CN101397756B - Preparation and application of fibroin strengthening protecting agent - Google Patents
Preparation and application of fibroin strengthening protecting agent Download PDFInfo
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- CN101397756B CN101397756B CN200810122093XA CN200810122093A CN101397756B CN 101397756 B CN101397756 B CN 101397756B CN 200810122093X A CN200810122093X A CN 200810122093XA CN 200810122093 A CN200810122093 A CN 200810122093A CN 101397756 B CN101397756 B CN 101397756B
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- fibroin
- silk
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- ethylene glycol
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Abstract
The invention discloses a preparation of a protective agent for reinforcing fibroin and an application thereof. The protective agent is formed by two parts of fibroin solution and an auxiliary agent, namely, an ethylene glycol diglycidyl ether aqueous solution, and the preparation of the protective agent is that A) silk fiber is put into Na2CO3 solution and boiled for degumming; B) the silk fiberafter the treatment is put into a CaCl2 solution for dissolution at high temperature, and then dissolving liquor is cooled and filtered, and filtrate is put into a dialysis bag and arranged in deionized water for dialysis to obtain pure fibroin solution; C) the obtained fibroin solution is arranged in a spray drier for spraying and drying to form soluble fibroin powder, and reserved for later use; D) the soluble fibroin powder is used for preparing the fibroin solution by the deionized water; and E) the ethylene glycol diglycidyl ether aqueous solution is prepared; when in use, the fibroin solution is sprayed on silk to be reinforced and then the ethylene glycol diglycidyl ether aqueous solution is sprayed on the silk to be reinforced; the preparation can substantially improve the strength of fragile silk and is applied to the protection of silk cultural relics, and has the advantages of simple method, convenient operation, no influence on the appearance of the silk cultural relics, and the like.
Description
Technical field
That the present invention relates to is the protectant preparation method of a kind of fibroin reinforcement, belongs to the technical field of historical relic's protection.
Background technology
Silk is the symbol of Chinese mature culture.China all has a large amount of silk historical relics to be unearthed every year, these silk historical relics have been crossed over 6,000 years up and down, having very high history, archaeology and scientific value, is the important component part of China's historical relic, is research China successive dynasties politics, economy, art, the very important data in kind of scientific and technological aspects.Because silk protein is a kind of bioabsorbable polymer material, be easy to be subjected to multiple factor affecting and damaged, different factors such as extraneous water, heat, oxygen, illumination, acid, alkali, microorganism, the fracture of silk protein generation sex change and macromolecular chain is caused in the capital, make silk fiber tender, fracture easily, mechanical strength obviously descends.Manyly seem intact harmless, bright in colour silk historical relic when unearthed; actual in various with the acting in conjunction of external factor under; serious aging, embrittlement; that is to say that serious sex change has taken place silk protein and with the fracture of a large amount of macromolecular chains; if processing can not effectively be protected, be easy to damage.Inquiring into the method for reinforcing and protecting of silk historical relic, is urgent, an important problem of departments in charge of cultural and historical relics.
Both at home and abroad the past to the reinforcement protection of silk historical relic mainly contain the braiding method for strengthening, mount the holder method, coating method, silk net reinforcing method, resin method for strengthening, adhesive method for strengthening, group draw synthetic fibre vacuum coating method, grafting copolymerization process etc.
On the Chinese patent communique, disclose that propose by the Hubei Provincial Museum a, number of patent application and be 200410012737 application for a patent for invention, it relates to a kind of " the microorganism reinforcement means of no intensity silk ", this method is that carbohydrate and organic acid are converted into cellulose with acetobacter, thereby reaches the purpose of reinforcing no intensity silk.Also disclosing one on the Chinese patent communique is 200810063254.2 application for a patent for invention by common that propose, the number of patent application of Institutes Of Technology Of Zhejiang, China Silk Museum, it relates to a kind of " preparation method of fibroin strengthening agent ", this method is utilized with the historical relic identical materials--fibroin prepares strengthening agent, and this strengthening agent is made of fibroin solution and auxiliary agent glutaraldehyde solution two parts.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, and a kind of higher security that not only has is provided, and reinforce the protectant preparation of fibroin reinforcement and the application of the aspect better effects if such as color and luster of back silk historical relic.
The objective of the invention is to finish by following technical solution, this fibroin strengthening agent is made of fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts, and following steps are adopted in its preparation:
A) be to put into the Na of 0.5% weight percent concentration at 1: 40-60 by weight with silk fiber
2CO
3In the solution, boil and come unstuck 25-35 minutes;
B) will put into weight percent concentration by weight 1: 30～70 through the silk fiber of above-mentioned processing is 45-55% CaCl
2In the solution,, with the lysate cooling, filter, and filtrate packed in the bag filter, place deionized water to dialyse, promptly obtain pure fibroin solution after 72 hours 98 ± 2 ℃ of down dissolvings 30～120 minutes;
C) the fibroin solution that obtains being placed spray dryer, is 180～220 ℃ at EAT, carry out spray drying under the condition that leaving air temp is 70～95 ℃ after, make the solubility silk fibroin powder, stand-by;
B) before consolidation process, it is 0.1%～5% fibroin solution that above-mentioned solubility silk fibroin powder is configured to weight percent concentration with deionized water;
E) the ethylene glycol diglycidylether aqueous solution of preparation 0.01～10% weight percent concentration;
F) through above preparation process, obtain the fibroin reinforcement protective agent that constitutes by fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts.
