CN111286049A - Cellulose porous spherulite microspheres and preparation method thereof - Google Patents
Cellulose porous spherulite microspheres and preparation method thereof Download PDFInfo
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 108
- 239000001913 cellulose Substances 0.000 title claims abstract description 108
- 239000004005 microsphere Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002608 ionic liquid Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 29
- 229920000875 Dissolving pulp Polymers 0.000 claims abstract 2
- 235000010980 cellulose Nutrition 0.000 claims description 102
- 238000002425 crystallisation Methods 0.000 claims description 19
- 230000008025 crystallization Effects 0.000 claims description 19
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 150000001298 alcohols Chemical class 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000643 oven drying Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- -1 1-allyl-3-methylimidazole chloride salt Chemical class 0.000 claims description 3
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 3
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 3
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- IAZSXUOKBPGUMV-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CCCC[NH+]1CN(C)C=C1 IAZSXUOKBPGUMV-UHFFFAOYSA-N 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims description 2
- 239000002159 nanocrystal Substances 0.000 claims description 2
- 238000002210 supercritical carbon dioxide drying Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000011268 retreatment Methods 0.000 abstract 1
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920005615 natural polymer Polymers 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- XIYUIMLQTKODPS-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CC[N+]=1C=CN(C)C=1 XIYUIMLQTKODPS-UHFFFAOYSA-M 0.000 description 1
- QVRCRKLLQYOIKY-UHFFFAOYSA-M 1-methyl-3-prop-2-enylimidazol-1-ium;chloride Chemical compound [Cl-].C[N+]=1C=CN(CC=C)C=1 QVRCRKLLQYOIKY-UHFFFAOYSA-M 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/14—Powdering or granulating by precipitation from solutions
-
- 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
- B01J13/02—Making microcapsules or microballoons
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a cellulose porous spherulite microsphere and a preparation method thereof. The method comprises the steps of dissolving cellulose by using ionic liquid, carrying out isothermal retreatment, and carrying out ultrasonic stripping to obtain the cellulose porous spherical microsphere. The cellulose spherulite microsphere material is completely composed of cellulose, and has controllable size, small and uniform pore diameter. The method overcomes the defect that cellulose microspheres prepared by adding a forming agent are difficult to recycle and degrade, and simplifies the preparation process.
Description
Technical Field
The invention belongs to the technical field of biomass material utilization and high polymer materials, and particularly relates to a cellulose porous spherical crystal microsphere and a preparation method thereof.
Background
In recent years, with the rapid depletion of non-renewable resources such as petroleum, natural gas, and coal mine, much attention has been paid to the development and utilization of natural polymers. Cellulose is used as a natural polymer material, has the most abundant reserves, and is always a research hotspot for development and utilization of cellulose materials due to the advantages of good biocompatibility, higher mechanical strength, easy derivatization, biodegradability and the like. The natural cellulose can be converted into materials in various forms such as films, gels, microspheres and the like through regeneration, and the application of the cellulose in daily life is greatly widened. The cellulose microspheres can be applied to the fields of chromatography, carriers, adsorption, catalysts and the like.
At present, solvent systems commonly used for preparing cellulose microspheres comprise an alkali/urea system, ionic liquid, copper ammonia solution and the like. In recent years, ionic liquids have attracted much attention due to their advantages of being non-toxic, recyclable, excellent in stability, and the like. The invention patent with publication number CN101612540 uses ionic liquid as solvent for the first time, and prepares the cellulose microsphere by reversed phase suspension and programmed cooling method, but the invention needs to add inert particles to promote the microsphere forming, the preparation process is more complicated, and the existence of the inert particles leads the microsphere to be incapable of completely processing through biodegradation. In the invention patent with the publication number of CN108745219A, the cellulose microspheres are prepared by emulsifying and regenerating a cellulose/thiourea solution, but in order to obtain the spherical shape, chemical substances such as a cross-linking agent, an emulsifying agent, a surfactant and the like are added in the preparation process, so that the environmental pollution is easily caused and the subsequent recovery and treatment of the cellulose microspheres are also not facilitated. In the invention patent with publication number CN102504285A, ionic liquid is used as cellulose solvent, and the cellulose microspheres are prepared by inverse suspension and programmed cooling, but the invention needs to add oil, emulsifier, etc., which results in waste of chemical reagents and complex post-treatment process.
