CN101613937A - The bionical method for strengthening of silk-fibroin compound system of silk historical relic - Google Patents
The bionical method for strengthening of silk-fibroin compound system of silk historical relic Download PDFInfo
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- CN101613937A CN101613937A CN200910101493A CN200910101493A CN101613937A CN 101613937 A CN101613937 A CN 101613937A CN 200910101493 A CN200910101493 A CN 200910101493A CN 200910101493 A CN200910101493 A CN 200910101493A CN 101613937 A CN101613937 A CN 101613937A
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Abstract
A kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic is characterized in that adopting following steps: A) put silk into boiled Na
2CO
3Come unstuck in the solution, 30min pulls out and wrings out, and repeats once; Clean oven dry; B) above-mentioned silk is placed salting liquid, 70 ℃ are stirred 5～90min, and cold filtration was dialysed 3 days, evaporate silk fibroin solution; C) above-mentioned solution is mixed with ethylene glycol bisthioglycolate glycidyl diethyl ether solution, stir; D) the silk historical relic is placed above-mentioned mixed liquor, 20～60 ℃, 20～60min takes out, the silk historical relic after obtaining reinforcing.Advantage of the present invention is: intensity, the minimizing that 1) can increase the silk historical relic are reinforced the historical relic Effect on Performance; 2) method is easy, and cost is low, effective; 3) under the condition of normal temperature and neutrality, repair the fibroin molecule that ruptures, and historical relic is not produced harmful effect; 4) strengthening agent is nontoxic, harmless, pollution-free, meets the trend of environmental protection development.
Description
Technical field
The present invention relates to a kind of guard method of silk historical relic, particularly a kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic.
Background technology
Raw material-the silk of silk is natural protein fibre, and it borrows the peptide bond effect to connect the natural macromolecular material that forms by amino acid.Comparing with the historical relic of inorganic classifications such as pottery, metal, because the organic material characteristic of silk goods is determining it very easily to be subjected to the infringement of microorganism and insect, is the source of nutrition of microbial reproduction growth; Thermo-oxidative ageing, light aging effect very easily take place in these organic high molecular compounds, make high molecular strand take place to destroy and degrade; Simultaneously, hydrophilic radicals such as the hydroxyl in these amino acid, carboxyl and amino make fabric have stronger hygroscopicity, very easily absorb the moisture in air or the soil, thereby have quickened the aging of silk goods, and its intensity is reduced greatly.Although look complete as new as the silk goods that are unearthed in the Han tomb at Mawangdui of Changsha, the dyeing floridity, and in fact the chemical constitution of fiber and physical property are damaged already or weaken, tentacle becomes mud, is unable to undergo disturbance.For a long time, how these silk historical relics are protected processing, be that archaeological circle faces a difficult problem of one always.
At present both at home and abroad the method for reinforcing and protecting to the silk historical relic mainly contains the needlework method, mounts the holder method, braiding method for strengthening, silk net reinforcing method, group draw synthetic fibre vacuum coating method, resin method for strengthening, grafting copolymerization process etc.; but all there is certain defective in these methods, and application is restricted.
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 on the Chinese patent communique by common that propose, the number of patent application of Institutes Of Technology Of Zhejiang, China Silk Museum is 200810063254.2 application for a patent for invention, 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; By common that propose, the number of patent application of Institutes Of Technology Of Zhejiang, China Silk Museum is the application for a patent for invention of 200810122093.X; it relates to a kind of " protectant preparation of fibroin reinforcement and application "; this method utilization and silk historical relic identical materials-fibroin prepare strengthening agent, and described fibroin strengthening agent is made of fibroin solution and auxiliary agent diglycidyl diethyl ether solution two parts.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists; provide a kind of method easy; low, the effective silk historical relic's protection of cost method, intensity, the minimizing that can effectively increase the silk historical relic are reinforced the historical relic Effect on Performance, help the protection of silk historical relic.The present invention utilizes fibroin albumen in the silk as the stock of bionical reinforcing, selects eco-friendly ethylene glycol bisthioglycolate glycidyl ethyl ether Polyethylene GlycolDigycidyl Ether (PGDE) as reinforcing auxiliary agent, forms the silk-fibroin compound system.At first with the big Molecular Adsorption of the fibroin in the silk fibroin solution to the silk historical relic, utilize the acting in conjunction of big molecule of fibroin and auxiliary agent ethylene glycol bisthioglycolate glycidyl ethyl ether that the silk historical relic is reinforced then.
A kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic is characterized in that adopting following steps:
A) silk is put into to boil concentration expressed in percentage by weight be 0.5% Na
2CO
3Come unstuck in the aqueous solution, behind the 30min silk is pulled out and wrung out; Repeat aforesaid operations once, will clean to there not being soapy feeling through the silk that comes unstuck after handling with deionized water then, carry out again in 50～80 ℃ of oven dry of temperature; The weight of silk is that concentration expressed in percentage by weight is 0.5% Na
2CO
31% of aqueous solution weight;
B) will be through A) silk fiber after handling places salting liquid, at 70 ℃ of following stirring and dissolving 5～90min of temperature, cool off then, filter, the filtrate that the obtains bag filter of packing into was placed deionized water dialysis 3 days, again the dialysis solution that obtains is carried out evaporation and concentration and obtain the higher silk fibroin solution of concentration; Salting liquid is LiBr, CH
3OH and H
2The mixed liquor of O, wherein the weight of LiBr is 40%～60% of mixed liquor weight, CH
3The weight of OH is 20%～40% of mixed liquor weight, H
2The weight of O is 10%～30% of mixed liquor weight, and the weight of silk fiber is 2% of salting liquid weight;
C) will be by B) concentration expressed in percentage by weight that obtains be 0.5%～4% silk fibroin solution with concentration expressed in percentage by weight is that 2%～20% ethylene glycol bisthioglycolate glycidyl diethyl ether solution mixes, and stirs 1～3min, obtains mixed solution; The weight of ethylene glycol bisthioglycolate glycidyl diethyl ether solution is 0.5～10 times of silk fibroin solution weight;
D) the silk historical relic is immersed C) handle in the mixed solution that obtains, at 20～60 ℃ of temperature dipping 20～60min down, take out the silk historical relic then, under 20～50 ℃ of temperature, dried in the air the silk historical relic after promptly obtaining reinforcing 2 days.
Described silk fiber is a kind of silk cocoon, perhaps useless silk.
Compared with the prior art, advantage of the present invention is: intensity, the minimizing that 1) can effectively increase the silk historical relic are reinforced the historical relic Effect on Performance, help the protection of silk historical relic; 2) method is easy, and cost is low, effective; 3) under the pH condition of normal temperature and neutrality, repair the fibroin molecule of fracture, and silk fabrics is not produced harmful effect; 4) strengthening agent is nontoxic, harmless, pollution-free to environment, meets the trend of environmental protection development.
The specific embodiment
Embodiment 1:
A kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic is characterized in that adopting following steps:
A) silk is put into to boil concentration expressed in percentage by weight be 0.5% Na
2CO
3Come unstuck in the aqueous solution, behind the 30min silk is pulled out and wrung out; Repeat aforesaid operations once, will clean to there not being soapy feeling through the silk that comes unstuck after handling with deionized water then, carry out again in 50 ℃ of oven dry of temperature; The weight of silk is that concentration expressed in percentage by weight is 0.5% Na
2CO
31% of aqueous solution weight;
B) will be through A) silk fiber after handling places salting liquid, at 70 ℃ of following stirring and dissolving 5min of temperature, cool off then, filter, the filtrate that the obtains bag filter of packing into was placed deionized water dialysis 3 days, again the dialysis solution that obtains is carried out evaporation and concentration and obtain the higher silk fibroin solution of concentration; Salting liquid is LiBr, CH
3OH and H
2The mixed liquor of O, wherein the weight of LiBr is 40% of mixed liquor weight, CH
3The weight of OH is 40% of mixed liquor weight, H
2The weight of O is 20% of mixed liquor weight, and the weight of silk fiber is 2% of salting liquid weight;
C) will be by B) concentration expressed in percentage by weight that obtains be 0.5% silk fibroin solution with concentration expressed in percentage by weight is that 2% ethylene glycol bisthioglycolate glycidyl diethyl ether solution mixes, and stirs 1min, obtains mixed solution; The weight of ethylene glycol bisthioglycolate glycidyl diethyl ether solution is 0.5 times of silk fibroin solution weight;
D) the silk historical relic is immersed C) handle in the mixed solution that obtains, at 20 ℃ of temperature dipping 20min down, take out the silk historical relic then, under 20 ℃ of temperature, dried in the air the silk historical relic after promptly obtaining reinforcing 2 days.
