CN104532365B - A kind of preparation method of silk nanofiber - Google Patents
A kind of preparation method of silk nanofiber Download PDFInfo
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- CN104532365B CN104532365B CN201510019809.3A CN201510019809A CN104532365B CN 104532365 B CN104532365 B CN 104532365B CN 201510019809 A CN201510019809 A CN 201510019809A CN 104532365 B CN104532365 B CN 104532365B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01B—MECHANICAL TREATMENT OF NATURAL FIBROUS OR FILAMENTARY MATERIAL TO OBTAIN FIBRES OF FILAMENTS, e.g. FOR SPINNING
- D01B7/00—Obtaining silk fibres or filaments
Abstract
The present invention relates to a kind of preparation method of silk nanofiber, belong to technical field of nanometer material preparation.Described preparation method refers to that the silk after by degumming process is transferred in the solution be made up of the micromolecular compound of inorganic salts or weak acid or weak base, deionized water, alcohols, after soaking the adhesion weakened in silk between nanometer fibril, again this silk solution is transferred in the disintegrating machine of high-pressure cell crusher or emulsifying machine or refiner or high speed agitator, by soak after silk Mechanical Crushing both described silk nanofiber.The silk nanofiber solution obtained by this method is that class water-setting is gluey, and adopt centrifugal or isolated by filtration to obtain silk nanofiber, preparation time is short, and equipment is simple, and operating influence factor is few, is convenient to control.The micromolecular compound adopted avoids strong acid or highly basic on the impact of silk nanometer fibril and described disintegrating machine can prepare silk nanofiber by rapid batch.
Description
Technical field
The present invention relates to a kind of preparation method of silk nanofiber, belong to technical field of nanometer material preparation.
Technical background
Silk is one of human use's protein the earliest, has good hygroscopicity and graceful gloss, very popular.Constantly further investigate along with to it, its research field developed also constantly is widened, and extends to the fields such as food fermentation, bio-pharmaceuticals, environmental protection, using energy source gradually.And fibroin albumen will be utilized, first just need the size reducing fibroin albumen to micron or nanoscale.For reaching this object, fibroin albumen normally dissolves in a solvent by people, the solvent that generally can dissolve fibroin comprises acid, alkali, salt or enzyme solutions, fibroin is degraded to Small molecular peptide chain by wherein acid, alkali, enzyme, being unfavorable for forming the large molecular staties such as film, also can there is larger change in protein structure.Therefore the salt of some high concentrations, the multicomponent solvent of salt-organic solvent is the conventional neutral flux of fibroin albumen, as being called in " Novelsilkfibroinfilmspreparedbyformicacid/hydroxyapatite dissolutionmethod " in name disclosed in document Mater.Sci.Eng.C the 37th phase 48 ~ 53 pages of 2014, boiled silk is dissolved in the mixed solution of formic acid and 1% ~ 5% hydroxyapatite composition, finally solution drying is obtained regenerated silk film, but in this process, owing to there is dissolving and the desalting processing subsequently of fibroin albumen, and be unfavorable for the industrialization of this technique.In addition, silk can also be dissolved methods such as adopting electrostatic spinning and prepare silk fiber, as China Patent Publication No. CN1587459A, publication date is on September 7th, 2004, denomination of invention is " manufacture method of regenerated fibroin superfine fibre ", just dissolve with inorganic salts, method concentrated after desalination is obtained high concentration (10% ~ 45%) first, the regenerated silk protein aqueous solution of good spinnability, through electrostatic spinning directly obtained regenerated fibroin superfine fibre (between 50 ~ 3000nm), but prepare silk fiber not only apparatus expensive by electrostatic spinning, and preparation influence factor is a lot.Fibroin albumen has very high mechanical strength, therefore be difficult to by the method for physics fibroin albumen is broken, if but the adhesion in silk between nanometer fibril was reduced by chemical reagent before being separated by fibroin albumen, fragmentation will be relatively easy, as U.S. Patent Publication No. 5853764, publication date is on October 29th, 1998, denomination of invention is " Processforpreparingfinepowderofsilkfibroin ", first boiled silk is soaked in the alkaline solution of 95 DEG C or more, then adopt two step mechanical disruption that fibroin albumen is broken; Disclosed in document Mater.Sci.Eng.C the 48th phase 444 ~ 452 pages of 2015, name is called " Processingandcharacterizationofpowderedsilkmicro-andnano fibersbyultrasonication ", and boiled silk is ultrasonic broken by fibroin albumen in the mixed solution of hydrochloric acid or formic acid or hydrochloric acid and formic acid.Although these methods also can be broken by silk, all complete in strong acid or strong base solution, inevitably can destroy the structure of silk, affect its follow-up use.