Disclosure of Invention
The invention designs a preparation method of a novel cellulose porous spherical crystal microsphere in order to solve the problem that the existence of chemicals in the cellulose microsphere causes difficult recovery and treatment. The invention adopts ionic liquid to dissolve cellulose, cellulose spherulites are obtained by means of self-assembly of molecular chains in the cellulose crystallization process, and then amorphous regions and the ionic liquid are removed by ultrasound to obtain the cellulose spherulites microspheres completely consisting of the cellulose.
The invention utilizes ionic liquid to dissolve cellulose, obtains cellulose spherulites by culturing, removes amorphous areas and ionic liquid by ultrasonic in solvent, and obtains cellulose porous spherulites completely composed of cellulose by washing and drying.
The invention only depends on the self-assembly of molecular chains in the cellulose crystallization process to obtain cellulose spherulites, and then removes amorphous regions and ionic liquid by ultrasound to obtain the cellulose spherulites without adding other forming agents, the preparation process is simple and convenient, and the invention is a new green and environment-friendly process.
The method comprises the following steps:
1) taking cellulose and ionic liquid as raw materials, heating and stirring to obtain a cellulose/ionic liquid homogeneous phase solution;
2) carrying out isothermal crystallization on the solution obtained in the step 1) to obtain cellulose/ionic liquid gel;
3) carrying out ultrasonic treatment on the gel obtained in the step 2) in a solvent to separate cellulose spherulites from an amorphous area and ionic liquid, and stripping the cellulose spherulites;
4) and fully washing the cellulose spherulites obtained by stripping in the previous step to remove residual ionic liquid, and drying to obtain the cellulose porous spherulites.
It is preferable that: in the step 1), the heating temperature is 70-130 ℃, the stirring speed is 100--1The dissolving time is 1-24 h;
it is preferable that: in the step 1), the mass of the cellulose accounts for 5-25% of the mass of the ionic liquid.
It is preferable that: in the step 2), the isothermal crystallization temperature is 40-70 ℃, and the isothermal crystallization time is 3-30 days.
It is preferable that: in the step 3), the mixture accounts for 2-20% of the solvent by mass, and is subjected to ultrasonic treatment for 2-15min under the ultrasonic power of 90-400W to separate cellulose spherulites from an amorphous area and ionic liquid, and the spherulites are stripped;
it is preferable that: in the step 3), the solvent used for ultrasonic treatment is water, acetone, dimethyl sulfoxide, alcohols or a mixture of the water, the acetone, the dimethyl sulfoxide and the alcohols;
it is preferable that: in the step 3), the ultrasonic time is 2-15 min.
It is preferable that: in the step 4), the solvent used for washing the ionic liquid remained in the cellulose spherulites is water, acetone, dimethyl sulfoxide, alcohols or the mixture of the water, the acetone, the dimethyl sulfoxide and the alcohols;
preferably, the drying means includes room temperature air drying, forced air oven drying, vacuum oven drying, freeze drying, supercritical carbon dioxide drying.
It is preferable that: the cellulose includes at least one of pulp, microcrystalline cellulose, and cellulose nanocrystals.
It is preferable that: the ionic liquid comprises at least one of 1-allyl-3-methylimidazole chloride salt and 1-butyl-3-methylimidazole chloride salt.
It is another object of the present invention to prepare a porous spherulitic microsphere consisting entirely of cellulose. The microsphere prepared by the method completely consists of cellulose, is nontoxic and good in biocompatibility, and is convenient to recycle and degrade after use. The size of the microspheres can be controlled by crystallization humidity, temperature and crystallization time. The method can regulate and control the size of the microsphere by changing the humidity, the temperature and the time of crystallization, and the size range is between 100 and 400 microns. A large number of nano-scale holes exist on the surface and inside of the microsphere due to the removal of the amorphous region and the ionic liquid, and the pore size is between 2 and 50 nanometers, so that the microsphere has wide application prospects in the fields of adsorption and carriers.
The invention has the beneficial effects that:
1. the preparation method is simple and convenient: cellulose grows in ionic liquid to obtain spherulites, and then cellulose spherulites can be obtained only by ultrasonic stripping, thereby overcoming the defect that cellulose microspheres prepared by adding a forming agent are difficult to recycle and degrade, simplifying the preparation process
2. Green and no pollution: the cellulose and the ionic liquid which are used as main raw materials are green chemicals, the ionic liquid can be recovered, and the prepared cellulose spherical microsphere can be completely biodegraded and is harmless to the environment.
