CN1313015C - Method for producing powder for refining silk - Google Patents
Method for producing powder for refining silk Download PDFInfo
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- CN1313015C CN1313015C CNB2003101061837A CN200310106183A CN1313015C CN 1313015 C CN1313015 C CN 1313015C CN B2003101061837 A CNB2003101061837 A CN B2003101061837A CN 200310106183 A CN200310106183 A CN 200310106183A CN 1313015 C CN1313015 C CN 1313015C
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Abstract
The present invention discloses a production method for refined silk powder, which is characterized in that hot water is firstly used for boiling and removing gum; sulfuric acid is used for acid hydrolysis until the test result shows that most of amino acid and a small amount of dipeptide and tripeptide are contained, and alkali is added for neutralization until the pH value is 7.0; a purifying agent is added after press filtration and decoloring; the filtered clear liquid is dried by spraying, and a powdery substance which is the refined silk powder is obtained. Because any auxiliary agent or sodium carbonate is used for removing gum when the production method is used for removing gum, impurities can not be introduced, and the obtained product has the advantages of low salt content, little ash, and low harmful impurity content; the obtained product is suitable for making cosmetics, health-care products and foods.
Description
Technical field
The present invention relates to a kind of is the manufacture method of the powder for refining silk of raw material with silk, and the powder for refining silk that is obtained is the mixture of free amino acid and dipeptides and tripeptides.
Background technology
Because international market demand changes, the silk industry gets into a difficult position, and people begin to try to explore the new purposes of silk.Contain several amino acids in the fibroin albumen, mainly form by amino acid such as aminoacetic acid, alanine, serine, tyrosine, and the serine that includes, lysine, arginine, asparatate, glutamic acid all are the nutritional factors of skin, yet, the fibroin molecular weight is bigger, only swelling taking place and do not dissolve, thereby is difficult to utilize in water.
Be directed to this, Chinese invention patent application CN1152410 discloses a kind of fibroin albumen hydrolyzed product silk essence and preparation method thereof, silk smart by amino acid and minute quantity two, tripeptides forms, silk after will coming unstuck is put into hydrochloric acid and is dissolved, through processes such as back hydrolysis, filtration, decolouring, neutralization, precipitations, it is smart to obtain silk, because silk is smart soluble in water, thereby can be used for making cosmetics, food, medicine etc.
Yet owing to adopt hydrochloric acid hydrolysis, neutralization back salt is difficult to remove, and can cause the too much problem of product ash content, simultaneously, can contain a certain amount of harmful substance in the product, as lead, arsenic, mercury etc., has influenced the smart application of silk.
Summary of the invention
The object of the invention provides a kind of manufacture method of powder for refining silk, reduces the ash content of coal and harmful substance contents in the powder for refining silk that is obtained.
For achieving the above object, the technical solution used in the present invention is: a kind of manufacture method of powder for refining silk comprises the following steps:
(1) come unstuck, silkworm cocoon or leftover bits and pieces silk are boiled the processing of coming unstuck in 3-4 hour with boiling water in bath raio 1: 15～20 earlier, add hot water again after degumed silk is dried and boiled 2～4 hours in bath raio 1: 15～20, water cleaning and degumming silk also takes off dried;
(2) acidolysis, the degumed silk after will washing drying adds 20～30% sulphuric acid hydrolysis, bath raio is 5～10, little boiling reflux, hydrolysis 15～20 hours, until testing result be major part be amino acid and contain a small amount of dipeptides, tripeptides till;
(3) add the alkali neutralization in the silk acid hydrolysis liquid that obtained in last step, to the pH value be 7.0;
(4) press filtration, decolouring;
(5) clear liquid after filtering is carried out spray-drying, obtain powdered substance, be powder for refining silk.
In the technique scheme, in the described step 1, the method for cleaning and degumming silk is that the silk after will coming unstuck cleans with warm water, uses centrifuge dewatering, soaks centrifugal dehydration again, 2～3 times repeatedly then with pure water.
