CN113637217A - Nano cellulose aerogel, preparation method thereof and application of nano cellulose aerogel in cigarettes - Google Patents
Nano cellulose aerogel, preparation method thereof and application of nano cellulose aerogel in cigarettes Download PDFInfo
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- CN113637217A CN113637217A CN202110750567.0A CN202110750567A CN113637217A CN 113637217 A CN113637217 A CN 113637217A CN 202110750567 A CN202110750567 A CN 202110750567A CN 113637217 A CN113637217 A CN 113637217A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 239000000178 monomer Substances 0.000 claims abstract description 17
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- FEPCMSPFPMPWJK-OLPJDRRASA-N maleopimaric acid Chemical compound C([C@]12C=C([C@H](C[C@@H]11)[C@H]3C(OC(=O)[C@@H]23)=O)C(C)C)C[C@@H]2[C@]1(C)CCC[C@@]2(C)C(O)=O FEPCMSPFPMPWJK-OLPJDRRASA-N 0.000 claims description 2
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 19
- 239000000243 solution Substances 0.000 description 34
- 239000005708 Sodium hypochlorite Substances 0.000 description 23
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
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- 244000166124 Eucalyptus globulus Species 0.000 description 6
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- MHVJRKBZMUDEEV-UHFFFAOYSA-N (-)-ent-pimara-8(14),15-dien-19-oic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(C=C)(C)C=C1CC2 MHVJRKBZMUDEEV-UHFFFAOYSA-N 0.000 description 2
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 2
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
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Images
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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
- C08J9/286—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 the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
- A24D3/10—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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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
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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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
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a preparation method of nano-cellulose aerogel, which comprises the following steps: adding a rosin-based polymerized monomer and methyl methacrylate into a mixed solution of nano-cellulose and nano-silica, uniformly mixing, adding an initiator, and reacting for 3-5 hours at 75-85 ℃; and (3) freeze-drying the obtained product to obtain the nano-cellulose aerogel. The invention also discloses the nano cellulose aerogel and application thereof. The nano cellulose aerogel disclosed by the invention has excellent elasticity and mechanical strength, higher hydrophobicity and better adsorption performance.
Description
Technical Field
The invention belongs to the field of cigarette filter additives, and particularly relates to high-adsorbability nano-cellulose aerogel, a preparation method thereof and application thereof in cigarettes.
Background
Benzopyrene (BaP) is used as nonpolar polycyclic aromatic hydrocarbon, has larger steric hindrance based on the molecular structure and functional groups, and is reduced mainly by the selective adsorption of physical adsorption and pi-pi conjugated adsorption modes when mainstream smoke passes through the filter stick. At present, in the aspect of reducing the release amount of cigarette smoke BaP, the interception and adsorption of the BaP are improved mainly by adopting the modes of adjusting the chemical components of leaf groups and processing technology, adding functional nano materials into cigarette filters, or modifying filter rod tows by high-specific-surface-area fiber materials and the like. According to the reports of the existing documents, the main action mechanisms of reducing phenol comprise hydrogen bond action, pi-pi conjugated adsorption of benzene rings, electrostatic adsorption and the like, and in addition, the main action mechanisms also comprise pore structure adsorption of porous materials. In the tobacco industry, adding functional harm-reducing adsorption materials into filters is an important research direction for reducing the two components. Besides selective adsorption and interception of target components BaP and phenol, modification and correction can be carried out on the mainstream smoke. However, in the meantime, cigarettes are products for mouth touch and smoking, the safety of the filter tip additive material is of great importance, and under the background, the safety consideration is taken as the primary choice of the filter tip additive material of the cigarettes.
Aerogel is a substance with a porous network structure, has the characteristics of low density, high porosity, large specific surface area, strong adsorbability and the like, and becomes a new adsorbent. Cellulose is a natural organic polymer compound, and is widely applied to the field of polymer functional materials due to the advantages of biological reproducibility, no toxicity, no pollution, easy modification and the like, and particularly, the construction of a cellulose aerogel material based on natural cellulose becomes a research hotspot. The cellulose aerogel has the advantages of wide source, degradability, biocompatibility and the like, and becomes a research hotspot in recent years when being used as an additive material of cigarette filters. However, the elasticity and mechanical strength of the existing cellulose aerogel are poor, and the structure collapses and cannot recover the original appearance after being extruded or bent under the action of external force, so that the application of the cellulose aerogel in cigarettes is greatly limited. In order to further widen the variety and practical application of cellulose aerogel, hydrophobic cellulose aerogel with low density, high specific surface area, good elasticity and strong mechanical property needs to be developed to improve the application performance of the cellulose aerogel in cigarettes.