3. The size of the microsphere can be regulated and controlled: the size of the microsphere is regulated and controlled by changing crystallization humidity, crystallization temperature and crystallization time, and the size range is between 100 and 400 microns.
4. Porous structure: the prepared cellulose spherulite microspheres are completely composed of cellulose, the size is controllable, the pore diameter is small and uniform, a large number of nano-scale holes exist on the surfaces and inside of the cellulose spherulite microspheres, the pore diameter range is 2-50 nanometers, and the cellulose spherulite microspheres have application potential in the fields of adsorption materials and carriers.
Drawings
1. FIG. 1 is a schematic representation of cellulose spherulites obtained in example 1, wherein uniform microsphere sizes around 200 microns are observed;
2. FIG. 2 is a scanning electron micrograph of the cellulose microsphere obtained in example 1 taken at high magnification, wherein a nano-scale microporous structure can be observed;
3. FIG. 3 is an X-ray diffraction pattern of cellulose spherical microspheres obtained in example 1, the crystallinity of the microspheres being 42% as calculated by the Segal method;
4. fig. 4 is a comparison of the infrared spectrum of the cellulose spherulites obtained in example 1 with the infrared spectrum of cellulose, and it can be seen that the infrared peak of the cellulose spherulites is consistent with the cellulose and no other peak appears, which indicates that the microspheres of the present invention are completely composed of cellulose and do not contain other substances.
Detailed Description
The invention is further described below with reference to examples. The scope of the invention is not limited thereto.
Example 1
Adding 1.5g microcrystalline cellulose and 10g 1-allyl-3-methylimidazolium chloride into a single-neck flask, heating in an oil bath at 80 deg.C, mechanically stirring at 600r min-1The dissolution time was 4h, resulting in a homogeneous cellulose/ionic liquid solution. The mixed solution was poured into a glass dish, and crystallized in an oven at 60 ℃ for 14 days at moderate temperature, and the formation of cellulose spherulites was observed under a polarizing microscope. And (3) taking 5g of cellulose/ionic liquid gel subjected to isothermal crystallization in a 100ml beaker, adding 60ml of deionized water, treating for 5min under the ultrasonic power of 180W, separating spherulites from an amorphous region, and stripping to obtain cellulose spherulites. And washing the stripped spherulites with water to fully remove the ionic liquid, and freeze-drying to obtain the cellulose porous spherulites. On the upper partThe diameter of the cellulose spherulites prepared by the method is about 200 microns, and the average pore diameter is about 6 nanometers.
Example 2
The materials and the process flow are the same as example 1, except that the cellulose raw material is 1.5g of paper pulp, and the cellulose porous spherulites are obtained by washing, freezing and drying the spherulites obtained by stripping.
Example 3
The materials and the process flow are the same as the example 1, except that the dissolving temperature is 100 ℃, and the cellulose porous spherulite microspheres are obtained by washing, freezing and drying the spherulites obtained by stripping.
Example 4
The materials and the process flow are the same as those in the example 1, except that the isothermal crystallization time is 21 days, and the cellulose porous spherulites are obtained by washing, freezing and drying the separated spherulites.
Example 5
The materials and the process flow are the same as the example 1, except that the reagent used for ultrasonic treatment is 60ml of dimethyl sulfoxide, the ultrasonic power is 225W, the ultrasonic time is 2min, and the cellulose porous spherulite microspheres are obtained by washing, freezing and drying the spherulites obtained by stripping.
Example 6
The materials and the process flow are the same as those in the example 1, except that the cellulose spherulites obtained by ultrasonic stripping are washed by water and dried at room temperature to obtain the spherulites.
Comparative example 1
The materials and process flow used were the same as in example 1, except that the ionic liquid used was 1-ethyl-3-methylimidazolium acetate. After 30 days of isothermal crystallization, no spherulites were formed, and thus cellulose spherulites could not be obtained.
Comparative example 2
The materials and the process flow are the same as example 1, except that the isothermal crystallization time is 1 day, no visible spherulites are observed in a polarizing microscope, and the cellulose spherulites cannot be obtained by subsequent separation.
Comparative example 3
The materials and process flow used were the same as in example 1, except that the sonication time was 20 min. And the cellulose spherulites are broken due to the overlong ultrasonic time, so that the cellulose spherulites cannot be obtained.
Claims (10)
1. A preparation method of cellulose porous spherulite microspheres is characterized by comprising the following steps: dissolving cellulose by using ionic liquid, obtaining cellulose spherulites by means of self-assembly of molecular chains in the cellulose crystallization process, and then removing amorphous regions and the ionic liquid by ultrasonic waves to obtain the cellulose spherulites which are completely composed of the cellulose.
