CN103074794A - Method for preparing cellulose nanoparticles from waste cotton wool - Google Patents
Method for preparing cellulose nanoparticles from waste cotton wool Download PDFInfo
- Publication number
- CN103074794A CN103074794A CN2013100446605A CN201310044660A CN103074794A CN 103074794 A CN103074794 A CN 103074794A CN 2013100446605 A CN2013100446605 A CN 2013100446605A CN 201310044660 A CN201310044660 A CN 201310044660A CN 103074794 A CN103074794 A CN 103074794A
- Authority
- CN
- China
- Prior art keywords
- cellulose
- waste cotton
- nano particle
- cotton velvet
- prepare
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing cellulose nanoparticles from waste cotton wool. The method comprises the following steps of: hydrolyzing waste cotton wool serving as a raw material; preparing a hydrolysis product into a cellulose dispersion liquid with a certain concentration; stirring the cellulose dispersion liquid under the action of ultrasonic waves to form a cellulose colloidal solution; and performing freeze drying on the cellulose colloidal solution to obtain the cellulose nanoparticles. The particle diameters of the prepared cellulose nanoparticles are 70-100 nanometers; moreover, the cellulose nanoparticles are obtained by shearing or performing ultrasonic dispersion without using any emulsifying agent, i.e., the cellulose nanoparticles are obtained by adopting a relatively direct way and a simple method; the polymerization degrees of the cellulose nanoparticles are 20-100; and the waste cotton wool is taken as the raw material, so that the resource utilization efficiency is increased.
Description
Technical field
The present invention relates to the preparation technology of nano-grade cellulosic, relate in particular to a kind of method of utilizing waste cotton velvet to prepare the cellulose nano particle.
Background technology
Except information technology and biotechnology, nanometer technology is considered to our these epoch important technical development.Generally, nanometer technology is concerned about is size in properity and the impact of hundreds of nanometer and following material.More and more extensive in its daily life that is applied in us, relate to for example energy technology, Environmental Technology, information technology and pharmacy medical field.
Cellulose is boiomacromolecule the most common on the earth, is global most important circular regeneration raw material.As composition main in the Plant holdfast, cellulose has excellent molecular characterization.Have orderly zone (crystal region) in the cellulose, these zones have the typical sizes (wide 3-10nm, long 100m) of nano particle, and are connected with each other by noncrystalline large molecule and secondary bond (hydrogen bond).
Prior art can only obtain the good stable nano-cellulose of one dimension usually, and the product that namely obtains just has nano level size in cross-sectional direction, but fibre length is all more than 200nm.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of method of utilizing waste cotton velvet to prepare the cellulose nano particle, the particle diameter of the fiber nano particle of the method preparation is at 70～100nm.
Technical scheme provided by the invention is:
A kind of method of utilizing waste cotton velvet to prepare the cellulose nano particle may further comprise the steps:
Step 1, waste cotton velvet is carried out preliminary treatment;
Step 2, adopt sulfuric acid to processings that be hydrolyzed of the preliminary treatment product of described step 1, the sulfuric acid consumption with the mass ratio of processing product is: 1: 6～15, and hydrolysis time is 1～2h, and hydrolysis temperature is 30～60 ℃, and sulfuric acid concentration is 45～70%;
Step 3, utilize the hydrolysate of described step 2 to prepare the cellulose dispersion liquid, the mass concentration of described cellulose dispersion liquid is 0.1～10%;
Step 4, described cellulose dispersion liquid is carried out ultrasonic processing and stir process, open and ultrasonic processing and stir process are carried out simultaneously, speed of agitator is 800～1000rpm, ultrasonic power is at 1000～1500w, processing time is 30～60min, obtain the cellulose gum liquid solution, wherein, the particle diameter of cellulose colloid is 70～100nm;
Step 5, the cellulose gum liquid solution that described step 4 is obtained carry out freeze drying, obtain the cellulose nano particle, and the particle diameter of described cellulose nano particle is 70～100nm.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 1, the contained cellulosic degree of polymerization is 6000～6500 in the described waste cotton velvet.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 6, the degree of polymerization of described cellulose nano particle is 20～100.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 1, waste cotton velvet is carried out preliminary treatment, comprise: step (1) is removed the impurity in the waste cotton velvet, step (2) adopts organic solvent that the product of step (1) is carried out the extracting dewaxing, and step (3) is dry with the product of step (2).
