboxymethyl cellulose to the chitosan is 0.2-4:l; the mass ratio of the nickel chloride hexahydrate to the carboxymethyl cellulose is 0.1-0.48:1; the mass ratio of the nickel chloride to the chitosan is 0.1-3:1.
As a preferred embodiment of the present invention, the biomass aerogel material is prepared by the following method: adding carboxymethyl cellulose and nickel chloride hexahydrate into distilled water according to a proportion, and stirring to obtain a colloidal solution I containing carboxymethyl cellulose; dissolving chitosan and lithium bromide in an acidic solution according to a proportion, and stirring to obtain a colloid solution II containing chitosan; and mixing the two solutions in proportion, and freeze-drying to obtain the biomass aerogel material.
As a preferred embodiment of the invention, the mass concentration of the carboxymethyl cellulose in the colloidal solution I is 1-20%; in the colloid solution II, the mass concentration of the chitosan is 1-10%.
As a preferred embodiment of the present invention, the carboxymethyl cellulose has a viscosity average molecular weight of 5 to 30 ten thousand; the viscosity average molecular weight of the chitosan is 5-30 ten thousand.
As a preferred embodiment of the present invention, the carboxymethyl cellulose has a viscosity average molecular weight of 15 to 30 ten thousand; the viscosity average molecular weight of the chitosan is 15-30 ten thousand.
As a preferred embodiment of the present invention, the carboxymethyl cellulose has a viscosity average molecular weight of 25 to 30 ten thousand; the viscosity average molecular weight of the chitosan is 25-30 ten thousand.
The preparation method of the biomass aerogel material based on the color response mechanism comprises the following steps:
(1) Preparation of colloidal solution I: adding carboxymethyl cellulose and nickel chloride hexahydrate into distilled water, stirring for dissolving, and adjusting the mass concentration of the carboxymethyl cellulose to 1-20%;
(2) Preparation of colloidal solution II: dissolving chitosan and lithium bromide in an acidic solution, stirring and dissolving, and adjusting the mass concentration of the chitosan to be 1-10%, wherein the mass ratio of the lithium bromide to the chitosan is 0.1-3:1;
(3) Adding the colloidal solution I into the colloidal solution II according to the mass ratio of the carboxymethyl cellulose to the chitosan of 0.2-4:l, continuously stirring until the mixed solution is completely and uniformly stirred to form hydrogel, and then freeze-drying.
As a preferred embodiment of the present invention, the method for preparing a biomass aerogel material comprises the following steps:
(1) Preparation of colloidal solution I: adding carboxymethyl cellulose and nickel chloride hexahydrate into distilled water according to a proportion, stirring for 1-6 hours at 500-1000rpm at room temperature, adjusting the concentration of the carboxymethyl cellulose to 1-20%, and fully dissolving the concentration of the nickel chloride hexahydrate to 0.1-48%, wherein the solution is in a green colloid shape;
(2) Preparation of colloidal solution II: dissolving chitosan and lithium bromide in an acid solution according to a proportion, and stirring for 10-48 hours at 300-1000rpm to obtain a chitosan colloid solution II containing 1-10%;
(3) Adding the colloidal solution I into the colloidal solution II, continuously stirring at 500-1000rpm until the mixed solution is completely and uniformly stirred to form hydrogel, and freeze-drying the formed hydrogel.
In a preferred embodiment of the present invention, in the step (2), the acid solution is a hydrochloric acid solution or an acetic acid solution having a mass concentration of 0.1 to 2%.
In a preferred embodiment of the present invention, in step (3), the freeze-drying is performed by: freezing the obtained hydrogel at the temperature of minus 20 ℃ for 8-24 hours, and freeze-drying the reacted solid for 1-3d to obtain the biomass aerogel material.
The biomass aerogel material or the biomass aerogel material prepared by the preparation method disclosed by the invention is applied to ammonia adsorbents.
The beneficial effects are that: according to the invention, the metal-loaded polymer biomass composite adsorbent is prepared by mixing and copolymerizing two polymer biomass materials by taking natural biomacromolecules as a base material, so that the aerogel material with higher specific surface area and lower density is prepared. And the color can be intuitively seen to be changed from yellow to blue-green before and after ammonia adsorption.
Drawings
FIG. 1 is a Fourier infrared spectrum of the composite biomass aerogel synthesized in example 1 before and after adsorption;
FIG. 2 ammonia adsorption capacity under laboratory conditions for examples 1-8;
fig. 3 shows the color change before and after adsorption of the composite biomass aerogel in example 1.
Detailed Description
Example 1: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 3:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to water is 1:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) Weighing chitosan and lithium bromide, putting the chitosan and the lithium bromide into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan to the hydrochloric acid to the lithium bromide to the water is 3:1:1:100), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the chitosan.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 1:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Fourier infrared spectra of the biomass aerogel prepared in the example 1 before and after adsorption are shown in fig. 1, and color changes before and after adsorption of ammonia gas are shown in fig. 3.
Example 2: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 4:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to the water is 1.2:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) Weighing chitosan and lithium bromide, putting the chitosan and the lithium bromide into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan to the hydrochloric acid to the lithium bromide to the water is 3:1:1:100), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the chitosan.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 1:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 3: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to the water is 1.4:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) Weighing chitosan and lithium bromide, putting the chitosan and the lithium bromide into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan to the hydrochloric acid to the lithium bromide to the water is 3:1:1:100), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the chitosan.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 1:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 4: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to the water is 1.6:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) Weighing chitosan and lithium bromide, putting the chitosan and the lithium bromide into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan to the hydrochloric acid to the lithium bromide to the water is 3:1:1:100), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the chitosan.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 2:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 5: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to the water is 1.8:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) The chitosan and lithium bromide are weighed and put into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan, the hydrochloric acid, the lithium bromide and the water is 3:1:1:100), and stirring is carried out (the magnetic rotation speed is 500 r/min), so that the chitosan is fully dissolved.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 2:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 6: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to water is 2:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) The chitosan and lithium bromide are weighed and put into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan, the hydrochloric acid, the lithium bromide and the water is 3:1:1:100), and stirring is carried out (the magnetic rotation speed is 500 r/min), so that the chitosan is fully dissolved.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 2:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 7: preparation of biomass aerogel materials
(1) And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to water is 2:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) The chitosan and lithium bromide are weighed and put into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan, the hydrochloric acid, the lithium bromide and the water is 3:1:1:100), and stirring is carried out (the magnetic rotation speed is 500 r/min), so that the chitosan is fully dissolved.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 3:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
Example 8: preparation of biomass aerogel materials
And (3) weighing carboxymethyl cellulose, adding the carboxymethyl cellulose into an aqueous solution with the pH value of 7 (the viscosity average molecular weight is 30 ten thousand, the mass ratio of the carboxymethyl cellulose to water is 5:100), taking nickel chloride hexahydrate, adding the nickel chloride hexahydrate into water (the mass ratio of the nickel chloride hexahydrate to the water is 2.4:10), and stirring (the magnetic rotation speed is 500 r/min) to fully dissolve the nickel chloride hexahydrate and the carboxymethyl cellulose into a green colloid solution.
(2) The chitosan and lithium bromide are weighed and put into an acid solution (the viscosity average molecular weight of the chitosan is 30 ten thousand, the mass ratio of the chitosan, the hydrochloric acid, the lithium bromide and the water is 3:1:1:100), and stirring is carried out (the magnetic rotation speed is 500 r/min), so that the chitosan is fully dissolved.
(3) Adding the mixed colloidal solution of the carboxymethyl cellulose and the nickel chloride hexahydrate prepared in the step (1) into the chitosan and lithium bromide colloidal solution prepared in the step (2), and fully stirring (the mass ratio of the two colloidal solutions is 3:1) to fully mix the two colloids to form a green colloid. Freezing the obtained hydrogel into a block solid at the temperature of minus 20 ℃, and then placing the block solid in a freeze dryer for freeze drying for 2 days to form the porous composite biomass aerogel material.
