CN104878468A - Nano-titanium dioxide-feeding silkworm rearing method for preparing high-performance silk and product prepared by nano-titanium dioxide-feeding silkworm rearing method - Google Patents
Nano-titanium dioxide-feeding silkworm rearing method for preparing high-performance silk and product prepared by nano-titanium dioxide-feeding silkworm rearing method Download PDFInfo
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- CN104878468A CN104878468A CN201510214730.6A CN201510214730A CN104878468A CN 104878468 A CN104878468 A CN 104878468A CN 201510214730 A CN201510214730 A CN 201510214730A CN 104878468 A CN104878468 A CN 104878468A
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Abstract
The invention relates to a nano-titanium dioxide-feeding silkworm rearing method for preparing a high-performance silk and a product prepared by the nano-titanium dioxide-feeding silkworm rearing method. The nano-titanium dioxide-feeding silkworm rearing method comprises the following specific steps: adding nano-titanium dioxide to a silkworm artificial feed; and entering the nano-titanium dioxide into sericterium of a silkworm employing the absorption and transformation functions of the silkworm, and cocooning by the silkworm, so as to obtain the high-performance silk containing the nano-titanium dioxide. According to the method provided by the invention, the silk is modified on the premise that the natural quality of the silk is not damaged, so that the obtained silk has relatively good mechanical property, and also has relatively good antibacterial and anti-ultraviolet abilities.
Description
Technical field
The invention belongs to silk fiber and modification field thereof, relate to a kind of nano titanium oxide preparing high-performance silk and freshen food and educate silkworm method and goods thereof.
Background technology
By the oozy spinning solution be made up of protein of sericterium when matured silkworm cocoons, the continuous fiber solidifying formation is in atmosphere called silk.As a kind of biological fiber, silk not only has good glossiness and comfortable sense of touch, also has stronger mechanical performance and good biocompatibility, is all widely used at weaving, medical science, cosmetics and biological field.
The fracture strength of boiled silk is about 400MPa, and elongation at break and energy to failure are 15% and about 30J/g, needs in actual applications to be improved further.Silk itself has certain uvioresistant and antibacterial ability, but not remarkable, as undressed natural silk does not show obvious inhibition zone in testing.Therefore in order to improve the performance of silk and widen its Application Areas, need to carry out modification to silk.
There is research by strengthening the performance of silk in the method for silk surface coated particle.Such as publication number is that the Chinese patent of CN103572585A discloses a kind of titania modified silk and preparation method thereof.In patent, inventor take titanate esters as reactant, makes solvent with benzinum, and the hydrated titanium dioxide of original position room temperature synthesis of densified, is covered in silk surface.Although can reach 22% by the elongation at break of the silk of the method modification, energy to failure is 22 ~ 74J/g, and intensity is 300 ~ 680MPa, and its uvioresistant and antibacterial ability are all significantly improved simultaneously.But the method for this modified natural silk needs with an organic solvent, produce if quantize and need more input in solvent recovery process.Moreover, titanium dioxide is covered in the one's best quality such as color and luster, sense of touch, gas permeability that silk itself can be damaged in silk surface.
Other some researchs then use the nano particle adding metal oxide in silk fibroin solution to be spun into the method for fiber more by artificial means to improve the performance of silk.Such as publication number is that the Chinese patent of CN102912470A discloses regenerated silk fiber of a kind of metal oxide nanoparticles activeness and quietness and preparation method thereof.In this invention, researcher makes regenerated silk fibroin solution after being come unstuck by natural silk, regulates its calcium ion concentration to 0.15 ~ 0.3mol/L, then with a certain proportion of metal oxide (TiO
2, Fe
3o
4, ZnO, Al
2o
3or ZrO
2) hydrosol mixing, concentrated, be at room temperature dry spun into silk, finally carry out post processing with ethanol-water mixture, the regenerated silk fiber elongation at break obtained is 50% ~ 150%, and energy to failure is 30 ~ 100J/g, and fracture strength is 50 ~ 250MPa.Publication number is that the Chinese patent of CN103572395A discloses a kind of activeness and quietness regenerated silk fiber and preparation method thereof.Researcher is on the basis of CN102912470A at aforementioned publication number, adds graphene oxide solution again, make the obtained regenerated fibroin fiber that uses the same method in regenerated silk fibroin solution.The regenerated silk fiber elongation at break that the method obtains is 20% ~ 150%, and energy to failure is 30 ~ 100J/g, and fracture strength is 70 ~ 380MPa.The toughness of these two kinds of methods to silk all improves a lot, but but fails to keep its fracture strength a good level, do not mention in patent yet silk can be made to obtain other are functional.And complicated by the process operation of regenerated silk fibroin solution-polymerized SBR, condition is harsh, the cycle is long, yield poorly, industrialized possibility is very little.
