CN112940336B - Preparation method and application of microfibrillated kapok cellulose aerogel - Google Patents
Preparation method and application of microfibrillated kapok cellulose aerogel Download PDFInfo
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- CN112940336B CN112940336B CN202110135508.2A CN202110135508A CN112940336B CN 112940336 B CN112940336 B CN 112940336B CN 202110135508 A CN202110135508 A CN 202110135508A CN 112940336 B CN112940336 B CN 112940336B
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/05—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur
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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
- C08J2301/08—Cellulose derivatives
Abstract
The invention discloses a preparation method and application of microfibrillated kapok cellulose aerogel, wherein the preparation method comprises the steps of firstly crushing kapok fibers, then dewaxing with alkali liquor, and then pulping to carry out microfibrillation; and then carrying out hydrophobic modification on the microfibrillated kapok cellulose to prepare the microfibrillated kapok cellulose aerogel. The aerogel material is prepared from kapok fibers which are rich in resources, low in cost and have a unique hollow structure, is low in cost and simple in preparation process, has good lipophilicity and hydrophobicity, has high porosity and low density, is easy to degrade, can effectively absorb various organic solvents and oil substances leaked in water, is high in adsorption rate and good in oil-retaining performance, is thorough in oil absorption, is not easy to leak for the second time, and can be recycled by extruding the adsorbed oil; the material can also be used as an oil-water separation or filtering material, and has wide application prospect.
Description
Technical Field
The invention relates to a preparation method and application of microfibrillated kapok cellulose, and belongs to the technical field of aerogel materials.
Background
In recent years, petroleum pollutants become one of the main pollutants in water, and cause serious damage to the water areas such as oceans, rivers and the like and the surrounding ecological environment. The adsorption method has become the main method for treating the problem of oil pollution, but the existing commonly used adsorption materials still have the problems of high cost, small adsorption capacity, incapability of recycling, difficulty in biodegradation, easiness in secondary pollution and the like. Therefore, a low-cost and environment-friendly preparation method is developed, so that the adsorbent with high adsorption multiplying power is prepared, and potential environmental and economic benefits are realized.
Disclosure of Invention
The invention solves the technical problems that: the existing oil absorption material has the technical problems of high preparation cost, small adsorption capacity, incapability of recycling, difficult biodegradation and easiness in secondary pollution.
In order to solve the technical problems, the invention provides a preparation method of microfibrillated kapok cellulose aerogel, which comprises the following steps:
step 1: crushing kapok fibers, dewaxing with alkali liquor, washing off residual alkali liquor with deionized water, and pulping to obtain microfibrillated kapok cellulose solution; the microfibrillation degree of the microfibrillated kapok fiber can be adjusted according to the beating degree;
step 2: taking a microfibrillated kapok cellulose solution, uniformly stirring, regulating the pH value to 4-5 by using acid, and then adding organosiloxane for reaction to carry out hydrophobic modification to obtain a modified microfibrillated kapok cellulose solution;
step 3: and freezing and molding the modified microfibrillated kapok cellulose solution, and drying to obtain the microfibrillated kapok cellulose aerogel.
Preferably, the alkali liquor in the step 1 is 10wt% NaOH solution, and the dewaxing treatment specifically comprises: stirring at 100 deg.c for 1-2 hr.
Preferably, the content of the microfibrillated kapok cellulose in the microfibrillated kapok cellulose solution in the step 2 is 0.05-3 wt%; the acid is at least one of hydrochloric acid, sulfuric acid, nitric acid and acetic acid.
Preferably, the organosiloxane in the step 2 is at least one of vinyl trimethoxy silane, methyl orthosilicate, ethyl orthosilicate, methyl triethoxy silane, ethyl trimethoxy silane and polysilicate; the reaction time is 3-5 h.
More preferably, the organosiloxane is vinyltrimethoxysilane.
Preferably, the addition amount of the organic siloxane in the step 2 is 0.1-5 mL of organic siloxane per 100mL of microfibrillated kapok cellulose solution.
