CN113087959A - Preparation method of crop straw full-component aerogel, product and application thereof - Google Patents
Preparation method of crop straw full-component aerogel, product and application thereof Download PDFInfo
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- CN113087959A CN113087959A CN202110541451.6A CN202110541451A CN113087959A CN 113087959 A CN113087959 A CN 113087959A CN 202110541451 A CN202110541451 A CN 202110541451A CN 113087959 A CN113087959 A CN 113087959A
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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
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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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
- C08J2201/044—Elimination of an inorganic solid phase
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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
- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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Abstract
The invention discloses a preparation method of crop straw full-component aerogel, a product and application thereof, belonging to the technical field of biomass aerogel materials, wherein the method comprises the following steps: pretreating crop straws to obtain straw powder, adding an inorganic salt solution, heating and dissolving, standing and aging the obtained dissolved solution, and then soaking and cleaning with water to obtain hydrogel; soaking the obtained hydrogel in alcohol to obtain alcohol gel, and freeze-drying to obtain the crop straw full-component aerogel; the aerogel prepared by the invention has stable property, has excellent performances of low density, high specific surface area, high porosity, low thermal conductivity coefficient and the like, and can be widely applied to the adsorption of water, oil or organic pollutants and the preparation of heat insulation materials; the invention takes inorganic salt as the solvent for preparing the straw full-component aerogel, has the advantages of no pollution, easy recovery, no toxicity, low cost and the like, and has simple preparation method and easy operation.
Description
Technical Field
The invention belongs to the technical field of biomass aerogel materials, and particularly relates to a preparation method of crop straw full-component aerogel, a product and application thereof.
Background
The crop straw is a renewable resource with high renewable speed and huge yield in northeast regions, and comprises corn straw, wheat straw, rice straw and the like, the straw incineration can generate gas polluting the atmosphere, so that the environment is polluted, and if waste straw resources can be utilized in a high-valued manner, the problem of unbalanced economic development caused by uneven distribution of fossil energy such as coal, petroleum, natural gas and the like can be relieved, and the problem of environment pollution caused by direct combustion of the straw can be reduced or even solved.
The aerogel material is a porous material with a rich three-dimensional network structure, and has the characteristics of extremely low density, high surface area, low thermal conductivity, low dielectric constant and the like. At present, a lot of documents on the preparation of aerogels use cellulose as a raw material, but the cost of pure cellulose is high, and many researchers separate and extract cellulose by pretreating a raw material containing cellulose. Reagents such as acid, alkali or ionic liquid can be used as solvents in the pretreatment process, so that the cost of the whole experiment is increased undoubtedly, the utilization rate of the straws can be reduced, and certain harm can be caused to the environment. Therefore, it is important to find a green and environment-friendly method for preparing aerogel materials with low density, high specific surface area and low thermal conductivity.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a crop straw full-component aerogel, and a product and application thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a crop straw full-component aerogel, which comprises the following steps: pretreating crop straws to obtain straw powder, adding an inorganic salt solution, heating and dissolving, standing and aging the obtained dissolved solution, and then soaking and cleaning with water to obtain hydrogel; and soaking the obtained hydrogel in alcohol to obtain alcohol gel, and freeze-drying to obtain the crop straw full-component aerogel.
Furthermore, the crop straws are corn straws, wheat straws or rice straws.
Further, the pretreatment is to cut off the crop straws, remove dust, clean, dry, crush and screen the crop straws.
Furthermore, the cutting length is 2-10 cm, and the sieving is performed by sieving with a 60-100-mesh sieve.
Further, the inorganic salt solution is one or more of a lithium bromide solution, a zinc chloride solution or a calcium bromide solution, and the inorganic salt solution is heated to 70-150 ℃.
Further, the concentration of the inorganic salt solution is 50-80 wt%, and the mass ratio of the straw powder to the inorganic salt solution is (1-5) to 50.
Further, the dissolving is carried out under stirring for 10-70 min, and the stirring speed is 200-1000 r/min.
Further, the standing aging specifically comprises: firstly, standing at 20-120 ℃ until the solution inclines for 45 degrees, losing fluidity, and then continuously aging at room temperature for 0.01-12 h.
Further, soaking and cleaning with water until the obtained cleaning solution is detected by silver nitrate and no precipitate is generated.
Further, the alcohol soaking is carried out by sequentially adopting alcohol with the concentration of 0-30 wt%, 30-60 wt%, 60-90 wt% and 90-100 wt%. Furthermore, when four concentration gradients of 0-30 wt%, 30-60 wt%, 60-90 wt% and 90-100 wt% of alcohol are used for soaking in sequence, the soaking time of the alcohol in each concentration gradient is 24 hours.
