CN104651964A - Preparation method of cellulose nanofiber - Google Patents
Preparation method of cellulose nanofiber Download PDFInfo
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- CN104651964A CN104651964A CN201510040590.5A CN201510040590A CN104651964A CN 104651964 A CN104651964 A CN 104651964A CN 201510040590 A CN201510040590 A CN 201510040590A CN 104651964 A CN104651964 A CN 104651964A
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Abstract
The invention relates to a preparation method of a cellulose nanofiber. The method comprises the following steps: with wood fiber biomass as a raw material, presoaking, and carrying out steam explosion pretreatment; carrying out high-temperature hydro-thermal treatment on pretreated materials; hydrolyzing hemicellulose, and carrying out washing suction filtration to obtain hemicellulose hydrolysate and filter residues rich in lignin; putting the filter residues into a high-pressure reaction kettle, adding an ethylene glycol solution, heating and extracting the lignin from the residues with ethylene glycol; extracting and carrying out solid-liquid separation to obtain a lignin extract liquid and cellulose solid; carrying out enzymolysis on the cellulose solid with cellulase and removing an amorphous region of the cellulose to obtain cellulose crystal; and carrying out high-pressure homogenizing on the cellulose crystal to obtain a cellulose nanofiber product. The cellulose nanofiber prepared by the method has the advantages of nanoscale, large specific surface area, high activity and high security.
Description
Technical field
The present invention relates to resources technology field, be specifically related to a kind of cellulose nano-fibrous preparation method.
Background technology
Nano-cellulose is a kind of novel polymer-function material, has unique structure and excellent performance, all has good application prospect in a lot of field.In biologic applications, nano-cellulose has larger development in carrier and biology sensor; And at medical domain, nano-cellulose and inorganic matter composite manufacturing artificial organ are focuses; The application of nano-cellulose in purification, conduction and ion-exchange simultaneously also comes into one's own; Food industry is also a key areas of nano-cellulose application, and source and the scope of application have the trend of expansion; Nano-cellulose and magnetic material compound are also new focuses in addition.
The current nano-cellulose preparation chemical method that adopts carries out preliminary treatment to lignocellulose more, and chemical method not only contaminated environment but also produce a lot of side reaction product, exists certain risk at secure context, be not suitable for being applied to food, medicine and health field.Most of nano-cellulose adopts the method for sulphuric acid hydrolysis to obtain, and produces a large amount of spent acid and impurity in preparation process, the more difficult recovery of residue after reaction.
Summary of the invention
Cellulose nano-fibrous preparation method provided by the invention, solves chemical method and uses strong acid and strong base and toxic reagent contaminated environment, and produce a lot of side reaction product, there is the problem of security risk.
To achieve these goals, technical scheme of the present invention is as follows:
A cellulose nano-fibrous preparation method, it comprises the steps:
A, wood fiber biomass raw material is dipped to water saturation in water after, be forced into 1.0 ~ 2.5Mpa, after dimension pressure 2 ~ 15min, instant decompression release, carries out steam blasting preliminary treatment, obtains the quick-fried raw material of vapour;
Add water in b, product in step a, process 10 ~ 30min within the scope of 170 ~ 190 DEG C after, carry out suction filtration, collect the filter residue being rich in cellulose and lignin;
Add glycol water in c, the filter residue that obtains in step b, within the scope of 200 ~ 220 DEG C, extract 1.5 ~ 2.5h, after extraction terminates, carry out Separation of Solid and Liquid, collect solids product, be cellulose solids;
Add acidic cellulase in d, the cellulose solids that obtains in step c, the dosage controlling to add in described every gram of cellulose solids acidic cellulase is 100 ~ 350U, and at 40 ~ 70 DEG C, enzymolysis 5 ~ 15h, obtains cellulose crystals;
E, by the cellulose crystals that obtains in steps d after high speed dispersion, at the pressure of 90 ~ 120MPa, carry out homogeneous cooling processing at 10 ~ 25 DEG C, this step repeats 4 ~ 10 times, obtains cellulose nano-fibrous finished product.