Preferably, the specific conditions of the step 3 of cold forming are as follows: freezing for 12h at-20-25 ℃ or freezing for 5min at-196 ℃ with liquid nitrogen.
Preferably, the drying method in the step 3 is vacuum freeze drying.
Preferably, the conditions of the vacuum freeze drying are: the temperature is between minus 60 ℃ and minus 70 ℃, the pressure is between 0.02 and 0.06mbar, and the time is between 24 and 48 hours.
The invention also provides application of the microfibrillated kapok cellulose aerogel prepared by the preparation method of the microfibrillated kapok cellulose aerogel.
It can be used as oil absorption material, oil-water separation material or filtering material.
Compared with the prior art, the invention has the following beneficial effects:
1. the density of the microfibrillated kapok cellulose aerogel prepared by the invention is 2.1-16.1mg/cm 3 Can effectively absorb various oil liquids such as mineral oil, soybean oil, vacuum pump oil, engine oil, chloroform, DMF, ethanol and the like and organic solvents, and the adsorption multiplying power reaches 112-220 g/g at normal temperature; the oil-retaining property is better and reaches 95.4 percent; the hydrophobic effect is good, and the contact angle reaches 140-158 degrees;
2. the invention takes natural absorbent material kapok fiber with unique hollow structure, wide sources and low price as raw material, and the prepared microfibrillated kapok cellulose aerogel has high porosity and low density, can be reused by a direct extrusion method, and can be biodegraded;
3. the preparation method is simple, the cost is low, and the prepared aerogel material has good lipophilicity and hydrophobicity, can be used as an oil-water separation or filtering material, and has wide application prospect.
Detailed Description
In order to make the present invention more comprehensible, preferred embodiments accompanied with the present invention are described in detail below.
The raw materials used in the following examples are all commercially available products.
Example 1
A method for preparing microfibrillated kapok cellulose aerogel, comprising the following steps:
(1) Dewaxing and microfibrillating the kapok fiber powder after mechanical crushing; putting kapok fiber powder into 10wt% NaOH solution, stirring at 100 ℃ for 1.5h to remove wax on the surface layer of the kapok fiber, and then washing alkali liquor on the fiber by deionized water; pulping the kapok fiber by using a pulping machine, namely microfibrillating treatment, wherein the microfibrillating degree of the kapok fiber can be realized by controlling the pulping degree; taking 100mL of microfibrillated kapok cellulose solution with the microfibrillated kapok fiber content of 1.5wt% into a beaker, and stirring for 1-2 h at normal temperature by using a magnetic stirrer to obtain a uniform solution of microfibrillated kapok cellulose;
(2) Hydrophobic modification of microfibrillated kapok cellulose solution; adjusting the pH value of the solution obtained in the step (1) to be between 4 and 5 by using glacial acetic acid, sucking 0.4ml of vinyltrimethoxysilane by using a pipetting gun, dripping the vinyltrimethoxysilane into the solution, and stirring the solution for 4 hours by using a magnetic stirrer at normal temperature, wherein the rotating speed is 800rpm;
(3) Preparing kapok cellulose aerogel; putting the modified solution into a mould, and freezing for 12h at the temperature of-20 to-25 ℃ in a refrigerator (or freezing for 5min at the temperature of liquid nitrogen-196 ℃); and freeze-drying the mixture for 24 to 48 hours at the temperature of-60 to-70 ℃ and the pressure of 0.04mbar by using a freeze dryer to obtain the microfibrillated kapok cellulose aerogel.
