CN1019808B - Extract the method for silk-protein from carpet leftover bits and pieces waste silk - Google Patents
Extract the method for silk-protein from carpet leftover bits and pieces waste silkInfo
- Publication number
- CN1019808B CN1019808B CN90108729A CN90108729A CN1019808B CN 1019808 B CN1019808 B CN 1019808B CN 90108729 A CN90108729 A CN 90108729A CN 90108729 A CN90108729 A CN 90108729A CN 1019808 B CN1019808 B CN 1019808B
- Authority
- CN
- China
- Prior art keywords
- silk
- carpet
- protein
- waste silk
- leftover bits
- 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.)
- Expired
Links
Landscapes
- Peptides Or Proteins (AREA)
Abstract
Present method utilizes carpet leftover bits and pieces waste silk to be raw material, and the water-soluble silk-protein of Development and Production high-quality has that technology is simplified, cost reduces, the characteristics of no waste water.After it is characterized in that the acid hydrolysis waste silk, the minimum argon barium oxide of solubleness is neutralization materials in the employing bases, make it precipitation fully, be easy to purify, and filter once more with gac, one step of decolorization and purification finishes, and rejects residual trace huge sum of money prime element simultaneously, and quality product and purity are further enhanced.Present method is easy to apply in hand-made carpet industry and daily-use chemical industry industry.
Description
The present invention relates in natural materials, extract the method for water-soluble silk-protein, relate in particular to the method for from the silk carpet tankage, extracting silk-protein.
Natural silk contains rich in protein, and wherein eight seed amino acids of needed by human nearly all have.Therefore, silk fibroin is the good raw material of production high-quality makeup and other dietetic products.
Prior art is to extract silk-protein from the silk mill's tankage and a piques of breeding silkworms, and its method or processing step are more, or cost investment is higher, and raw material is with ash impurity residual quantity to be difficult to the greatest extent, and final product quality is relative with purity to be difficult to raising.As CN1038282 and CN8510742 two examples, the former will adopt ion exchange method further to purify, and the latter will use organic solvent extraction, and step is more beyond doubt, and cost is higher.The more important thing is that these two kinds of prior aries all can not be with carpet, the leftover bits and pieces waste silk is a raw material.
The used real silk raw material of silk carpet is 100% mulbery spun silk.The leftover bits and pieces waste silk that silk carpet produces in the course of processing is that staple length is silk head and the silk powder about 5mm, and the processing of can't respinning for a long time, is abandoned it as refuse entirely.Because the carpet waste silk is process dyeing and other processing entirely, has various dye well auxiliary agents, the composition complexity.Utilize prior art, can not obtain purified silk peptide product, so be difficult to use.
The invention reside in and utilize carpet leftover bits and pieces waste silk to be raw material, the water-soluble silk-protein of high-quality (silk peptide, fibroin amino acid) is extracted in processing, both the carpet waste silk can be used, and can be the production silk-protein again and opens up abundant resource.The invention provides a kind of method, comprise the acid hydrolysis waste silk, in the alkali and after-filtration, use the gac heating and filtering again after it is characterized in that filtering, decolorization and purification becomes liquid product, and perhaps revaporization is dried to solid phase prod subsequently.Its technology is:
1, with clean carpet leftover bits and pieces waste silk, with 4-8N sulfuric acid (H
2SO
4) hydrolysis, be heated to 37 ℃-110 ℃, kept 15-40 hour, obtain the complete aqueous solution.By the antacid concentration of used water, Heating temperature and the control of the difference of hold-time, can finally obtain the different product of molecular weight.
2, with hydrated barta-Ba(OH)
2Add aqueous solution neutralization, add-on is the 1.0-3.0 of aqueous solution acid equivalent: 1, be heated to 30 ℃-50 ℃, and constant temperature 1-2 hour, the adjustment pH value was 6.8-7.2.Used hydrated barta is a solubleness minimum in the bases, so precipitation, is convenient to purify fully.Therefore, can save ion-exchange step and alcohol extraction technology.
3, with 100 orders with upper screen cloth vacuum filtration or press filtration, filter is precipitated solid impurity to the greatest extent, clear liquid.Add 100 order to the 400 order gacs of the 30%-50% of clear liquid weightmeasurement ratio, be heated to 30 ℃-50 ℃, dyestuff that raw material is with is fully adsorbed by gac.Select for use the above gac of 200 orders preferable, and 300 orders are above best.
4, with vacuum filtration or press filtration, filter is the dye well auxiliary agent to the greatest extent, must be the light amber liquid product, and then, as required, but reconcentration, crystallization get solid phase prod.
Adopt above method, utilize carpet lower temple processing silk-protein (silk peptide, fibroin amino acid), waste silk utilization ratio height, liquid and solid phase prod are respectively 2 to 3 times and 0.2 to 0.4 times of waste silk raw material; The product purity height, quality is good, and the liquid product protein content is 12.5% to 16.9%, and the solid phase prod protein content is more than 99%, and the ash foreign matter content is less than 1%, and trace elements lead, mercury, arsenic are all less than 1ppa; Technology is easy, and cost savings are purified simultaneously with activated carbon decolorizing, saves ion-exchange or alcohol extraction technology; No waste water does not need attached sewage disposal device.Therefore, present method has technology simplifies, and cost reduces, and advantages such as no waste water are easy to apply at hand-made carpet and daily-use chemical industry industry.
