CN86107142A - A kind of method of from broken silkworm cocoon, extracting silk fibroin powder - Google Patents
A kind of method of from broken silkworm cocoon, extracting silk fibroin powder Download PDFInfo
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- CN86107142A CN86107142A CN 86107142 CN86107142A CN86107142A CN 86107142 A CN86107142 A CN 86107142A CN 86107142 CN86107142 CN 86107142 CN 86107142 A CN86107142 A CN 86107142A CN 86107142 A CN86107142 A CN 86107142A
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- silk fibroin
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Abstract
A kind of method of extracting silk fibroin powder that provides is provided, present method is raw material with the broken silkworm cocoon, with hydrogen peroxide dipping handle, extract fibroin, produce the hydrolyzed-silk fibroin, ethanol purification secondary, three vacuum filtrations, freeze-day with constant temperature pulverize, be silk fibroin powder product after 120 mesh sieves handled, product can be widely used in daily-use chemical industry and medicine and other fields.
Description
The invention belongs to a kind of method of extracting silk fibroin powder from broken silkworm cocoon in the chemical industry technology, products obtained therefrom can be widely used in daily-use chemical industry, medicine and other fields.
Silk fibroin powder is by extracting in the silk (cocoon), contain multiple essential amino acid, as the nutritional additive of serial cosmetics, skin being had good maintenance action; Add in the tetter externally used paste,, significantly auxiliary curative effect is also arranged treating for skin disease.
Present domestic production silk fibroin powder, be raw material mainly with reeling waste thing such as waste silk, recotti, long tell etc., add steam boiling with the diluted alkaline immersion, to remove impurity and part silk gum, after rinsing with 5～6% caustic lye of soda heating hydrolysis, after adjusting pH value with hydrochloric acid, the silk fibroin precipitation is separated out, promptly as rough silk fibroin as modulation used for cosmetic base-material.Extract silk fibroin with above-mentioned raw materials and method, because of adopting basic hydrolysis, make amino acid produce racemization, partly amino acid is destroyed, add the high temperature cocoon drying of reeling waste thing behind cocoon purchasing, so the silk fibroin color and luster that extracts jaundice, bad dispersibility in water and oil phase, inner quality is poor.The useful 1.2N hydrochloric acid of Japan under 60-70 ℃, heats 24 hours hydrolyzed-silk fibroins, with powerful stir (10000rpm), obtain powdery precipitate again, the dilute sodium hydroxide rinsing of centrifugal back, until neutrality or slight alkalinity, be ground into the raw silk pulvis with 200 order ball mills behind the centrifuge dripping.Aforesaid method is because of without coming unstuck and purifying, and impurities is more, and products obtained therefrom only is the raw silk pulvis.
At above-mentioned deficiency, the objective of the invention is to utilize broken silkworm cocoon (silkworm production of hybrid seeds field byproduct) is raw material, by safe and reliable method, extracts still and can perfection keep natural silk characteristic, the silk fibroin powder that use value is higher.
Main points of the present invention are: be raw material with the broken silkworm cocoon, through hydrogen peroxide dipping handle, extract fibroin, produce the hydrolyzed-silk fibroin, ethanol purification secondary, three vacuum filtrations.Its technology is as follows:
1. broken silkworm cocoon is handled with hydrogen peroxide dipping, and hydrogen peroxide concentration is 0.5-1.2%, and under 50-60 ℃ of temperature, constant temperature is protected 40-65 minute, pulls out with water extracter to dry.
2. extraction fibroin.With the broken silkworm cocoon after the hydrogen peroxide dipping processing; put into glass-lined reactor; add the 0.3-0.9% sodium hydrogen carbonate solution; pH value is 9-11; under 80-100 ℃ of temperature, constant temperature protection 25-60 minute is pulled out with water extracter and is dried the after washing dealkalize; making pH value is 6-7, is purer fibroin after the thorough drying.
3. produce the hydrolyzed-silk fibroin.With above-mentioned dry fibroin; put into glass-lined reactor; adding 0.5-1.1N hydrochloric acid is hydrolyzed; temperature is 50-60 ℃; constant temperature protection 25-32 hour; pulling out and drying the back with water extracter is 6-7 with 0.15-0.32N sodium hydroxide adjustment pH value, does with the vacuum filtration filter after washing, and is rough hydrolyzed-silk fibroin.