Further, the 0-30 wt%, 30-60 wt% and 60-90 wt% of alcohol is ethanol or tert-butyl alcohol, and the 90-100 wt% of alcohol is tert-butyl alcohol.
Further, the freeze drying is carried out under the vacuum degree of 1-20 Pa, the temperature is-20 to-80 ℃, and the time is 10-48 hours.
The invention also provides the crop straw full-component aerogel prepared by the preparation method.
The invention also provides application of the full-component aerogel containing the crop straws in water, oil or organic pollutant adsorption.
The invention also provides application of the crop straw full-component aerogel in preparation of a heat-insulating material.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses the whole straw components as raw materials, takes inorganic salt as a solvent for preparing the whole straw component aerogel, successfully prepares aerogel, and the prepared aerogel has stable property, low density, high specific surface area, high porosity, low heat conductivity coefficient and other excellent performances, can be widely applied to the adsorption of water, oil or organic pollutants and the preparation of heat insulation materials, and has wide application prospect in the industries of sewage treatment, solar water heaters, heat insulation, oil storage and the like.
The invention does not need to carry out cellulose extraction pretreatment on the straws, can improve the utilization rate of the straws, changes waste straws into valuables, saves the cost and reduces the pollution to the environment.
The method takes the inorganic salt as the solvent for preparing the straw full-component aerogel, is environment-friendly, has the advantages of no pollution, easy recovery, no toxicity, low cost and the like, and is simple in preparation method and easy to operate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIGS. 1a to d are actual effect diagrams of the straw full-component aerogel prepared in examples 1 to 4, which is placed on grass blades in sequence;
FIGS. 2a to d are scanning electron microscope images of the straw full-component aerogel prepared in examples 1 to 4 in sequence.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
The preparation method of the corn straw full-component aerogel comprises the following steps:
(1) straw pretreatment: cutting corn stalks into small sections of 3cm, dedusting, cleaning, drying, crushing by a crusher, and sieving by a 60-mesh sieve to obtain corn stalk powder.
(2) Dissolving: putting the corn straw powder obtained in the step (1) into a zinc chloride solution with the mass concentration of 70%, wherein the mass ratio of the corn straw powder to the zinc chloride solution is 1: 25, and stirring and dissolving the corn straw powder and the zinc chloride solution in an oil bath pan at the temperature of 80 ℃ at the speed of 550r/min for 45min to obtain a dissolved solution.
(3) Preparing corn straw full-component gel: and (3) pouring the solution obtained in the step (2) into a beaker, standing at room temperature until the solution loses fluidity when the beaker is inclined at 45 degrees, and standing at room temperature for 60min for aging to obtain the corn straw full-component gel.
(4) Preparing a corn straw full-component hydrogel: and (4) repeatedly soaking and cleaning the corn straw full-component gel obtained in the step (3) by using deionized water until no precipitate is generated when the cleaning solution is detected by using silver nitrate, which shows that inorganic salt is completely removed, so as to obtain the corn straw full-component hydrogel.
(5) Preparing corn straw full-component alcohol gel: and (3) sequentially soaking the corn straw complete component hydrogel obtained in the step (4) for 24h by using tert-butyl alcohol with the mass fractions of 25%, 50%, 75% and 100%, and replacing the tert-butyl alcohol with the same mass fraction every 12h to obtain the corn straw complete component alcohol gel.
(6) Preparing the corn straw full-component aerogel: and (4) freeze-drying the corn straw full-component alcohol gel obtained in the step (5) for 24 hours at the temperature of minus 60 ℃ and the drying vacuum degree of 10Pa to obtain the corn straw full-component aerogel.
Example 2
The preparation method of the wheat straw full-component aerogel comprises the following steps:
(1) straw pretreatment: cutting wheat straws into 5cm small sections, dedusting, cleaning, drying, crushing by a crusher, and sieving by a 60-mesh sieve to obtain wheat straw powder.
(2) Dissolving: and (2) putting the wheat straw powder obtained in the step (1) into a lithium bromide solution with the mass concentration of 65%, wherein the mass ratio of the wheat straw powder to the lithium bromide solution is 1: 45, stirring and dissolving the wheat straw powder and the lithium bromide solution in an oil bath pan at the temperature of 130 ℃ at the speed of 550r/min for 45min to obtain a dissolved solution.
(3) Preparing the whole-component gel of the wheat straw: and (3) pouring the solution obtained in the step (2) into a beaker, standing at room temperature until the solution loses fluidity when the beaker is inclined at 45 degrees, and then standing at room temperature for 60min for aging to obtain the wheat straw full-component gel.
(4) Preparing wheat straw full-component hydrogel: and (4) repeatedly soaking and cleaning the wheat straw full-component gel obtained in the step (3) by using deionized water until no precipitate is generated when the cleaning solution is detected by using silver nitrate, so that the wheat straw full-component hydrogel is obtained.
