CN1477141A - Production method of water soluble sericin - Google Patents
Production method of water soluble sericin Download PDFInfo
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- CN1477141A CN1477141A CNA031320236A CN03132023A CN1477141A CN 1477141 A CN1477141 A CN 1477141A CN A031320236 A CNA031320236 A CN A031320236A CN 03132023 A CN03132023 A CN 03132023A CN 1477141 A CN1477141 A CN 1477141A
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Abstract
The method for preparing water soluble sericin with different molecular weights by using cocoon as raw material includes the following steps: soaking cleaned cocoon crust and waste silk in water or alkalescency solution, regulating pH value of said solution to 8-12 and making high-temp. high-pressure degrading treatment, regulating temp. or pressure, treatment time and pH value of boiling solution and controlling requirement molecular weight of water soluble sericin so as to prepare water soluble sericin solution or powder. The product can be extensively used in the fields of biological material, textile finishing agent.
Description
Technical field
The present invention relates to a kind ofly make the proteic method of the different water-soluble silk glue of various molecular weight ranges for raw material with silk cocoon (comprising cocoon shell, husks, waste silk etc.).
Background technology
The main component of silk is silk gum and fibroin, is a kind of natural polymer albumen of being produced by silkworm, and silk gum accounts for silk-protein total amount 20～30%.During silkworms spin silk cocooning, silk gum is overlayed on the fibroin fiber outside and is played the effect of protection and gluing fibroin fiber.In processings such as filature, silk white silk dye, need the processing of coming unstuck in various degree.In the processing of silk flosssilk wadding, silk spinning or in the research and development of the new functional materials of silk fibroin, must remove silk gum wholly or in part and just can carry out following process and processing.At present, in the above-mentioned silk production and the course of processing, the silk gum of sloughing does not almost all reclaim, all get rid of as waste liquid, because protein content is too high in the sewage effluent, flowing into the river course will the mass consumption oxygen in water, makes water body forfeiture self-purification capacity, causes a large amount of environmental pollutions and energy dissipation.So,, will produce huge economic benefit and social benefit if in the processing of silk and treating processes, can reclaim and utilize silk gum efficiently to exempt pollution to environment.
Contain the necessary aminoacids content of human body in the silk gum up to more than 17%, in 18 seed amino acids of forming silk gum, have 8 kinds to be essential amino acid.There are some researches show recently myelencephalon stellate cell excretory non-essential amino acid one Serine and glycine all be the nutritional factor that produces by neurogliocyte (Mitoma J et al, Neurosci Res 30 (2): 195-199,1998; Mitoma J et al, J Biol Chem 273 (31): 19363-19366,1998), it promotes cerebellar neuron existence, the dendron cultivated to take place and electric physiological development (Furuya S et al, Porc Natl Acad SciUSA, 97 (21): 11528-11533,2000).The L-Serine accounts for total amino acid content 33.3% in the sericin, and glycine also contains 16.05%, this two seed amino acid account for total amount half.Therefore, absorbing sericin or silk gum hydrolysate can improve man memory power, prevents brain aging, prevent dementia etc. more.Studies show that silk gum and silk gum hydrolysate thereof have the skin care of beauty treatment, beauty treatment, hair care function, antioxygenation and tyrosinase activity restraining effect (Japanese kokai publication sho 10-140154,10-265403, European patent 0841065), (spy opens clear 10-245345 to dermatitis, 11-193210), the growth of skin carcinoma, intestinal cancer restraining effect (spy opens clear 2000-256210) arranged, can promote the absorption and digestion or the like function (spy open clear 2000-312568) of stomach to mineral nutrition.And along with going deep into of research, new utility value and many unknown functions of the different degraded products of silk gum peptide or silk gum will constantly be found.
Studies show that the sericin that molecular weight is bigger can be used for making the textiles hygienic function top finish of bio-medical material or synthon and natural fiber; Less silk gum peptide, small molecular weight oligopeptide and some aminoacid mixtures of molecular weight can be used for makeup, medical bio medicine, functional health-care food, nourishing drink etc.