Above-mentioned rough silk fibroin with the ethanol secondary of purifying, further to remove residual impurity, the concentration of ethanol purification for the first time is 60-85%, through 1.5-6 hour, do with the vacuum filtration filter, the concentration of ethanol purification for the second time is 60-85%, after 1.5-6 hour, do with the vacuum filtration filter, be refining sik fibroin.
5. with above-mentioned refining sik fibroin, with 55-68 ℃ of freeze-day with constant temperature, to pulverize after behind 120 mesh sieves, be silk fibroin powder product, yield is 60-66%.
Embodiment 1.(raw material is a broken silkworm cocoon, in 7.5 kilograms)
(1), broken silkworm cocoon handles with 0.55% hydrogen peroxide dipping earlier, temperature is 57 ℃, constant temperature is protected 60 fens, pulls out with water extracter to dry.(2), extract fibroin.Broken silkworm cocoon after hydrogen peroxide dipping is handled is put into glass-lined reactor, use 0.85% sodium hydrogen carbonate solution, pH value is 10.5, and under 82 ℃ of temperature, constant temperature protection 35 minutes is pulled out with the water extracter drying, and it is 6.5 that the washing dealkalize makes pH value, thorough drying.(3), produce the hydrolyzed-silk fibroin.With above-mentioned dry fibroin, put into glass-lined reactor, add 0.55N hydrochloric acid and be hydrolyzed, under 59 ℃ of temperature, constant temperature protection 31 hours, pulling the back out is 6 with 0.18N sodium hydroxide adjustment pH value, does with the vacuum filtration filter after washing, and promptly gets rough silk fibroin.(4), above-mentioned rough silk fibroin is purified with 65% ethanol, the time is 4.5 hours, after the vacuum filtration filter is done, puts into 75% ethanol again and carries out second time and purify, and is through 2.5 hours, dried with the vacuum filtration filter.(5), with the back silk fibroin oven dry of will purifying of 57 ℃ of constant temperature, pulverize after 120 mesh sieves are silk fibroin powder product, yield is 62%.
According to above-mentioned implementation method and raw material gained silk fibroin powder, through item-dividing test, wherein contained essential amino acid of its protein content＞97%(such as Threonine are 1.1%, leucine 0.6%, Isoleucine 1.0%, phenylalanine 1.3%), whiteness 70-75 degree, weight loss on drying≤3%, ignition residue≤1.2%, poisonous micro-AS, Hg do not detect Pb＜0.05PPm, skin feel: profit, sliding, refreshing, good dispersion property in water, oil phase.
Embodiment 2(raw material is in 10 kilograms of broken silkworm cocoons)
(1), broken silkworm cocoon handles with 1.1% hydrogen peroxide dipping earlier, under 57 ℃ of temperature, constant temperature is protected 45 minutes, pulls out with water extracter to dry.(2), extract fibroin.Put into glass-lined reactor with above-mentioned with the broken silkworm cocoon after the hydrogen peroxide dipping processing, add 0.4% sodium hydrogen carbonate solution, pH value is 9; under 98 ℃ of temperature, constant temperature is protected 55 minutes, pulls out with water extracter to dry; the washing dealkalize, making pH value is 6.5, is purer fibroin after the thorough drying.(3), produce the hydrolyzed-silk fibroin.With above-mentioned dry fibroin, put into glass-lined reactor, add 1.0N hydrochloric acid and be hydrolyzed; temperature is 52 ℃, and constant temperature protection 25 hours is pulled out with after the water extracter drying; adjusting pH value with 0.30N sodium hydroxide is 6.5, and the filter of washing final vacuum suction filtration is done, and is rough silk fibroin.(4), above-mentioned silk fibroin is purified with 65% ethanol, further to remove residual impurity, through 4 hours, after doing with the vacuum filtration filter, put into 80% ethanol again and carry out second time and purify, through 2.5 hours, the vacuum filtration filter was dried.(5), with 64 ℃ of constant temperature, the silk fibroin oven dry with after purifying through 120 mesh sieves, is silk fibroin powder product after the pulverizing, yield is 64.5%.