In the technique scheme, described discoloration method is to add activated carbon decolorizing 1～2 hour in the clear liquid after filter residue is removed in press filtration, bleaching temperature is 60～70 ℃, and the active carbon addition is 5～8% of a destainer, carries out press filtration then and separates, remove residue, get it and cross cleaner liquid.
Further technical scheme can purify once more to the cleaner liquid after the decolouring, and described purification method is, adds in filtrate after 0.05%～0.1% cleanser handles, by the cleanser of filter screen removal effect.The purpose that filtrate purifies, it is the harmful substance of removing in the filtrate, as lead, arsenic, mercury ion, usually, can adopt ion-exchange process, but, existing ion exchange column mode product yield is lower, and therefore, what adopt among the present invention is to add a certain amount of cleanser, realize ion-exchange, remove the mode of cleanser again with filter screen.
Wherein, the cleanser that is added can be an ion exchange cellulose, also can be ion exchange resin.
In the technique scheme, before described spray-drying, filter the smart solution of silk that obtains with accurate filter earlier, spray-dired EAT scope is 180 ℃～200 ℃, and leaving air temp is 70～80 ℃.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. because the present invention adopts boiling water treating when coming unstuck, do not add any auxiliary agent or soda ash and come unstuck, thereby introduce impurity at the Shi Buhui that comes unstuck, simultaneously, clean after coming unstuck, the silk impurity content after can guaranteeing to come unstuck reduces, be convenient to subsequent treatment, and improve the purity of product;
2. what the present invention added when acidolysis is sulfuric acid, after this use in the alkali and the time because multiple sulfate is insoluble matter, be easy to remove with the press filtration mode, make the salt content in the product low, ash is few;
3. adopt the mode that adds cleanser to carry out ion-exchange, remove objectionable impurities, effective, detect through Zhejiang Center For Disease Control and Prevention, the content of lead, arsenic, mercury reaches the allowed band of export food.
The specific embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment one: follows these steps to handle,
(1) come unstuck: take by weighing 10 kilograms of silkworm cocoon or leftover bits and pieces silks, add pure water, boiled 3 hours with boiling water earlier, bath raio is 1: 15; Boiled 2.5 hours adding hot water again after the degumed silk drying, bath raio is 1: 15, obtains boiled silk;
(2) cleaning and degumming silk: the silk after will coming unstuck is used centrifuge dewatering after cleaning with warm water, soaks half an hour approximately, centrifugal dehydration again, 2～3 times repeatedly with pure water then;
(3) acidolysis: will wash and dry degumed silk and add 20～30% sulphuric acid hydrolysis, bath raio is 1: 5～10, little boiling reflux, hydrolysis 15～20 hours, until testing result be major part be amino acid and contain a certain amount of dipeptides, tripeptides till;
(4) neutralization: adding alkali in the silk acid hydrolysis liquid, to be neutralized to the pH value be till 7.0, and alkali can be selected the hydroxide of metal, with its sulfate indissoluble or water insoluble being advisable;
(5) press filtration, decolouring: filter residue is removed in the neutralizer press filtration, in clear liquid, added activated carbon decolorizing 1 hour, 60～70 ℃ of bleaching temperatures, the active carbon addition is 5～8% of a destainer, carries out press filtration then and separates, and removes residue, gets it and crosses cleaner liquid;
(6) filtrate purifies: add 0.05%～0.1% cleanser in filtrate, handle, by the cleanser of filter screen removal effect, cleanser wherein generally can be selected ion exchange cellulose, also can be ion exchange resin;
(7) spray-drying: filter (filtrate of accurate filter is the microporous polyethylene sheet stock) with accurate filter earlier, use hig h-speed centrifugal spray drying device drying again, EAT is about 180～200 ℃, and leaving air temp is at 70～80 ℃;
(8) packing of sieving: with the silk essence that obtains after the spray-drying sieve, vacuum packaging, promptly obtain the finished product powder for refining silk.