At present, proteic preparation of water-soluble silk glue or the way that from the waste liquid that contains sericin, reclaims, particularly prepare the proteic method of low-molecular-weight water-soluble silk glue, mostly be to carry out extracting with some inorganic salt, organic salt equal solvent, or with acid, alkali is hydrolyzed, dialyse then, desalination or ultrafiltration purification, decolouring make water-soluble silk glue albumen, or again through concentrating, dry, make the sericin powder.For example, be used for cosmetic material (spy opens clear 58-26809) with the water-soluble silk glue that alkaline, inorganic salts, the surfactivity aqueous solution, aqueous solution of urea carry out the boiling of silk gum, extracting, filtration, purifying, concentrate, dry back obtains, also useful carboxylic acid such as citric acid etc. carry out coming unstuck of raw silk and fabric.From scouring waste, reclaim water-soluble silk glue as the method (spy opens clear 1-168906) of precipitations such as poly-propionic acid diethylamino ethyl ester collection or by hyperfiltration process (spy opens clear 4-202435) by inorganic agglutinant such as poly aluminium chloride etc., organic polymer agglutinant.The ionized water that generates by water electrolysis is used for coming unstuck of silk, thus the higher silk gum peptide solution (spy opens clear 10-29909) of preparation purity.
The above-mentioned method for preparing sericin, owing to add the difference of solvent and the difference of dissolution conditions, the sericin of preparation has plenty of macromole insoluble sericin, have plenty of the very little water-soluble silk glue peptide of molecular weight, be difficult to the palliating degradation degree of control sericin and the molecular weight ranges of sericin.And since the ion of high density exist must through dialysis, desalination or repeatedly ultrafiltration purification, the sericin that operation could obtain practicality such as concentrate.At present, the water-soluble silk glue albumen particularly silk gum production of molecular weight less (generally below 5 kilodaltons) mainly is to obtain by enzymolysis or acidolysis, this enzymolysis or acidolysis are difficult to the palliating degradation degree of control silk gum, cannot obtain the water-soluble silk glue of various different purposes, different molecular weight ranges.So, more than these methods mostly exist complicated process of preparation, cost recovery height, organic efficiency low, be not suitable for the recovery or the proteic preparation of water-soluble silk glue of industrialization silk gum.
Summary of the invention
The objective of the invention is to overcome the deficiency that above-mentioned prior art exists, provide that a kind of technology is simple, clean environment firendly, and can effectively control the proteic manufacture method of water-soluble silk glue of sericin molecular weight ranges.
The technical scheme that realizes the object of the invention is to have adopted following procedure of processing: 1. come unstuck: clean cocoon shell, waste silk, husks etc. make insoluble silk gum solution through the processing of coming unstuck of 110～140 ℃ or 0.05～0.26MPa High Temperature High Pressure after 1～5 hour in water or pH value are 8～12 the aqueous solution; 2. silk gum degraded: with alkali the pH value of above-mentioned insoluble silk gum solution is transferred to 8～12, degradation treatment is 1～5 hour under 110～140 ℃ or 0.05～0.26MPa condition, the different various water-soluble silk glue protein solutions of acquisition molecular weight ranges.
The described solution that comes unstuck of technique scheme is carried out drying treatment make powder, before the silk gum degradation treatment, use hot water earlier the silk gum powder dissolution.
To adopt the water-soluble silk glue protein solution that technique scheme obtained to transfer to neutrality with acid.
After adopting the water-soluble silk glue protein solution drying that technique scheme obtained, make the water-soluble silk glue protein powder.
Compared with prior art, the proteic method of manufacturing water-soluble silk glue provided by the present invention has following tangible beneficial effect:
1. owing to adopted comparatively gentle silk gum to come unstuck and degradation technique, only need just silk gum liquid to be transferred to pH8～12 with the alkali of minute quantity, after under high-temperature and high-pressure conditions, handling, obtain degraded silk gum liquid as long as just can transfer to neutrality with a spot of acid, do not need to dialyse again, operation such as desalination, ultrafiltration just can be applicable to many fields, greatly reduce production cost, improved efficient.Have 95% silk gum to degrade to the following polypeptide of molecular weight 10kDa after the degradation treatment approximately, all the other are total free aminoacids and a spot of taurine.This sericin fines is soluble in water, can all dissolve in the water more than 0 ℃.
2. sericin molecular weight ranges size can realize the effective control to required various sericin molecular weight ranges easily by the pressure or the processing condition such as temperature, degradation treatment time and sericin pH value of solution value of control degradation processing.
3. discarded without any sericin in the whole course of processing do not have deleterious processing waste water and produces and pollute, and do not use a large amount of chemicalses as additive yet.Therefore, but high-level efficiency reclaims the sericin of silk in producing, and accomplishes low cost, pollution-free, suitability for industrialized production water-soluble silk glue albumen.
