CN101613936B - Method for compound-enhancing fibroin-self-crosslinking adhesive of silk antiquity - Google Patents
Method for compound-enhancing fibroin-self-crosslinking adhesive of silk antiquity Download PDFInfo
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- CN101613936B CN101613936B CN2009101014918A CN200910101491A CN101613936B CN 101613936 B CN101613936 B CN 101613936B CN 2009101014918 A CN2009101014918 A CN 2009101014918A CN 200910101491 A CN200910101491 A CN 200910101491A CN 101613936 B CN101613936 B CN 101613936B
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Abstract
The invention relates to a method for compound-enhancing a fibroin-self-crosslinking adhesive of a silk antiquity which is characterized by adopting the following steps: A) placing silk in Na2CO3 solution for decementation, taking the silk out after 30 min, wringing the silk, repeating the previous actions once, and cleaning and drying the silk; B) placing the silk in CaCl2 solution, dissolving the silk for 10-90 min at 90 DEGC, carrying out cooling and filtration, and obtaining fibroin solution after 72-hour dialysis; C) spraying the fibroin solution on the silk antiquity and thoroughly wetting the silk antiquity, airing the silk antiquity, repeating the previous actions for one to three times; and D) placing the silk antiquity in a self-crosslinking adhesive, taking out the silk antiquity after the treatment for 1-30 min at 30 DEG C, and obtaining the enhanced silk antiquity. The method has the advantages that 1) the method can increase the strength of the silk antiquity and reduce the influence of the enhancement upon the properties of the antiquity; 2) the method is simple and has low cost and good effect; 3) the method repairs broken silk protein molecules at the normal temperature and in a neutral condition and does not cause negative influences; and 4) the enhancing agent used in the method has no toxicity or harm, does not cause pollution and conforms to the trend of environment-friendly development.
Description
Technical field
What the present invention relates to is a kind of fibroin-self-crosslinking adhesive composite reinforcing method of silk historical relic, belongs to the Techniques of Relics Protection field.
Background technology
Ancient Silk Textile is an important part in China culture treasure-house, is the important topic that the historical relic's protection worker pays close attention to exploration to the reinforcing of the poor rotten silk historical relic that is unearthed always.In order to satisfy the requirement of collection research and display, need carry out necessary reinforcing to increase its intensity to silk goods.Silk goods are reinforced follow following basic principle: (1) keeps original appearance principle, (2) ageing-resistant principle, (3) to intervene principle, (4) invertibity principle less.The main body of silk is a fibroin, and the big molecule of fibroin has strong suction-operated to silk product again, and therefore using the silk fibroin solution reparation is the optimal path that poor rotten silk fabric is realized self-perfection.The big molecule of fibroin is a kind of natural polymer protein that comes from silk, and is safe and reliable to the effect of human non-toxic evil, has excellent biological compatibility, obtains a large amount of developments and utilizations in recent years.With silk fibroin solution unearthed relics being reinforced, can when effectively improving silk historical relic intensity, do not influenced the outward appearance and the feel of historical relic, is a kind of more promising reinforcement technique.
Summary of the invention
The object of the invention is overcoming the deficiency that prior art exists, and a kind of new method of reinforcing the silk historical relic with fibroin albumen is provided.The silk-fibroin reinforcement technique of silk historical relic with fibroin albumen as the material of main part of reinforcing, with crosslinking agent as auxiliary agent.Self-crosslinking adhesive KG-101 of the present invention be a kind of be the polynary emulsion copolymers of main raw material with the butyl acrylate, be mainly used in the silk fabrics printing adhesive.It has following advantage: need not high temperature and bake, as long as air drying just can obtain good set fastness, epithelium is transparent, and through the not yellowing of finalizing the design, feel is superior to general auto crosslinking binder, therefore can satisfy the requirement that historical relic is reinforced, and convenient in application.