(5) Preparing the whole-component alcohol gel of the wheat straws: and (3) sequentially soaking the wheat straw full-component hydrogel obtained in the step (4) with 25% of ethanol, 50% of ethanol, 75% of ethanol and 100% of tert-butyl alcohol for 24 hours, and replacing the tert-butyl alcohol with the same mass fraction every 12 hours to obtain the wheat straw full-component alcohol gel.
(6) Preparing the whole-component aerogel of the wheat straws: and (4) freeze-drying the wheat straw full-component alcohol gel obtained in the step (5) for 24 hours at the temperature of minus 60 ℃ and the drying vacuum degree of 10Pa to obtain the wheat straw full-component aerogel.
Example 3
The preparation method of the rice straw full-component aerogel comprises the following steps:
(1) straw pretreatment: cutting rice straws into 8cm small sections, dedusting, cleaning, drying, crushing by a crusher, and sieving by a 60-mesh sieve to obtain rice straw powder.
(2) Dissolving: putting the rice straw powder obtained in the step (1) into a calcium bromide solution with the mass concentration of 75%, wherein the mass ratio of the rice straw powder to the calcium bromide solution is 1: 20, stirring and dissolving the rice straw powder and the calcium bromide solution in an oil bath pan at the temperature of 150 ℃ at the speed of 550r/min for 20min to obtain a dissolved solution.
(3) Preparing rice straw full-component gel: and (3) pouring the solution obtained in the step (2) into a beaker, standing at 20 ℃ until the solution loses fluidity when the beaker is inclined at 45 ℃, and standing at room temperature for 12 hours to age the beaker, thus obtaining the rice straw full-component gel.
(4) Preparing rice straw full-component hydrogel: and (4) repeatedly soaking and cleaning the rice straw full-component gel obtained in the step (3) by using deionized water until no precipitate is generated when the cleaning solution is detected by using silver nitrate, so that the rice straw full-component hydrogel is obtained.
(5) Preparing rice straw full-component alcohol gel: and (3) sequentially soaking the rice straw full-component hydrogel obtained in the step (4) for 24h by using tert-butyl alcohol with the mass fractions of 25%, 50%, 75% and 100%, and replacing the tert-butyl alcohol with the same mass fraction every 12h to obtain the rice straw full-component alcohol gel.
(6) Preparing the whole-component aerogel of the rice straws: and (4) freeze-drying the rice straw full-component alcohol gel obtained in the step (5) for 10 hours at the temperature of minus 80 ℃ and the drying vacuum degree of 1Pa to obtain the rice straw full-component aerogel.
Example 4
The preparation method of the corn straw full-component aerogel comprises the following steps:
(1) straw pretreatment: cutting corn stalks into 10cm small sections, dedusting, cleaning, drying, crushing by a crusher, and sieving by a 90-mesh sieve to obtain corn stalk powder.
(2) Dissolving: putting the corn straw powder obtained in the step (1) into a lithium bromide solution with the mass concentration of 80%, wherein the mass ratio of the corn straw powder to the lithium bromide solution is 1: 10, and stirring and dissolving the corn straw powder and the lithium bromide solution in an oil bath kettle at the temperature of 110 ℃ at the speed of 650r/min for 40min to obtain a dissolved solution.
(3) Preparing corn straw full-component gel: and (3) pouring the solution obtained in the step (2) into a beaker, standing at 120 ℃ until the solution loses fluidity when the beaker is inclined at 45 degrees, and standing at room temperature for 36s for aging to obtain the corn straw full-component gel.
(4) Preparing a corn straw full-component hydrogel: and (4) repeatedly soaking and cleaning the corn straw full-component gel obtained in the step (3) by using deionized water until no precipitate is generated when the cleaning solution is detected by using silver nitrate, so that the corn straw full-component hydrogel is obtained.
(5) Preparing corn straw full-component alcohol gel: and (3) sequentially soaking the corn straw complete component hydrogel obtained in the step (4) for 24h by using tert-butyl alcohol with the mass fractions of 25%, 50%, 75% and 100%, and replacing the tert-butyl alcohol with the same mass fraction every 12h to obtain the corn straw complete component alcohol gel.
(6) Preparing the corn straw full-component aerogel: and (4) freeze-drying the corn straw full-component alcohol gel obtained in the step (5) for 48 hours at the temperature of minus 20 ℃ and the drying vacuum degree of 20Pa to obtain the corn straw full-component aerogel.
Comparative example 1
The same as example 1 except that t-butanol in step (5) was entirely replaced with ethanol.