Carry out steam blasting after adopting preimpregnation and preliminary treatment is carried out to raw material, its principle is that high-pressure hot steam enters in fibrous raw material, and the space of infiltrated fiber inside, because steam and hot synergy produce class acid degradation and the thermal degradation of fibrous raw material, lower-molecular substance stripping, fibrous polymer degree declines; During high steam release, the high speed of fibrous inside and around vapours flows instantaneously, makes fiber generation mechanical breaking to a certain extent, and the inner hydrogen bond of cellulose is destroyed, and unformed area and partially crystallizable district are destroyed.Avoid the electroplating effluent recycling and using strong acid and strong base and toxic reagent, Product Safety improves greatly.
The hydrothermal treatment consists adopted is in fact the differentiation of dilute acid pretreatment method, hydrothermal treatment consists destroys acetyl group, furfural acid substituent etc. on hemicellulose, generate acetic acid and other organic acids, the organic acids such as acetic acid are formed with the ehter bond that helps break fibrous raw material cell membrane and connect, and serve catalytic action to the formation of compound sugar and removal; In addition, the dielectric constant of temperature appreciable impact aqueous water, under high temperature action, water also serves the effect of acid, polysaccharide is hemicellulose particularly, can be hydrolyzed into monose, the stripping of hemicellulose can improve the reactivity of lignin and the penetrating power of reagent, thus improves the extraction degree of lignin.
Adopt ethylene glycol high-temperature extraction lignin, utilize ethylene glycol to the good dissolubility of lignin and high boiling feature, avoid the shortcoming with Small molecule organic solvents volatile in extraction process, easy leakage, inflammable and explosive and high-voltage operation, substantially increase the security of extraction process.
Adopt cellulase to carry out enzymolysis to the raw material removing hemicellulose and lignin, cellulase acts preferentially on cellulosic amorphous region, selects suitable cellulase, consumption and enzymolysis time, obtains cellulose crystals after enzymolysis.
Preferably, in step a, described wood fiber biomass raw material is at least one in agricultural crop straw, wheat bran, bean dregs, bagasse, straw.
Preferably, in step b, the mass ratio of the quick-fried raw material of described vapour and water is 1:16 ~ 1:8.
Preferably, in step c, the mass fraction of described glycol water is 70 ~ 90%.
Preferably, in step c, the fibre length of described wood fiber biomass raw material is 2 ~ 10mm.
Preferably, in step c, the volume ratio of described filter residue and glycol water is 1:7 ~ 1:10.
The present invention adopts cellulase to carry out enzymolysis to the raw material removing hemicellulose and lignin, and cellulase acts preferentially on cellulosic amorphous region, selects suitable cellulase, consumption and enzymolysis time, obtains cellulose crystals after enzymolysis.
Prepared by the present invention cellulose nano-fibrous compared with general fibre, has nano-scale, large, the active stronger advantage of specific area.The cellulose nano-fibrous diameter of preparation is at 10 ~ 20nm, and length is between 200 ~ 400nm.High-pressure homogeneously have obvious broken wall effect to fiber, along with the increase of homogenization cycles, the specific area of fiber increases gradually.Cellulose chain segment a large amount of in preparation process is destroyed and rupture, and surface exposes a large amount of hydroxyls, and reactivity is enhanced.Cellulose nano-fibrous is a kind of novel polymer-function material, has unique structure and excellent performance, has application in a lot of fields.
Beneficial effect of the present invention is mainly reflected in: the present invention adopts steam blasting preliminary treatment, eliminate most of hemicellulose and partial lignin, add its molecule accessibility and reactivity, and the quick-fried rear cellulose crystallity of vapour improves, the degree of polymerization declines, and removes hemicellulose through high-temperature-hot-water process, then through ethylene glycol extraction lignin, then cellulose unformed area is taken off through cellulose enzyme, cellulose nano-fibrous finally by high-pressure homogeneous preparation.This method reagent used is simple and safe, and reacted residue recoverable, reduces production cost.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Fig. 2 is that cellulose nano-fibrous TEM schemes.