Summary of the invention
The present invention is directed to prior art Problems existing, object is the preparation method providing a kind of silk nanofiber.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation method of silk nanofiber, described preparation method refers to that the silk after by degumming process is transferred in the solution be made up of micromolecular compound, deionized water, alcohols, after soaking the adhesion weakened in silk between nanometer fibril, again the solution immersed with silk is transferred in disintegrating machine, by soak after silk Mechanical Crushing both described silk nanofiber, preparation method carries out according to the following steps:
After a gets the silk washed with de-ionized water after degumming process, dry at 20 ~ 30 DEG C;
B will join micromolecular compound with deionized water quality than being 0:1 ~ 1:200 through the dried boiled silk of a step, the mass ratio of alcohols and deionized water is soak 3 ~ 7h in the solution that forms of 0:1 ~ 1:200, swelling silk is to weaken the adhesion in silk between nanometer fibril, wherein, after solution and degumming process, the mass ratio of silk is 2000:1 ~ 1000:1;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 2 ~ 6h in disintegrating machine by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, again by after the product washed with de-ionized water of collection, at 20 ~ 30 DEG C drying both described silk nanofiber, gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Described micromolecular compound is the one in inorganic salts or weak acid or weak base.
Described inorganic salts are the one in calcium sulfate or calcium chloride or ammonium chloride or ammonium sulfate or ammonium acetate or ammonium nitrate.
Described weak acid is the one in acetic acid or propionic acid or butyric acid or valeric acid or oxalic acid.
Described weak base is ammoniacal liquor or aniline or hexa.
Described alcohols is the one in methyl alcohol or ethanol or propyl alcohol or butanols.
Described disintegrating machine is the one in high-pressure cell crusher or mulser or refiner or high speed agitator.
Owing to have employed above technical scheme, the preparation method of a kind of silk nanofiber of the present invention, be by degumming process after Silk Soaking micromolecular compound, deionized water, alcohols composition solution in, wherein alcohols can accelerate the swelling of silk, reduce soak required for time.Because silk is not only containing acidic-group (-COOH) but also containing basic group (-NH
2,-OH), in the process that silk soaks in the solution, micromolecular compound or its ion enter into amorphous area between silk nanometer fibril and are combined with corresponding group, reduce the adhesion between silk nanometer fibril.The silk reducing adhesion between silk nanometer fibril just can by it fragmentation by physical method, the silk solution obtained by physical method is that class water-setting is gluey, adopt centrifugal or isolated by filtration just can obtain the nanofiber of silk, do not need as the process of silk nanofiber just must will can be obtained after solution drying in chemolysis, shorten preparation time, be conducive to the industrialization of this technique, and equipment is simple, operating influence factor is few, is convenient to control.The appearance structure of traditional strong acid or highly basic destructible silk nanometer fibril in the immersion process of silk is unfavorable for the preparation of later stage long nanofiber.The micromolecular compound of faintly acid or alkalescent or weakly acidic pH inorganic salts is adopted to avoid strong acid or highly basic to the impact of silk nanometer fibril, in the process of Mechanical Crushing, disintegrating machine is step unlatching, therefore at room temperature just can be broken by silk, it also avoid the impact of high temperature on silk.The disintegrating machine simultaneously adopted is that high-pressure cell crusher or emulsifying machine or refiner or high speed agitator can prepare silk nanofiber by rapid batch.