The powder for refining silk that present embodiment obtains, extremely faint yellow for white, be crystalloid or pulverulent solids, detect through Zhejiang Center For Disease Control and Prevention, do not detect heavy metal and arsenic, total plate count＜10cfu/kg, coliform＜30MPN/100g.
This powder for refining silk has remarkable moisture-keeping functions, and the skin corium that very easily penetrates to the skin is absorbed very soon by skin, for skin provides rich nutrient contents, and participates in the activity of body endoenzyme, plays skin care, grows the effect of skin, skin makeup, thereby can be used as cosmetic material.
Simultaneously, contain unique physiologically active peptide in the silk essence, easily be absorbed by the body; blood sugar in the reduction blood of human body, cholesterol etc. had certain prevention and health care function; its contained abundant alanine, the effect that has the protection liver and sober up, thereby also can be used for making health products.
The amino acid content of the powder for refining silk that present embodiment obtains detects:
In the hydrochloric acid of 6mol/L, hydrochloric acid is removed in 110 ℃ of following hydrolysis 24 hours, draws the hydrolyzate of a certain amount of volume with obtaining powder for refining silk, measures with the 835-50 of Hitachi type amino-acid analyzer, and the amino acid composition situation of acquisition is as shown in table 1 below.As can be seen, the amino acid of fibroin is formed basic identical in the amino acid composition of silk essence and the silk.
The amino acid of table 1 embodiment 1 powder for refining silk that obtains is formed (%)
| Amino acid | ％ | Amino acid | ％ |
| Asparatate threonine serine glutamic acid aminoacetic acid alanine valine tyrosine | 4.43 1.61 12.51 1.13 39.42 34.92 1.11 0.41 | Isoleucine leucine phenylalanine arginine lysine histidine proline | 0.07 0.18 0.08 0.79 0.17 0.90 0.26 |
Claims (7)
1. the manufacture method of a powder for refining silk is characterized in that, comprises the following steps:
(1) come unstuck, silkworm cocoon or leftover bits and pieces silk are boiled the processing of coming unstuck in 3-4 hour with boiling water in bath raio 1: 15～20 earlier, add hot water again after degumed silk is dried and boiled 2～4 hours in bath raio 1: 15～20, water cleaning and degumming silk also takes off dried;
(2) acidolysis, the degumed silk after will washing drying adds 20～30% sulphuric acid hydrolysis, bath raio is 5～10, little boiling reflux, hydrolysis 15～20 hours, until testing result be major part be amino acid and contain a small amount of dipeptides, tripeptides till;
(3) add the alkali neutralization in the silk acid hydrolysis liquid that obtained in last step, to the pH value be 7.0;
(4) press filtration, decolouring;
(5) clear liquid after the decolouring is carried out spray-drying, obtain powdered substance, be powder for refining silk.
2. the manufacture method of powder for refining silk according to claim 1, it is characterized in that: in the described step of coming unstuck, the method for cleaning and degumming silk is, silk after will coming unstuck cleans with warm water, uses centrifuge dewatering, soaks with pure water then, centrifugal dehydration again, 2～3 times repeatedly.
3. the manufacture method of powder for refining silk according to claim 1, it is characterized in that: described discoloration method is, added activated carbon decolorizing 1～2 hour in the clear liquid after filter residue is removed in press filtration, bleaching temperature is 60～70 ℃, the active carbon addition is 5～8% of a destainer, carry out press filtration then and separate, remove residue, get it and cross cleaner liquid.
4. according to the manufacture method of claim 1 or 3 described powder for refining silk, it is characterized in that: the cleaner liquid after the decolouring is purified once more, described purification method is, adds in filtrate after 0.05%～0.1% cleanser handles, by the cleanser of filter screen removal effect.
5. the manufacture method of powder for refining silk according to claim 4, it is characterized in that: the cleanser that is added is an ion exchange cellulose.