Detailed description of the invention
Process chart of the present invention as shown in Figure 1.
embodiment 1
The maize straw that 2 ~ 10mm is long is dipped to water saturation in water, then loads steam-explosion jar, dimension pressure 10min under the pressure of 1.8Mpa, and instant decompression release afterwards, obtains the quick-fried maize straw of vapour; Add the quick-fried maize straw of vapour and water in a kettle., the mass ratio of the quick-fried maize straw of vapour and water is 1:8, at the temperature of 180 DEG C, be hydrolyzed 20min, carries out suction filtration after cooling with vavuum pump, obtains hydrolyzate and steam puffed stalk filter residue; Steam puffed stalk filter residue is placed in autoclave through washing, then adds the ethylene glycol solution of 80% mass concentration by solid-to-liquid ratio 1:7, is heated to 210 DEG C of extraction 2.5h, carries out Separation of Solid and Liquid, obtain extraction solution and cellulose solids after cooling; Extraction solution obtains ethylene glycol solution and lignin after decompression distillation, and wherein ethylene glycol can be back to cycling extraction lignin; The cellulose solids obtained adds acidic cellulase and carries out enzymolysis after washing, and the addition of acidic cellulase is 200U/g substrate, enzymolysis 7h at the temperature of 60 DEG C, and carry out Inactivation in Water after enzymolysis terminates and wash, then Separation of Solid and Liquid obtains cellulose crystals; Add a small amount of water in cellulose crystals and make cellulose suspension, through high-pressure homogeneous under high speed disperser, carry out low temperature (25 DEG C) cooling, homogenization pressure 100Mpa in homogenizing process, circulate 6 times to obtain high purity cellulose nanofiber simultaneously.As Fig. 2, obtained cellulose nano-fibrous diameter is at 10 ~ 20nm, and length is between 200 ~ 400nm.
embodiment 2
Wheat bran is dipped to water saturation in water, then loads steam-explosion jar, dimension pressure 5min under the pressure of 2.2Mpa, instant decompression release afterwards, obtains the quick-fried wheat bran of vapour; Add the quick-fried wheat bran of vapour and water in a kettle., the mass ratio of the quick-fried wheat bran of vapour and water is 1:10, at the temperature of 190 DEG C, be hydrolyzed 10min, carries out suction filtration after cooling with vavuum pump, obtains hydrolyzate and the quick-fried wheat bran filter residue of vapour; The quick-fried wheat bran filter residue of vapour is placed in autoclave through washing suction filtration, then adds the ethylene glycol solution of 80% mass concentration by solid-to-liquid ratio 1:8, is heated to 215 DEG C of extraction 2h, carries out Separation of Solid and Liquid, obtain extraction solution and cellulose solids after cooling; Extraction solution obtains ethylene glycol solution and lignin after decompression distillation, and wherein ethylene glycol can be back to cycling extraction lignin; The cellulose solids obtained adds acidic cellulase and carries out enzymolysis after washing, and the addition of acidic cellulase is 150U/g substrate, enzymolysis 12h at the temperature of 50 DEG C, and carry out Inactivation in Water after enzymolysis terminates and wash, then Separation of Solid and Liquid obtains cellulose crystals; Add a small amount of water in cellulose crystals and make cellulose suspension, through high-pressure homogeneous under high speed disperser, carry out low temperature (10 DEG C) cooling, homogenization pressure 120Mpa in homogenizing process, circulate 10 times to obtain high purity cellulose nanofiber simultaneously.
