CN116856188A - Method for preparing cellulose fiber from camellia oleifera and typha and prepared cellulose fiber - Google Patents
Method for preparing cellulose fiber from camellia oleifera and typha and prepared cellulose fiber Download PDFInfo
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- CN116856188A CN116856188A CN202310852480.3A CN202310852480A CN116856188A CN 116856188 A CN116856188 A CN 116856188A CN 202310852480 A CN202310852480 A CN 202310852480A CN 116856188 A CN116856188 A CN 116856188A
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 36
- 241000526900 Camellia oleifera Species 0.000 title claims abstract description 30
- 241000233948 Typha Species 0.000 title claims description 17
- 238000005406 washing Methods 0.000 claims abstract description 45
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000835 fiber Substances 0.000 claims abstract description 19
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 238000004061 bleaching Methods 0.000 claims abstract description 11
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 230000007935 neutral effect Effects 0.000 claims description 17
- 229920002678 cellulose Polymers 0.000 claims description 13
- 239000001913 cellulose Substances 0.000 claims description 13
- 241001122767 Theaceae Species 0.000 claims description 11
- 239000010779 crude oil Substances 0.000 claims description 9
- 229920005610 lignin Polymers 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- NWIPPCMREQXKRU-UHFFFAOYSA-N ethanol nitrate Chemical compound CCO.[O-][N+]([O-])=O NWIPPCMREQXKRU-UHFFFAOYSA-N 0.000 claims description 2
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 240000001398 Typha domingensis Species 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000001914 filtration Methods 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 4
- 240000003553 Leptospermum scoparium Species 0.000 description 4
- 235000015459 Lycium barbarum Nutrition 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000000703 high-speed centrifugation Methods 0.000 description 4
- 238000010297 mechanical methods and process Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 238000000265 homogenisation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/16—Bleaching ; Apparatus therefor with per compounds
- D21C9/163—Bleaching ; Apparatus therefor with per compounds with peroxides
Abstract
The application relates to a method for preparing cellulose fibers from camellia oleifera and the prepared cellulose fibers, and belongs to the technical field of nano material preparation. The method takes camellia oleifera as a raw material, removes hemicellulose and impurities through acid washing and alkali washing, obtains crude fibers through bleaching, and obtains cellulose fibers through sulfuric acid hydrolysis, centrifugation and dispersion. The cellulose fiber prepared by the application has high length-diameter ratio, and the length-diameter ratio is 50-100; the device is in a network structure, has uniform size distribution and is beneficial to subsequent industrial utilization. The preparation method eliminates a large-sized instrument, and adopts a mode with smaller energy consumption to discard and utilize the camellia oleifera cattail.
Description
Technical Field
The application relates to the technical field of nano material preparation, in particular to a method for preparing cellulose fibers from camellia oleifera and the prepared cellulose fibers.
Background
The camellia oleifera is a part wrapping the camellia oleifera fruits, the whole fruits occupy 25%, the camellia oleifera fruits mainly comprise cellulose, tea saponin, lignin and hemicellulose, the cellulose content is about 15.5%, and biomass resources are enriched. In the comprehensive utilization of the biomass resources of the camellia oleifera and the typha oleifera, the contained cellulose resources can be further developed into cellulose fibers, and the prepared cellulose fibers are paid attention to because of the unique advantages of high mechanical strength, high length-diameter ratio, degradability, biocompatibility and the like.
The preparation of cellulose fiber can be mainly divided into chemical method and mechanical method, and common mechanical methods include high-pressure homogenization, micro-jet, grinding, ultrasonic wave, freezing and crushing, PFI beating, steam explosion, high-pressure fluid and the like, but the single method has low impurity treatment efficiency, and the mechanical method has high requirement on instruments and high cost requirement. The chemical method comprises acid hydrolysis, alkali hydrolysis, TEMPO oxidation, ionic liquid dissolution and other methods, so as to remove impurities hemicellulose, lignin and the like, and oxidize surface groups to weaken intermolecular hydrogen bonds to prepare cellulose.
Chinese patent No. 113004426A discloses a method for preparing cellulose nanocrystals and cellulose nanofibers simultaneously from camellia oleifera, which comprises hydrolyzing crude fibers with hydrochloric acid and sulfuric acid, centrifuging, wherein the upper layer is cellulose nanocrystal suspension, and the lower layer is cellulose nanofiber suspension obtained by high-pressure homogenization treatment. The method introduces chloride ions in the process, has great influence on environmental pollution, and has high instrument requirement and energy consumption requirement by utilizing high-pressure homogenization treatment.
