CN114011345A - Nano-cellulose aerogel and preparation method and application thereof - Google Patents
Nano-cellulose aerogel and preparation method and application thereof Download PDFInfo
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- CN114011345A CN114011345A CN202111337884.6A CN202111337884A CN114011345A CN 114011345 A CN114011345 A CN 114011345A CN 202111337884 A CN202111337884 A CN 202111337884A CN 114011345 A CN114011345 A CN 114011345A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 202
- 239000001913 cellulose Substances 0.000 title claims abstract description 202
- 239000004964 aerogel Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000001914 filtration Methods 0.000 claims abstract description 25
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 229920001046 Nanocellulose Polymers 0.000 claims description 134
- 239000007864 aqueous solution Substances 0.000 claims description 80
- 239000000017 hydrogel Substances 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 238000004108 freeze drying Methods 0.000 claims description 32
- 239000000499 gel Substances 0.000 claims description 30
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 17
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 15
- 125000000524 functional group Chemical group 0.000 claims description 15
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 claims description 15
- 238000007873 sieving Methods 0.000 claims description 15
- 238000002791 soaking Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 6
- 238000006467 substitution reaction Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 15
- 238000003786 synthesis reaction Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- 239000011521 glass Substances 0.000 description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 26
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 26
- 238000003756 stirring Methods 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 16
- 239000005708 Sodium hypochlorite Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 238000007710 freezing Methods 0.000 description 13
- 230000008014 freezing Effects 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 13
- 239000000126 substance Substances 0.000 description 13
- 238000005406 washing Methods 0.000 description 13
- 230000007613 environmental effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229920002749 Bacterial cellulose Polymers 0.000 description 2
- 239000005016 bacterial cellulose Substances 0.000 description 2
- 239000008104 plant cellulose Substances 0.000 description 2
- 241000700605 Viruses Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
Classifications
-
- 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
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/02—Loose filtering material, e.g. loose fibres
- B01D39/04—Organic material, e.g. cellulose, cotton
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a nano-cellulose aerogel and a preparation method and application thereof, belonging to the technical field of material synthesis; the nano-cellulose aerogel provided by the technical scheme of the invention has a porous net structure in the interior, has the properties of high porosity, high mechanical strength and the like, can be effectively applied to the field of air filtration, and has the removal efficiency of particles with the particle size of 0.01-2 mu m in air of more than 99.9%; meanwhile, as the nano-cellulose aerogel has high specific surface area and porosity, the nano-cellulose aerogel has small filtration resistance outside particles in the air are effectively intercepted, namely the product provided by the technical scheme of the invention can give consideration to both resistance pressure drop and filtration efficiency; meanwhile, the nano-cellulose aerogel provided by the technical scheme of the invention takes nano-cellulose as a raw material, wherein the nano-cellulose also has a pore structure and has a certain interception effect on particulate matters, and the nano-cellulose is taken as the raw material, so that the nano-cellulose aerogel is simple and easy to obtain, and the acquisition approach is green and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of material synthesis, and particularly relates to a nano-cellulose aerogel and a preparation method and application thereof.
Background
At present, the haze problem becomes a very serious environmental problem faced by people, and the preparation of a material for effectively filtering small particles in air becomes a problem to be solved urgently. However, the existing air filter material generally has the defects of low filter efficiency, large resistance pressure drop and the like. HEPA (High-Efficiency Particulate Air) filter materials are very efficient Air filter materials at present, the filter Efficiency of common HEPA materials can reach 99.99%, but the technology is still in the exploration stage in china. Most of the air filtration materials commonly used today are fibrous materials such as polytetrafluoroethylene films, nonwoven materials of polymer fibers and glass fiber materials. Although the materials have better filtering efficiency, the materials have the defects of greenness, environmental protection, low functionality, large resistance pressure drop and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the nano-cellulose aerogel which can filter particles, viruses and the like in the air and meet the requirements of environmental protection, and the preparation method and the application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the nano-cellulose aerogel has a porous reticular structure, the average pore diameter of the nano-cellulose aerogel is 100-240nm, and the porosity of the nano-cellulose aerogel is 69% -88%; the nano-cellulose aerogel is prepared from nano-cellulose, wherein the length of the nano-cellulose is 200-800nm, the diameter of the nano-cellulose is 5-80nm, and the content of surface carboxyl functional groups is 0.3-1.0 mmol/g.