Cocoon shell, waste silk, husks etc. the first time High Temperature High Pressure come unstuck and handle the degumed silk fiber that the back obtains, cleaning, fair and clear, its degumed silk output and quality are not affected, and can be used as various uses such as silk flosssilk wadding, silk spinning.
Description of drawings
Fig. 1 adopts different processing condition to make the proteic SDS-PAGE collection of illustrative plates of water-soluble silk glue of different molecular weight ranges in the embodiment of the invention.
Fig. 2 is that the amino acid of a kind of water-soluble silk glue albumen and hydrolyzate thereof in the embodiment of the invention is formed collection of illustrative plates.
Embodiment
Below in conjunction with drawings and Examples technical solutions according to the invention are further described.
Embodiment 1:
Take by weighing raw materials such as cocoon shell, husks, waste silk, impurity and dust are removed in rinsing in warm water or in weak alkaline aqueous solution earlier, add the pure water of 20 times of amounts (V/W) then or transfer in pH7～8 aqueous solution and flood with NaOH, after making husks or the abundant swelling of cocoon shell, placing high temperature and high pressure containers, is to handle 1 hour under the condition of 120 ℃ (0.1MPa pressure) in temperature, boiled silk is taken out in the cooling back, water washes repeatedly, and washings and come unglued liquid are merged, and makes insoluble silk gum solution.
Transfer to above-mentioned insoluble silk gum solution with NaOH, the pH value is respectively pH=10.0, pH=11.0 and pH=12.0; Perhaps the direct spraying drying of above-mentioned degumed silk sol solution is made insoluble silk gum powder, this silk gum powder is used the hot water dissolving earlier, transfer to pH=10.0, pH=11.0 and pH=12.0 respectively with NaOH equally.
The insoluble silk gum solution of above-mentioned adjustment pH value is carried out the High Temperature High Pressure degradation treatment second time, handled respectively 1 hour, 2.5 hours and 5 hours, transfer to neutrality with the HCl solution silk gum liquid of will degrading respectively again after the cooling, after filtration, obtain the different water-soluble silk glue protein solution of various molecular weight ranges behind the purifying, perhaps obtain various water-soluble silk glue protein powders with this solution spray is dry.Referring to accompanying drawing 1, can be clear that the proteic molecular weight ranges of various water-soluble silk glues by the SDS-PAGE collection of illustrative plates.The pH value that A4, A5, A6 correspond respectively to sericin solution is 10.0,11.0 and 12.0, is that 120 ℃, pressure are resulting sericin molecular weight ranges under 1 hour the processing condition of 0.1Mpa degradation treatment in temperature; The pH value that B4, B5, B6 correspond respectively to sericin solution is 10.0,11.0 and 12.0, is that 120 ℃, pressure are resulting sericin molecular weight ranges under 2.5 hours the processing condition of 0.1MPa degradation treatment in temperature; The pH value that C4, C5, C6 correspond respectively to sericin solution is 10.0,11.0 and 12.0, is that 120 ℃, pressure are resulting sericin molecular weight ranges under 5 hours the processing condition of 0.1MPa degradation treatment in temperature.Analyze through the SDS-of accompanying drawing 1 polyacrylamide gel electrophoresis, the proteic method of preparation water-soluble silk glue that the embodiment of the invention provided, by changing processing condition, as the pH value of sericin solution, temperature or pressure, the treatment time etc. of degradation treatment, just can reach the purpose of the prepared sericin molecular weight ranges of control.
At the following sericin that obtains of various different technology conditions, also can add the acetone treatment 10～20 hours of 1～5 times of volume to above-mentioned, after filtration, make the water-soluble silk glue powder of degreasing after the oven dry, be convenient to store, transport or satisfy some special needs.The particle size distribution range of this water-soluble silk glue powder is at 0.5～20 μ m, and median size for white or micro-yellow powder slightly, can be dissolved in water more than 0 ℃ about 10 μ m fully.By the fuchsin(e)test to this silk gum powder, the result shows that its wettability power is very strong.
Referring to accompanying drawing 2; this water-soluble silk glue protein powder shows through amino acid analysis, contains the total free aminoacids about 5%, also contains 13.7% taurine in these total free aminoacidss; therefore, this water-soluble silk glue albumen have anti-oxidant, suppress multiple effect such as tyrosine activity.