The microfibrillated kapok cellulose aerogel is prepared into an oil absorption material with the size of 2cm multiplied by 1.2cm, and the density is measured to be 3.6mg/cm 3 The contact angle is 149 degrees, the oil is soaked in oil for 10 minutes, the saturated oil absorption multiplying power is 145g/g, and after the oil is taken out from the oil and kept stand for 24 hours, the oil retention rate is 96.1 percent; after 20g of spilled oil is added into a mixture of spilled oil and water with the area of 40cm multiplied by 40cm, 0.2g of prepared oil absorption material is added, 99% of oil can be absorbed within 5min, and the absorption is thorough.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing microfibrillated kapok cellulose aerogel, comprising the steps of:
step 1: crushing kapok fibers, dewaxing with alkali liquor, washing off residual alkali liquor with deionized water, and pulping to obtain microfibrillated kapok cellulose solution;
step 2: taking a microfibrillated kapok cellulose solution, uniformly stirring, regulating the pH value to 4-5 by using acid, and then adding organosiloxane for reaction to carry out hydrophobic modification to obtain a modified microfibrillated kapok cellulose solution;
step 3: freezing and molding the modified microfibrillated kapok cellulose solution, and drying to obtain microfibrillated kapok cellulose aerogel;
the dewaxing treatment specifically comprises the following steps: stirring at 100 deg.c for 1-2 hr.
2. The method for preparing microfibrillated kapok cellulose aerogel according to claim 1, wherein the alkali solution in the step 1 is 10wt% NaOH solution.
3. The method for preparing microfibrillated kapok cellulose aerogel according to claim 1, wherein the content of microfibrillated kapok cellulose in the microfibrillated kapok cellulose solution in the step 2 is 0.05 to 3wt%; the acid is at least one of hydrochloric acid, sulfuric acid, nitric acid and acetic acid.
4. The method for preparing microfibrillated kapok cellulose aerogel according to claim 1, wherein the organosiloxane in step 2 is at least one of vinyltrimethoxysilane, methyltriethoxysilane and ethyltrimethoxysilane; the reaction time is 3-5 h.
5. The method of preparing a microfibrillated kapok cellulose aerogel of claim 4, wherein the organosiloxane is vinyltrimethoxysilane.
6. The method for preparing a microfibrillated kapok cellulose aerogel according to claim 1, wherein the addition amount of the organosiloxane in the step 2 is 0.1 to 5mL per 100mL of microfibrillated kapok cellulose solution.
7. The method for preparing microfibrillated kapok cellulose aerogel according to claim 1, wherein the specific conditions of the step 3 of cold forming are: freezing for 12h at-20-25 ℃ or freezing for 5min at-196 ℃ with liquid nitrogen.
8. The method for preparing microfibrillated kapok cellulose aerogel according to claim 1, wherein the drying method in the step 3 is vacuum freeze drying.
9. The method for preparing microfibrillated kapok cellulose aerogel of claim 8, wherein the vacuum freeze drying conditions are: the temperature is between minus 60 ℃ and minus 70 ℃, the pressure is between 0.02 and 0.06mbar, and the time is between 24 and 48 hours.
10. Use of a microfibrillated kapok cellulose aerogel prepared by the method of preparation of a microfibrillated kapok cellulose aerogel according to any one of claims 1 to 9.
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| CN113429617B (en) * | 2021-06-24 | 2022-07-05 | 东华大学 | Kapok nano-cellulose aerogel and preparation method and application thereof |
| CN114437399A (en) * | 2022-01-04 | 2022-05-06 | 南京工业大学 | Preparation method of starch-biomass cellulose composite aerogel |
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| JP5162752B2 (en) * | 2007-03-20 | 2013-03-13 | 国立大学法人 東京大学 | Cellulose airgel and method for producing the same |
| EP2644566A1 (en) * | 2012-03-30 | 2013-10-02 | Construction Research & Technology GmbH | Method for producing aerogels |
| CN103980547B (en) * | 2014-05-27 | 2015-12-30 | 哈尔滨工业大学 | A kind of method being prepared magnetic cellulose aerogel by waste paper |
| CN104710647A (en) * | 2015-04-14 | 2015-06-17 | 海南大学 | Preparation method of super-hydrophobic cellulose aerogel and application of super-hydrophobic cellulose aerogel in oil stain treatment |
| CN109865482B (en) * | 2019-04-02 | 2020-08-25 | 江南大学 | Antibacterial oil-water separation nano aerogel composite material and preparation method and application thereof |
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| 林亲录等.粮食工程导论.中国轻工业出版社,2019,165. * |
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