Also there is researcher in feed of mulberry silkworm, add some functional particles, thus obtain the silk with some specific function.Publication number is that the Chinese patent of CN1395861A discloses a kind of silkworm feed containing functional particle and the silk produced with this feed feeding and the goods using this silk.In this patent, the functional particle such as mineral, pigment is added feeding silkworm in silkworm feed by inventor, spins function silk by the effect of silkworm sorption enhanced.Publication number be the Chinese patent of CN1608489 disclose a kind of silkworm feed and feed raise the silk that this feed is produced and the squeeze using this.This patent is then water-soluble for the functional particles such as the zeolite of ormal weight, noctilucence stone or other solvents are added feeding silkworm in silkworm feed again obtain silk.These two patents need functional particle used to carry out screening and processing freshening in food process, and because diameter of particle is comparatively large, the feed being easy to affect silkworm grows, and causes silk quality and production declining.Its result shows again, and functional particle is more to be present in silk gum, and silk in use, and mostly need to come unstuck, so its modified effect is just very little.And the two does not all provide the Mechanical Characteristics of gained silk, only represent that gained silk has the function of the particulate that some add, can range of application narrow.
Summary of the invention
The object of this invention is to provide a kind of nano titanium oxide preparing high-performance silk to freshen food and educate silkworm method and goods thereof, better for fields such as organization bracket engineering, weaving and medical science.In the present invention, nano titanium oxide is blended in feeding silkworm in silkworm feed, by the absorption of silkworm self, makes nano titanium oxide be mixed into silk, to improve the mechanical performance of silk and antibacterial and uvioresistant ability.The high-performance silk that this method obtains, the multivalence titanium elements in nano titanium oxide occurs interact and form boundary layer by hydrogen bond, chelating mode and fibroin albumen, and degumed silk can keep good modified effect.This method, while the mechanical performance improving silk, can also improve its antibacterial and uvioresistant ability, and can not damage other fine quality of silk.Whole process environmental protection, simple and easy to do, can implement in normal silkworm rearing process, can suitability for industrialized production be realized.
A kind of nano titanium oxide preparing high-performance silk of the present invention freshens food and educates silkworm method, in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorb nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 0.5 ~ 2% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons.Silkworm five the length of times body of gland proportion anxious to increase, five age forage protein be increased to 96% in the retention ratio of its sericterium gradually by 9%, the synthesis of its silk-fibroin is mainly carried out in five length of times as seen.Therefore select to add food nano titanium oxide five length of times and can obtain the highest raw material availability and optimum efficiency.
There is research by multiple-pulse vapor infiltration method, the elements such as titanium, aluminium, zinc to be penetrated in the natural spider's thread, be connected with covalent bond or coordinate bond with protein molecule after reactant enters, form metal-protein complex compound.Protein molecule in spider silk unformed area is connected by metal, and therefore its mechanical property improves greatly.The present invention then educates silkworm method and is added in silk by freshening food by nano titanium oxide, and titanium elements is connected with covalent bond or coordinate bond with silk fibroin molecular, forms titanium-protein complex, improves the mechanical property of silk; Meanwhile, because titanium elements and silk fibroin molecular can form coordinate bond and hydrogen bond, hinder random conformation and alpha helical conformation to the transformation of β-pleated sheet conformation, cause the degree of crystallinity of silk to reduce; Therefore, consider, if the addition of nano titanium oxide is too high, the nanoparticle concentration entering sericterium is too high, be then unfavorable for silk-fibroin crystallization; And too much additive will inevitably affect the normal growth of silkworm, therefore the addition of nano titanium oxide required for the present invention is lower, mass percent is only 0.5 ~ 2%, experiment show this addition do not affect silkworm normal food-intake, eating speed, grow and cocoon.
As preferred technical scheme:
The nano titanium oxide preparing high-performance silk as above freshens food and educates a silkworm method, and described mixed feed refers to and in silkworm feed, is evenly mixed into a certain amount of nano titanium oxide and the feed heating shortening; The concrete preparation process of described mixed feed comprises the following steps:
(1) nano titanium oxide is soluble in water, make nanometer titanium dioxide titanium solution;
(2) nanometer titanium dioxide titanium solution and silkworm feed are stirred, then heat, after cooling, namely make mixed feed;
Wherein, the quality of water is 2 ~ 3 times of silkworm feed.