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, described step 1 also comprises: step (4) adopts ball mill that the product of described step (3) is carried out ball-milling treatment, and ball mill power is 11kw, rotating speed is 88rpm, and Ball-milling Time is 16h.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step (2), organic solvent is the mixed liquor of toluene and ethanol, and the volume ratio of toluene and ethanol is 1: 1, and the extracting dewaxing treatment is carried out under 70 ℃.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 4, wash the hydrolysate of described step 3 with ultra-pure water, until the pH value of hydrolysate reaches 7, prepare the aqueous solution of hydrolysate, the aqueous solution of hydrolysate is described cellulose dispersion liquid again.
Preferably, the described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 6, the particle diameter of described cellulose nano particle is recorded by the dynamic laser scattering.
The particle diameter of the fiber nano particle of the present invention's preparation is at 70～100nm; And the present invention does not need emulsifying agent, but utilizes shearing or ultrasonic dispersion to obtain, and namely adopts comparatively direct mode to obtain, and method is simple; The cellulose nano particle has 20～100 the degree of polymerization; Take waste cotton velvet as raw material, improve the utilization ratio of resource.
The specific embodiment
Below the present invention is described in further detail, can implement according to this with reference to the specification literal to make those skilled in the art.
The invention provides a kind of method of utilizing waste cotton velvet to prepare the cellulose nano particle, may further comprise the steps:
Step 1, waste cotton velvet is carried out preliminary treatment;
Step 2, adopt sulfuric acid to processings that be hydrolyzed of the preliminary treatment product of described step 1, the sulfuric acid consumption with the mass ratio of processing product is: 1: 6～15, and hydrolysis time is 1～2h, and hydrolysis temperature is 30～60 ℃, and sulfuric acid concentration is 45～70%;
Step 3, utilize the hydrolysate of described step 2 to prepare the cellulose dispersion liquid, the mass concentration of described cellulose dispersion liquid is 0.1～10%;
Step 4, described cellulose dispersion liquid is carried out ultrasonic processing and stir process, and ultrasonic processing and stir process are carried out simultaneously, speed of agitator is 800～1000rpm, ultrasonic power is at 1000～1500w, processing time is 30～60min, obtain the cellulose gum liquid solution, wherein, the particle diameter of cellulose colloid is 70～100nm;
Step 5, the cellulose gum liquid solution that described step 4 is obtained carry out freeze drying, obtain the cellulose nano particle, and the particle diameter of described cellulose nano particle is 70～100nm.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 1, the contained cellulosic degree of polymerization is 6000～6500 in the described waste cotton velvet.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 6, the degree of polymerization of described cellulose nano particle is 20～100.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 1, waste cotton velvet is carried out preliminary treatment, comprise: step (1) is removed the impurity in the waste cotton velvet, step (2) adopts organic solvent that the product of step (1) is carried out the extracting dewaxing, and step (3) is dry with the product of step (2).
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, described step 1 also comprises: step (4) adopts ball mill that the product of described step (3) is carried out ball-milling treatment, ball mill power is 11kw, and rotating speed is 88rpm, and Ball-milling Time is 16h.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step (2), organic solvent is the mixed liquor of toluene and ethanol, and the volume ratio of toluene and ethanol is 1: 1, and the extracting dewaxing treatment is carried out under 70 ℃.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 4, wash the hydrolysate of described step 3 with ultra-pure water, until the pH value of hydrolysate reaches 7, prepare the aqueous solution of hydrolysate, the aqueous solution of hydrolysate is described cellulose dispersion liquid again.
The described utilization in the method that waste cotton velvet prepares the cellulose nano particle, in the described step 6, the particle diameter of described cellulose nano particle is recorded by the dynamic laser scattering.
Waste cotton velvet utilizes ball mill to carry out ball mill grinding and processes through after certain preliminary treatment, under the ball milling condition that the present invention provides, the size of preliminary treatment product can be reduced to 115～180 μ m, in order to carry out follow-up processing.In the said process, the size of cellulose granules also mainly is the variation that macroscopic view occurs.
Hydrolysis process will shorten cellulosic chain length, reduce the cellulosic degree of polymerization.
Under the acting in conjunction of ultrasonic and stirring, then the fibre structure of the cellulose granules in the cellulose dispersion liquid further can be divided, at this moment, this division mainly is to carry out in microcosmic point.Through repetition test, determine that speed of agitator is 800～1000rpm, ultrasonic power is at 1000～1500w, and the processing time is 30～60min, has finally obtained the cellulose gum liquid solution, and wherein, the colloidal particle size in the cellulose gum liquid solution has reached 70～100nm.The raising of ultrasonic and stirring intensity, and the prolongation in processing time all helps lend some impetus to the cellulose grain quantum splitting, makes it form the less particle of particle diameter.