Described silk fiber is a kind of cocoon layer or useless silk.
The present invention when using, earlier with the fibroin solution spraying to waiting to reinforce on the silk, again the ethylene glycol diglycidylether aqueous solution is sprayed to wait to reinforce on the silk and can reach the reinforcing purpose.
The present invention prepares fibroin strengthening agent with the fibroin solution and the ethylene glycol diglycidylether aqueous solution, reinforces fragile silk with it, can improve the intensity of fragile silk significantly, is used for the protection of silk historical relic.The present invention compared with the prior art, have following outstanding advantage: 1) method is simple, and is easy to operate; 2) do not influence the outward appearance of silk historical relic, and can partly recover the silky luster of historical relic; 3) outstanding superiority is arranged high temperature resistant aspect aging.
The specific embodiment
The present invention will be described in detail below in conjunction with specific embodiment.
Embodiment 1, and fibroin strengthening agent of the present invention is to be made of fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts, and following steps are adopted in its preparation:
A) be to put into the Na of 0.5% weight percent concentration at 1: 50 by weight with silk fiber
2CO
3In the solution, boil and come unstuck 30 minutes;
B) will put into weight percent concentration by weight 1: 50 through the silk fiber of above-mentioned processing is 50% CaCl
2In the solution,, with the lysate cooling, filter, and filtrate packed in the bag filter, place deionized water to dialyse, promptly obtain pure fibroin solution after 72 hours 98 ℃ of down dissolvings 80 minutes;
C) the fibroin solution that obtains being placed spray dryer, is 200 ℃ at EAT, carry out spray drying under the condition that leaving air temp is 70 ℃ after, make the solubility silk fibroin powder, stand-by;
D) before consolidation process, it is 2% fibroin solution that above-mentioned solubility silk fibroin powder is configured to weight percent concentration with deionized water;
E) the ethylene glycol diglycidylether aqueous solution of preparation 1% weight percent concentration;
F) through above preparation process, obtain the fibroin reinforcement protective agent that constitutes by fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts;
Described silk fiber is a kind of cocoon layer;
The present invention when using, earlier with the fibroin solution spraying to waiting to reinforce on the silk, again the ethylene glycol diglycidylether aqueous solution is sprayed to wait to reinforce on the silk and can reach the reinforcing purpose.
Embodiment 2, and fibroin strengthening agent of the present invention is to be made of fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts, and following steps are adopted in its preparation:
A) be to put into the Na of 0.5% weight percent concentration at 1: 40 by weight with silk fiber
2CO
3In the solution, boil and come unstuck 25 minutes;
B) will put into weight percent concentration by weight 1: 30 through the silk fiber of above-mentioned processing is 45% CaCl
2In the solution,, with the lysate cooling, filter, and filtrate packed in the bag filter, place deionized water to dialyse, promptly obtain pure fibroin solution after 72 hours 96 ℃ of down dissolvings 30 minutes;
C) the fibroin solution that obtains being placed spray dryer, is 180 ℃ at EAT, carry out spray drying under the condition that leaving air temp is 70 ℃ after, make the solubility silk fibroin powder, stand-by;
B) before consolidation process, it is 0.1% fibroin solution that above-mentioned solubility silk fibroin powder is configured to weight percent concentration with deionized water;
E) the ethylene glycol diglycidylether aqueous solution of preparation 0.01% weight percent concentration;
F) through above preparation process, obtain the fibroin reinforcement protective agent that constitutes by fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts;
Described silk fiber is a kind of useless silk;
The present invention when using, earlier with the fibroin solution spraying to waiting to reinforce on the silk, again the ethylene glycol diglycidylether aqueous solution is sprayed to wait to reinforce on the silk and can reach the reinforcing purpose.
Embodiment 3, and fibroin strengthening agent of the present invention is to be made of fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts, and following steps are adopted in its preparation:
A) be to put into the Na of 0.5% weight percent concentration at 1: 60 by weight with silk fiber
2CO
3In the solution, boil and come unstuck 35 minutes;
B) will put into weight percent concentration by weight 1: 70 through the silk fiber of above-mentioned processing is 55% CaCl
2In the solution,, with the lysate cooling, filter, and filtrate packed in the bag filter, place deionized water to dialyse, promptly obtain pure fibroin solution after 72 hours 100 ℃ of down dissolvings 120 minutes;
C) the fibroin solution that obtains being placed spray dryer, is 220 ℃ at EAT, carry out spray drying under the condition that leaving air temp is 95 ℃ after, make the solubility silk fibroin powder, stand-by;
B) before consolidation process, it is 5% fibroin solution that above-mentioned solubility silk fibroin powder is configured to weight percent concentration with deionized water;
E) the ethylene glycol diglycidylether aqueous solution of preparation 10% weight percent concentration;
F) through above preparation process, obtain the fibroin reinforcement protective agent that constitutes by fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts;
Described silk fiber is a kind of cocoon layer or useless silk;
The present invention when using, earlier with the fibroin solution spraying to waiting to reinforce on the silk, again the ethylene glycol diglycidylether aqueous solution is sprayed to wait to reinforce on the silk and can reach the reinforcing purpose.