Embodiment 2:
Take by weighing raw material 1Kg such as cocoon shell, husks, waste silk, impurity and dust are removed in rinsing in warm water or in weak alkaline aqueous solution earlier, add then in the pure water of 20 times of amounts (V/W) and flood, after making husks or the abundant swelling of cocoon shell, placing high temperature and high pressure containers, is to handle 1 hour under the condition of 120 ℃ (0.1MPa pressure) in temperature, boiled silk is taken out in the cooling back, water washes repeatedly, and washings and come unglued liquid are merged, and makes insoluble silk gum solution.
With NaOH the insoluble silk gum solution that makes is transferred to pH11.0; Perhaps the direct spraying drying of insoluble silk gum solution that makes is made insoluble silk gum powder, this silk gum powder is used the hot water dissolving earlier, transfer to pH11.0 with NaOH equally.Then, insoluble silk gum solution after the above-mentioned adjustment pH value is divided into two groups of D and E, the D group is at 110 ℃ (or 0.05MPa pressure), E group is carried out the High Temperature High Pressure degradation treatment 2.5 hours second time respectively under 125 ℃ of (or 0.135MPa pressure) conditions, all transfer to neutrality after the cooling with the HCl solution silk gum liquid of will degrading, after filtration, obtain the water-soluble silk glue protein solution of two kinds of different molecular weights behind the purifying, perhaps with the dry water-soluble silk glue protein powder that obtains of this solution spray.Analyze through the SDS-polyacrylamide gel electrophoresis, the proteic molecular weight ranges of D group water-soluble silk glue is below the 90kDa, and the proteic molecular weight ranges of E group water-soluble silk glue is below the 15kDa.
China produces silk big country, has a large amount of waste silks to utilize in silkworm and mulberry, filature and weaving are produced.The present invention is specially adapted to the recovery of silk flosssilk wadding factory, silk spinning filature silk glue and the production of water-soluble silk glue albumen (powder), also is applicable to from silk mill's cocoon cooking and dyes the experienced filature silk silk fabric scouring waste and to reclaim insoluble silk gum, produces water-soluble silk glue albumen.This sericin can be widely used in fields such as biological medicine, Biofunctional materials, healthcare products, makeup and food.This invention will have obvious economic benefit and great social significance.
Claims (4)
1. proteic manufacture method of water-soluble silk glue is characterized in that procedure of processing is as follows:
1. come unstuck: clean cocoon shell, waste silk, husks etc. make insoluble silk gum solution through the processing of coming unstuck of 110～140 ℃ or 0.05～0.26MPa High Temperature High Pressure after 1～5 hour in water or pH value are 8～12 the aqueous solution;
2. silk gum degraded: with alkali the pH value of above-mentioned insoluble silk gum solution is transferred to 8～12, degradation treatment is 1～5 hour under 110～140 ℃ or 0.05～0.26MPa condition, the different various water-soluble silk glue protein solutions of acquisition molecular weight ranges.
2. the proteic manufacture method of water-soluble silk glue according to claim 1 is characterized in that: described insoluble silk gum solution carries out drying treatment and makes powder, before the silk gum degradation treatment, uses hot water the silk gum powder dissolution earlier.
3. the proteic manufacture method of water-soluble silk glue according to claim 1 is characterized in that: the water-soluble silk glue protein solution that obtains is transferred to neutrality with acid.
4. the proteic manufacture method of water-soluble silk glue according to claim 1 and 2 is characterized in that: will make the water-soluble silk glue protein powder after the water-soluble silk glue protein solution drying that obtain.