The concentration of above-mentioned cellulose dispersion liquid is 0.1～10%, and the excessive dispersion that is unfavorable for cellulose granules of concentration affects reducing of particle diameter.
Carry out freeze drying for the cellulose gum liquid solution, obtain the cellulose nano particle.Freeze drying can not cause reassembling of colloid.The particle diameter of cellulose nano particle of the present invention is 70～100nm.The present invention has not only obtained being at three-dimensional the cellulose granules of nano-scale, and the particle diameter of particle is evenly distributed.
Embodiment one
A kind of method of utilizing waste cotton velvet to prepare the cellulose nano particle may further comprise the steps:
Step 1, waste cotton velvet is carried out preliminary treatment, preliminary treatment comprises: step (1) is removed the impurity in the waste cotton velvet, step (2) adopts organic solvent that 70 ℃ of the products of step (1) are carried out lower extracting dewaxing, organic solvent is the mixed liquor of toluene and ethanol, and the volume ratio of toluene and ethanol is 1: 1, and step (3) is dry with the product of step (2);
Step 2, employing ball mill carry out ball-milling treatment to the preliminary treatment product of described step 1, and ball mill power is 11kw, and rotating speed is 88rpm, and Ball-milling Time is 16h;
Step 3, adopt sulfuric acid to processings that be hydrolyzed of the processing product of described step 2, the sulfuric acid consumption with the mass ratio of processing product is: 1: 10, hydrolysis time was 2h, and hydrolysis temperature is 50 ℃, and sulfuric acid concentration is 65%;
Step 4, wash the hydrolysate of described step 3 with ultra-pure water, until the pH value of hydrolysate reaches 7, prepare the aqueous solution of hydrolysate again, the aqueous solution of hydrolysate is described cellulose dispersion liquid, and the mass concentration of described cellulose dispersion liquid is 0.1%;
Step 5, described cellulose dispersion liquid is carried out ultrasonic processing and stir process, and ultrasonic processing and stir process are carried out simultaneously, speed of agitator is 850rpm, ultrasonic power is at 1200w, processing time is 30min, obtain the cellulose gum liquid solution, wherein, the particle diameter of cellulose colloid is 80～100nm;
Step 6, the cellulose gum liquid solution that described step 2 is obtained carry out freeze drying, obtain the cellulose nano particle, and the particle diameter of described cellulose nano particle is 80～100nm.
Embodiment two
Step 1, waste cotton velvet is carried out preliminary treatment, preliminary treatment comprises: step (1) is removed the impurity in the waste cotton velvet, step (2) adopts organic solvent that 70 ℃ of the products of step (1) are carried out lower extracting dewaxing, organic solvent is the mixed liquor of toluene and ethanol, and the volume ratio of toluene and ethanol is 1: 1, and step (3) is dry with the product of step (2);
Step 2, employing ball mill carry out ball-milling treatment to the preliminary treatment product of described step 1, and ball mill power is 11kw, and rotating speed is 88rpm, and Ball-milling Time is 16h;
Step 3, adopt sulfuric acid to processings that be hydrolyzed of the processing product of described step 2, the sulfuric acid consumption with the mass ratio of processing product is: 1: 15, hydrolysis time was 2h, and hydrolysis temperature is 50 ℃, and sulfuric acid concentration is 65%;
Step 4, wash the hydrolysate of described step 4 with ultra-pure water, until the pH value of hydrolysate reaches 7, prepare the aqueous solution of hydrolysate again, the aqueous solution of hydrolysate is described cellulose dispersion liquid, and the mass concentration of described cellulose dispersion liquid is 10%;
Step 5, described cellulose dispersion liquid is carried out ultrasonic processing and stir process, and ultrasonic processing and stir process are carried out simultaneously, speed of agitator is 1000rpm, ultrasonic power is at 1500w, processing time is 60min, obtain the cellulose gum liquid solution, wherein, the particle diameter of cellulose colloid is 70～80nm;
Step 6, the cellulose gum liquid solution that described step 5 is obtained carry out freeze drying, obtain the cellulose nano particle, and the particle diameter of described cellulose nano particle is 70～80nm.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification and the embodiment, it can be applied to various suitable the field of the invention fully, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details.
