CN105504335A - Preparation method of biomass micro-nano fiber aerogel - Google Patents
Preparation method of biomass micro-nano fiber aerogel Download PDFInfo
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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Abstract
The invention discloses a preparation method of a biomass micro-nano fiber aerogel, and belongs to the field of aerogel preparation. The preparation method comprises the following steps: using shrimp shells to prepare purified chitin, obtaining chitin nanofiber through ultrasonic fibrillation treatment, then preparing a gel through dialysis concentration, and finally drying to obtain the biomass micro-nano fiber aerogel. The method is simple in operation and novel, the purified chitin is prepared by using the shrimp shells as raw materials, so that the utilization of waste materials is realized, the waste of resources is reduced, and the prepared aerogel can be self-degraded; moreover, the chitin nanofiber is obtained by using the ultrasonic fibrillation treatment, and the chitin nanofiber is taken as a one-dimensional nano-assembling unit while the chemical structure of alpha-chitin is maintained to have high mechanical performance and form a support with sufficient strength, so that the aerogel is firm in structure and unlikely to fracture, and the tensile and compressive properties of the material are increased.
Description
Technical field
The invention discloses a kind of preparation method of biomass micro-nano fiber aerogel, belong to aerogel preparation field.
Background technology
Lignocellulose is the material that on the earth, content is the abundantest, is extensively present in woody with herbaceous plant.In timber, micro-fibril not only has very high length-to-diameter ratio, also there is the recyclability of natural molecule, recyclability and biodegradable, but micro-fibril is but closely embedded by hemicellulose and xylogen in plant cell wall, this just makes people start to find various means to isolate the nano-sized aggregates of micro-fibril or several micro-fibril, namely desirable 1-dimention nano assembled unit, nanofibrils cellulose NFC.In addition, chitin is second largest biomass resource on the earth, most chitin does not carry out effective exploitation and just abandons as industrial refuse (dried small shrimp and crab shell), and the annual global output of these biomass resources, more than 2,000 hundred million tons, effectively can be utilized as natural polymer raw material.
Natural polymer goods can meet the demand of people to novel material environment-friendly type and biocompatibility, are the natural polymeric materials that a class has broad development prospect, such as natural polymer aerogel material.
Aerogel is a kind of novel low density of structure-controllable, the nano-porous materials of high porosity, there is continuous print network structure, the bore hole size of nanometer scale and particle diameter are the lightest known at present solid materials, are also heat-insulating property best materials up to now.There is because of it features such as nano-porous structure, low density, low-k, low thermal conductivity, high porosity, high-specific surface area.Aerogel is obviously different from its corresponding macroscopical vitreous material, all there is unique character in mechanics, acoustics, calorifics, optics etc., as extremely low solid-state and gas thermal conductivity, low-refraction, low elastic modulus, low acoustic impedance, strong absorption property etc., have a wide range of applications in fields such as aerospace, chemical industry, energy saving building, military affairs, communication, electronics, metallurgy.
Although natural polymer aerogel material possesses the characteristic of traditional aerogel extremely-low density, unified nano level aperture, high porosity and high-specific surface area, but the performance of self haves much room for improvement, as good mechanical characteristics and degradability, in addition, aerogel by capillary pressure function, easily causes contraction, capillary tension and breaks in drying process.
Therefore, prepare and a kind of there is good mechanical characteristics, can to degrade voluntarily and the natural polymer aerogel material not easily broken is necessary.