Disclosure of Invention
The invention provides a high-adsorbability nano-cellulose aerogel, a preparation method thereof and application thereof in cigarettes, and the cellulose aerogel obtained by the invention has the characteristics of low density, high specific surface area, good elasticity, strong mechanical property and hydrophobicity; the preparation method has the advantages of simple operation, low cost and environmental protection, and solves the technical problem of poor elasticity and mechanical strength of the cellulose aerogel obtained by the traditional preparation method; the obtained nano-cellulose aerogel is used in cigarettes, and the release amount of harmful ingredients in cigarette smoke can be effectively reduced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows, and the technologies not mentioned in the invention refer to the prior art.
The invention discloses a preparation method of nano-cellulose aerogel, which comprises the following steps: adding a rosin-based polymerized monomer and methyl methacrylate into a mixed solution of nano-cellulose and nano-silica, uniformly mixing, adding an initiator, and reacting for 3-5 hours at 75-85 ℃; freeze-drying the obtained product to obtain the nano-cellulose aerogel; according to the requirement, the product is generally placed in a silica gel mold for freeze drying treatment to obtain the nano cellulose aerogel with different shapes; the silica gel mold can be in a block shape, a spherical shape or a columnar shape, so that the block-shaped, spherical-shaped or columnar nano cellulose aerogel is obtained; the diameter of the spherical nano cellulose aerogel is 0.3 cm-0.7 cm generally; the diameter of the columnar nano cellulose aerogel is 0.4-0.7 cm, and the height of the columnar nano cellulose aerogel is 0.8-1.2 cm.
Preferably, the mixed solution of the nano-cellulose and the nano-silica is formed by mixing 2.5 wt% of nano-cellulose water dispersion and nano-silica aerogel, wherein the mass of the nano-silica aerogel is 10-30% of that of the nano-cellulose; the specific surface area of the nano silicon dioxide aerogel is more than or equal to 600m2/g。
Preferably, the rosin-based polymerized monomer is one or two of propylene pimaric acid ethylene glycol acrylate or maleopimaric acid ethylene glycol acrylate; the hydrophobicity and the mechanical property of the obtained material can be improved after the rosin-based polymerized monomer is polymerized.
Preferably, in order to achieve both the adsorption performance and the mechanical property of the obtained material, the mass ratio of the rosin-based polymerized monomer to the methyl methacrylate is 1: (3-5); the mass ratio of the nano-cellulose to the rosin-based polymerized monomer is 1: (0.05-1.5).
Preferably, in order to improve the reaction efficiency and ensure the quality of the obtained product, the initiator is one or more of potassium persulfate, sodium persulfate or ammonium persulfate, and the mass of the initiator is 0.1-10% of that of the rosin-based polymerization monomer.
Preferably, the freezing temperature of the freeze drying is-20 +/-2 ℃, and the time is 8-12 hours; or a liquid nitrogen quick freezing method is adopted, and the freeze drying time is 2-3 days.
Preferably, the mixing is stirring mixing, and the stirring is carried out for 30-60 min under the condition of 800-1200 r/min; to ensure homogeneity of the resulting material.
Preferably, the nano-cellulose is treated by a TEMPO oxidation process, and then is washed by deionized water to obtain nano-cellulose water dispersion; wherein the cellulose is one or more of regenerated cellulose, bamboo cellulose, hemp cellulose or coconut shell cellulose; the regenerated cellulose is one or more of wood pulp, cotton linter pulp, paper pulp or bagasse pulp;
a specific example of a method for preparing an aqueous dispersion of nanocellulose is: adding 1 part by weight of cellulose, 0.01-0.015 part by weight of 2,2,6, 6-tetramethylpiperidine-1-oxygen radical and 0.1-0.15 part by weight of sodium bromide into 70-80 parts by weight of deionized water, and dropwise adding a sodium hypochlorite solution for reaction to obtain a nano-cellulose aqueous dispersion; the mass content of active chlorine in the sodium hypochlorite is 6-14%.
The invention also discloses a nano cellulose aerogel prepared by the preparation method.
Preferably, the nanocellulose aerogel has resilience; the specific surface area is more than 200m2G, porosity of more than 96.00 percent and density of less than 0.035g/cm3The contact angle is greater than 150 deg..