Claims (6)
1, a kind of extracting method of silk fibroin powder is characterized in that with the broken silkworm cocoon being raw material, with hydrogen peroxide dipping handle, extract fibroin, produce the hydrolyzed-silk fibroin, ethanol purification secondary, three vacuum filtrations.
2, by the extracting method of the described a kind of silk fibroin powder of claim 1, it is characterized in that broken silkworm cocoon 0.5-1.2% hydrogen peroxide dipping processing, temperature is 50-60 ℃, constant temperature protection 40-65 minute.
3, by the extracting method of the described a kind of silk fibroin powder of claim 1, it is characterized in that extracting the broken silkworm cocoon after fibroin is handled with hydrogen peroxide dipping, add the 0.3-0.9% sodium hydrogen carbonate solution, under 80-100 ℃ of temperature, constant temperature protection 25-60 minute.
4, by the extracting method of the described a kind of silk fibroin powder of claim 1, it is characterized in that producing the hydrolyzed-silk fibroin after extracting fibroin, be hydrolyzed with 0.5-1.1N hydrochloric acid, temperature is 50-60 ℃, constant temperature protection 25-32 hour.
5, press the extracting method of the described a kind of silk fibroin powder of claim 1, it is characterized in that ethanol purification secondary, extraction using alcohol is after producing the hydrolyzed-silk fibroin for the first time, for the second time ethanol purify the first time ethanol purify and vacuum filtration after, ethanol purification secondary concentration is 60-80%, and the time is 1.5-6 hour.
6, by the described a kind of silk fibroin powder extracting method of claim 1, it is characterized in that vacuum filtration three times, for the first time after producing the hydrolyzed-silk fibroin, for the second time after the first time, ethanol was purified, for the third time after the second time, ethanol was purified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86107142 CN86107142A (en) | 1986-10-11 | 1986-10-11 | A kind of method of from broken silkworm cocoon, extracting silk fibroin powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86107142 CN86107142A (en) | 1986-10-11 | 1986-10-11 | A kind of method of from broken silkworm cocoon, extracting silk fibroin powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN86107142A true CN86107142A (en) | 1988-04-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86107142 Pending CN86107142A (en) | 1986-10-11 | 1986-10-11 | A kind of method of from broken silkworm cocoon, extracting silk fibroin powder |
Country Status (1)
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| CN (1) | CN86107142A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005085327A1 (en) * | 2004-03-04 | 2005-09-15 | Yuqing Zhang | A method of producing nanosize fibroin particle |
| CN1313015C (en) * | 2003-10-31 | 2007-05-02 | 湖州澳特丝生物化工有限公司 | Method for producing powder for refining silk |
| CN101718007B (en) * | 2009-11-26 | 2012-05-02 | 郭筱洁 | Production method of regenerated silk protein fiber |
| CN103897021A (en) * | 2013-02-04 | 2014-07-02 | 中国科学院上海有机化学研究所 | Silk peptide as well as preparation method and application thereof |
| CN110551192A (en) * | 2019-09-16 | 2019-12-10 | 姚建林 | extraction method of silk peptide protein |
-
1986
- 1986-10-11 CN CN 86107142 patent/CN86107142A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313015C (en) * | 2003-10-31 | 2007-05-02 | 湖州澳特丝生物化工有限公司 | Method for producing powder for refining silk |
| WO2005085327A1 (en) * | 2004-03-04 | 2005-09-15 | Yuqing Zhang | A method of producing nanosize fibroin particle |
| CN101718007B (en) * | 2009-11-26 | 2012-05-02 | 郭筱洁 | Production method of regenerated silk protein fiber |
| CN103897021A (en) * | 2013-02-04 | 2014-07-02 | 中国科学院上海有机化学研究所 | Silk peptide as well as preparation method and application thereof |
| CN103897021B (en) * | 2013-02-04 | 2016-06-29 | 中国科学院上海有机化学研究所 | Silk peptide, preparation method and application |
| CN110551192A (en) * | 2019-09-16 | 2019-12-10 | 姚建林 | extraction method of silk peptide protein |
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Correction item: Agency|Agent Correct: Yantai Patent Agency|Zhang Yaping False: Missing agency|Agent Number: 16 Page: 25 Volume: 4 |
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