The nano-cellulose aerogel provided by the technical scheme of the invention has a porous reticular structure in the interior, has the properties of high porosity, high mechanical strength and the like, can be effectively applied to the field of air filtration, and has the removal efficiency of particulate matters with the particle size of 0.01-2um in air of more than 99.9%; meanwhile, the nanocellulose for preparing the nanocellulose aerogel also has a pore structure, has a certain interception effect on particles, is simple and easy to obtain by taking the nanocellulose as a raw material, and is green and environment-friendly.
In addition, the invention also provides a preparation method of the nano cellulose aerogel, which comprises the following steps:
(1) preparing a nano cellulose aqueous solution: treating cellulose by using a TEMPO oxidation system to obtain cellulose pulp, crushing the cellulose pulp, sieving the crushed cellulose pulp, and adding water to obtain a nano cellulose aqueous solution;
(2) preparing the nano-cellulose hydrogel: rotatably and dropwise adding the nano-cellulose aqueous solution obtained in the step (1) into a solution containing chloride ions to obtain a nano-cellulose hydrogel;
(3) preparation of nanocellulose alcogel: continuously replacing the nano-cellulose hydrogel obtained in the step (2) with a replacement solvent to obtain nano-cellulose alcohol gel;
(4) preparing the nano-cellulose aerogel: and (4) freeze-drying the nano-cellulose alcohol gel obtained in the step (3) to obtain the nano-cellulose aerogel.
As a preferred embodiment of the preparation method of the present invention, in the step (1), the cellulose includes bacterial cellulose or natural plant cellulose.
The bacterial cellulose and the natural plant cellulose have wide sources, simple acquisition ways and environmental protection.
In a preferred embodiment of the preparation method of the present invention, in the step (1), the mass percentage concentration of the nanocellulose in the nanocellulose aqueous solution is 0.2 to 1.0%.
When the mass percentage concentration of the nano-cellulose in the nano-cellulose aqueous solution is in the range, the prepared nano-cellulose aerogel has proper average pore diameter and moderate porosity, and when the nano-cellulose aerogel is applied to air filtration, the filtering efficiency of the nano-cellulose aerogel on particles with the particle size of 0.01-2um in air is up to more than 99.9%.
As a preferable embodiment of the preparation method of the present invention, in the step (2), the solution containing chloride ions includes a zinc chloride solution, a calcium chloride solution, or a sodium chloride solution.
As a preferable embodiment of the production method of the present invention, in the step (2), the concentration of chloride ions in the solution containing chloride ions is 0.8 to 1.6 mol/L.
As a preferred embodiment of the preparation method of the present invention, in the step (2), the volume ratio of the solution containing chloride ions to the nanocellulose aqueous solution is 1: (1-5).
As a preferred embodiment of the preparation method of the present invention, in the step (3), the substitution solvent includes t-butanol or ethanol.
As a preferred embodiment of the preparation method of the present invention, in the step (3), the specific process of continuous substitution is as follows: and continuously soaking the nano-cellulose hydrogel in 25 percent, 50 percent, 75 percent and 100 percent of replacement solvent by mass for 12 to 24 hours respectively.
As a preferred embodiment of the preparation process according to the present invention, in the step (4), the time for lyophilization is 12 to 24 hours, and the temperature for lyophilization is (-24) - (-20) deg.C.
