CN111269455A - Preparation method of novel cellulose aerogel - Google Patents
Preparation method of novel cellulose aerogel Download PDFInfo
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- CN111269455A CN111269455A CN202010296745.2A CN202010296745A CN111269455A CN 111269455 A CN111269455 A CN 111269455A CN 202010296745 A CN202010296745 A CN 202010296745A CN 111269455 A CN111269455 A CN 111269455A
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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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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/096—Nitrogen containing compounds
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/097—Sulfur containing compounds
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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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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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
- C08J2301/02—Cellulose; Modified cellulose
Abstract
The invention discloses a preparation method of a novel cellulose aerogel, which comprises the steps of adding cellulose into a solvent, stirring until the cellulose is completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, defoaming after the cellulose is dissolved to prepare a uniform cellulose solution, feeding the cellulose solution into a coagulating bath through a forming die for regeneration forming, and repeatedly replacing the cellulose solution with desalted water until the solvent is cleaned, so as to obtain a cellulose hydrogel; and drying the obtained cellulose hydrogel to remove the contained water to obtain the cellulose aerogel. The solvent in the preparation process of the spinning solution is a mixed solvent of a DMSO (dimethyl sulfoxide) dissolving aid and a TBAH organic alkali solvent, the preparation of the cellulose aerogel with lower density can be realized by matching a coagulating bath and a specific forming die, and the preparation method has the advantages of simple process, low cost, environmental friendliness, capability of being carried out at normal temperature and the like.
Description
Technical Field
The invention belongs to the technical field of cellulose aerogel, and particularly relates to a preparation method of novel cellulose aerogel.
Background
Aerogels are a method of replacing the liquid in a gel with a gas without substantially altering the gelThe special gel of the self-network structure of the gel is a product obtained after drying hydrogel or organogel. The aerogel has the characteristics of nano-scale porous structure, high porosity and the like, and the density range is 3-600Kg/m3Is one of the currently known solid materials with the smallest density. The aerogel has low thermal conductivity, low dielectric constant, high specific surface area, excellent impact resistance and the like, and the unique property steps lead the material to attract interest in basic research and have wide application prospects in many fields.
The cellulose has wide source, is the most abundant high molecular material in nature, and has degradability, reproducibility and good biocompatibility. The cellulose aerogel prepared by using cellulose can be widely applied to the fields of chemical industry, building, papermaking, materials and the like. The traditional cellulose aerogel production process has the defects of high cost, serious pollution and the like.
Disclosure of Invention
The invention solves the technical problem of providing the preparation method of the novel cellulose aerogel, which has simple process, low cost, environmental protection and normal temperature.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the novel cellulose aerogel is characterized by comprising the following specific processes:
step S1: preparation of cellulose hydrogels
Adding cellulose into a solvent, stirring until the cellulose is completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, the DMSO dissolution auxiliary agent accounts for 0-90% of the total mass of the mixed solvent, the purity of the DMSO dissolution auxiliary agent is more than 90wt%, the DMSO dissolution auxiliary agent is used for fully infiltrating an amorphous region and a sub-crystalline region in a cellulose structure, the competitive relationship between the DMSO dissolution auxiliary agent and the TBAH organic alkali solvent is avoided to the utmost extent, the diffusion of the solvent into the cellulose is promoted, the balance regulation between the solvent diffusion and the cellulose dissolution is realized, so that the cellulose is more efficiently dissolved, the DMSO dissolution auxiliary agent is used for improving the stability of the obtained cellulose solution, the DMSO dissolution auxiliary agent can be stably adsorbed on the surface of the dissolved cellulose molecules, so that the regeneration of the dissolved cellulose is effectively inhibited, and the DMSO dissolution auxiliary agent can effectively reduce the viscosity of the cellulose solution, the cellulose hydrogel is prepared by dissolving and defoaming a TBAH organic alkali solution with the concentration of more than 40wt% into a uniform cellulose solution, feeding the cellulose solution into a coagulating bath through a forming die for regeneration and forming, and then repeatedly replacing the cellulose solution with desalted water until the solvent is cleaned;
step S2: preparation of cellulose aerogels
And (4) drying the cellulose hydrogel obtained in the step (S1) to remove the contained water to obtain the cellulose aerogel.