Comparative example 2
The method is similar to example 1, except that step (5) is that the corn straw complete component hydrogel obtained in step (4) is sequentially soaked in tertiary butyl alcohol with the mass fractions of 50%, 75% and 100% for 24h, and the tertiary butyl alcohol with the same mass fraction is replaced every 12h, so that the corn straw complete component alcohol gel is obtained.
Comparative example 3
The difference from example 1 is that the freeze-drying in step (6) is carried out under normal pressure.
Effect verification
1. Observing the straw full-component aerogel prepared in the examples 1, 2, 3 and 4 and placing the straw full-component aerogel on a piece of grass blades, the results are shown in fig. 1, wherein fig. 1a is an actual effect diagram of the example 1, fig. 1b is an actual effect diagram of the example 2, fig. 1c is an actual effect diagram of the example 3, and fig. 1d is an actual effect diagram of the example 4, as can be seen from fig. 1, the grass blades are not bent, which indicates that the prepared straw full-component aerogel has excellent characteristics of light weight and low density.
The straw full-component aerogel prepared in the examples 1 to 4 is placed in a normal environment of normal temperature and normal pressure for three days and three nights, and the fact that the quality is slightly increased probably due to the fact that moisture in the air is absorbed does not change in appearance indicates that the aerogel prepared in the examples 1 to 4 is stable in property.
2. The straw full-component aerogels prepared in examples 1 to 4 and comparative examples 1 to 3 were observed, the length, width and height were measured by a vernier caliper, the mass was weighed by a precision electronic scale, and the density was calculated according to the formula ρ ═ m/v, as shown in table 1.
3. Observing the full-component straw aerogel prepared in the examples 1 to 4 and observing the microscopic morphology of the full-component straw aerogel by using a scanning electron microscope, wherein the results are shown in fig. 2, fig. 2a is a scanning electron microscope image of the example 1, fig. 2b is a scanning electron microscope image of the example 2, fig. 2c is a scanning electron microscope image of the example 3, and fig. 2d is a scanning electron microscope image of the example 4, as can be seen from fig. 2, the sample surface has obvious wrinkles and pore structures, and the specific surface area and the porosity of the full-component straw aerogel prepared in the examples 1 to 4 and the comparative examples 1 to 3 are tested, and the results are shown in table 1.
4. The heat conductivity coefficients of the straw full-component aerogels prepared in examples 1 to 4 and comparative examples 1 to 3 were tested, and the results are shown in table 1.
5. The adsorption effect of the straw full-component aerogel prepared in the embodiments 1-4 and the comparative examples 1-3 on water, oil and organic pollutants is verified: the straw full-component aerogel prepared in the examples 1 to 4 and the comparative examples 1 to 3 is put into water, diesel oil and organic pollutant chloroform, and the adsorption results are tested and shown in table 1.
TABLE 1
The above description is only for the preferred embodiment of the present invention, and the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention, the technical solution and the inventive concept of the present invention equivalent or change within the technical scope of the present invention.
Claims (9)
1. The preparation method of the crop straw full-component aerogel is characterized by comprising the following steps of: pretreating crop straws to obtain straw powder, adding an inorganic salt solution, heating and dissolving, standing and aging the obtained dissolved solution, and then soaking and cleaning with water to obtain hydrogel; and soaking the obtained hydrogel in alcohol to obtain alcohol gel, and freeze-drying to obtain the crop straw full-component aerogel.
2. The preparation method according to claim 1, wherein the inorganic salt solution is one or more of a lithium bromide solution, a zinc chloride solution and a calcium bromide solution, and the heating is performed to 70-150 ℃.
3. The preparation method of claim 1, wherein the concentration of the inorganic salt solution is 50-80 wt%, and the mass ratio of the straw powder to the inorganic salt solution is (1-5) to 50.
4. The method according to claim 1, wherein the static aging is specifically: firstly, standing at 20-120 ℃ until the solution inclines for 45 degrees, losing fluidity, and then continuously aging at room temperature for 0.01-12 h.
5. The method according to claim 1, wherein the alcohol soaking is performed by sequentially using 0 to 30 wt%, 30 to 60 wt%, 60 to 90 wt%, and 90 to 100 wt% alcohol.
6. The preparation method according to claim 1, wherein the freeze-drying is carried out under a vacuum degree of 1 to 20Pa, at a temperature of-20 to-80 ℃ and for a time of 10 to 48 hours.
7. The crop straw full-component aerogel prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the crop straw full component aerogel of claim 7 in water, oil or organic pollutant adsorption.
9. Use of the crop straw full component aerogel of claim 7 in the preparation of thermal insulation materials.
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| CN103554548A (en) * | 2013-10-24 | 2014-02-05 | 华南理工大学 | Preparation method of wood fiber biomass aerogel |
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