Summary of the invention
The technical problem that the present invention mainly solves: though possess the characteristic of traditional aerogel extremely-low density, unified nano level aperture, high porosity and high-specific surface area at present conventional natural polymer aerogel material, but the mechanical property of self, degradability are poor, and it is very fragile, the present situation of easily breaking, providing one utilizes shrimp shell to prepare purifying chitin, chitin nano fiber is obtained by ultrasonic fibrillation process, after again by the concentrated obtained gel of dialysis, final drying, thus the preparation method obtaining biomass micro-nano fiber aerogel.The present invention is simple to operate, method is novel, shrimp shell is not only utilized to prepare purifying chitin for raw material, achieve utilization of waste material, decrease the waste of resource, the aerogel obtained can be degraded voluntarily, and utilize ultrasonic fibrillation process to obtain chitin nano fiber, while maintenance α-chitin chemistry structure, it can be used as 1-dimention nano assembled unit, there is stronger mechanical property, form the support with sufficient intensity, make aerogel structure firm, not easily break, add the resistance to compression tensile property of material, there is more wide application prospect.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) take 500 ~ 600g shrimp shell and put into agate mortar, after grinding 20 ~ 30min shrimp shell meal, then being moved in Soxhlet extraction device, is that 92% ethanolic soln is as extract and heating in water bath is warming up to 75 ~ 85 DEG C using mass concentration, extracting backflow 5 ~ 7h, carries out decolouring, degreasing;
(2) measuring 1 ~ 2L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 3 ~ 4, then to add 3 ~ 5mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 4 ~ 6h, be 85 ~ 95 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 1 ~ 2h repeatedly, removes shrimp glutelin matter;
(3) the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, microwave-assisted dipping 2 ~ 3h at 70 ~ 90 DEG C, remove mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 105 ~ 110 DEG C, obtain purifying chitin;
(4) taking 20 ~ 30g purifying chitin is scattered in 2 ~ 3L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 30 ~ 40min is carried out with 200 ~ 300W power, wherein the ultrasound works time is 0.1 ~ 0.2s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous;
(5) chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 36 ~ 48h, obtains clear gum chitin micro-nano fiber hydrogel;
(6) the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, to be placed in-15 ~-10 DEG C of refrigerators after precooling 10 ~ 15min, use freeze drier again under 20 ~ 30Pa pressure after lyophilize 3 ~ 4h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
The biomass micro-nano fiber aerogel aperture that the present invention obtains is 18 ~ 28nm, and contact angle is 127.5 ~ 134.8 °, and density is 5.6 ~ 6.8mg/cm
3, specific inductivity is 1.2 ~ 2.2, and thermal conductivity is 0.012 ~ 0.022w/mk, and porosity is 85 ~ 93%, specific surface area 350 ~ 650m
2/ g.
Application method of the present invention is: biomass micro-nano fiber aerogel the present invention obtained joins in ink printer, utilize its high-specific surface area, be used as additive, wherein add-on is add 1 ~ 3g aerogel in every 500 ~ 1200mL ink,, not only can expand ink microparticle surfaces tension force after using, and strengthen adsorptive power and make the pattern that prints more clear, more true to nature.
The invention has the beneficial effects as follows:
(1) present invention process is simple, and easy to operate, controllability is good, can not produce environment unfavorable factor in preparation process, not containing to harm composition, is applicable to large-scale production and application;
(2) the present invention utilizes shrimp shell to prepare purifying chitin for raw material, achieves utilization of waste material, decreases the waste of resource, the aerogel obtained can be degraded voluntarily;
(3) the present invention utilizes ultrasonic fibrillation process to obtain chitin nano fiber, and while maintenance α-chitin chemistry structure, it can be used as 1-dimention nano assembled unit, have stronger mechanical property, aerogel is not easily broken, and physicals is better.