6. the manufacture method of powder for refining silk according to claim 4, it is characterized in that: the cleanser that is added is an ion exchange resin.
7. the manufacture method of powder for refining silk according to claim 1 is characterized in that: before described spray-drying, filter the smart solution of silk that obtains with accurate filter earlier, spray-dired EAT scope is 180 ℃～200 ℃, and leaving air temp is 70～80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101061837A CN1313015C (en) | 2003-10-31 | 2003-10-31 | Method for producing powder for refining silk |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101061837A CN1313015C (en) | 2003-10-31 | 2003-10-31 | Method for producing powder for refining silk |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1539309A CN1539309A (en) | 2004-10-27 |
| CN1313015C true CN1313015C (en) | 2007-05-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003101061837A Expired - Fee Related CN1313015C (en) | 2003-10-31 | 2003-10-31 | Method for producing powder for refining silk |
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| CN (1) | CN1313015C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1620887B (en) * | 2004-12-15 | 2010-05-12 | 汤兴然 | Edible fatless animal protein and its preparation method and uses |
| CN100376170C (en) * | 2006-04-06 | 2008-03-26 | 浙江省农业科学院 | Edible watural silk protein powder and preparation method of natural silk extract |
| CN104099202A (en) * | 2014-07-10 | 2014-10-15 | 无锡蚕魅科技有限公司 | Mixed fibroin amino acid beer and production technology thereof |
| CN106420431A (en) * | 2016-11-25 | 2017-02-22 | 江苏爱西施科技服务咨询股份有限公司 | Anti-senescence silk cosmetic and preparation method thereof |
| CN108244657A (en) * | 2018-01-12 | 2018-07-06 | 海南蛛王药业有限公司 | A kind of method for hydrolysis of spider silk |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107142A (en) * | 1986-10-11 | 1988-04-20 | 山东省烟台桑蚕原种场 | A kind of method of from broken silkworm cocoon, extracting silk fibroin powder |
| CN1152410A (en) * | 1995-12-21 | 1997-06-25 | 无锡永新日用化学品有限公司 | Nutritious foodstuff-silk extract made from natural silk and making method |
| JP2000093091A (en) * | 1998-09-25 | 2000-04-04 | Gakuei O | Wild silkworm water-soluble silk powder and its production |
| KR20010079286A (en) * | 2001-07-03 | 2001-08-22 | 주육현 | Method of manufacturing by hydrochloric acid hydrolysis method in the production of functional silk amino acid peptide material using cocoon |
-
2003
- 2003-10-31 CN CNB2003101061837A patent/CN1313015C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107142A (en) * | 1986-10-11 | 1988-04-20 | 山东省烟台桑蚕原种场 | A kind of method of from broken silkworm cocoon, extracting silk fibroin powder |
| CN1152410A (en) * | 1995-12-21 | 1997-06-25 | 无锡永新日用化学品有限公司 | Nutritious foodstuff-silk extract made from natural silk and making method |
| JP2000093091A (en) * | 1998-09-25 | 2000-04-04 | Gakuei O | Wild silkworm water-soluble silk powder and its production |
| KR20010079286A (en) * | 2001-07-03 | 2001-08-22 | 주육현 | Method of manufacturing by hydrochloric acid hydrolysis method in the production of functional silk amino acid peptide material using cocoon |
Non-Patent Citations (3)
| Title |
|---|
| 丝素粉的功能性及其研究进展 孔祥东等，蚕桑通报，第31卷第4期 2000 * |
| 丝素粉的功能性及其研究进展 蚕桑通报，第31卷第4期 2000 * |
| 丝素粉的功能性及其研究进展 蚕桑通报，第31卷第4期 2000;丝素粉的功能性及其研究进展 孔祥东等，蚕桑通报，第31卷第4期 2000 * |
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| CN1539309A (en) | 2004-10-27 |
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Granted publication date: 20070502 Termination date: 20091130 |