Embodiment 2:
A kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic is characterized in that adopting following steps:
A) silk is put into to boil concentration expressed in percentage by weight be 0.5% Na
2CO
3Come unstuck in the aqueous solution, behind the 30min silk is pulled out and wrung out; Repeat aforesaid operations once, will clean to there not being soapy feeling through the silk that comes unstuck after handling with deionized water then, carry out again in 80 ℃ of oven dry of temperature; The weight of silk is that concentration expressed in percentage by weight is 0.5% Na
2CO
31% of aqueous solution weight;
B) will be through A) silk fiber after handling places salting liquid, at 70 ℃ of following stirring and dissolving 90min of temperature, cool off then, filter, the filtrate that the obtains bag filter of packing into was placed deionized water dialysis 3 days, again the dialysis solution that obtains is carried out evaporation and concentration and obtain the higher silk fibroin solution of concentration; Salting liquid is LiBr, CH
3OH and H
2The mixed liquor of O, wherein the weight of LiBr is 60% of mixed liquor weight, CH
3The weight of OH is 20% of mixed liquor weight, H
2The weight of O is 20% of mixed liquor weight, and the weight of silk fiber is 2% of salting liquid weight;
C) will be by B) concentration expressed in percentage by weight that obtains be 4% silk fibroin solution with concentration expressed in percentage by weight is that 20% ethylene glycol bisthioglycolate glycidyl diethyl ether solution mixes, and stirs 3min, obtains mixed solution; The weight of ethylene glycol bisthioglycolate glycidyl diethyl ether solution is 10 times of silk fibroin solution weight;
D) the silk historical relic is immersed C) handle in the mixed solution that obtains, at 60 ℃ of temperature dipping 60min down, take out the silk historical relic then, under 50 ℃ of temperature, dried in the air the silk historical relic after promptly obtaining reinforcing 2 days.
Embodiment 3:
A kind of bionical method for strengthening of silk-fibroin compound system of silk historical relic is characterized in that adopting following steps:
A) silk is put into to boil concentration expressed in percentage by weight be 0.5% Na
2CO
3Come unstuck in the aqueous solution, behind the 30min silk is pulled out and wrung out; Repeat aforesaid operations once, will clean to there not being soapy feeling through the silk that comes unstuck after handling with deionized water then, carry out again in 65 ℃ of oven dry of temperature; The weight of silk is that concentration expressed in percentage by weight is 0.5% Na
2CO
31% of aqueous solution weight;
B) will be through A) silk fiber after handling places salting liquid, at 70 ℃ of following stirring and dissolving 50min of temperature, cool off then, filter, the filtrate that the obtains bag filter of packing into was placed deionized water dialysis 3 days, again the dialysis solution that obtains is carried out evaporation and concentration and obtain the higher silk fibroin solution of concentration; Salting liquid is LiBr, CH
3OH and H
2The mixed liquor of O, wherein the weight of LiBr is 50% of mixed liquor weight, CH
3The weight of OH is 30% of mixed liquor weight, H
2The weight of O is 20% of mixed liquor weight, and the weight of silk fiber is 2% of salting liquid weight;
C) will be by B) concentration expressed in percentage by weight that obtains be 2% silk fibroin solution with concentration expressed in percentage by weight is that 11% ethylene glycol bisthioglycolate glycidyl diethyl ether solution mixes, and stirs 2min, obtains mixed solution; The weight of ethylene glycol bisthioglycolate glycidyl diethyl ether solution is 5 times of silk fibroin solution weight;
D) the silk historical relic is immersed C) handle in the mixed solution that obtains, at 40 ℃ of temperature dipping 40min down, take out the silk historical relic then, under 35 ℃ of temperature, dried in the air the silk historical relic after promptly obtaining reinforcing 2 days.
Claims (2)
1. the bionical method for strengthening of silk-fibroin compound system of a silk historical relic is characterized in that adopting following steps:
A) silk is put into to boil concentration expressed in percentage by weight be 0.5% Na
2CO
3Come unstuck in the aqueous solution, behind the 30min silk is pulled out and wrung out; Repeat aforesaid operations once, will clean to there not being soapy feeling through the silk that comes unstuck after handling with deionized water then, carry out again in 50～80 ℃ of oven dry of temperature; The weight of silk is that concentration expressed in percentage by weight is 0.5% Na
2CO
31% of aqueous solution weight;
B) will be through A) silk fiber after handling places salting liquid, at 70 ℃ of following stirring and dissolving 5～90min of temperature, cool off then, filter, the filtrate that the obtains bag filter of packing into was placed deionized water dialysis 3 days, again the dialysis solution that obtains is carried out evaporation and concentration and obtain the higher silk fibroin solution of concentration; Salting liquid is LiBr, CH
3OH and H
2The mixed liquor of O, wherein the weight of LiBr is 40%～60% of mixed liquor weight, CH
3The weight of OH is 20%～40% of mixed liquor weight, H
2The weight of O is 10%～30% of mixed liquor weight, and the weight of silk fiber is 2% of salting liquid weight;
C) will be by B) concentration expressed in percentage by weight that obtains be 0.5%～4% silk fibroin solution with concentration expressed in percentage by weight is that 2%～20% ethylene glycol bisthioglycolate glycidyl diethyl ether solution mixes, and stirs 1～3min, obtains mixed solution; The weight of ethylene glycol bisthioglycolate glycidyl diethyl ether solution is 0.5～10 times of silk fibroin solution weight;
D) the silk historical relic is immersed C) handle in the mixed solution that obtains, at 20～60 ℃ of temperature dipping 20～60min down, take out the silk historical relic then, under 20～50 ℃ of temperature, dried in the air the silk historical relic after promptly obtaining reinforcing 2 days.
2. the bionical method for strengthening of silk-fibroin compound system of silk historical relic according to claim 1 is characterized in that: silk fiber is a kind of silk cocoon, perhaps useless silk.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274089A (en) * | 2011-05-24 | 2011-12-14 | 苏州大学 | Silk fibroin tubular bracket and preparation method thereof |
| CN102359019A (en) * | 2011-08-18 | 2012-02-22 | 浙江理工大学 | Fibroin reinforcing method for fragile silk cultural relic |
| CN102359015A (en) * | 2011-08-18 | 2012-02-22 | 浙江理工大学 | Preparation method for biomimetic reinforcing agent of silk relics |
| CN102634972A (en) * | 2012-04-20 | 2012-08-15 | 浙江理工大学 | Method for preparing seriously contaminated antique silk substitution sample |
| CN102877299A (en) * | 2012-10-22 | 2013-01-16 | 中国科学技术大学 | Application of superoxide dismutase and trehalose mixture for textile ashing reaction inhibitor to textiles |
| CN103726306A (en) * | 2013-12-28 | 2014-04-16 | 杭州泛林科技有限公司 | Functional silk fiber preparation method using husks |
| CN109667176A (en) * | 2019-01-07 | 2019-04-23 | 梅丽玲 | The preparation method of modified fibroin albumen color fixing agent and its application in silk fixation |
| CN115478437A (en) * | 2022-10-14 | 2022-12-16 | 陕西科技大学 | Method for in-situ reinforcement of aged silk by silk fibroin/carboxymethyl chitosan composite material |
| CN115787297A (en) * | 2022-12-08 | 2023-03-14 | 达利(中国)有限公司 | Method for preparing fibroin finishing liquid and weight-increasing silk fabric by using waste silk fabric |
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2009
- 2009-08-10 CN CN200910101493A patent/CN101613937A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274089A (en) * | 2011-05-24 | 2011-12-14 | 苏州大学 | Silk fibroin tubular bracket and preparation method thereof |
| CN102359019A (en) * | 2011-08-18 | 2012-02-22 | 浙江理工大学 | Fibroin reinforcing method for fragile silk cultural relic |
| CN102359015A (en) * | 2011-08-18 | 2012-02-22 | 浙江理工大学 | Preparation method for biomimetic reinforcing agent of silk relics |
| CN102359015B (en) * | 2011-08-18 | 2013-04-17 | 浙江理工大学 | Preparation method for biomimetic reinforcing agent of silk relics |
| CN102634972A (en) * | 2012-04-20 | 2012-08-15 | 浙江理工大学 | Method for preparing seriously contaminated antique silk substitution sample |
| CN102877299B (en) * | 2012-10-22 | 2014-07-23 | 中国科学技术大学 | Application of superoxide dismutase and trehalose mixture for textile ashing reaction inhibitor to textiles |
| CN102877299A (en) * | 2012-10-22 | 2013-01-16 | 中国科学技术大学 | Application of superoxide dismutase and trehalose mixture for textile ashing reaction inhibitor to textiles |
| CN103726306A (en) * | 2013-12-28 | 2014-04-16 | 杭州泛林科技有限公司 | Functional silk fiber preparation method using husks |
| CN103726306B (en) * | 2013-12-28 | 2015-10-28 | 杭州泛林科技有限公司 | A kind of function silk fiber preparation method utilizing husks |
| CN109667176A (en) * | 2019-01-07 | 2019-04-23 | 梅丽玲 | The preparation method of modified fibroin albumen color fixing agent and its application in silk fixation |
| CN109667176B (en) * | 2019-01-07 | 2021-08-24 | 章华海 | Preparation method of modified silk fibroin color fixing agent and application of modified silk fibroin color fixing agent in silk color fixing |
| CN115478437A (en) * | 2022-10-14 | 2022-12-16 | 陕西科技大学 | Method for in-situ reinforcement of aged silk by silk fibroin/carboxymethyl chitosan composite material |
| CN115787297A (en) * | 2022-12-08 | 2023-03-14 | 达利(中国)有限公司 | Method for preparing fibroin finishing liquid and weight-increasing silk fabric by using waste silk fabric |
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Open date: 20091230 |