Further defined, the cellulose in step S1 is derived from wood, cotton linter, wheat straw, rice straw, reed, hemp, mulberry bark, paper mulberry bark, or bagasse.
Further defined, the dissolving of the cellulose pulp in step S1 includes: mixing a DMSO dissolving auxiliary agent and a TBAH organic alkali solvent, and then adding cellulose for dissolving; or soaking the cellulose by using a DMSO dissolving auxiliary agent, and then adding a TBAH organic alkali solvent for dissolving; or soaking the cellulose by using the DMSO dissolving auxiliary agent, and then adding the mixed solution of the residual DMSO dissolving auxiliary agent and the TBAH organic alkali solvent for dissolving.
Further, in step S1, the coagulation bath is water, an acidic solution, an alcohol solvent, a ketone solvent, or a mixed solvent thereof, and the temperature of the mixed regeneration liquid is 25 to 60 ℃.
Further defined, the coagulation bath in step S1 is water or a sulfuric acid solution.
Further defined, the cellulose content of the cellulose solution in step S1 is 1wt% to 25 wt%.
Further, the cellulose aerogel in the form of sheet, fiber or granule can be finally prepared by using different forming molds or methods in step S1.
Further defined, the drying process in step S2 is supercritical drying or freeze drying.
Further limited, the preparation method of the novel cellulose aerogel is characterized by comprising the following specific process steps:
step S1: preparation of cellulose hydrogels
Adding cellulose into a solvent, mechanically stirring until the cellulose is completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, the DMSO dissolution auxiliary agent accounts for 80% of the total mass of the mixed solvent, the purity of the DMSO dissolution auxiliary agent is 95wt%, the TBAH organic alkali solvent is a TBAH aqueous solution with the concentration of 50wt%, the content of the cellulose in the cellulose solution is 10wt%, preparing a uniform cellulose solution by centrifugation or negative pressure defoaming after dissolution, mixing the obtained cellulose solution with a coagulating bath, regenerating and molding the cellulose solution by a molding die, and repeatedly replacing the cellulose solution by desalted water until the solvent is cleaned, so as to obtain the cellulose hydrogel;
step S2: preparation of cellulose aerogels
Removing the water content of the cellulose hydrogel obtained in the step S1 through supercritical drying or freeze drying to obtain the cellulose aerogel, wherein the density of the cellulose aerogel is 0.03-0.5g/cm3Specific surface area of more than 80m2(iv) a porosity of greater than 85%.
The solvent selected in the process of preparing the spinning solution is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolving aid. Here, the DMSO dissolution aid functions not only to dissolve a conventional solvent for preparing a spinning dope from cellulose but also to simply combine a TBAH organic base solvent with a DMSO dissolution aid, wherein the DMSO dissolution aid functions mainly in the following three aspects:
1) the DMSO dissolution aid can increase the accessibility of the cellulose, thereby allowing the solvent to penetrate into the interior of the cellulose and, in turn, dissolve the cellulose. One of the key problems involved in the dissolution process of cellulose is the swelling of the aggregated polymer, i.e. the diffusion of the solvent into the cellulose crystals. The dissolving process of cellulose in TBAH organic alkali solvent is a process of dissolving and diffusing simultaneously; the dissolution of cellulose causes a significant increase in the viscosity of the solution in the dissolution region, which is not favorable for the solvent to further diffuse into the cellulose, and thus the dissolution efficiency of the solvent system is low. The viscosity of a cellulose solution is very dependent on the degree of polymerization of cellulose. By introducing the dissolving auxiliary agent, the invention can fully infiltrate the amorphous region and the sub-crystalline region in the cellulose structure, promote the solvent to diffuse into the cellulose, realize the balance regulation between the solvent diffusion and the cellulose dissolution, and further more efficiently dissolve the cellulose. In this process, in addition to the competitive action between the dissolution aid and the cellulose and the competitive action between the organic alkali solvent and the cellulose, there is a competitive relationship between the dissolution aid and the organic alkali solvent. Among these, the latter is disadvantageous for the dissolution of cellulose and therefore needs to be avoided as much as possible. This means that not all dissolution aids commonly used in the art play a positive role in dissolution; if the intermolecular force between the dissolution auxiliary agent and the organic alkali solvent is too strong, the cellulose solubility of the organic alkali solvent is negatively affected.