The third aspect of the invention discloses the application of the nano-cellulose aerogel in cigarettes.
Preferably, the dosage of the nano cellulose aerogel is 10-20 mg added into each cigarette filter; one test result is: the release amounts of phenol, benzopyrene and tar in the main stream smoke are respectively reduced to 53.6 wt%, 19.9 wt% and 17.5 wt%.
The invention has the beneficial effects that:
the cellulose aerogel disclosed by the invention has the characteristics of low density, high specific surface area, large porosity, good rebound resilience, strong mechanical property and high hydrophobicity, and has high adsorbability on phenol, benzopyrene and tar in mainstream smoke when being used for cigarettes. The preparation method disclosed by the invention has the advantages of simplicity and convenience in operation, low cost and environmental friendliness, has a wide application prospect in the field of cigarette filter additives, and can also be used in other environmental protection fields.
Drawings
Fig. 1 is a physical diagram of nano-cellulose aerogels with different shapes prepared in embodiment 3 of the present invention.
Fig. 2 is a scanning electron microscope image of the surface (upper) and cross-section (lower) of the nanocellulose aerogel prepared in example 3 of the present invention.
Fig. 3 is a cyclic compressive stress-strain curve of the bulk nanocellulose aerogel prepared in example 3 of the present invention.
Fig. 4 is a real image of the bulk nanocellulose aerogel prepared in example 3 of the present invention when being squeezed and bent under an external force.
Fig. 5 is a hydrophilic-hydrophobic physical diagram of the bulk nanocellulose aerogels prepared in example 3 and comparative example 2 of the present invention.
Fig. 6 is a schematic diagram of the water contact angle of the bulk nanocellulose aerogel prepared in example 3 of the present invention.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (6-14% of available chlorine, 5mmol/g) solution to about 10 by 0.1mol/L HCl at 25 ℃; dropwise adding 5mL of sodium hypochlorite solution into a flask at the speed of 1 drop/second, simultaneously adjusting the pH of a reaction system by using 0.5mol/L NaOH to keep about 10, continuously stirring after the sodium hypochlorite solution is dripped within 2 hours until the pH is not obviously changed, then washing the solution to be neutral by using deionized water to obtain 2.5 wt% of nano-cellulose water dispersion, adding nano-SiO with the mass of 10% of the nano-cellulose2Aerogel (purchased from gallery Tougo nanomaterial Co., Ltd.) to obtain nano cellulose-SiO2Mixing the solution;
then 0.5g of ethylene glycol propyleneapimaric acid acrylateAnd 2.5g of methyl methacrylate to 50g of the above nanocellulose-SiO2Stirring the mixed solution for 40min at 1000 r/min; and then adding 0.5g of ammonium persulfate into the system, reacting for 4 hours at 80 ℃, placing the product into silica gel molds (block, column and sphere) with different shapes after the reaction is finished, and freeze-drying to obtain the block, column and sphere nano-cellulose aerogel.
The specific surface area of the nano-cellulose aerogel with different shapes is 292m determined by a nitrogen adsorption method2Per g, porosity 96.54%, density 0.034g/cm3(ii) a The contact angle is 151 degrees; the diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm.
Example 2
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (6-14% of available chlorine, 5mmol/g) solution to about 10 by 0.1mol/L HCl at 25 ℃; dropwise adding 5mL of sodium hypochlorite solution into a flask at the speed of 1 drop/second, simultaneously adjusting the pH of a reaction system by using 0.5mol/L NaOH to keep about 10, continuously stirring after the sodium hypochlorite solution is dripped within 2 hours until the pH is not obviously changed, then washing the solution to be neutral by using deionized water to obtain 2.5 wt% of nano-cellulose water dispersion, adding nano-SiO with the mass of 20% of the nano-cellulose2Aerogel (purchased from gallery Tougo nanomaterial Co., Ltd.) to obtain nano cellulose-SiO2Mixing the solution;
0.5g of ethylene glycol propyleneapinoate acrylate and 2.5g of methyl methacrylate were then added to 50g of the above nanocellulose-SiO2Stirring the mixed solution for 40min at 1000 r/min; and then adding 0.5g of ammonium persulfate into the system, reacting for 4 hours at 80 ℃, placing the product into silica gel molds (block, column and sphere) with different shapes after the reaction is finished, and freeze-drying to obtain the block, column and sphere nano cellulose aerogel.