A kind of fibroin of silk historical relic-self-crosslinking adhesive composite reinforcing method is characterized in that adopting following steps:
A) silk fiber being put into concentration expressed in percentage by weight is 0.5% Na
2CO
3In the solution, silk fiber is pulled out and wrung out after boiling the 30min that comes unstuck, repeat aforesaid operations once, fully wash with deionized water then, 50～80 ℃ of oven dry down, silk fiber and concentration expressed in percentage by weight are 0.5% Na
2CO
3The weight ratio of solution is 1: 100;
B) to place concentration expressed in percentage by weight be 50% CaCl to the silk fiber after will coming unstuck
2In the solution, under 90～100 ℃ of conditions, dissolve 10～90min, filter the fibroin lysate through cooling off, crossing, silk fiber after coming unstuck and concentration expressed in percentage by weight are 50% CaCl
2The weight ratio of solution is 1: 30～50; The fibroin lysate is packed in the bag filter, place deionized water to dialyse, the volume of deionized water is 8～10 times of fibroin lysate volume, and per 4～6h changes deionized water one time, after the 72h dialysis, obtains the pure silk cellulose solution;
C) be that 0.5%～2% silk fibroin solution evenly is sprayed onto on the silk historical relic to be reinforced with concentration expressed in percentage by weight, drenched until evenly, dry, take out, by this operation 1～3 time;
D) will pass through step C) to be impregnated into concentration expressed in percentage by weight be in 1%～20% the self-crosslinking adhesive solution, to handle 1～30min down at 25～35 ℃ for silk historical relic after handling, taking-up is dried in the shade, the silk historical relic after obtaining to reinforce.
Characteristic of the present invention also is: the self-crosslinking adhesive adopts low-temperature self-crosslinking adhesive KG-101A, perhaps in warm self-crosslinking adhesive KG-101B.
With prior art relatively, 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 environmental protection Development Trend.
The specific embodiment
Embodiment 1:
A kind of fibroin of silk historical relic-self-crosslinking adhesive composite reinforcing method is characterized in that adopting following steps:
A) silk fiber being put into concentration expressed in percentage by weight is 0.5% Na
2CO
3In the solution, silk fiber is pulled out and wrung out after boiling the 30min that comes unstuck, repeat aforesaid operations once, fully wash with deionized water then, 50 ℃ of oven dry down, silk fiber and concentration expressed in percentage by weight are 0.5% Na
2CO
3The weight ratio of solution is 1: 100;
B) to place concentration expressed in percentage by weight be 50% CaCl to the silk fiber after will coming unstuck
2In the solution, under 90 ℃ of conditions, dissolve 10min, filter the fibroin lysate through cooling off, crossing, silk fiber after coming unstuck and concentration expressed in percentage by weight are 50% CaCl
2The weight ratio of solution is 1: 30; The fibroin lysate is packed in the bag filter, place deionized water to dialyse, the volume of deionized water is 8 times of fibroin lysate volume, and every 4h changes deionized water one time, after the 72h dialysis, obtains the pure silk cellulose solution;
C) be that 0.5% silk fibroin solution evenly is sprayed onto on the silk historical relic to be reinforced with concentration expressed in percentage by weight, drenched until evenly, dry, take out, by this operation 1 time;
D) will pass through step C) to be impregnated into concentration expressed in percentage by weight be in 1% the self-crosslinking adhesive solution, to handle 1min down at 25 ℃ for silk historical relic after handling, taking-up is dried in the shade, the silk historical relic after obtaining to reinforce.
Embodiment 2:
A kind of fibroin of silk historical relic-self-crosslinking adhesive composite reinforcing method is characterized in that adopting following steps:
A) silk fiber being put into concentration expressed in percentage by weight is 0.5% Na
2CO
3In the solution, silk fiber is pulled out and wrung out after boiling the 30min that comes unstuck, repeat aforesaid operations once, fully wash with deionized water then, 80 ℃ of oven dry down, silk fiber and concentration expressed in percentage by weight are 0.5% Na
2CO
3The weight ratio of solution is 1: 100;
B) to place concentration expressed in percentage by weight be 50% CaCl to the silk fiber after will coming unstuck
2In the solution, under 100 ℃ of conditions, dissolve 10～90min, filter the fibroin lysate through cooling off, crossing, silk fiber after coming unstuck and concentration expressed in percentage by weight are 50% CaCl
2The weight ratio of solution is 1: 50; The fibroin lysate is packed in the bag filter, place deionized water to dialyse, the volume of deionized water is 10 times of fibroin lysate volume, and every 6h changes deionized water one time, after the 72h dialysis, obtains the pure silk cellulose solution;
C) be that 2% silk fibroin solution evenly is sprayed onto on the silk historical relic to be reinforced with concentration expressed in percentage by weight, drenched until evenly, dry, take out, by this operation 3 times;
D) will pass through step C) to be impregnated into concentration expressed in percentage by weight be in 20% the self-crosslinking adhesive solution, to handle 30min down at 35 ℃ for silk historical relic after handling, taking-up is dried in the shade, the silk historical relic after obtaining to reinforce.