In addition, the invention also provides application of the nano cellulose aerogel in the field of air filtration.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the method comprises the following steps: the nano-cellulose aerogel provided by the technical scheme of the invention has a porous reticular structure in the interior, has the properties of high porosity, high mechanical strength and the like, can be effectively applied to the field of air filtration, and has the removal efficiency of particulate matters with the particle size of 0.01-2um in air of more than 99.9%; meanwhile, as the nano-cellulose aerogel has high specific surface area and porosity, the nano-cellulose aerogel has small filtration resistance outside particles in the air are effectively intercepted, namely the product provided by the technical scheme of the invention can give consideration to both resistance pressure drop and filtration efficiency;
secondly, the method comprises the following steps: the nano-cellulose aerogel provided by the technical scheme of the invention takes nano-cellulose as a raw material, wherein the nano-cellulose also has a pore structure, has a certain interception effect on particles, is simple and easy to obtain by taking the nano-cellulose as the raw material, and is green and environment-friendly in acquisition approach.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 2
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.016g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 1.6g of sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) for 5 minutes by using a homogenizer, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 13nm, the length of the nano-cellulose is about 320nm, and the content of surface carboxyl functional groups is 0.5 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 3
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably and dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of CaCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 4
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: will be provided withRotatably dropwise adding the nano-cellulose aqueous solution in the step (2) to 200mL of ZnCl with the concentration of 0.8mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 5
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding a filtered product into 1000g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 6
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 4g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.6 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 7
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) for 5 minutes by using a homogenizer, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 45nm, the length is about 560nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Example 8
The specific synthesis steps of the nanocellulose aerogel provided in this example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 80nm, the length of the nano-cellulose is about 740nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Comparative example 1
The specific synthesis steps of the nano-cellulose aerogel provided by the comparative example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) for 1 minute by using a homogenizer, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 160nm, the length of the nano-cellulose is about 940nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Comparative example 2
The specific synthesis steps of the nano-cellulose aerogel provided by the comparative example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably and dropwise adding the nano cellulose aqueous solution obtained in the step (2) to200mL of ZnCl with the concentration of 2.0mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Comparative example 3
The specific synthesis steps of the nano-cellulose aerogel provided by the comparative example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding a filtered product into 1500g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.9 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Comparative example 4
The specific synthesis steps of the nano-cellulose aerogel provided by the comparative example are as follows:
(1) preparation of nano cellulose pulp: adding 0.032g of TEMPO and 0.2g of NaBr into 200mL of water, adding 10g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring for 10 minutes at room temperature, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 0.2 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Comparative example 5
The specific synthesis steps of the nano-cellulose aerogel provided by the comparative example are as follows:
(1) preparation of nano cellulose pulp: adding 0.096g of TEMPO and 0.6g of NaBr into 200mL of water, adding 2g of cellulose, adding 3.2g of a sodium hypochlorite solution with the mass percent of 12%, stirring at room temperature for 10 minutes, dropwise adding a NaOH aqueous solution with the mass percent of 1% into a reaction system under the condition of stirring until the pH value of the system is 10, and stopping the reaction to obtain cellulose pulp;
(2) preparing a nano cellulose aqueous solution: crushing the cellulose pulp prepared in the step (1) by using a homogenizer for 10 minutes, then sieving the crushed substances by using a 100-mesh sieve, and adding the filtered product into 400g of water to obtain a nano cellulose aqueous solution; the diameter of the obtained nano-cellulose is about 6nm, the length of the nano-cellulose is about 420nm, and the content of the surface carboxyl functional group is 1.5 mmol/g;
(3) preparing the nano-cellulose hydrogel: rotatably dropwise adding the nano-cellulose aqueous solution obtained in the step (2) to 200mL of ZnCl with the concentration of 0.4mol/L2Obtaining nano cellulose hydrogel in the solution, and washing with deionized water;
(4) preparation of nanocellulose alcogel: soaking the nano-cellulose hydrogel obtained in the step (3) in a tertiary butanol aqueous solution with the mass percentage of 25%, 50%, 75% and 100% for 20 hours at one time to obtain nano-cellulose alcohol gel;
(5) preparing the nano-cellulose aerogel: and (3) pouring the nano cellulose alcohol gel obtained in the step (4) into a glass bottle, unscrewing the bottle cap, firstly putting the glass bottle into liquid nitrogen for 5 minutes for freezing, then putting the glass bottle into a freeze dryer for 24 hours for freeze drying, setting the temperature to be (-20) DEG C, and freeze-drying to obtain the nano cellulose aerogel.