Claims (3)
1. protectant preparation method of fibroin reinforcement, described fibroin strengthening agent is made of fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts, and following steps are adopted in its preparation:
A) be 1 by weight with silk fiber: 40-60 puts into the Na of 0.5% weight percent concentration
2CO
3In the solution, boil and come unstuck 25-35 minute;
B) will put into the CaCl that weight percent concentration is 45-55% by weight 1: 30～70 through the silk fiber of above-mentioned processing
2In the solution,, with the lysate cooling, filter, and filtrate packed in the bag filter, place deionized water to dialyse, promptly obtain pure fibroin solution after 72 hours 98 ± 2 ℃ of down dissolvings 30～120 minutes;
C) the fibroin solution that obtains being placed spray dryer, is 180～220 ℃ at EAT, carry out spray drying under the condition that leaving air temp is 70～95 ℃ after, make the solubility silk fibroin powder, stand-by;
D) before consolidation process, it is 0.1%～5% fibroin solution that above-mentioned solubility silk fibroin powder is configured to weight percent concentration with deionized water;
E) the ethylene glycol diglycidylether aqueous solution of preparation weight percent concentration 0.01～10%;
F) through above preparation process, obtain the fibroin reinforcement protective agent that constitutes by fibroin solution and auxiliary agent ethylene glycol diglycidylether aqueous solution two parts.
2. the protectant preparation method of fibroin reinforcement according to claim 1 is characterized in that described silk fiber is a kind of cocoon layer or useless silk.
3. protectant application of fibroin reinforcement as claimed in claim 1 or 2, it be earlier with the fibroin solution spraying to waiting to reinforce on the silk, again the ethylene glycol diglycidylether aqueous solution is sprayed to wait to reinforce on the silk and can reach the reinforcing purpose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810122093XA CN101397756B (en) | 2008-11-03 | 2008-11-03 | Preparation and application of fibroin strengthening protecting agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810122093XA CN101397756B (en) | 2008-11-03 | 2008-11-03 | Preparation and application of fibroin strengthening protecting agent |
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| CN101397756A CN101397756A (en) | 2009-04-01 |
| CN101397756B true CN101397756B (en) | 2010-09-08 |
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|---|---|---|---|
| CN200810122093XA Expired - Fee Related CN101397756B (en) | 2008-11-03 | 2008-11-03 | Preparation and application of fibroin strengthening protecting agent |
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| CN103603196B (en) * | 2013-10-24 | 2015-11-18 | 浙江理工大学 | A kind of keratin EGDE reinforces the method for fragile wool fabric |
| CN103572598B (en) * | 2013-10-24 | 2015-11-18 | 浙江理工大学 | A kind of keratin reinforcement process going out the fragile wool fabric of soil scene for historical relic |
| CN103614914B (en) * | 2013-10-24 | 2015-09-16 | 浙江理工大学 | A kind of keratin reinforcement method for fragile wool fabric |
| CN103668982A (en) * | 2013-11-29 | 2014-03-26 | 南通市通州区大达麻纺织有限公司 | Preparation method of fibroin finishing agent |
| CN103726336B (en) * | 2013-12-28 | 2015-10-28 | 杭州泛林科技有限公司 | A kind of preparation method of raw silk material |
| CN103911854B (en) * | 2013-12-28 | 2015-08-26 | 杭州泛林科技有限公司 | A kind of preparation method of health care silk clothes |
| CN104372611B (en) * | 2014-10-30 | 2016-05-18 | 浙江理工大学 | A kind of preparation technology who simulates classical Chinese painting on silk historical relic in ancient times |
| CN104372612B (en) * | 2014-10-30 | 2016-06-01 | 浙江理工大学 | A kind of preparation technology simulating ripe classical Chinese painting on silk historical relic in ancient times |
| CN105582744B (en) * | 2015-01-28 | 2017-12-19 | 武汉纺织大学 | A kind of silk nanofiber filtration material, its preparation method and its application |
| CN107419430A (en) * | 2015-09-01 | 2017-12-01 | 苏州先蚕丝绸生物科技有限公司 | A kind of feature silk non-woven fabric and its production method |
| CN105671958B (en) * | 2016-01-21 | 2017-11-28 | 苏州纳百奥生物科技有限公司 | The reinforcing liquid and reinforcement means of a kind of silk fabric cultural relics and application |
| CN110409179A (en) * | 2019-08-29 | 2019-11-05 | 浙江理工大学 | A kind of rotten silk quality historical relic strengthening agent of grain and its reinforcement means |
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| CN1116227A (en) * | 1994-08-05 | 1996-02-07 | 李秀芬 | Usage of sericin in durable material |
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| CN101397756A (en) | 2009-04-01 |
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