2. Ammonia adsorption experiment
The ammonia adsorption experiment method comprises taking a cuboid-like adsorbent of 1.5cm×1cm×0.1cm from the porous composite biomass aerogel materials prepared in examples 1-8, and placing ammonia gas with concentration of 3000mg/m 3 In an 8L sealed organic glass cover, the residual concentration of ammonia gas was measured after 12 hours, and the adsorption amount (mg/g) of ammonia gas per gram of porous material was calculated, and the result was shown in FIG. 2.
The variation of the porous composite biomass aerogel material of example 1 before and after adsorption is shown in fig. 3.
Claims (7)
1. The application of the biomass aerogel material based on the color response mechanism in ammonia gas adsorption is characterized in that the biomass aerogel material is prepared by the following steps: adding carboxymethyl cellulose and nickel chloride hexahydrate into distilled water according to a proportion, and stirring to obtain a colloidal solution I containing carboxymethyl cellulose; dissolving chitosan and lithium bromide in an acidic solution according to a proportion, and stirring to obtain a colloid solution II containing chitosan; mixing the two solutions in proportion, and freeze-drying to obtain a biomass aerogel material; the mass ratio of the carboxymethyl cellulose to the chitosan is 0.2-4:l; the mass ratio of the nickel chloride hexahydrate to the carboxymethyl cellulose is 0.1-4.8:1; the mass ratio of the lithium bromide to the chitosan is 0.1-3:1.
2. The use of a color response mechanism based biomass aerogel material in ammonia gas adsorption according to claim 1, wherein the mass concentration of carboxymethyl cellulose in the colloidal solution i is 1-20%; in the colloid solution II, the mass concentration of the chitosan is 1-10%.
3. The application of the biomass aerogel material based on the color response mechanism in ammonia adsorption according to claim 1, wherein the viscosity average molecular weight of the carboxymethyl cellulose is 5-30 ten thousand; the viscosity average molecular weight of the chitosan is 5-30 ten thousand.
4. The use of a color response mechanism based biomass aerogel material in ammonia adsorption according to claim 1, wherein the preparation method of the biomass aerogel material comprises the following steps:
(1) Preparation of colloidal solution I: adding carboxymethyl cellulose and nickel chloride hexahydrate into distilled water, stirring at 500-1000rpm at room temperature for 1-6h, and adjusting the mass concentration of the carboxymethyl cellulose to 1-20% to obtain green colloid solution I;
(2) Preparation of colloidal solution II: dissolving chitosan and lithium bromide in an acid solution, stirring for 10-48h at 300-1000rpm, and adjusting the mass concentration of the chitosan to 1-10% to obtain a chitosan colloid solution II;
(3) Adding the colloidal solution I into the colloidal solution II according to the mass ratio of the carboxymethyl cellulose to the chitosan of 0.2-4:l, continuously stirring at 500-1000rpm until the mixed solution is completely and uniformly stirred to form hydrogel, and then freeze-drying.
5. The use of a color response mechanism based biomass aerogel material in ammonia adsorption according to claim 4, wherein in step (1), the mass concentration of nickel chloride hexahydrate is 0.1-48%.
6. The application of the biomass aerogel material based on the color response mechanism in ammonia gas adsorption according to claim 4, wherein in the step (2), the acidic solution is a hydrochloric acid solution or an acetic acid solution with a mass concentration of 0.1-2%.
7. The use of a color response mechanism based biomass aerogel material in ammonia adsorption according to claim 4, wherein in step (3), the freeze drying is: freezing the obtained hydrogel at the temperature of minus 20 ℃ for 8-24 hours, and freeze-drying the reacted solid for 1-3d to obtain the biomass aerogel material.
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