Nitrogen gasThe specific surface area of the nano-cellulose aerogel with different shapes is 258m through the measurement of an adsorption method2G, porosity 97.85%, density 0.033g/cm3(ii) a The contact angle is 152 degrees; the diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm.
Example 3
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (6-14% of available chlorine, 5mmol/g) solution to about 10 by 0.1mol/L HCl at 25 ℃; dropwise adding 5mL of sodium hypochlorite solution into a flask at the speed of 1 drop/second, simultaneously adjusting the pH of a reaction system by using 0.5mol/L NaOH to keep about 10, continuously stirring after the sodium hypochlorite solution is dripped within 2 hours until the pH is not obviously changed, then washing the solution to be neutral by using deionized water to obtain 2.5% of nano-cellulose water dispersion, adding nano-SiO with the mass of 30% of the nano-cellulose2Aerogel (purchased from gallery Tougo nanomaterial Co., Ltd.) to obtain nano cellulose-SiO2Mixing the solution;
then 0.5g of ethylene glycol propyleneapinoate acrylate and 2.5g of methyl methacrylate were added to 50g of the above nanocellulose-SiO2Stirring the mixed solution for 40min at 1000 r/min; and then adding 0.5g of ammonium persulfate into the system, reacting for 4 hours at 80 ℃, placing the product into silica gel molds (block, column and sphere) with different shapes after the reaction is finished, and freeze-drying to obtain the block, column and sphere nano cellulose aerogel.
The specific surface area of the nano-cellulose aerogel with different shapes is 355m determined by a nitrogen adsorption method2G, porosity 97.92%, density 0.032g/cm3(ii) a The contact angle was 154 °; the diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm.
As shown in fig. 1, the nano-cellulose aerogel prepared in this embodiment has a relatively complete macro-morphology, and nano-cellulose aerogels with different shapes and sizes can be constructed. As shown in fig. 2, the cellulose aerogel prepared in example 3 of the present invention had a porous three-dimensional network structure.
FIG. 3 is a cyclic compressive stress-strain curve of the highly adsorptive nano-cellulose aerogel prepared in example 3 of the present invention; the cellulose aerogel is compressed to 50% deformation, and after 4 times of cyclic compression, the cellulose aerogel still has higher deformation recovery rate. As shown in fig. 4, when the nanocellulose aerogel is extruded and bent under the action of external force, the cellulose aerogel does not collapse in microscopic pores and break in macroscopic morphology, can recover to the original morphology well, and shows excellent elasticity and mechanical properties.
Comparative example 1, nanocellulose only, no SiO2Rosin-based polymerized monomers and methyl methacrylate.
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (effective chlorine is 6-14%, 5mmol/g) solution to be about 10 by 0.1mol/L HCl at 25 ℃, dropwise adding 5mL of the sodium hypochlorite solution into a flask at the speed of 1 drop/second, adjusting the pH value of a reaction system to be about 10 by 0.5mol/LNaOH, continuously stirring the sodium hypochlorite solution after the sodium hypochlorite solution is dropwise added within 2 hours until the pH value is not obviously changed, washing the solution to be neutral by deionized water to obtain 2.5 wt% of nano-cellulose aqueous dispersion, placing the nano-cellulose aqueous dispersion into silica gel molds (blocks, columns and spheres) with different shapes, and freeze-drying the nano-cellulose aerogel to obtain the block, column and sphere nano-cellulose aerogel.
The specific surface area of the high-adsorbability nano-cellulose aerogel with different shapes is 121m determined by a nitrogen adsorption method2Per g, porosity 96.20%, density 0.043g/cm3(ii) a The diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm. The specific surface area is lower and the density is higher.
Comparative example 2, only nanocellulose and SiO2And no rosin-based monomer and methyl methacrylate.
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (effective chlorine is 6-14%, 5mmol/g) solution to be about 10 by 0.1mol/L HCl at 25 ℃, dropwise adding 5mL of the sodium hypochlorite solution into a flask at the speed of 1 drop/second, adjusting the pH value of a reaction system to be about 10 by 0.5mol/L NaOH, continuously stirring the sodium hypochlorite solution after the sodium hypochlorite solution is dropwise added within 2 hours until the pH value is not obviously changed, and then washing the solution to be neutral by deionized water to obtain 2.5 wt% of nano-cellulose aqueous dispersion;
then adding nano SiO with the mass of 30 percent of nano cellulose2Aerogel to obtain nano-cellulose-SiO2Mixing the solution, placing the solution in silica gel molds (blocks, columns and spheres) with different shapes, and freeze-drying to obtain the nano cellulose aerogel with blocks, columns and spheres.