Embodiment (one) (in carpet waste silk 1000 grams)
With 2700ml4N sulphuric acid hydrolysis waste silk, be heated to 100 ℃, kept 38 hours, get the aqueous solution.Add 1800 gram hydrated barta neutralizations, be heated to 60 ℃, adjust PH=6.8, get clear liquid with 300 screen cloth suction filtrations.Add 300 order gacs, 1000 grams, be heated to 60 ℃, decolorization and purification must be light amber liquid product 2800ml through vacuum filtration.Evaporation drying gets solid phase prod 400 grams then.The product protein content is more than 99%, lead, mercury, arsenic content＜1ppm, no ash, salt.
Embodiment (two) (in carpet waste silk 1000 grams)
With 2400ml6N sulphuric acid hydrolysis waste silk, be heated to 90 ℃, kept 30 hours, get the aqueous solution.Add 2200 gram hydrated barta neutralizations again, be heated to 60 ℃ and adjust PH=7.1, get clear liquid with 200 eye mesh screen suction filtrations.Add 300 order gacs, 1000 grams, be heated to 60 ℃ of decolorization and purification, get light amber liquid product 2400ml through vacuum filtration.Product test value: nitrogen content 2.5, (protein content is about 15.6%), lead, mercury, arsenic content＜1ppm, no ash, salt.
Embodiment (three) (in carpet waste silk 1000 grams)
With the sulphuric acid hydrolysis carpet waste silk of 1900ml8N, ordinary-temp hydrolysis 3 hours is heated to 80 ℃, keeps 15 hours, gets the aqueous solution.Add hydrated barta 3000 gram neutralizations, be heated to 60 ℃, adjust PH=6.8, get clear liquid with 300 eye mesh screen suction filtrations.Add 100 order gacs, 1000 grams, be heated to 60 ℃, decolorization and purification must be light amber liquid product 1900ml through vacuum filtration.Its molecular-weight average 150, nitrogen content are 2.2, (protein content is about 13.8%), lead, mercury, arsenic content＜1ppm, the ash content of coal＜1.
Claims (5)
1, a kind of method of extracting water-soluble silk-protein from carpet leftover bits and pieces waste silk comprises the acid hydrolysis waste silk, desalts with after-filtration in the alkali, use the gac heating and filtering again after it is characterized in that filtering, one step of decolorization and purification finishes, and becomes liquid product, or reheat evaporation subsequently, drying crystalline becomes solid phase prod.
2, according to the method for claim 1, it is characterized in that used acid is sulfuric acid, concentration is 4-8N, is heated to 37 ℃-110 ℃, keeps 15-40 hour.
3, according to the method for claim 1, it is characterized in that adopting the hydrated barta neutralization, consumption is the 1.0-3.0 of acid equivalent: 1.
4, according to the process of claim 1 wherein that alkali is neutralized to PH=6.8-7.2.
5, according to the process of claim 1 wherein the gac that uses at 100 order to 400 orders, consumption is the 30%-50% of hydrolysis clear liquid weightmeasurement ratio (W/V), is heated to 30 ℃-50 ℃, keeps 1-2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90108729A CN1019808B (en) | 1990-10-31 | 1990-10-31 | Extract the method for silk-protein from carpet leftover bits and pieces waste silk |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90108729A CN1019808B (en) | 1990-10-31 | 1990-10-31 | Extract the method for silk-protein from carpet leftover bits and pieces waste silk |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1050197A CN1050197A (en) | 1991-03-27 |
| CN1019808B true CN1019808B (en) | 1992-12-30 |
Family
ID=4881100
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90108729A Expired CN1019808B (en) | 1990-10-31 | 1990-10-31 | Extract the method for silk-protein from carpet leftover bits and pieces waste silk |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1019808B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061685C (en) * | 1995-05-24 | 2001-02-07 | 复旦大学 | Regenerated silk protein and complex material thereof for fixation of enzyme and bio-active substance |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101402C (en) * | 1998-12-01 | 2003-02-12 | 浙江丝绸工学院 | Sericin polypeptide extracted from frison, husks and waste silk and its extracting method |
| CN1099424C (en) * | 1998-12-22 | 2003-01-22 | 金明官 | Catalytic circular preparation of fibroin peptide |
| CN102584430B (en) * | 2012-01-10 | 2013-07-24 | 广西工学院 | Method for manufacturing amino-acid fishpond fertilizer water aqua by waste bave protein |
| CN108276484B (en) * | 2018-04-03 | 2021-08-03 | 辽宁省农业科学院大连生物技术研究所 | Method for preparing tussah silk fibroin peptide by step temperature-controlled hydrolysis |
-
1990
- 1990-10-31 CN CN90108729A patent/CN1019808B/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061685C (en) * | 1995-05-24 | 2001-02-07 | 复旦大学 | Regenerated silk protein and complex material thereof for fixation of enzyme and bio-active substance |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1050197A (en) | 1991-03-27 |
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| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application |