Claims (8)
1. a method of utilizing waste cotton velvet to prepare the cellulose nano particle is characterized in that, may further comprise the steps:
Step 1, waste cotton velvet is carried out preliminary treatment;
Step 2, adopt sulfuric acid to processings that be hydrolyzed of the preliminary treatment product of described step 1, the sulfuric acid consumption with the mass ratio of processing product is: 1: 6～15, and hydrolysis time is 1～2h, hydrolysis temperature is 30～60.℃, sulfuric acid concentration is 45～70%;
Step 3, utilize the hydrolysate of described step 2 to prepare the cellulose dispersion liquid, the mass concentration of described cellulose dispersion liquid is 0.1～10%;
Step 4, described cellulose dispersion liquid is carried out ultrasonic processing and stir process, and ultrasonic processing and stir process are carried out simultaneously, speed of agitator is 800～1000rpm, ultrasonic power is at 1000～1500w, processing time is 30～60min, obtain the cellulose gum liquid solution, wherein, the particle diameter of cellulose colloid is 70～100nm;
Step 5, the cellulose gum liquid solution that described step 4 is obtained carry out freeze drying, obtain the cellulose nano particle, and the particle diameter of described cellulose nano particle is 70～100nm.
2. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 1 is characterized in that, in the described step 1, the contained cellulosic degree of polymerization is 6000～6500 in the described waste cotton velvet.
3. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 2 is characterized in that, in the described step 6, the degree of polymerization of described cellulose nano particle is 20～100.
4. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 3, it is characterized in that, in the described step 1, waste cotton velvet is carried out preliminary treatment, comprise: step (1) is removed the impurity in the waste cotton velvet, step (2) adopts organic solvent that the product of step (1) is carried out the extracting dewaxing, and step (3) is dry with the product of step (2).
5. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 4, it is characterized in that, described step 1 also comprises: step (4) adopts ball mill that the product of described step (3) is carried out ball-milling treatment, ball mill power is 11kw, rotating speed is 88rpm, and Ball-milling Time is 16h.
6. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 4, it is characterized in that in the described step (2), organic solvent is the mixed liquor of toluene and ethanol, and the volume ratio of toluene and ethanol is 1: 1, and the extracting dewaxing treatment is carried out under 70 ℃.
7. the method for utilizing waste cotton velvet to prepare the cellulose nano particle as claimed in claim 5, it is characterized in that, in the described step 4, wash the hydrolysate of described step 3 with ultra-pure water, until the pH value of hydrolysate reaches 7, prepare the aqueous solution of hydrolysate, the aqueous solution of hydrolysate is described cellulose dispersion liquid again.
8. such as each described method of utilizing waste cotton velvet to prepare the cellulose nano particle in the claim 1 to 7, it is characterized in that in the described step 6, the particle diameter of described cellulose nano particle is recorded by the dynamic laser scattering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310044660.5A CN103074794B (en) | 2013-02-04 | 2013-02-04 | Method for preparing cellulose nanoparticles from waste cotton wool |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310044660.5A CN103074794B (en) | 2013-02-04 | 2013-02-04 | Method for preparing cellulose nanoparticles from waste cotton wool |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103074794A true CN103074794A (en) | 2013-05-01 |
| CN103074794B CN103074794B (en) | 2015-01-07 |
Family
ID=48151485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310044660.5A Active CN103074794B (en) | 2013-02-04 | 2013-02-04 | Method for preparing cellulose nanoparticles from waste cotton wool |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103074794B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104558639A (en) * | 2015-01-15 | 2015-04-29 | 四川大学 | Regenerated cellulose nano-particles and preparation method thereof |
| CN103304673B (en) * | 2013-07-01 | 2016-01-13 | 青岛科技大学 | A kind of method optimized Ascidian nano-cellulose and prepare |
| CN106810614A (en) * | 2017-01-21 | 2017-06-09 | 深圳市优普惠药品股份有限公司 | A kind of preparation technology of nanocrystal cellulose |
| WO2018157453A1 (en) * | 2017-03-03 | 2018-09-07 | 曾济天 | Nanocellulose, preparation method therefor, and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