Embodiment 3:
A kind of fibroin of silk historical relic-self-crosslinking adhesive composite reinforcing method is characterized in that adopting following steps:
A) silk fiber being put into concentration expressed in percentage by weight is 0.5% Na
2CO
3In the solution, silk fiber is pulled out and wrung out after boiling the 30min that comes unstuck, repeat aforesaid operations once, fully wash with deionized water then, 65 ℃ of oven dry down, silk fiber and concentration expressed in percentage by weight are 0.5% Na
2CO
3The weight ratio of solution is 1: 100;
B) to place concentration expressed in percentage by weight be 50% CaCl to the silk fiber after will coming unstuck
2In the solution, under 95 ℃ of conditions, dissolve 50min, filter the fibroin lysate through cooling off, crossing, silk fiber after coming unstuck and concentration expressed in percentage by weight are 50% CaCl
2The weight ratio of solution is 1: 40; The fibroin lysate is packed in the bag filter, place deionized water to dialyse, the volume of deionized water is 9 times of fibroin lysate volume, and every 5h changes deionized water one time, after the 72h dialysis, obtains the pure silk cellulose solution;
C) be that 1% silk fibroin solution evenly is sprayed onto on the silk historical relic to be reinforced with concentration expressed in percentage by weight, drenched until evenly, dry, take out, by this operation 2 times;
D) will pass through step C) to be impregnated into concentration expressed in percentage by weight be in 10% the self-crosslinking adhesive solution, to handle 15min down at 30 ℃ for silk historical relic after handling, taking-up is dried in the shade, the silk historical relic after obtaining to reinforce.
Claims (1)
1. the fibroin of a silk historical relic-self-crosslinking adhesive composite reinforcing method is characterized in that adopting following steps:
A) silk fiber being put into concentration expressed in percentage by weight is 0.5% Na
2CO
3In the solution, silk fiber is pulled out and wrung out after boiling the 30min that comes unstuck, repeat aforesaid operations once, fully wash with deionized water then, 50～80 ℃ of oven dry down, silk fiber and concentration expressed in percentage by weight are 0.5% Na
2CO
3The weight ratio of solution is 1: 100;
B) to place concentration expressed in percentage by weight be 50% CaCl to the silk fiber after will coming unstuck
2In the solution, under 90～100 ℃ of conditions, dissolve 10～90min, filter the fibroin lysate through cooling off, crossing, silk fiber after coming unstuck and concentration expressed in percentage by weight are 50% CaCl
2The weight ratio of solution is 1: 30～50; The fibroin lysate is packed in the bag filter, place deionized water to dialyse, the volume of deionized water is 8～10 times of fibroin lysate volume, and per 4～6h changes deionized water one time, after the 72h dialysis, obtains the pure silk cellulose solution;
C) be that 0.5%～2% silk fibroin solution evenly is sprayed onto on the silk historical relic to be reinforced with concentration expressed in percentage by weight, drenched until evenly, dry, take out, by this operation 1～3 time;
D) will pass through step C) to be impregnated into concentration expressed in percentage by weight be in 1%～20% the self-crosslinking adhesive solution, to handle 1～30min down at 25～35 ℃ for silk historical relic after handling, taking-up is dried in the shade, the silk historical relic after obtaining to reinforce; The self-crosslinking adhesive adopts low-temperature self-crosslinking adhesive KG-101A, perhaps in warm self-crosslinking adhesive KG-101B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101014918A CN101613936B (en) | 2009-08-10 | 2009-08-10 | Method for compound-enhancing fibroin-self-crosslinking adhesive of silk antiquity |
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|---|---|---|---|
| CN2009101014918A CN101613936B (en) | 2009-08-10 | 2009-08-10 | Method for compound-enhancing fibroin-self-crosslinking adhesive of silk antiquity |
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| CN101613936A CN101613936A (en) | 2009-12-30 |
| CN101613936B true CN101613936B (en) | 2012-03-07 |
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| CN102965932B (en) * | 2012-11-19 | 2014-12-03 | 浙江理工大学 | Silk peptide-amino acid grafting and reinforcing method for decayed silk fabric cultural relic |
| CN103205885A (en) * | 2012-11-28 | 2013-07-17 | 苏州大学 | Silk degumming/scouring agent and applications thereof |
| CN113846485A (en) * | 2021-10-26 | 2021-12-28 | 厦门大学 | Simple and efficient aged silk fibroin fiber repairing method |
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