The specific surface area of the high-adsorbability nano-cellulose aerogel with different shapes is 346m determined by a nitrogen adsorption method2A porosity of 97.81% and a density of 0.034g/cm3(ii) a The diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm.
Comparative example 3, with nanocellulose, methyl methacrylate and rosin-based monomer, no SiO2。
0.025g of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 0.25g of sodium bromide are weighed into a 250mL three-necked flask containing 150mL of deionized water and stirred to dissolve, and 1g of eucalyptus pulp (available from Dalian Yangrun Co., Ltd.) is added; adjusting the pH value of a sodium hypochlorite (effective chlorine is 6-14%, 5mmol/g) solution to be about 10 by 0.1mol/L HCl at 25 ℃, dropwise adding 5mL of the sodium hypochlorite solution into a flask at the speed of 1 drop/second, adjusting the pH value of a reaction system to be about 10 by 0.5mol/L NaOH, continuously stirring the sodium hypochlorite solution after the sodium hypochlorite solution is dropwise added within 2 hours until the pH value is not obviously changed, and then washing the solution to be neutral by deionized water to obtain 2.5 wt% of nano-cellulose aqueous dispersion;
then 0.5g of propylene pimaric acid ethylene glycol acrylate and 2.5g of methyl methacrylate are added into 50g of the nano-cellulose solution, and the mixture is stirred for 40min at the speed of 1000 r/min; and then adding 0.5g of ammonium persulfate into the system, reacting for 4 hours at 80 ℃, placing the product into silica gel molds (block, spherical and columnar) with different shapes after the reaction is finished, and freeze-drying to obtain the block, spherical and columnar nano cellulose aerogel.
The specific surface area of the nano-cellulose aerogel with different shapes is 129m determined by a nitrogen adsorption method2A porosity of 96.18%, a density of 0.042g/cm3(ii) a The contact angle is 148 degrees; the diameter of the spherical nano cellulose aerogel is 0.6 cm; the diameter of the columnar nano cellulose aerogel is 0.6 cm, and the height of the columnar nano cellulose aerogel is 1.0 cm.
FIG. 5 is a hydrophilic-hydrophobic physical diagram of the cellulose aerogels prepared in example 3 and comparative example 2 of the present invention, and the cellulose aerogels without rosin-based polymerized monomers introduced exhibit hydrophilicity (comparative example 2), and rapidly absorb water in deionized water to be immersed in water; the cellulose aerogel introduced with the rosin-based polymerized monomer shows super-strong hydrophobic characteristics and floats on the water surface (example 3); fig. 6 is a schematic diagram of a water contact angle of the cellulose aerogel prepared in example 3 of the present invention, where the water contact angle is greater than 150 °.
Performance characterization
The nano-cellulose aerogels with different shapes prepared in the example 3 and the comparative example 3 are added into a filter segment of a cigarette filter in an adding amount of 20 mg/cigarette to obtain a sample cigarette, a common cigarette is used as a blank control sample, a cigarette smoking experiment is carried out on a smoking machine according to standard smoking conditions, the release amount of phenol, benzopyrene and tar in mainstream smoke is tested, the reduction rate of corresponding components is calculated, and the test result is shown in table 1.
TABLE 1 cigarette test and control samples of the amount of phenol, benzopyrene and tar released in the smoke
| Sample (I) | Blank control | Example 3 | Comparative example 3 |
| Phenol release (microgram/count) | 8.4 | 3.9 | 4.2 |
| Reduction rate of phenol | -- | 53.6％ | 50％ |
| Released amount of benzopyrene (microgram/count) | 8.64 | 6.92 | 7.13 |
| Reduction ratio of benzopyrene (%) | -- | 19.9％ | 17.5％ |
| Tar release (mg/count) | 9.7 | 8.0 | 8.4 |
| Reduction ratio of Tar (%) | -- | 17.5％ | 13.4％ |
As can be seen from the above table, the nanocellulose aerogel (without nano SiO) prepared in comparative example 3 of the present application2Aerogel) has a certain adsorption effect on phenol and benzopyrene which are harmful components in cigarette smoke, but has a common effect; the nano-cellulose aerogel prepared in example 3 has a more obvious harmful substance reduction effect, and the nano-SiO is proved2After the aerogel is introduced into cellulose, the specific surface area of the nano cellulose aerogel is obviously improved, so that the nano cellulose aerogel has better adsorption effect on harmful components such as phenol, benzopyrene and tar in smoke.
The nano cellulose aerogel obtained in the examples 1-3 and the comparative examples 1-3 is prepared into a cigarette for testing, and common cigarettes are used as blank control samples for comparison, and the cigarette is balanced for 48 hours under the conditions of the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-2 percent, so that the sensory evaluation of cigarette smoking is carried out. The results are shown in Table 2.
TABLE 2 cigarette sensory comparative evaluation
| Gloss (5) | Aroma (32) | Harmonicity (6) | Miscellaneous gas (12) | Irritation (20) | Aftertaste (25) | General score (100) | |
| Blank control | 4.5 | 27.0 | 5.0 | 10.0 | 17.0 | 21.0 | 84.5 |
| Example 1 | 5 | 27.5 | 6.0 | 11.5 | 18.5 | 22.0 | 90.5 |
| Example 2 | 5 | 27.5 | 6.0 | 11.5 | 18.5 | 21.5 | 90.0 |
| Example 3 | 5 | 27.5 | 6.0 | 11.5 | 18.5 | 22.0 | 90.5 |
| Comparative example 1 | 5 | 27.0 | 5.0 | 10.5 | 17.5 | 21.0 | 86.5 |
| Comparative example 2 | 5 | 27.0 | 5.0 | 11.0 | 18.0 | 21.5 | 87.0 |
| Comparative example 3 | 4.5 | 27.0 | 5.0 | 10.5 | 17.5 | 21.5 | 85.5 |
As can be seen from table 2, the nanocellulose aerogel disclosed by the invention can obviously improve the aroma quality of cigarettes, reduce smoke irritation, improve aftertaste and miscellaneous gases, and has better smoking comfort as a whole; a product superior to the comparative example; but all outperformed the ordinary cigarettes of the blank control sample.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (11)
1. The preparation method of the nano-cellulose aerogel is characterized by comprising the following steps: adding a rosin-based polymerized monomer and methyl methacrylate into a mixed solution of nano-cellulose and nano-silica, uniformly mixing, adding an initiator, and reacting for 3-5 hours at 75-85 ℃; and (3) freeze-drying the obtained product to obtain the nano-cellulose aerogel.
2. The preparation method according to claim 1, wherein the mixed solution of the nano-cellulose and the nano-silica is prepared by mixing 2.5 wt% of nano-cellulose water dispersion and nano-silica aerogel, wherein the nano-silica aerogel accounts for 10-30% of the nano-cellulose by mass; the specific surface area of the nano silicon dioxide aerogel is more than or equal to 600m2/g。
3. The method of claim 1, wherein the rosin-based polymerized monomer is one or both of ethylene glycol acrylpimaric acid or ethylene glycol maleopimaric acid.
4. The production method according to claim 1, wherein the mass ratio of the rosin-based polymerized monomer to the methyl methacrylate is 1: (3-5); the mass ratio of the nano-cellulose to the rosin-based polymerized monomer is 1: (0.05-1.5).
5. The preparation method according to claim 1, wherein the initiator is one or more of potassium persulfate, sodium persulfate or ammonium persulfate, and the mass of the initiator is 0.1-10% of that of the rosin-based polymerized monomer.
6. The method according to claim 1, wherein the freeze-drying is carried out at a freezing temperature of-20 ± 2 ℃ for 8 to 12 hours; or a liquid nitrogen quick freezing method is adopted, and the freeze drying time is 2-3 days.
7. The method according to claim 1, wherein the mixing is stirring mixing under the condition of stirring at 800 to 1200r/min for 30 to 60 min.
8. The preparation method according to claim 2, characterized in that the nanocellulose is treated by a TEMPO oxidation process and then washed with deionized water to obtain a nanocellulose aqueous dispersion; wherein the cellulose is one or more of regenerated cellulose, bamboo cellulose, hemp cellulose or coconut shell cellulose; the regenerated cellulose is one or more of wood pulp, cotton linter pulp, paper pulp or bagasse pulp;
9. the nanocellulose aerogel prepared by the preparation method of claim 1.
10. The nanocellulose aerogel of claim 9, wherein said nanocellulose aerogel is resilient; the specific surface area is more than 200m2G, porosity of more than 96.00 percent and density of less than 0.035g/cm3The contact angle is greater than 150 deg..
11. Use of the nanocellulose aerogel according to any of claims 9 or 10 in cigarettes.
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