Accompanying drawing explanation
Fig. 1 is that after Mechanical Crushing, silk nanofiber amplifies the scanning electron microscope (SEM) photograph of 5000 times.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail, sees accompanying drawing.
A kind of preparation method of silk nanofiber, described preparation method refers to that the silk after by degumming process is transferred in the solution be made up of micromolecular compound, deionized water, alcohols, after soaking the adhesion weakened in silk between nanometer fibril, again the solution immersed with silk is transferred in disintegrating machine, by soak after silk Mechanical Crushing both described silk nanofiber, preparation method carries out according to the following steps:
After a gets the silk washed with de-ionized water after degumming process, dry at 20 ~ 30 DEG C;
B will join micromolecular compound with deionized water quality than being 0:1 ~ 1:200 through the dried boiled silk of a step, the mass ratio of alcohols and deionized water is soak 3 ~ 7h in the solution that forms of 0:1 ~ 1:200, swelling silk is to weaken the adhesion in silk between nanometer fibril, wherein, after solution and degumming process, the mass ratio of silk is 2000:1 ~ 1000:1;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 2 ~ 6h in disintegrating machine by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, again by after the product washed with de-ionized water of collection, at 20 ~ 30 DEG C drying both described silk nanofiber, gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Described micromolecular compound is the one in inorganic salts or weak acid or weak base.
Described inorganic salts are the one in calcium sulfate or calcium chloride or ammonium chloride or ammonium sulfate or ammonium acetate or ammonium nitrate.
Described weak acid is the one in acetic acid or propionic acid or butyric acid or valeric acid or oxalic acid.
Described weak base is ammoniacal liquor or aniline or hexa.
Described alcohols is the one in methyl alcohol or ethanol or propyl alcohol or butanols.
Described disintegrating machine is the one in high-pressure cell crusher or mulser or refiner or high speed agitator.
Specific embodiment
Embodiment 1
After a gets 1g boiled silk washed with de-ionized water, the silk after cleaning is dry at 30 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 9.9g calcium chloride, 1980.2g ionized water, 9.9g ethanol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 4h in refiner by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 20 DEG C drying both described silk nanofiber.As shown in Figure 1, accompanying drawing 1 is the scanning electron microscope (SEM) photograph that gained silk nanofiber amplifies 5000 times, and the diameter of silk nanofiber is 50 ~ 150nm, and length is 100nm ~ 100 μm, the interlaced formation network structure of nanofiber.
Embodiment 2
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 5h in the solution going 1g calcium sulfate, 1492.6g ionized water, 6.4g ethanol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 6h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 20 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 3
After a gets 1g boiled silk washed with de-ionized water, the silk after cleaning is dry at 30 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 9.9g ammonium sulfate, 1980.2g ionized water, 9.9g methyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 2h in high speed agitator by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 20 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 4
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 7.5g ammonium acetate, 1395.8g ionized water, 96.7g methyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 4h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 25 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 5
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 5g ammonium nitrate, 990g ionized water, 5g ethanol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 25 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 6
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 3.7g acetic acid, 1492.6g ionized water, 3.7g propyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 7
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 4.8g propionic acid, 1440.6g ionized water, 54.6g propyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 8
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 7.5g butyric acid, 1395.8g ionized water, 96.7g propyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 9
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 9.9g valeric acid, 1980.2g ionized water, 9.9g propyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 10
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 7.5g oxalic acid, 1395.8g ionized water, 96.7g propyl alcohol to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 11
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 3.7g ammoniacal liquor, 1492.6g ionized water, 3.7g butanols to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 12