2) The DMSO dissolution aid can improve the stability of the obtained cellulose solution. Since the organic base solvent is a non-derivatized cellulose solution, the cellulose is in an unstable state in solution, i.e., there is a possibility that the dissolved cellulose molecules are regenerated in a solution environment to form aggregates. The problem of poor stability of the cellulose solution exists in the dissolution of cellulose by a single organic alkali solvent. With the addition of the dissolving assistant, the dissolving assistant can be stably adsorbed on the surface of the dissolved cellulose molecules, so that the regeneration agglomeration of the dissolved cellulose is effectively inhibited. Too strong intermolecular interaction between the dissolution aid and the organic base solvent also needs to be avoided in order not to affect the solubility of the organic base to the cellulose. The invention comprehensively considers the competitive relationship among the organic alkali solvent, the dissolving assistant and the cellulose, and finally selects the organic alkali solvent and the dissolving assistant with ideal effect as the mixed solvent for dissolving the cellulose with high polymerization degree (more than 400 polymerization degree).
3) The DMSO dissolution auxiliary agent can effectively reduce the viscosity of the cellulose solution, is beneficial to realizing the long-distance transportation of the cellulose solution at normal temperature, reduces the transmission energy consumption and cost, and is beneficial to realizing the industrial production. Meanwhile, with the addition of the DMSO dissolving assistant, the alkali content of the cellulose solution is relatively reduced, the proportion of acid in the coagulating bath can be further optimized, the use amount of the acid is greatly reduced, the pollution is reduced, and meanwhile, the working environment of operators is improved.
In addition, natural cellulose presents a complex multilayer structure. Cellulose raw materials from different sources have significant differences in aggregation structure, degree of polymerization and the like, and also have significant differences in trace element content, non-cellulose components (hemicellulose, lignin and the like), combination modes thereof and the like. Thus, there is a clear difference in the ease of dissolution of cellulosic raw materials of different origin from a technical point of view. For cellulose raw materials having a high polymerization degree (such as cotton pulp, wood pulp, etc.), the organic alkali solvent does not dissolve these celluloses well. Due to the key synergistic effect of the dissolution auxiliary agent, the dissolving capacity of the mixed solvent to the cellulose is remarkably improved, which is particularly shown in that the mixed solvent can well dissolve the cellulose raw material with higher polymerization degree.
The solvent in the preparation process of the spinning solution is a mixed solvent of a DMSO (dimethyl sulfoxide) dissolving aid and a TBAH organic alkali solvent, the preparation of the cellulose aerogel with lower density can be realized by matching a coagulating bath and a specific forming die, and the preparation method has the advantages of simple process, low cost, environmental friendliness, capability of being carried out at normal temperature and the like.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
The process flow of the invention is as follows: adding cellulose into a solvent, stirring until the cellulose is completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, the DMSO dissolution auxiliary agent accounts for 0-90% of the total mass of the mixed solvent, the purity of the DMSO dissolution auxiliary agent is more than 90wt%, the TBAH organic alkali solvent is a TBAH aqueous solution with the concentration of more than 40wt%, the content of the cellulose in the cellulose solution is 1-25 wt%, preparing a uniform cellulose solution through centrifugation or negative pressure deaeration after dissolution, then putting the cellulose solution into a coagulating bath through a forming die for regeneration forming, and then repeatedly replacing with desalted water until the solvent is cleaned, thereby obtaining the cellulose hydrogel; and carrying out supercritical drying or freeze drying on the obtained cellulose hydrogel to remove contained water to obtain the cellulose aerogel.
The DMSO dissolution auxiliary agent selected in the following specific examples has a purity of 95wt%, the TBAH organic alkali solvent is TBAH aqueous solution with a concentration of 50wt%, cotton pulp is used as raw material, and cellulose solution with a content of 10wt% alpha cellulose is prepared.
Due to the improvement of the proportion of the DMSO dissolution auxiliary agent to the TBAH aqueous solution in the embodiment, a lower-viscosity cellulose solution can be obtained, the use amount of acid can be effectively reduced, and a lower-density cellulose aerogel can be obtained. Wherein the DMSO dissolution auxiliary agent and the TBAH organic alkali solvent have the best effect when the mass ratio is 8/2.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, the invention further resides in various changes and modifications which fall within the scope of the invention as claimed.