Disclosure of Invention
In order to overcome the defects of the prior art, the application provides a method for preparing cellulose fibers from camellia oleifera and the prepared cellulose fibers, wherein the method is used for extracting cellulose from the camellia oleifera, preparing the cellulose fibers by combining a chemical method and a mechanical method, performing centrifugal ultrasonic treatment after sulfuric acid hydrolysis, and the method has the advantages of simple and low-cost used instruments, low energy consumption and capability of avoiding larger pollution in reagents to obtain chlorine-containing reagents. The technical proposal is as follows:
a method for preparing cellulose fiber from camellia oleifera is characterized in that camellia oleifera is used as a raw material, semi-fiber and impurities are removed through acid washing and alkali washing, crude fiber is obtained through bleaching, and cellulose fiber is obtained through sulfuric acid hydrolysis, centrifugation and dispersion.
Further, the method specifically comprises the following steps:
s1, mechanical treatment: cleaning and drying the camellia oleifera and the cattail, pulverizing into 100 meshes, and sieving to remove large particles and impurities;
s2, acid washing: adding the powder obtained in the step S1 into a nitric acid-ethanol mixed solution, heating and stirring to react, removing hemicellulose and lignin, washing filter residues with water to be neutral, and drying;
s3, alkali washing: taking filter residues obtained in the step S2, adding NaOH solution, heating and stirring to react, removing hemicellulose, and water
Washing the filter residue to neutrality and drying;
s4, bleaching: adding hydrogen peroxide solution into the filter residue obtained in the step S3, removing lignin after heating reaction, washing the filter residue to be neutral and drying to obtain crude oil tea tree seed-tail fibers;
s5, sulfuric acid hydrolysis: dispersing the crude fiber obtained in the step S4 into H2SO4 solution, heating for reaction, and adding deionized water to terminate the reaction to obtain acidolysis material;
s6, centrifuging: transferring the acidolysis material obtained in the step S5 to a centrifuge tube, and centrifugally washing with water for several times until the material is neutral to obtain a lower layer material;
s7, dispersing: and (3) dispersing the lower-layer material after centrifugation in the step (S6) into deionized water, and carrying out ultrasonic treatment by using a cell disruption instrument to prepare the cellulose fiber suspension.
Preferably, in the pickling process of step S2, the mass ratio of the filter residue to the ethanol nitrate solution is 1:10 to 20, heating to 60 to 80 ℃, heating and stirring for 120 to 240min, and drying filter residues at 50 to 70 ℃.
In the pickling step, lignin in the camellia oleifera is nitrified and oxidized, the generated nitrified lignin and oxidized lignin are soluble in an ethanol solution, hemicellulose is hydrolyzed and oxidized and is also soluble in the ethanol solution, a cellulose product is left, and hydrolysis and oxidation of nitric acid on cellulose are reduced by adopting an ethanol medium.
Preferably, in the alkaline washing process of the step S3, the mass fraction of the NaOH solution is 2-5%, the mass ratio of the filter residue to the NaOH solution is 1:10-20, the filter residue is heated to 80-95 ℃, the filter residue is heated and stirred for 120-180 min, and the drying temperature of the filter residue is 50-70 ℃.
Preferably, in the bleaching in the step S4, H 2 O 2 The mass fraction of the solution is 2-5%, and the filter residue and H 2 O 2 The mass ratio of the solution is 1:20-30, the solution is heated to 40-60 ℃, and simultaneously stirred for 3-6 hours, and the drying temperature of the crude fiber is 50-70 ℃.
Preferably, in the sulfuric acid hydrolysis of the step S5, H 2 SO 4 The mass fraction of the solution is 45-60%, and the crude cellulose and H 2 SO 4 The mass ratio of the solution is 1:10-20, heating to 40-60 ℃, stirring for 30-120 min, and adding at least 10 times of deionized water to terminate the reaction.
Preferably, in the step S6, a centrifugal machine is adopted for centrifugal treatment, and the rotation speed of the centrifugal machine is 7000-10000 r/min.
Preferably, in the dispersing process of the step S7, the ultrasonic power is 360-720W, and the ultrasonic time is 15-30 min.