Examples of effects
The nanocellulose aerogels prepared in examples 1 to 8 and comparative examples 1 to 5 were subjected to measurement of average pore size and porosity, and average filtration efficiency and resistance pressure drop when the prepared nanocellulose aerogels were applied to air filtration were simultaneously measured, wherein the filtration efficiency of particulate matters having a particle size of 0.01 to 2um when the nanocellulose aerogels were applied to air filtration was counted, and the results are shown in table 1;
table 1: characterization and application data of nanocellulose aerogel
As can be seen from Table 1, when the technical scheme provided by the invention is adopted, the average filtration efficiency of the prepared nano-cellulose aerogel is over 99.9%, and the average resistance pressure drop is smaller and is below 81%; as can be seen from examples 1 to 8, the larger the porosity, the higher the filtration efficiency, but at the same time, the resistance pressure drop will also increase, and in the preparation process, parameters such as the mass percentage of the nanocellulose in the nanocellulose aqueous solution, the volume ratio of the nanocellulose to the solution containing chloride ions, the mass percentage of the chloride ions in the solution containing chloride ions will all affect the average pore size and the porosity of the product; as can be seen from example 1 and comparative example 1, when the diameter of the prepared nanocellulose was too large, the filtration efficiency was significantly reduced, as can be seen from example 1 and comparative example 2, when the mass percentage of chloride ions in the chloride ion-containing solution was too high, the pore size of the obtained nanocellulose aerogel was too small, and although good filtration efficiency was secured, the filtration efficiency was caused to be too high, as can be seen from example 1 and comparative example 3, when the mass percentage of nanocellulose in the nanocellulose aqueous solution was too low, the pore size of nanocellulose was too low, and the filtration efficiency was significantly reduced, as can be seen from example 1 and comparative example 4, when the mass percentage of nanocellulose in the nanocellulose aqueous solution was too high, the filtration efficiency was caused to be too high, as can be seen from example 1 and comparative example 5, when the surface carboxyl group content in the nanocellulose aqueous solution was too high, causing the drag pressure drop to be too high.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The nano-cellulose aerogel is characterized in that the inside of the nano-cellulose aerogel is of a porous network structure, the average pore diameter of the nano-cellulose aerogel is 100-240nm, and the porosity of the nano-cellulose aerogel is 69% -88%; the nano-cellulose aerogel is prepared from nano-cellulose, wherein the length of the nano-cellulose is 200-800nm, the diameter of the nano-cellulose is 5-80nm, and the content of surface carboxyl functional groups is 0.3-1.0 mmol/g.
2. The method for preparing nanocellulose aerogel according to claim 1, comprising the steps of:
(1) preparing a nano cellulose aqueous solution: treating cellulose by using a TEMPO oxidation system to obtain cellulose pulp, crushing the cellulose pulp, sieving the crushed cellulose pulp, and adding water to obtain a nano cellulose aqueous solution;
(2) preparing the nano-cellulose hydrogel: rotatably and dropwise adding the nano-cellulose aqueous solution obtained in the step (1) into a solution containing chloride ions to obtain a nano-cellulose hydrogel;
(3) preparation of nanocellulose alcogel: continuously replacing the nano-cellulose hydrogel obtained in the step (2) with a replacement solvent to obtain nano-cellulose alcohol gel;
(4) preparing the nano-cellulose aerogel: and (4) freeze-drying the nano-cellulose alcohol gel obtained in the step (3) to obtain the nano-cellulose aerogel.
3. The method according to claim 2, wherein in the step (1), the concentration of the nanocellulose in the nanocellulose aqueous solution is 0.2 to 1.0% by mass.
4. The method according to claim 2, wherein in the step (2), the solution containing chloride ions comprises a zinc chloride solution, a calcium chloride solution or a sodium chloride solution.
5. The production method according to claim 2, wherein in the step (2), the concentration of the chloride ion in the solution containing chloride ion is 0.8 to 1.6 mol/L.
6. The method according to claim 2, wherein in the step (2), the volume ratio of the solution containing chloride ions to the nanocellulose aqueous solution is 1: (1-5).
7. The method according to claim 2, wherein in the step (3), the substitution solvent comprises t-butanol or ethanol.
8. The method according to claim 2, wherein in the step (3), the continuous substitution is carried out by the following specific steps: and continuously soaking the nano-cellulose hydrogel in 25 percent, 50 percent, 75 percent and 100 percent of replacement solvent by mass for 12 to 24 hours respectively.
9. The process according to claim 2, wherein in the step (4), the freeze-drying time is 12 to 24 hours and the freeze-drying temperature is (-24) - (-20) C.
10. Use of the nanocellulose aerogel of claim 1 in the field of air filtration.
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