embodiment 3
Bean dregs are dipped to water saturation in water, then steam-explosion jar is loaded, dimension pressure 12min under the pressure of 1.5Mpa, instant decompression release afterwards, obtains vapour pop beans slag, adds vapour pop beans slag and water in a kettle., the mass ratio of vapour pop beans slag and water is 1:16, at the temperature of 170 DEG C, be hydrolyzed 30min, after cooling, carry out suction filtration with vavuum pump, obtain hydrolyzate and vapour pop beans slag filter residue; Vapour pop beans slag filter residue is placed in autoclave through washing suction filtration, then adds the ethylene glycol solution of 90% mass concentration by solid-to-liquid ratio 1:9, is heated to 200 DEG C of extraction 2h, carries out Separation of Solid and Liquid, obtain extraction solution and cellulose solids after cooling; Extraction solution obtains ethylene glycol solution and lignin after decompression distillation, and wherein ethylene glycol can be back to cycling extraction lignin; The cellulose solids obtained adds acidic cellulase and carries out enzymolysis after washing, and the addition of acidic cellulase is 100U/g substrate, enzymolysis 15h at the temperature of 65 DEG C, and carry out Inactivation in Water after enzymolysis terminates and wash, then Separation of Solid and Liquid obtains cellulose crystals; Add a small amount of water in cellulose crystals and make cellulose suspension, through high-pressure homogeneous under high speed disperser, carry out low temperature 20 DEG C cooling, homogenization pressure 100Mpa in homogenizing process simultaneously, circulate 6 times to obtain high purity cellulose nanofiber.
embodiment 4
The straw that 2 ~ 10mm is long is dipped to water saturation in water, then steam-explosion jar is loaded, dimension pressure 8min under the pressure of 2.0Mpa, instant decompression release afterwards, obtains the quick-fried straw of vapour, adds the quick-fried straw of vapour and water in a kettle., the mass ratio of the quick-fried straw of vapour and water is 1:14, at the temperature of 180 DEG C, be hydrolyzed 20min, after cooling, carry out suction filtration with vavuum pump, obtain hydrolyzate and the quick-fried straw filter residue of vapour; The quick-fried straw filter residue of vapour is placed in autoclave through washing suction filtration, then adds the ethylene glycol solution of 70% mass concentration by solid-to-liquid ratio 1:10, is heated to 220 DEG C of extraction 1.5h, carries out Separation of Solid and Liquid, obtain extraction solution and cellulose solids after cooling; Extraction solution obtains ethylene glycol solution and lignin after decompression distillation, and wherein ethylene glycol can be back to cycling extraction lignin; The cellulose solids obtained adds acidic cellulase and carries out enzymolysis after washing, and the addition of acidic cellulase is 300U/g, enzymolysis 6h at the temperature of 45 DEG C, and carry out Inactivation in Water after enzymolysis terminates and wash, then Separation of Solid and Liquid obtains cellulose crystals; Add a small amount of water in cellulose crystals and make cellulose suspension, through high-pressure homogeneous under high speed disperser, carry out low temperature (15 DEG C) cooling, homogenization pressure 120Mpa in homogenizing process, circulate 5 times to obtain high purity cellulose nanofiber simultaneously.
In sum, be only preferred embodiment of the present invention, not be used for limiting scope of the invention process, all equalizations of doing according to shape, structure, feature and the spirit described in the claims in the present invention scope change and modify, and all should be included in right of the present invention.
Claims (6)
1. a cellulose nano-fibrous preparation method, is characterized in that, comprises the steps:
A, wood fiber biomass raw material is dipped to water saturation in water after, be forced into 1.0 ~ 2.5Mpa, after dimension pressure 2 ~ 15min, instant decompression release, carries out steam blasting preliminary treatment, obtains the quick-fried raw material of vapour;
Add water in b, product in step a, process 10 ~ 30min within the scope of 170 ~ 190 DEG C after, carry out suction filtration, collect the filter residue being rich in cellulose and lignin;
Add glycol water in c, the filter residue that obtains in step b, within the scope of 200 ~ 220 DEG C, extract 1.5 ~ 2.5h, after extraction terminates, carry out Separation of Solid and Liquid, collect solids product, be cellulose solids;
Add acidic cellulase in d, the cellulose solids that obtains in step c, the dosage controlling to add in described every gram of cellulose solids acidic cellulase is 100 ~ 350U, and at 40 ~ 70 DEG C, enzymolysis 5 ~ 15h, obtains cellulose crystals;
E, by the cellulose crystals that obtains in steps d after high speed dispersion, at the pressure of 90 ~ 120MPa, carry out homogeneous cooling processing at 10 ~ 25 DEG C, this step repeats 4 ~ 10 times, obtains cellulose nano-fibrous finished product.