The cellulose fiber prepared by the method has the width of 180-600 nanometers, the length of 8-13 micrometers and the length-diameter ratio of 50-100.
Compared with the prior art, the application has the following beneficial effects:
the preparation process eliminates larger instruments, adopts a mode of lower energy consumption to discard and utilize the camellia oleifera cattail, and has higher economic and practical values.
The cellulose fiber prepared by the application has high length-diameter ratio, width of 180-600 nanometers, length of 8-13 micrometers and length-diameter ratio of 50-100, and can be seen to be in a network structure, and uniform in size distribution, thereby being beneficial to subsequent industrial utilization. The produced cellulose fiber has good biodegradability, biocompatibility and mechanical property, and can be used as a reinforcing material in the fields of biological medicine, paper and food packaging.
Drawings
Fig. 1 is an SEM image of the cellulose fiber prepared in example 1 of the present application.
Detailed Description
The process scheme of the application is described in further detail below with reference to the accompanying drawings and specific examples.
Example 1
A method for preparing cellulose fiber from camellia oleifera abel cattail comprises the following specific steps:
s1, mechanical treatment: taking 20g of camellia oleifera and crushing, and sieving with a 100-mesh sieve;
s2, acid washing: taking 20g of the oil tea Pu Fenmo obtained in the step S1, adding 200mL of a nitric acid/ethanol=1:2 mixed solution, heating to 60 ℃ in a water bath, stirring for 2 hours at the same time, filtering after the reaction is finished, washing filter residues with deionized water, washing the filter residues to be neutral, and drying at 50 ℃;
s3, alkali washing: taking 10g of filter residue obtained in the step S2, adding 100mL of 2% NaOH solution, heating to 80 ℃ in a water bath, stirring for 2 hours at the same time, filtering after the reaction is finished, washing the filter residue to be neutral, and drying at 50 ℃;
s4, bleaching: taking 5g of filter residue obtained in the step S3, adding 100mL of 2% H 2 O 2 Heating the solution to 40 ℃ in a water bath, stirring for 3 hours, filtering after the reaction is finished, washing filter residues to be neutral, and drying at 50 ℃ to obtain crude oil tea tree seed-tail fibers;
s5, sulfuric acid hydrolysis: 20mL of 45% H 2 SO 4 Heating the solution to 40 ℃ in a water bath, preheating for 15min, adding 2g of crude oil tea cattail fiber obtained in the step S4, stirring at a high speed for 30min, and adding 10 times of deionized water to terminate the reaction;
s6, centrifuging: transferring the acidolysis material obtained in the step S5 to a centrifuge tube, centrifuging for 5min at 7000r/min, removing supernatant, and washing the lower-layer material for several times to neutrality;
s7, dispersing: dispersing the lower-layer material after high-speed centrifugation in the step S6 into a proper amount of deionized water, treating by a cell disruption instrument, and obtaining the cellulose fiber suspension, wherein the ultrasonic power is 360W and the ultrasonic time is 15 min.
Example 2
A method for preparing cellulose fiber from camellia oleifera abel cattail comprises the following specific steps:
s1, mechanical treatment: taking 20g of camellia oleifera and crushing, and sieving with a 100-mesh sieve;
s2, acid washing: taking 20g of the oil tea Pu Fenmo obtained in the step S1, adding 300mL of a nitric acid/ethanol=1:4 mixed solution, heating to 70 ℃ in a water bath, stirring for 3 hours at the same time, filtering after the reaction is finished, washing filter residues with deionized water, washing the filter residues to be neutral, and drying at 60 ℃;
s3, alkali washing: taking 10g of filter residue obtained in the step S2, adding 200mL of 4% NaOH solution, heating to 90 ℃ in a water bath, stirring for 2.5h, filtering after the reaction is finished, washing the filter residue to be neutral, and drying at 60 ℃;
s4, bleaching: taking 5g of filter residue obtained in the step S3, adding 125mL of 3%H 2 O 2 Heating the solution to 50 ℃ in a water bath, stirring for 4 hours, filtering after the reaction is finished, washing filter residues to be neutral, and drying at 60 ℃ to obtain crude oil tea tree seed-tail fibers;
s5, sulfuric acid hydrolysis: 30mL of 50% H 2 SO 4 Heating the solution to 50 ℃ in a water bath, preheating for 15min, adding 2g of crude oil tea cattail fiber obtained in the step S4, stirring at a high speed for 60min, and adding 10 times of deionized water to terminate the reaction;
s6, centrifuging: transferring the acidolysis material obtained in the step S5 to a centrifuge tube, centrifuging for 5min at 8000r/min, removing supernatant, and washing the lower-layer material for several times to neutrality;
s7, dispersing: dispersing the lower-layer material after high-speed centrifugation in the step S6 into a proper amount of deionized water, treating by a cell disruption instrument, and obtaining the cellulose fiber suspension, wherein the ultrasonic power is 540W and the ultrasonic time is 20 min.