Embodiment
First take 500 ~ 600g shrimp shell and put into agate mortar, after grinding 20 ~ 30min shrimp shell meal, then being moved in Soxhlet extraction device, is that 92% ethanolic soln is as extract and heating in water bath is warming up to 75 ~ 85 DEG C using mass concentration, extracting backflow 5 ~ 7h, carries out decolouring, degreasing; Then measuring 1 ~ 2L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 3 ~ 4, then to add 3 ~ 5mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 4 ~ 6h, be 85 ~ 95 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 1 ~ 2h repeatedly, removes shrimp glutelin matter; Subsequently the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, and at 70 ~ 90 DEG C, microwave-assisted dipping 2 ~ 3h, removes mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 105 ~ 110 DEG C, obtain purifying chitin; Next taking 20 ~ 30g purifying chitin is scattered in 2 ~ 3L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 30 ~ 40min is carried out with 200 ~ 300W power, wherein the ultrasound works time is 0.1 ~ 0.2s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous; Afterwards chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 36 ~ 48h, obtains clear gum chitin micro-nano fiber hydrogel; Finally the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, to be placed in-15 ~-10 DEG C of refrigerators after precooling 10 ~ 15min, use freeze drier again under 20 ~ 30Pa pressure after lyophilize 3 ~ 4h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
Example 1
First take 500g shrimp shell and put into agate mortar, after grinding 20min shrimp shell meal, then is moved in Soxhlet extraction device, using mass concentration be 92% ethanolic soln as extract and heating in water bath is warming up to 75 DEG C, extracting refluxes 5h, carries out decolouring, degreasing; Then measuring 1L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 3, then to add 3mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 4h, be 85 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 1h repeatedly, removes shrimp glutelin matter; Subsequently the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, and at 70 DEG C, microwave-assisted dipping 2h, removes mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 105 DEG C, obtain purifying chitin; Next taking 20g purifying chitin is scattered in 2L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 30min is carried out with 200W power, wherein the ultrasound works time is 0.1s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous; Afterwards chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 36h, obtains clear gum chitin micro-nano fiber hydrogel; Finally the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, be placed in-15 DEG C of refrigerators after precooling 10min, then use freeze drier under 20Pa pressure after lyophilize 3h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
This case method is unique novel, during use, biomass micro-nano fiber aerogel the present invention obtained joins in ink printer, utilize its high-specific surface area, be used as additive, wherein add-on is add 1g aerogel in every 500mL ink, not only can expand ink microparticle surfaces tension force after using, and strengthen adsorptive power and make the pattern that prints more clear, more true to nature.
Example 2
First take 550g shrimp shell and put into agate mortar, after grinding 25min shrimp shell meal, then is moved in Soxhlet extraction device, using mass concentration be 92% ethanolic soln as extract and heating in water bath is warming up to 80 DEG C, extracting refluxes 6h, carries out decolouring, degreasing; Then measuring 1.5L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 3.5, then to add 4mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 5h, be 90 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 1.5h repeatedly, removes shrimp glutelin matter; Subsequently the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, and at 80 DEG C, microwave-assisted dipping 2.5h, removes mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 108 DEG C, obtain purifying chitin; Next taking 25g purifying chitin is scattered in 2.5L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 35min is carried out with 250W power, wherein the ultrasound works time is 0.15s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous; Afterwards chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 42h, obtains clear gum chitin micro-nano fiber hydrogel; Finally the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, be placed in-13 DEG C of refrigerators after precooling 13min, then use freeze drier under 25Pa pressure after lyophilize 3.5h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
This case method is unique novel, during use, biomass micro-nano fiber aerogel the present invention obtained joins in ink printer, utilize its high-specific surface area, be used as additive, wherein add-on is add 2g aerogel in every 800mL ink, not only can expand ink microparticle surfaces tension force after using, and strengthen adsorptive power and make the pattern that prints more clear, more true to nature.
Example 3
First take 600g shrimp shell and put into agate mortar, after grinding 30min shrimp shell meal, then is moved in Soxhlet extraction device, using mass concentration be 92% ethanolic soln as extract and heating in water bath is warming up to 85 DEG C, extracting refluxes 7h, carries out decolouring, degreasing; Then measuring 2L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 4, then to add 5mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 6h, be 95 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 2h repeatedly, removes shrimp glutelin matter; Subsequently the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, and at 90 DEG C, microwave-assisted dipping 3h, removes mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 110 DEG C, obtain purifying chitin; Next taking 30g purifying chitin is scattered in 3L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 40min is carried out with 300W power, wherein the ultrasound works time is 0.2s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous; Afterwards chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 48h, obtains clear gum chitin micro-nano fiber hydrogel; Finally the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, be placed in-10 DEG C of refrigerators after precooling 15min, then use freeze drier under 30Pa pressure after lyophilize 4h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
This case method is unique novel, during use, biomass micro-nano fiber aerogel the present invention obtained joins in ink printer, utilize its high-specific surface area, be used as additive, wherein add-on is add 3g aerogel in every 1200mL ink, not only can expand ink microparticle surfaces tension force after using, and strengthen adsorptive power and make the pattern that prints more clear, more true to nature.