2. preparation method as claimed in claim 1, it is characterized in that, in step a, described wood fiber biomass raw material is at least one in agricultural crop straw, wheat bran, bean dregs, bagasse, straw.
3. preparation method as claimed in claim 1, it is characterized in that, in step b, the mass ratio of the quick-fried raw material of described vapour and water is 1:16 ~ 1:8.
4. preparation method as claimed in claim 1, it is characterized in that, in step c, the mass fraction of described glycol water is 70 ~ 90%.
5. preparation method as claimed in claim 1 or 2, it is characterized in that, in step c, the fibre length of described wood fiber biomass raw material is 2 ~ 10mm.
6. the preparation method as described in claim 1 or 5, is characterized in that, in step c, the volume ratio of described filter residue and glycol water is 1:7 ~ 1:10.
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Cited By (19)
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| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
| CN106149433A (en) * | 2016-06-24 | 2016-11-23 | 华南理工大学 | Nano-cellulose and preparation method thereof |
| CN106472577A (en) * | 2016-09-30 | 2017-03-08 | 桂林茗兴生物科技有限公司 | Double season Chinese scholartree plantation disease control flushing liquors |
| CN106472576A (en) * | 2016-09-30 | 2017-03-08 | 桂林茗兴生物科技有限公司 | A kind of pair of season Chinese scholartree plantation disease control flushing liquor |
| CN106472578A (en) * | 2016-09-30 | 2017-03-08 | 桂林茗兴生物科技有限公司 | A kind of pair of season Chinese scholartree plantation pest control flushing liquor |
| CN106508901A (en) * | 2016-09-30 | 2017-03-22 | 桂林茗兴生物科技有限公司 | Pest control spray solution for plantation of dual-season sophora japonica |
| CN106690332A (en) * | 2017-01-20 | 2017-05-24 | 成都衔石科技有限公司 | Novel process for preparing dietary fiber by adopting straws |
| CN107345372A (en) * | 2016-05-05 | 2017-11-14 | 中国农业科学院农业环境与可持续发展研究所 | It is a kind of that cellulose nano-fibrous method is prepared based on biomass material |
| CN108350226A (en) * | 2015-11-24 | 2018-07-31 | 因比肯公司 | Include the bituminous composition of lignin |
| CN109024031A (en) * | 2018-10-12 | 2018-12-18 | 山东金胜粮油集团有限公司 | The method that steam blasting combination ultrasonic treatment prepares peanut shell nano-cellulose |
| CN109024036A (en) * | 2018-07-10 | 2018-12-18 | 盐城工学院 | A method of preparing nano-cellulose |
| CN109322201A (en) * | 2018-09-20 | 2019-02-12 | 上海同化新材料科技有限公司 | A kind of cellulose pyrolysis purifying extrusion device and the purification process based on the device |
| CN109338781A (en) * | 2018-10-12 | 2019-02-15 | 山东金胜粮油集团有限公司 | A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose |
| CN109629293A (en) * | 2018-12-28 | 2019-04-16 | 合肥工业大学 | A method of extracting cellulose from bean dregs dietary fiber |
| US10538012B2 (en) | 2015-12-07 | 2020-01-21 | Timothee Boitouzet | Process for partial delignification and filling of a lignocellulosic material, and composite material structure able to be obtained by this process |
| CN110857538A (en) * | 2018-08-22 | 2020-03-03 | 中南大学 | Method for synchronously preparing cellulose crystals and lignin nanoparticles |
| CN113388652A (en) * | 2021-07-07 | 2021-09-14 | 西南林业大学 | Preparation method of green efficient nano-cellulose |
| US11656756B2 (en) | 2018-02-09 | 2023-05-23 | Sas Woodoo | Touch detection device with touch interface made of composite material |
| US11820041B2 (en) | 2017-06-07 | 2023-11-21 | Sas Woodoo | Process for supercritical or subcritical partial delignification and filling of a lignocellulosic material |
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| CN108350226A (en) * | 2015-11-24 | 2018-07-31 | 因比肯公司 | Include the bituminous composition of lignin |
| CN108350226B (en) * | 2015-11-24 | 2021-12-31 | 因比肯公司 | Asphalt composition comprising lignin |
| US11254026B2 (en) | 2015-12-07 | 2022-02-22 | Timothée BOITOUZET | Process for partial delignification and filling of a lignocellulosic material, and composite material structure able to be obtained by this process |
| US10538012B2 (en) | 2015-12-07 | 2020-01-21 | Timothee Boitouzet | Process for partial delignification and filling of a lignocellulosic material, and composite material structure able to be obtained by this process |
| CN105568744A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Cornstalk nanocellulose whiskers and preparation method and application thereof |
| CN107345372B (en) * | 2016-05-05 | 2019-05-28 | 中国农业科学院农业环境与可持续发展研究所 | A method of it is prepared based on biomass material cellulose nano-fibrous |
| CN107345372A (en) * | 2016-05-05 | 2017-11-14 | 中国农业科学院农业环境与可持续发展研究所 | It is a kind of that cellulose nano-fibrous method is prepared based on biomass material |
| CN106149433B (en) * | 2016-06-24 | 2018-08-10 | 华南理工大学 | Nano-cellulose and preparation method thereof |
| CN106149433A (en) * | 2016-06-24 | 2016-11-23 | 华南理工大学 | Nano-cellulose and preparation method thereof |
| CN106472578A (en) * | 2016-09-30 | 2017-03-08 | 桂林茗兴生物科技有限公司 | A kind of pair of season Chinese scholartree plantation pest control flushing liquor |
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| CN106472577A (en) * | 2016-09-30 | 2017-03-08 | 桂林茗兴生物科技有限公司 | Double season Chinese scholartree plantation disease control flushing liquors |
| CN106508901A (en) * | 2016-09-30 | 2017-03-22 | 桂林茗兴生物科技有限公司 | Pest control spray solution for plantation of dual-season sophora japonica |
| CN106690332A (en) * | 2017-01-20 | 2017-05-24 | 成都衔石科技有限公司 | Novel process for preparing dietary fiber by adopting straws |
| US11820041B2 (en) | 2017-06-07 | 2023-11-21 | Sas Woodoo | Process for supercritical or subcritical partial delignification and filling of a lignocellulosic material |
| US11656756B2 (en) | 2018-02-09 | 2023-05-23 | Sas Woodoo | Touch detection device with touch interface made of composite material |
| US11662899B2 (en) | 2018-02-09 | 2023-05-30 | Sas Woodoo | Touch detection device with touch interface made of composite material |
| CN109024036A (en) * | 2018-07-10 | 2018-12-18 | 盐城工学院 | A method of preparing nano-cellulose |
| CN110857538A (en) * | 2018-08-22 | 2020-03-03 | 中南大学 | Method for synchronously preparing cellulose crystals and lignin nanoparticles |
| CN109322201A (en) * | 2018-09-20 | 2019-02-12 | 上海同化新材料科技有限公司 | A kind of cellulose pyrolysis purifying extrusion device and the purification process based on the device |
| CN109338781A (en) * | 2018-10-12 | 2019-02-15 | 山东金胜粮油集团有限公司 | A kind of steam blasting combines the high-pressure homogeneous method for preparing peanut shell nano-cellulose |
| CN109024031A (en) * | 2018-10-12 | 2018-12-18 | 山东金胜粮油集团有限公司 | The method that steam blasting combination ultrasonic treatment prepares peanut shell nano-cellulose |
| CN109629293A (en) * | 2018-12-28 | 2019-04-16 | 合肥工业大学 | A method of extracting cellulose from bean dregs dietary fiber |
| CN113388652A (en) * | 2021-07-07 | 2021-09-14 | 西南林业大学 | Preparation method of green efficient nano-cellulose |
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Application publication date: 20150527 |