2. The method for preparing cellulose porous spherical crystalline microspheres according to claim 1, wherein: the method comprises the following steps:
1) taking cellulose and ionic liquid as raw materials, heating and stirring to obtain a cellulose/ionic liquid homogeneous phase solution;
2) carrying out isothermal crystallization on the solution obtained in the step 1) to obtain cellulose/ionic liquid gel;
3) carrying out ultrasonic treatment on the gel obtained in the step 2) in a solvent to separate cellulose spherulites from an amorphous area and ionic liquid, and stripping the cellulose spherulites;
4) and fully washing the cellulose spherulites obtained by stripping in the previous step to remove residual ionic liquid, and drying to obtain the cellulose porous spherulites.
3. The method for preparing cellulose porous spherical crystalline microspheres according to claim 2, wherein: in the step 1), the heating temperature is 70-130 ℃, the stirring speed is 100--1The dissolving time is 1-24 h;
it is preferable that: in the step 1), the mass of the cellulose accounts for 5-25% of the mass of the ionic liquid.
4. The method for preparing cellulose porous spherical crystalline microspheres according to claim 2, wherein: in the step 2), the isothermal crystallization temperature is 40-70 ℃, and the isothermal crystallization time is 3-30 days.
5. The method for preparing cellulose porous spherical crystalline microspheres according to claim 2, wherein: in the step 3), the mixture accounts for 2-20% of the solvent by mass, and is subjected to ultrasonic treatment for 2-15min under the ultrasonic power of 90-400W to separate cellulose spherulites from an amorphous area and ionic liquid, and the spherulites are stripped;
it is preferable that: in the step 3), the solvent used for ultrasonic treatment is water, acetone, dimethyl sulfoxide, alcohols or a mixture of the water, the acetone, the dimethyl sulfoxide and the alcohols;
it is preferable that: in the step 3), the ultrasonic time is 2-15 min.
6. The method for preparing cellulose porous spherical crystalline microspheres according to claim 2, wherein: in the step 4), the solvent used for washing the ionic liquid remained in the cellulose spherulites is water, acetone, dimethyl sulfoxide, alcohols or the mixture of the water, the acetone, the dimethyl sulfoxide and the alcohols;
preferably, the drying means includes room temperature air drying, forced air oven drying, vacuum oven drying, freeze drying, supercritical carbon dioxide drying.
7. The method for preparing cellulose porous spherical crystalline microspheres according to claim 1, wherein: the cellulose includes at least one of pulp, microcrystalline cellulose, and cellulose nanocrystals.
8. The method for preparing cellulose porous spherical crystalline microspheres according to claim 1, wherein: the ionic liquid comprises at least one of 1-allyl-3-methylimidazole chloride salt and 1-butyl-3-methylimidazole chloride salt.
9. Cellulose porous spherulites produced by the method of any of claims 1 to 8, wherein: the microsphere is completely composed of cellulose, the diameter is between 100-400 microns, a large number of holes are formed in the surface and the interior of the microsphere, and the aperture is between 2 and 50 nanometers.
10. The porous cellulose microsphere of claim 9, which is used in the fields of adsorption and carrier.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114702732A (en) * | 2022-06-07 | 2022-07-05 | 江苏集萃智能液晶科技有限公司 | Polymer particle with double-size pore channel and preparation method thereof |
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|---|---|---|---|---|
| EP2022801A1 (en) * | 2007-08-10 | 2009-02-11 | Dow Wolff Cellulosics GmbH | Nanoparticles made of amorphous cellulose |
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| CN105037562A (en) * | 2015-07-09 | 2015-11-11 | 广西科开成林科技有限公司 | Preparation method for cellulose acetate succinate microsphere |
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| Title |
|---|
| HONGZAN SONG ，ET AL.: "Preparation and morphology of different types of cellulose spherulites from concentrated cellulose ionic liquid solutions" * |
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Cited By (2)
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| CN114702732A (en) * | 2022-06-07 | 2022-07-05 | 江苏集萃智能液晶科技有限公司 | Polymer particle with double-size pore channel and preparation method thereof |
| CN114702732B (en) * | 2022-06-07 | 2022-08-26 | 江苏集萃智能液晶科技有限公司 | Polymer particle with double-size pore channel and preparation method thereof |
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Application publication date: 20200616 |