Claims (8)
1. A preparation method of novel cellulose aerogel is characterized by comprising the following specific processes:
step S1: preparation of cellulose hydrogels
Mixing cellulose and a solvent, stirring until the cellulose and the solvent are completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, the DMSO dissolution auxiliary agent accounts for 0-90% of the total mass of the mixed solvent, the purity of the DMSO dissolution auxiliary agent is more than 90wt%, the DMSO dissolution auxiliary agent is used for fully infiltrating an amorphous region and a sub-crystalline region in a cellulose structure, the competitive relationship between the DMSO dissolution auxiliary agent and the TBAH organic alkali solvent is avoided to the utmost extent, the diffusion of the solvent to the inside of the cellulose is promoted, the balance regulation between the solvent diffusion and the cellulose dissolution is realized, so that the cellulose is more efficiently dissolved, the DMSO dissolution auxiliary agent is used for improving the stability of the obtained cellulose solution, the DMSO dissolution auxiliary agent can be stably adsorbed on the surface of the dissolved cellulose molecules, so that the regeneration of the dissolved cellulose is effectively inhibited, and the DMSO dissolution auxiliary agent can effectively reduce the viscosity of the cellulose solution, the cellulose hydrogel is prepared by dissolving and defoaming a TBAH organic alkali solution with the concentration of more than 40wt% into a uniform cellulose solution, feeding the cellulose solution into a coagulating bath through a forming die for regeneration and forming, and then repeatedly replacing the cellulose solution with desalted water until the solvent is cleaned;
step S2: preparation of cellulose aerogels
And (4) drying the cellulose hydrogel obtained in the step (S1) to remove the contained water to obtain the cellulose aerogel.
2. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: the cellulose in step S1 is derived from wood, cotton linter, wheat straw, stalk, straw, reed, hemp, mulberry bark, paper mulberry bark or bagasse.
3. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: the cellulose content in the cellulose solution in step S1 is 1wt% to 25 wt%.
4. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: in step S1, the coagulating bath is water, acidic solution, alcohol solvent, ketone solvent or their mixture, and the temperature of the mixed regeneration liquid is 25-60 deg.C.
5. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: the coagulation bath in step S1 is water or a sulfuric acid solution.
6. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: in step S1, a sheet-like, fibrous or granular cellulose aerogel can be finally prepared by using different forming molds or methods.
7. The method for preparing a novel cellulose aerogel according to claim 1, characterized in that: the drying process in step S2 is supercritical drying or freeze drying.
8. The method for preparing the novel cellulose aerogel according to claim 1, characterized by comprising the following specific process steps:
step S1: preparation of cellulose hydrogels
Adding cellulose into a solvent, mechanically stirring until the cellulose is completely dissolved, wherein the solvent is a mixed solvent of a TBAH organic alkali solvent and a DMSO dissolution auxiliary agent, the DMSO dissolution auxiliary agent accounts for 80% of the total mass of the mixed solvent, the purity of the DMSO dissolution auxiliary agent is 95wt%, the TBAH organic alkali solvent is a TBAH aqueous solution with the concentration of 50wt%, the content of the cellulose in the cellulose solution is 10wt%, preparing a uniform cellulose solution by centrifugation or negative pressure defoaming after dissolution, mixing the obtained cellulose solution with a coagulating bath, regenerating and molding the cellulose solution by a molding die, and repeatedly replacing the cellulose solution by desalted water until the solvent is cleaned, so as to obtain the cellulose hydrogel;
step S2: preparation of cellulose aerogels
Removing the water content of the cellulose hydrogel obtained in the step S1 through supercritical drying or freeze drying to obtain the cellulose aerogel, wherein the density of the cellulose aerogel is 0.03-0.5g/cm3Specific surface area of more than 80m2(iv) a porosity of greater than 85%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115322432A (en) * | 2022-08-30 | 2022-11-11 | 新乡化纤股份有限公司 | Environment-friendly preparation process for regenerating cellulose aerogel based on waste textile ionic liquid method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115322432A (en) * | 2022-08-30 | 2022-11-11 | 新乡化纤股份有限公司 | Environment-friendly preparation process for regenerating cellulose aerogel based on waste textile ionic liquid method |
| CN115322432B (en) * | 2022-08-30 | 2023-09-22 | 新乡化纤股份有限公司 | Green preparation process for regenerating cellulose aerogel based on waste textile ionic liquid method |
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Application publication date: 20200612 |