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| CN 03132023 CN1209395C (en) | 2003-07-09 | 2003-07-09 | Production method of water soluble sericin |
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| CN 03132023 CN1209395C (en) | 2003-07-09 | 2003-07-09 | Production method of water soluble sericin |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999545B (en) * | 2007-01-12 | 2010-09-08 | 东华大学 | Process of recovering sericine by ion exchanging |
| CN101857320A (en) * | 2010-05-25 | 2010-10-13 | 苏州大学 | Method for treatment of silk degumming wastewater and recovery of silk gum |
| CN103005564A (en) * | 2013-01-17 | 2013-04-03 | 李卫旗 | Method for making sweet tangelo sericin polypeptide juice |
| CN103141900A (en) * | 2013-03-06 | 2013-06-12 | 上海大学 | Sericin Chinese medicinal health-care beverage and preparation method thereof |
| CN103627367A (en) * | 2013-11-29 | 2014-03-12 | 郝飞麟 | Environment-friendly adhesive as well as preparation method and application thereof |
| CN104614277A (en) * | 2015-01-26 | 2015-05-13 | 浙江大学 | Method for utilizing sericin dissolution property to distinguish fresh cocoon raw silk from dried cocoon raw silk |
| CN106592229A (en) * | 2016-11-24 | 2017-04-26 | 江苏爱西施科技服务咨询股份有限公司 | Cashmere fabric anti-pilling finishing liquor containing modified sericin and preparation method of finishing liquor |
| CN106702741A (en) * | 2016-11-24 | 2017-05-24 | 江苏爱西施科技服务咨询股份有限公司 | Antibacterial finishing liquid containing modified sericin protein and preparation method of antibacterial finishing liquid |
| CN108547079A (en) * | 2018-06-08 | 2018-09-18 | 北京鹏盛天纤科技有限公司 | A kind of absorbent cotton green continous way production integrating device and technique |
| CN110551192A (en) * | 2019-09-16 | 2019-12-10 | 姚建林 | extraction method of silk peptide protein |
| CN112300257A (en) * | 2020-11-03 | 2021-02-02 | 西南大学 | Sericin with anti-inflammatory function and preparation method and application thereof |
| CN113150307A (en) * | 2021-04-30 | 2021-07-23 | 苏州大学 | Glycosylated sericin, preparation method and application thereof |
| CN113372426A (en) * | 2020-03-10 | 2021-09-10 | 森田生医股份有限公司 | Sericin extract, preparation method and use thereof, and antioxidant composition comprising the same |
Families Citing this family (1)
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| CN102250995B (en) * | 2011-03-25 | 2012-07-04 | 兴化市大地蓝绢纺有限公司 | Method for degumming from silk spinning raw material and recovering sericin |
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2003
- 2003-07-09 CN CN 03132023 patent/CN1209395C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999545B (en) * | 2007-01-12 | 2010-09-08 | 东华大学 | Process of recovering sericine by ion exchanging |
| CN101857320A (en) * | 2010-05-25 | 2010-10-13 | 苏州大学 | Method for treatment of silk degumming wastewater and recovery of silk gum |
| CN103005564A (en) * | 2013-01-17 | 2013-04-03 | 李卫旗 | Method for making sweet tangelo sericin polypeptide juice |
| CN103141900A (en) * | 2013-03-06 | 2013-06-12 | 上海大学 | Sericin Chinese medicinal health-care beverage and preparation method thereof |
| CN103627367A (en) * | 2013-11-29 | 2014-03-12 | 郝飞麟 | Environment-friendly adhesive as well as preparation method and application thereof |
| CN103627367B (en) * | 2013-11-29 | 2016-03-30 | 郝飞麟 | A kind of environment-protective adhesive and its preparation method and application |
| CN104614277A (en) * | 2015-01-26 | 2015-05-13 | 浙江大学 | Method for utilizing sericin dissolution property to distinguish fresh cocoon raw silk from dried cocoon raw silk |
| CN106702741A (en) * | 2016-11-24 | 2017-05-24 | 江苏爱西施科技服务咨询股份有限公司 | Antibacterial finishing liquid containing modified sericin protein and preparation method of antibacterial finishing liquid |
| CN106592229A (en) * | 2016-11-24 | 2017-04-26 | 江苏爱西施科技服务咨询股份有限公司 | Cashmere fabric anti-pilling finishing liquor containing modified sericin and preparation method of finishing liquor |
| CN108547079A (en) * | 2018-06-08 | 2018-09-18 | 北京鹏盛天纤科技有限公司 | A kind of absorbent cotton green continous way production integrating device and technique |
| CN108547079B (en) * | 2018-06-08 | 2023-10-10 | 北京鹏盛天纤科技有限公司 | Green continuous production integrated device and process for absorbent cotton |
| CN110551192A (en) * | 2019-09-16 | 2019-12-10 | 姚建林 | extraction method of silk peptide protein |
| CN113372426A (en) * | 2020-03-10 | 2021-09-10 | 森田生医股份有限公司 | Sericin extract, preparation method and use thereof, and antioxidant composition comprising the same |
| TWI756643B (en) * | 2020-03-10 | 2022-03-01 | 森田生醫股份有限公司 | Sericin extract, manufacturing method and use thereof, and antioxidant composition including the same |
| CN112300257A (en) * | 2020-11-03 | 2021-02-02 | 西南大学 | Sericin with anti-inflammatory function and preparation method and application thereof |
| CN113150307A (en) * | 2021-04-30 | 2021-07-23 | 苏州大学 | Glycosylated sericin, preparation method and application thereof |
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