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 3.7g aniline, 1492.6g ionized water, 3.7g butanols to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 13
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by soaking 7h in the solution going 3.7g hexamethyl tetramine, 1492.6g ionized water, 3.7g butanols to form;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 14
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by removing to soak in 7.4g ammonium chloride, 1492.6g ionized water, the solution that forms 7h;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 15
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B soaks 7h and weakens adhesion in silk between nanometer fibril by joining through the dried boiled silk of a step by removing 1492.6g ionized water, in solution that 7.4g ethanol forms;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 3h in mulser by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 30 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Embodiment 16
After a gets the silk washed with de-ionized water after 1g degumming process, dry at 25 DEG C;
B weakens adhesion in silk between nanometer fibril by soaking 7h in the solution joining 1000g deionized water composition through the dried boiled silk of a step;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 6h in high-pressure cell crusher by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, then by after the product washed with de-ionized water of collecting, at 20 DEG C drying both described silk nanofiber.Gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
Claims (7)
1. the preparation method of a silk nanofiber, it is characterized in that: described preparation method refers to that the silk after by degumming process is transferred in the solution be made up of micromolecular compound, deionized water, alcohols, after soaking the adhesion weakened in silk between nanometer fibril, again the solution immersed with silk is transferred in disintegrating machine, namely silk Mechanical Crushing after soaking is obtained described silk nanofiber, and preparation method carries out according to the following steps:
After a gets the silk washed with de-ionized water after degumming process, dry at 20 ~ 30 DEG C;
It is 0.00067 ~ 0.005 that b will join micromolecular compound with deionized water quality ratio through the dried boiled silk of a step, the mass ratio of alcohols and deionized water is soak 3 ~ 7h in 0.00248 ~ 0.005 solution formed, swelling silk is to weaken the adhesion in silk between nanometer fibril, wherein, after solution and degumming process, the mass ratio of silk is 2000:1 ~ 1000:1;
The solution being added with boiled silk after b step process is transferred to Mechanical Crushing 2 ~ 6h in disintegrating machine by c;
Solution through step c adopts centrifugation or isolated by filtration to collect product by d, again by after the product washed with de-ionized water of collection, at 20 ~ 30 DEG C, be drying to obtain described silk nanofiber, gained silk nanofiber diameter is 50 ~ 150nm, and length is 100nm ~ 100 μm.
2. the preparation method of a kind of silk nanofiber according to claim 1, is characterized in that: described micromolecular compound is the one in inorganic salts or weak acid or weak base.
3. the preparation method of a kind of silk nanofiber according to claim 2, is characterized in that: described inorganic salts are the one in calcium sulfate or calcium chloride or ammonium chloride or ammonium sulfate or ammonium acetate or ammonium nitrate.
4. the preparation method of a kind of silk nanofiber according to claim 2, is characterized in that: described weak acid is the one in acetic acid or propionic acid or butyric acid or valeric acid or oxalic acid.
5. the preparation method of a kind of silk nanofiber according to claim 2, is characterized in that: described weak base is ammoniacal liquor or aniline or hexa.
6. the preparation method of a kind of silk nanofiber according to claim 1, is characterized in that: described alcohols is the one in methyl alcohol or ethanol or propyl alcohol or butanols.
7. the preparation method of a kind of silk nanofiber according to claim 1, is characterized in that: described disintegrating machine is the one in high-pressure cell crusher or mulser or refiner or high speed agitator.
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| CN1609122A (en) * | 2003-10-20 | 2005-04-27 | 北京理工大学 | New method of preparing silk protein powder |
| CN101168763A (en) * | 2007-11-09 | 2008-04-30 | 重庆工学院 | Method for preparing nano natural silk protein powder |
| CN101445546A (en) * | 2008-12-31 | 2009-06-03 | 苏州大学 | Preparation for tussore silk fibroin solution and concentration method thereof |
| CN103290085A (en) * | 2013-05-13 | 2013-09-11 | 湖州新天丝生物技术有限公司 | Silk protein powder and preparation method thereof |
| CN103271835A (en) * | 2013-06-20 | 2013-09-04 | 南京信息工程大学 | Silk fibroin nanocrystalline and preparation method thereof |
| CN104263785A (en) * | 2014-09-03 | 2015-01-07 | 苏州印丝特纺织数码科技有限公司 | Preparation method of superfine silk protein powder |
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