Example 3
A method for preparing cellulose fiber from camellia oleifera abel cattail comprises the following specific steps:
s1, mechanical treatment: taking 20g of camellia oleifera and crushing, and sieving with a 100-mesh sieve;
s2, acid washing: taking 20g of the oil tea Pu Fenmo obtained in the step S1, adding 400mL of a nitric acid/ethanol=1:6 mixed solution, heating to 80 ℃ in a water bath, stirring for 4 hours at the same time, filtering after the reaction is finished, washing filter residues with deionized water, washing the filter residues to be neutral, and drying at 70 ℃;
s3, alkali washing: taking 10g of filter residue obtained in the step S2, adding 300mL of 2% NaOH solution, heating to 80 ℃ in a water bath, stirring for 2 hours at the same time, filtering after the reaction is finished, washing the filter residue to be neutral, and drying at 50 ℃;
s4, bleaching: taking 5g of filter residue obtained in the step S3, adding 100mL of 2% H 2 O 2 Heating the solution to 40 ℃ in a water bath, stirring for 3 hours, filtering after the reaction is finished, washing filter residues to be neutral, and drying at 50 ℃ to obtain crude oil tea tree seed-tail fibers;
s5, sulfuric acid hydrolysis: 50mL of 45% H 2 SO 4 Heating the solution to 40 ℃ in a water bath, preheating for 15min, adding 2g of crude oil tea cattail fiber obtained in the step S4, stirring at a high speed for 30min, and adding 10 times of deionized water to terminate the reaction;
s6, centrifuging: transferring the acidolysis material obtained in the step S5 to a centrifuge tube, centrifuging for 5min at 7000r/min, removing supernatant, and washing the lower-layer material for several times to neutrality;
s7, dispersing: dispersing the lower-layer material after high-speed centrifugation in the step S6 into a proper amount of deionized water, treating by a cell disruption instrument, and obtaining the cellulose fiber suspension, wherein the ultrasonic power is 360W and the ultrasonic time is 15 min.
Comparative example 1
A method for preparing cellulose fiber from camellia oleifera abel cattail comprises the following specific steps:
s1, mechanical treatment: 10g of camellia oleifera and typha are taken, dried and crushed, and sieved by a 100-mesh sieve;
s2, alkali washing: adding 200mL of 4% NaOH solution into 10g of the oil tea Pu Fenmo obtained in the step S1, heating to 90 ℃ in a water bath, stirring for 2.5h, filtering after the reaction is finished, washing filter residues to be neutral, and drying at 60 ℃;
s3, bleaching: taking 5g of filter residue obtained in the step S2, adding 125mL of 3%H 2 O 2 Heating the solution to 50 ℃ in water bath, stirring for 4 hours, filtering after the reaction is finished, and filtering residuesWashing with water to neutrality, and drying at 60deg.C to obtain crude fiber of Camellia oleifera;
s4, sulfuric acid hydrolysis: 30mL of 50% H 2 SO 4 Heating the solution to 50 ℃ in a water bath, preheating for 15min, adding 2g of crude oil tea cattail fiber obtained in the step S3, stirring at a high speed for 60min, and adding 10 times of deionized water to terminate the reaction;
s5, centrifuging: transferring the acidolysis material obtained in the step S4 to a centrifuge tube, centrifuging for 5min at 8000r/min, removing supernatant, and washing the lower-layer material for several times to neutrality;
s6, dispersing: dispersing the lower-layer material after high-speed centrifugation in the step S5 into a proper amount of deionized water, treating by a cell disruption instrument, and obtaining the cellulose fiber suspension, wherein the ultrasonic power is 540W and the ultrasonic time is 20 min.
SEM spectra of the cellulose fibers prepared in example 1 are shown in fig. 1, and yields and aspect ratios of examples 1 to 3 and comparative example 1 are shown in table 1.
TABLE 1
As can be seen from Table 1, comparative example 1 does not contain an acid washing step, and the resulting cellulose fibers have significantly lower aspect ratios than the examples.
In summary, the protection scope of the present application is not limited to this, and any simple changes or equivalent substitutions of the technical solutions, such as the preparation process of the thickener, the type and amount of the tea cattail, the type and amount of the alkali in the alkalization process, the choice of the swelling mode, such as the equipment used by ultrasound and the ultrasound time, can be obviously obtained by those skilled in the art within the technical scope of the present application.
Claims (9)
1. A method for preparing cellulose fibers from camellia oleifera is characterized by taking camellia oleifera as a raw material, removing hemicellulose and impurities through acid washing and alkali washing, bleaching to obtain crude fibers, and hydrolyzing with sulfuric acid, centrifuging and dispersing to obtain the cellulose fibers.
2. The method according to claim 1, comprising the steps of:
s1, mechanical treatment: cleaning and drying the camellia oleifera and the cattail, pulverizing into 100 meshes, and sieving to remove large particles and impurities;
s2, acid washing: adding the powder obtained in the step S1 into a nitric acid-ethanol mixed solution, heating and stirring to react, removing hemicellulose and lignin, washing filter residues with water to be neutral, and drying;
s3, alkali washing: taking filter residues obtained in the step S2, adding NaOH solution, heating and stirring to react, removing hemicellulose, washing the filter residues to be neutral, and drying;
s4, bleaching: taking filter residues obtained in the step S3, and adding H 2 O 2 Removing lignin after heating the solution, washing filter residues to be neutral and drying to obtain crude oil tea cattail fibers;
s5, sulfuric acid hydrolysis: dispersing the crude fiber obtained in the step S4 into H 2 SO 4 Adding deionized water into the solution to terminate the reaction after the heating reaction, so as to obtain a material after acidolysis;
s6, centrifuging: transferring the acidolysis material obtained in the step S5 to a centrifuge tube, and centrifugally washing with water for several times until the material is neutral to obtain a lower layer material;
s7, dispersing: and (3) dispersing the lower-layer material after centrifugation in the step (S6) into deionized water, and carrying out ultrasonic treatment by using a cell disruption instrument to prepare the cellulose fiber suspension.
3. The method according to claim 2, wherein in the step S2 of pickling, the mass ratio of the filter residue to the ethanol nitrate solution is 1:10-20, the filter residue is heated to 60-80 ℃, the filter residue is heated and stirred for 120-240 min, and the drying temperature of the filter residue is 50-70 ℃.
4. The method according to claim 2, wherein in the alkaline washing process of step S3, the mass fraction of NaOH solution is 2-5%, the mass ratio of the filter residue to NaOH solution is 1:10-20, the filter residue is heated to 80-95 ℃, the filter residue is heated and stirred for 120-180 min, and the drying temperature of the filter residue is 50-70 ℃.
5. The method according to claim 2, wherein in the step S4 bleaching process, H 2 O 2 The mass fraction of the solution is 2-5%, and the filter residue and H 2 O 2 The mass ratio of the solution is 1:20-30, the solution is heated to 40-60 ℃, and simultaneously stirred for 3-6 hours, and the drying temperature of the crude fiber is 50-70 ℃.
6. The method according to claim 2, wherein during the sulfuric acid hydrolysis of step S5, H 2 SO 4 The mass fraction of the solution is 45-60%, and the crude cellulose and H 2 SO 4 The mass ratio of the solution is 1: 10-20, heating to 40-60 ℃, stirring for 30-120 min, and adding at least 10 times of deionized water to terminate the reaction.
7. The method according to claim 2, wherein in the step S6 of centrifuging, a centrifuge is used for centrifuging, and the rotational speed of the centrifuge is 7000 to 10000r/min.
8. The method according to claim 2, wherein the ultrasonic power is 360-720W and the ultrasonic time is 15-30 min during the dispersion in step S7.
9. A cellulose fiber produced according to any one of claims 1 to 8, wherein the cellulose fiber has an aspect ratio of 50 to 100.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000061858A1 (en) * | 1999-04-12 | 2000-10-19 | Rhodia Acetow Gmbh | Method for separating lignocellulose-containing biomass |
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