Claims (1)
1. a preparation method for biomass micro-nano fiber aerogel, is characterized in that concrete preparation process is:
(1) take 500 ~ 600g shrimp shell and put into agate mortar, after grinding 20 ~ 30min shrimp shell meal, then being moved in Soxhlet extraction device, is that 92% ethanolic soln is as extract and heating in water bath is warming up to 75 ~ 85 DEG C using mass concentration, extracting backflow 5 ~ 7h, carries out decolouring, degreasing;
(2) measuring 1 ~ 2L mass concentration is 2% potassium chlorate solution, dropwise instill edible white vinegar wherein, until pH value of solution reaches 3 ~ 4, then to add 3 ~ 5mL mass concentration be 10% hydrogen peroxide solution, mix, obtain acidifying oxidation solution, above-mentioned shrimp shell after decolouring, skimming treatment is immersed in acidifying oxidation solution, leaves standstill, soak oxidation 4 ~ 6h, be 85 ~ 95 DEG C by filter residue temperature after filtration, mass concentration is that 5% potassium hydroxide solution rinses 1 ~ 2h repeatedly, removes shrimp glutelin matter;
(3) the shrimp shell after deproteination matter being immersed concentration is in 0.3mol/L hydrochloric acid soln, microwave-assisted dipping 2 ~ 3h at 70 ~ 90 DEG C, remove mineral salt wherein, after filtration, filter residue is put into baking oven and be dried to constant weight at 105 ~ 110 DEG C, obtain purifying chitin;
(4) taking 20 ~ 30g purifying chitin is scattered in 2 ~ 3L deionized water, form chitin dispersion liquid, moved in ultrasonic cell disintegration machine, nanometer fibrillation process 30 ~ 40min is carried out with 200 ~ 300W power, wherein the ultrasound works time is 0.1 ~ 0.2s, cycle time out is 0.4s, by micron-sized chitin fiber nanofibrils, obtains the chitin nanometer fibrillated fibers dispersion liquid of clear viscous;
(5) chitin nanometer fibrillated fibers dispersion liquid obtained above is loaded in dialysis tubing, with concentration be the 1mol/L trimethyl carbinol as dialysis displacement liquid, flowing dialysis 36 ~ 48h, obtains clear gum chitin micro-nano fiber hydrogel;
(6) the chitin micro-nano fiber hydrogel after dialysis displacement is poured in mould of plastics, to be placed in-15 ~-10 DEG C of refrigerators after precooling 10 ~ 15min, use freeze drier again under 20 ~ 30Pa pressure after lyophilize 3 ~ 4h, the demoulding, obtain a kind of biomass micro-nano fiber aerogel.
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Cited By (5)
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| CN106318020A (en) * | 2016-08-17 | 2017-01-11 | 郑文忠 | Wear-proof UV solidification ink composition |
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| CN110544430A (en) * | 2019-07-18 | 2019-12-06 | 浙江海洋大学 | preparation method of ductile substrate material |
| CN112680028A (en) * | 2021-01-09 | 2021-04-20 | 广州市印道理印刷有限公司 | Printing ink and preparation method thereof |
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2016
- 2016-02-02 CN CN201610072420.XA patent/CN105504335A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106046924A (en) * | 2016-08-17 | 2016-10-26 | 郑文忠 | Preparation method of wear-resisting UV-curing printing ink composition |
| CN106318020A (en) * | 2016-08-17 | 2017-01-11 | 郑文忠 | Wear-proof UV solidification ink composition |
| CN106046924B (en) * | 2016-08-17 | 2019-04-26 | 珠海恒格电子科技有限公司 | A kind of preparation method of wear-resisting type UV cured printing ink composition |
| CN110080025A (en) * | 2019-05-06 | 2019-08-02 | 南京林业大学 | Regulate and control the method and its application of cellulose size |
| CN110544430A (en) * | 2019-07-18 | 2019-12-06 | 浙江海洋大学 | preparation method of ductile substrate material |
| CN112680028A (en) * | 2021-01-09 | 2021-04-20 | 广州市印道理印刷有限公司 | Printing ink and preparation method thereof |
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