| CN102899950A (en) * | 2012-10-25 | 2013-01-30 | 福建农林大学 | Method for preparing nano cellulose by simultaneous assistance of ultrasonic waves and microwaves |
| CN102899949A (en) * | 2012-08-10 | 2013-01-30 | 襄垣县鑫瑞达连氏塑木制造有限公司 | Method for preparing cellulose nano-fibril film by utilizing wood powder |
-
2013
- 2013-02-04 CN CN201310044660.5A patent/CN103074794B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942102A (en) * | 2010-09-07 | 2011-01-12 | 东南大学 | Preparation method of powder nano cellulose |
| CN102899949A (en) * | 2012-08-10 | 2013-01-30 | 襄垣县鑫瑞达连氏塑木制造有限公司 | Method for preparing cellulose nano-fibril film by utilizing wood powder |
| CN102899950A (en) * | 2012-10-25 | 2013-01-30 | 福建农林大学 | Method for preparing nano cellulose by simultaneous assistance of ultrasonic waves and microwaves |
Non-Patent Citations (1)
| Title |
|---|
| WENSHUAI CHEN ETAL: "Individualization of cellulose nanofibers from wood using high-intensity ultrasonication combined with chemical pretreatment", 《CARBOHYDRATE POLYMERS》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304673B (en) * | 2013-07-01 | 2016-01-13 | 青岛科技大学 | A kind of method optimized Ascidian nano-cellulose and prepare |
| 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 |
| CN104558639A (en) * | 2015-01-15 | 2015-04-29 | 四川大学 | Regenerated cellulose nano-particles and preparation method thereof |
| CN106810614A (en) * | 2017-01-21 | 2017-06-09 | 深圳市优普惠药品股份有限公司 | A kind of preparation technology of nanocrystal cellulose |
| CN106810614B (en) * | 2017-01-21 | 2019-04-12 | 深圳市优普惠药品股份有限公司 | A kind of preparation process of nanocrystal cellulose |
| WO2018157453A1 (en) * | 2017-03-03 | 2018-09-07 | 曾济天 | Nanocellulose, preparation method therefor, and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103074794B (en) | 2015-01-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103074794B (en) | Method for preparing cellulose nanoparticles from waste cotton wool | |
| CN108659135B (en) | Preparation method of cellulose nanofiber or chitin nanofiber dispersion liquid | |
| CN102690358B (en) | Cellulose nanocrystal suspension and preparation method thereof | |
| Ioelovich | Study of cellulose interaction with concentrated solutions of sulfuric acid | |
| CN109705226B (en) | Method for preparing carboxylated nanocellulose by utilizing citric acid hydrolysis and combining ultrasonic assistance | |
| CN102505546B (en) | Method for preparing nanocellulose by using homogeneous method | |
| Hao et al. | Self-assembled nanostructured cellulose prepared by a dissolution and regeneration process using phosphoric acid as a solvent | |
| CN102220718B (en) | Method for preparing nano celluloses through high-pressure crushing and low-temperature cooling | |
| Xu et al. | Preparation and characterization of spherical cellulose nanocrystals with high purity by the composite enzymolysis of pulp fibers | |
| Chen et al. | Controlled enzymolysis preparation of nanocrystalline cellulose from pretreated cotton fibers | |
| CN105218836B (en) | A kind of method that emulsifying agent auxiliary biological enzyme prepares size tunable type starch nanometer granule | |
| CN103588886B (en) | A kind of Easily-water dispersible nanocrystalline cellulose and preparation method thereof | |
| CN102702365A (en) | Method for preparing micro-nano cellulose with ultra-low crystallinity | |
| CN103103847A (en) | Method for preparing cellulose nanocrystals by combining biological enzymolysis and mechanical shearing | |
| CN105754133A (en) | Nano cellulose based biological aerogel and preparation method and application thereof | |
| AU2020100319A4 (en) | Method for preparing cellulose nanofibrils by deep eutectic solvent pretreatment | |
| CN106905437B (en) | Redispersible powder Cellulose nanocrystal of high heat resistance and preparation method thereof | |
| CN104211036A (en) | Hydroxyapatite and preparation method thereof | |
| CN105562714A (en) | Nanometer material for SERS (Surface-Enhanced Raman Scattering) detection and preparing method of nanometer material | |
| CN106149433B (en) | Nano-cellulose and preparation method thereof | |
| CN113718543A (en) | Method for cleanly preparing cellulose nanocrystals by combining organic acid hydrolysis with nano-micro-jet homogenization one-step method and product | |
| CN103333262A (en) | Preparation method of modified starch nanocrystal | |
| CN105603020A (en) | Nanocrystalline cellulose preparation method | |
| CN103271835B (en) | Silk fibroin nanocrystalline and preparation method thereof | |
| CN103978223A (en) | Method for green synthesis of nano-gold by using water extract of eucommia ulmoides |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |