CN104988779A - Preparation method and application of Salix cheilophila nanocellulose - Google Patents

Preparation method and application of Salix cheilophila nanocellulose Download PDF

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Publication number
CN104988779A
CN104988779A CN201510289609.XA CN201510289609A CN104988779A CN 104988779 A CN104988779 A CN 104988779A CN 201510289609 A CN201510289609 A CN 201510289609A CN 104988779 A CN104988779 A CN 104988779A
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salix monogolica
nano
solution
cellulose
salix
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张克勤
盛卫
董伊航
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Suzhou Best Color Nano Technology Co Ltd
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Suzhou Best Color Nano Technology Co Ltd
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00Pretreatment of the finely-divided materials before digesting
    • D21C1/04Pretreatment of the finely-divided materials before digesting with acid reacting compounds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/04Pulping cellulose-containing materials with acids, acid salts or acid anhydrides
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-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
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-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
    • D21C9/02Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-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
    • D21C9/10Bleaching ; Apparatus therefor
    • D21C9/16Bleaching ; Apparatus therefor with per compounds

Abstract

The invention relates to the field of nanofiber materials, especially to a preparation method and application of a Salix cheilophila nanocellulose. The method comprises the steps of: (1) treating Salix cheilophila peel in an acid solution, controlling the bath ratio at 1:20-25 and the temperature at 80-110DEG C, performing stirring for 1h, after treatment, washing, drying and crushing the Salix cheilophila peel to obtain Salix cheilophila microcrystalline cellulose; and (2) placing the Salix cheilophila microcrystalline cellulose obtained in step (1) into an acid solution with a mass percent content of 55-65% to conduct treatment, controlling the bath ratio at 1:10-20, conducting stirring for 30-90min at 40-60DEG C, at the end of the treatment, diluting the solution by 10 times, and conducting centrifugation, dialysis and ultrasonic treatment to obtain the Salix cheilophila nanocellulose. According to the invention, the raw materials have abundant sources and are cheap in price, and the preparation process has the characteristics of simple operation and low cost.

Description

The preparation method of salix monogolica nano-cellulose and application thereof
Technical field
The present invention relates to nano-fiber material field, particularly relate to a kind of preparation method and application thereof of salix monogolica nano-cellulose.
Background technology
Cellulose, as the most general organic compound of nature, is considered to inexhaustible raw material, the chemical property superior due to it and biocompatibility, has been widely used in many fields.The micro-dimension cellulose of receiving extracted from natural plants not only has cellulosic basic structure and performance, also has the advantage of many uniquenesses: draw ratio is large, the specific area of super large, high-crystallinity, low-density, higher Young's modulus and TENSILE STRENGTH etc., and be widely used potentiality.
The main raw material of current production of cellulose is cotton and wood pulps, and cost is higher.And salix monogolica is the common desert shrub in NORTHWEST CHINA area, its content of cellulose is up to 48%, and lignin, hemicellulose are lower, extract its cellulose, Appropriate application biomass resource, huge economy, ecological benefits will be produced, utilize salix monogolica to extract cellulosic method mainly enzymatic isolation method and Mechanical Method at present, enzymatic isolation method process be complicated, high, the consuming time length of cost and expensive, Mechanical Method is high to equipment requirement, energy consumption is comparatively large, and obtained nano-cellulose domain size distribution is wider.
Because above-mentioned Problems existing, the present invention uses a kind of new method to carry out the preparation of salix monogolica nano-cellulose, more convenient, from natural plants, obtain nano-cellulose efficiently.This method may have the value in industry.
Summary of the invention
The invention provides a kind of preparation method and application thereof of salix monogolica nano-cellulose, adopt acid-hydrolyzed method to prepare salix monogolica nano-cellulose, salix monogolica abundant raw material is easy to get, and preparation process is simple to operate, with low cost.
The present invention proposes a kind of preparation method of salix monogolica nano-cellulose, comprises the following steps:
(1) salix monogolica skin is placed in acid solution to process, bath raio is 1:20-25, temperature 80-110 DEG C, stirs 1h, salix monogolica skin clean dry is pulverized, obtain salix monogolica microcrystalline cellulose after process;
(2) the salix monogolica microcrystalline cellulose obtained in described step (1) being placed in mass percentage is that the acid solution of 55-65% processes; bath raio is 1:10-20; at 40-60 DEG C of temperature, stir 30-90min; by solution dilution 10 times after being disposed, and obtains salix monogolica nano-cellulose through centrifugal, dialysis and ultrasonic process.
Further, in described step (1), acid solution is the mixed liquor of a kind of and ethanol in-nitric acid, hydrochloric acid, sulfuric acid, and acid is 1:4-9 with the volume ratio of ethanol, and in described step (2), acid solution is sulfuric acid or hydrochloric acid solution.
Further, in described step (1), the bath raio of salix monogolica skin and nitric acid/ethanolic solution is 1:25, temperature is 100 DEG C, the volume ratio of nitric acid and ethanol is 1:4, in described step (2), the sulfuric acid mass percentage of sulfuric acid solution is 64%, reaction temperature is 45 DEG C, and mixing time is 60min.
Further, salix monogolica skin is before the acid treatment in described step (1), also through preliminary treatment, come unstuck and bleaching.
Further, described preliminary treatment comprises the following steps:
A, salix monogolica branch is dried rear pulverizing, be then placed in warm water and soak 24h, clean post-drying, obtain salix monogolica drying sample;
B, the salix monogolica drying sample obtained in described steps A is placed in the acetic acid solution of 7g/L, at 50 DEG C of Water Unders bath 1h, bath raio is 1:15, and clear water is cleaned subsequently, dries.
Further, come unstuck described in and comprise the following steps:
A, first time soda boiling: will be placed in the NaOH solution of 15-25g/L through pretreated salix monogolica skin, bath raio is 1:10-1:30, and the soda boiling time is 90-210min, and temperature is 90-120 DEG C.
B, second time soda boiling: the NaOH solution salix monogolica skin through first time soda boiling being placed in 15-25g/L, containing mass percentage in solution is 0.1-0.2% anthraquinone and/or 5-10% tertiary sodium phosphate, and bath raio is 1:10-1:30, at 120 DEG C of insulation 3.5h.
Further, in described steps A, the concentration of NaOH is 20g/L, and bath raio is 1:15, and temperature is 110 DEG C, and the time is 150min, and in described step B, the concentration of NaOH is 20g/L, and containing mass percentage in solution is the anthraquinone of 0.1%, and bath raio is 1:15.
Further, described bleaching comprises the following steps:
Salix monogolica skin through coming unstuck is placed in liquid lime chloride, and described liquid lime chloride comprises the component of following mass percentage: 10-30%H 2o 2, 0.5%EDTA, 0.5%MgSO 4and the NaOH of 5-30g/L, bath raio are 1:15, temperature is 60-100 DEG C, and the time is 60-90min.
Further, the process of described bleaching repeats twice.
Present invention also offers a kind of application of salix monogolica nano-cellulose, will add in silk fibroin protein solution after above-mentioned salix monogolica nano-cellulose wiring solution-forming, air-dry film forming.
By such scheme, the present invention at least has the following advantages: the raw material that the present invention uses salix monogolica to prepare as nano-cellulose, the wide material sources of salix monogolica and cheap, greatly can save production cost, use acid-hydrolyzed method to prepare nano-cellulose, this process is simple, and the properties of product obtained are excellent.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of description, below with preferred embodiment of the present invention, and coordinate accompanying drawing to be described in detail as follows.
Accompanying drawing explanation
Fig. 1 is the grain size distribution of salix monogolica nano-cellulose in the embodiment of the present invention one;
Fig. 2 is the AFM figure of salix monogolica nano-cellulose in the embodiment of the present invention one;
Fig. 3 is the AFM figure of salix monogolica nano-cellulose in the embodiment of the present invention one;
Fig. 4 is the scanning electron microscope (SEM) photograph of salix monogolica nano-cellulose in the embodiment of the present invention one;
Fig. 5 is the light transmittance figure of fibroin protein film and composite membrane in the embodiment of the present invention four.
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment one:
1) preliminary treatment:
Salix monogolica branch is dried.First, salix monogolica branch is pulverized, remove flaw, in warm water, soak twenty four hours, clean, dry for standby.Then dry sample is put into 7g/L acetic acid solution at 50 DEG C of Water Under bath 1h, bath raio is 1:15, carries out sour prehydrolysis.Rinse with a large amount of clear water subsequently, dry.
2) degumming process:
First time soda boiling: time 150min, temperature 110 DEG C, NaOH concentration 20g/L, bath raio is 1:15;
Second time soda boiling: temperature 120 DEG C, time 3.5h, anthraquinone 0.1wt% (mass percentage), NaOH concentration 20g/L, bath raio is 1:15.
3) bleaching:
Add in liquid lime chloride by the salix monogolica skin after degumming process, the component of liquid lime chloride is: 30wt%H 2o 2, 5g/L NaOH, time 60min, temperature 90 DEG C, 0.5wt% ethylenediamine tetra-acetic acid (EDTA), 0.5wt%MgSO 4, bath raio is 1:15, repeats bleaching twice.4) salix monogolica microcrystalline cellulose is prepared:
Salix monogolica skin after bleaching and the nitric acid/ethanolic solution prepared are added thermal agitation 1h 80 DEG C of oil baths, nitric acid and ethanol contend are than being 1:4; bath raio is 1:20; react rear nitric acid and ethanol washing; in other embodiments, the acid solution in this step also can be hydrochloric acid or sulfuric acid, then extremely close neutral with hot wash; finally to use absolute ethanol washing twice, drain filtrate.Finally obtain microcrystalline cellulose by after dried sample comminution process, efficiency of pcr product 68% under this condition, average length is that 46 ± 15 μm of its width are at about 10 μm.
5) salix monogolica nano-cellulose is prepared:
Preparation 64wt% sulfuric acid is for subsequent use, joins in the 64wt% concentrated sulfuric acid by salix monogolica microcrystalline cellulose according to the bath raio of 1:10, and high speed magnetic stirring reaction 1h under 45 DEG C of water bath condition, in other embodiments, the acid solution in this step also can be hydrochloric acid.After reaction, add the deionized water dilution of 10 times, stop heating, leave standstill cooling, obtain oyster white nano whisker suspension.By aaerosol solution centrifugal treating, centrifuge washing ten minutes under 10000rpm speed, removes supernatant liquor, repeatedly centrifugal until upper solution variable color.Taken out on upper strata, put into bag filter deionized water and dialyse three days, molecular cut off is 8000-14000Da, until pH ~ 7.0.Solution after dialysis under putting into supersonic wave cleaning machine cold bath ultrasonic 30 minutes, makes nano whisker disperse.Finally obtain salix monogolica nano-cellulose suspension.
The salix monogolica nano-cellulose suspension blueing light obtained, after leaving standstill a period of time, solution is constant, and layering, precipitation do not occur, and obtained salix monogolica nano-cellulose suspension is highly stable.
Fig. 1 to 4 can find out, the salix monogolica nano-cellulose average length obtained is 274 ± 60nm, the distribution of lengths of the nano micro crystal cellulose of 80% concentrates between 200-400nm, and its width is between 10-50nm, has larger draw ratio (>5.0).
Embodiment two:
1) preliminary treatment:
Salix monogolica branch is dried.First, salix monogolica branch is pulverized, remove flaw, in warm water, soak twenty four hours, clean, dry for standby.Then dry sample is put into 7g/L acetic acid solution at 50 DEG C of Water Under bath 1h, bath raio is 1:15, carries out sour prehydrolysis.Rinse with a large amount of clear water subsequently, dry.
2) degumming process:
First time soda boiling: time 210min, temperature 90 DEG C, NaOH concentration 15g/L, bath raio is 1:10;
Second time soda boiling: temperature 120 DEG C, time 3.5h, anthraquinone 0.2wt% (mass percentage), tertiary sodium phosphate 5wt%, NaOH concentration 15g/L, bath raio is 1:10.
3) bleaching:
Add in liquid lime chloride by the salix monogolica skin after degumming process, the component of liquid lime chloride is: 10wt%H 2o 2, 15g/L NaOH, time 90min, temperature 60 C, 0.5wt% ethylenediamine tetra-acetic acid (EDTA), 0.5wt%MgSO 4, bath raio is 1:15, repeats bleaching twice.
4) salix monogolica microcrystalline cellulose is prepared:
Salix monogolica skin after bleaching and the nitric acid/ethanolic solution prepared are added thermal agitation 1h 80 DEG C of oil baths, nitric acid and ethanol contend are than being 1:5; bath raio is 1:20; react rear nitric acid and ethanol washing; then extremely neutral with hot wash; finally to use absolute ethanol washing twice, drain filtrate, repeat acid treatment constant to solution filtrate color.Finally obtain microcrystalline cellulose by after dried sample comminution process, efficiency of pcr product 74% under this condition, average length is 73 ± 32 μm, and width is at about 10 μm.
5) salix monogolica nano-cellulose is prepared:
Preparation 55wt% sulfuric acid is for subsequent use, joins in the 64wt% concentrated sulfuric acid by salix monogolica microcrystalline cellulose according to the bath raio of 1:15, high speed magnetic stirring reaction 30min under 60 DEG C of water bath condition.After reaction, add the deionized water dilution of 10 times, stop heating, leave standstill cooling, obtain oyster white nano whisker suspension.By aaerosol solution centrifugal treating, centrifuge washing ten minutes under 10000rpm speed, removes supernatant liquor, repeatedly centrifugal until upper solution variable color.Taken out on upper strata, put into bag filter deionized water and dialyse three days, molecular cut off is 8000-14000, until pH is neutral.Solution after dialysis under putting into supersonic wave cleaning machine cold bath ultrasonic 30 minutes, makes nano whisker disperse.Finally obtain salix monogolica nano-cellulose suspension.
The salix monogolica nano-cellulose average length obtained is 450 ± 90nm, and its width is between 50-100nm, has larger draw ratio.
Embodiment three:
1) preliminary treatment:
Salix monogolica branch is dried.First, salix monogolica branch is pulverized, remove hard object impurity, in warm water, soak twenty four hours, clean, dry for standby.Then dry sample is put into 7g/L acetic acid solution at 50 DEG C of Water Under bath 1h, bath raio is 1:15, carries out sour prehydrolysis.Use a large amount of deionized water rinsing subsequently, dry.
2) degumming process:
First time soda boiling: time 90min, temperature 120 DEG C, NaOH concentration 25g/L, bath raio is 1:30;
Second time soda boiling: temperature 120 DEG C, time 3.5h, anthraquinone 0.2wt% (mass percentage), NaOH concentration 25g/L, bath raio is 1:30.
3) bleaching:
Add in liquid lime chloride by the salix monogolica skin after degumming process, the component of liquid lime chloride is: 20wt%H 2o 2, 30g/L NaOH, time 70min, temperature 100 DEG C, 0.5wt% ethylenediamine tetra-acetic acid (EDTA), 0.5wt%MgSO 4, bath raio is 1:15, repeats bleaching twice.
4) salix monogolica microcrystalline cellulose is prepared:
Salix monogolica skin after bleaching and the nitric acid/ethanolic solution prepared are added thermal agitation 1h 80 DEG C of oil baths, nitric acid and ethanol contend are than being 1:4; bath raio is 1:20; react rear nitric acid and ethanol washing, in other embodiments, the acid solution in this step also can be hydrochloric acid or sulfuric acid; then extremely neutral with hot wash; finally to use absolute ethanol washing twice, drain filtrate, repeat acid treatment constant to filtrate color.Finally obtain microcrystalline cellulose by after dried sample comminution process, efficiency of pcr product 79% under this condition, average length is 95 ± 45 μm, and its width is at about 10 μm.
5) salix monogolica nano-cellulose is prepared:
Preparation 60wt% sulfuric acid is for subsequent use, joins in the 60wt% concentrated sulfuric acid by salix monogolica microcrystalline cellulose according to the bath raio of 1:20, and high speed magnetic stirring reaction 90min under 40 DEG C of water bath condition, in other embodiments, the acid solution in this step also can be hydrochloric acid.After reaction, add the deionized water dilution of 10 times, stop heating, leave standstill cooling, obtain oyster white nano whisker suspension.By aaerosol solution centrifugal treating, centrifuge washing ten minutes under 10000rpm speed, removes supernatant liquor, repeatedly centrifugal until upper solution variable color.Taken out on upper strata, put into bag filter deionized water and dialyse three days, molecular cut off is 8000-14000Da, until pH is neutral.Solution after dialysis under putting into supersonic wave cleaning machine cold bath ultrasonic 30 minutes, makes nano whisker disperse.Finally obtain salix monogolica nano-cellulose suspension.
The salix monogolica nano-cellulose average length obtained is 195 ± 21nm, and its width is between 10-50nm, has larger draw ratio.
Embodiment four:
Salix monogolica nanofiber is applied to silk fibroin protein solution:
Silk fibroin protein solution must be mixed by solution with the Cellulose nanocrystal prepared in embodiment one, wherein the mass ratio of fibroin albumen and nano-cellulose is 4:1, mixed solution is film forming after air-dry, comparing of performance is carried out with the film of the air-dry rear formation of silk fibroin protein solution, as can be drawn from Table 1, the ultimate strength adding the silk fibroin composite membrane of the salix monogolica nano-cellulose of 20wt% is 1.58 times of fibroin protein film, extension at break is 2.22 times of fibroin protein film, have and strengthen effect significantly, as can be seen from Figure 5, the light transmittance of fibroin protein film is approximately 92%, the light transmittance adding the silk fibroin composite membrane of 20wt% salix monogolica nano-cellulose is 86%, find out thus, add the light transmittance on fibroin protein film of nano-cellulose almost without impact, still there is very high light transmission.
Table 1 fibroin protein film compares with composite membrane performance
Ultimate strength (CN) Extension at break (%)
Fibroin protein film 2558.8 2.67
Composite membrane 4043.1 5.93
In sum, the present invention uses acid-hydrolyzed method to prepare salix monogolica nano-cellulose, simple to operate, and it is with low cost, the nano-cellulose draw ratio obtained is high, the suspension stable in properties be configured to, be applied to the preparation of silk fibroin composite membrane, strengthen fibroin albumen film strength, in addition, can also by freezing in-80 DEG C after its wiring solution-forming, cellulose aerogels is made after freeze drying, or add in poly-vinyl alcohol solution by after its wiring solution-forming, obtained biological tissue support after freeze drying, being widely used of the salix monogolica nano-cellulose that the present invention prepares, function admirable.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.

Claims (10)

1. a preparation method for salix monogolica nano-cellulose, is characterized in that: comprise the following steps:
(1) salix monogolica skin is placed in acid solution to process, bath raio is 1:20-25, temperature 80-110 DEG C, stirs 1h, salix monogolica skin clean dry is pulverized, obtain salix monogolica microcrystalline cellulose after process;
(2) the salix monogolica microcrystalline cellulose obtained in described step (1) being placed in mass percentage is that the acid solution of 55-65% processes; bath raio is 1:10-20; at 40-60 DEG C of temperature, stir 30-90min; by solution dilution 10 times after being disposed, and obtains salix monogolica nano-cellulose through centrifugal, dialysis and ultrasonic process.
2. the preparation method of salix monogolica nano-cellulose according to claim 1, it is characterized in that: in described step (1), acid solution is the mixed liquor of a kind of and ethanol in nitric acid, hydrochloric acid or sulfuric acid, acid is 1:4-9 with the volume ratio of ethanol, and in described step (2), acid solution is sulfuric acid or hydrochloric acid solution.
3. the preparation method of salix monogolica nano-cellulose according to claim 2, it is characterized in that: in described step (1), the bath raio of salix monogolica skin and nitric acid/ethanolic solution is 1:25, temperature is 100 DEG C, the volume ratio of nitric acid and ethanol is 1:4, in described step (2), the sulfuric acid mass percentage of sulfuric acid solution is 64%, reaction temperature is 45 DEG C, and mixing time is 60min.
4. the preparation method of salix monogolica nano-cellulose according to claim 1, is characterized in that: salix monogolica skin is before the acid treatment in described step (1), also through preliminary treatment, come unstuck and bleaching.
5. the preparation method of salix monogolica nano-cellulose according to claim 4, is characterized in that: described preliminary treatment comprises the following steps:
A, salix monogolica branch is dried rear pulverizing, be then placed in warm water and soak 24h, clean post-drying, obtain salix monogolica drying sample;
B, the salix monogolica drying sample obtained in described steps A is placed in the acetic acid solution of 7g/L, at 50 DEG C of Water Unders bath 1h, bath raio is 1:15, and clear water is cleaned subsequently, dries.
6. the preparation method of salix monogolica nano-cellulose according to claim 5, is characterized in that: described in come unstuck and comprise the following steps:
A, first time soda boiling: will be placed in the NaOH solution of 15-25g/L through pretreated salix monogolica skin, bath raio is 1:10-1:30, and the soda boiling time is 90-210min, and temperature is 90-120 DEG C.
B, second time soda boiling: the NaOH solution salix monogolica skin through first time soda boiling being placed in 15-25g/L, containing mass percentage in solution is 0.1-0.2% anthraquinone and/or 5-10% tertiary sodium phosphate, and bath raio is 1:10-1:30, at 120 DEG C of insulation 3.5h.
7. the preparation method of salix monogolica nano-cellulose according to claim 6, it is characterized in that: in described steps A, the concentration of NaOH is 20g/L; bath raio is 1:15; temperature is 110 DEG C; the time is 150min; in described step B, the concentration of NaOH is 20g/L, containing mass percentage in solution is the anthraquinone of 0.1%, and bath raio is 1:15.
8. the preparation method of salix monogolica nano-cellulose according to claim 7, is characterized in that: described bleaching comprises the following steps:
Salix monogolica skin through coming unstuck is placed in liquid lime chloride, and described liquid lime chloride comprises the component of following mass percentage: 10-30%H 2o 2, 0.5%EDTA, 0.5%MgSO 4and the NaOH of 5-30g/L, bath raio are 1:15, temperature is 60-100 DEG C, and the time is 60-90min.
9. the preparation method of salix monogolica nano-cellulose according to claim 8, is characterized in that: the process of described bleaching repeats twice.
10. an application for salix monogolica nano-cellulose, is characterized in that: add in silk fibroin protein solution by claim 1-9 after salix monogolica nano-cellulose wiring solution-forming described in any one, air-dry film forming.
CN201510289609.XA 2015-06-01 2015-06-01 Preparation method and application of Salix cheilophila nanocellulose Pending CN104988779A (en)

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CN106749687A (en) * 2016-12-23 2017-05-31 盐城工业职业技术学院 A kind of preparation method of ramulus mori bark nano cellulose whisker
CN113136093A (en) * 2021-05-13 2021-07-20 广西安全工程职业技术学院 Preparation method of reinforced polybutylene terephthalate material
CN115119678A (en) * 2022-06-27 2022-09-30 榆林市林业科学研究所 Pinus sylvestris forestation method

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CN104448007A (en) * 2014-11-14 2015-03-25 中国科学院青岛生物能源与过程研究所 Method for preparing nano-cellulose

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CN113136093A (en) * 2021-05-13 2021-07-20 广西安全工程职业技术学院 Preparation method of reinforced polybutylene terephthalate material
CN115119678A (en) * 2022-06-27 2022-09-30 榆林市林业科学研究所 Pinus sylvestris forestation method

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Application publication date: 20151021