The nano titanium oxide preparing high-performance silk as above freshens food and educates a silkworm method, and described nanometer titanium dioxide titanium solution is before mixing with silkworm feed, and first ultrasonic 15 ~ 30min, makes nanoparticle dispersion even.
The nano titanium oxide preparing high-performance silk as above freshens food and educates a silkworm method, and described heating refers to puts into micro-wave oven heating 3 ~ 6min, and the power output of micro-wave oven is 800 ~ 1000W.
The nano titanium oxide preparing high-performance silk as above freshens food and educates a silkworm method, and the size range of described nano titanium oxide is 50 ~ 400nm.
The present invention's nano titanium oxide used is small-sized, and has water-soluble preferably, is scattered in water, then mixes with feed through ultrasonic Absorbable organic halogens afterwards.Mixed feed is through heating using microwave, and cooling forming, can keep suitable humidity, is beneficial to silkworm feed.After nano titanium oxide is taken in body by silkworm, very fast diffusion enters each organ of its health, comprises sericterium.Nano titanium oxide is and protein bound, finally in the spinning process of silkworm, enters silk.Due to the sorption enhanced effect of silkworm self, nano titanium oxide can with fibroin stable bond, and be uniformly distributed in silk, effectively improve the performance of silk.
The nano titanium oxide preparing high-performance silk as above freshens food and educates a silkworm method, cocoons period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, and in described mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
The nano titanium oxide preparing high-performance silk adds the high-performance silk eaten and educate silkworm method and obtain, and the fracture strength of described high-performance silk monofilament after removing silk gum is 340 ~ 620MPa, and elongation at break is 15 ~ 23%, and energy to failure is 26 ~ 80J/g.Described high-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
Nano titanium oxide has good photocatalytic effect, and Absorbable rod ultraviolet light produces electron transition, and the hole of generation and electronics have very strong oxidability, therefore have antibiotic property.Except absorbing ultraviolet, nano titanium oxide also has very strong scatters ultraviolet ability.Therefore the silk antibiotic property and the uvioresistant performance that combine nano titanium oxide all improve a lot.
High-performance silk as above, described in remove silk gum detailed process comprise the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.5 ~ 1%
2cO
3in the aqueous solution, boil 20 ~ 30min, then use washed with de-ionized water;
(3) repeat (2) step 2 ~ 3 times, the silk come unstuck is hung on Indoor Natural air-dry.
Silk gum is little for the Effect on Mechanical Properties of silk fiber, in actual applications, mostly need to remove silk gum, therefore the present invention adopts the mechanical property of degumed silk to show modified effect, proves the interaction of nano titanium oxide and fibroin albumen in the present invention simultaneously and is effectively combined.
A kind of silk product, by high-performance silk through braiding or be formed by weaving.
Beneficial effect:
Nano titanium oxide of the present invention adds food and educates the method for modifying of silkworm method relative to prior art, eliminates expensive equipment support and complicated technological means, not only simple and easy to do, cost-saving, and is easy to control, Be very effective.
High-performance silk of the present invention, has and has better mechanical performance than natural silk, also has antibacterial and uvioresistant ability preferably simultaneously.
Detailed description of the invention
Below in conjunction with detailed description of the invention, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
The silkworm feed used in the present invention, in dry powdered, its main component and configuration proportion scope list in table 1.
The composition with silkworm feed tested by table 1
Embodiment 1
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 15min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 3min, the power output of micro-wave oven is 800W, namely makes mixed feed after cooling; Wherein, the quality of water is 2 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 0.5% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.5%
2cO
3in the aqueous solution, boil 20min, then use washed with de-ionized water;
(3) repeat (2) step 2 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 340MPa, and elongation at break is 15%, and energy to failure is 26J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
Silk product is formed through braiding by high-performance silk.
Experiment is composed as follows with silkworm feed:
Embodiment 2
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 30min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 6min, the power output of micro-wave oven is 1000W, namely makes mixed feed after cooling; Wherein, the quality of water is 3 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 2% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 1%
2cO
3in the aqueous solution, boil 30min, then use washed with de-ionized water;
(3) repeat (2) step 3 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 500MPa, and elongation at break is 22%, and energy to failure is 60J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
By high-performance silk through the silk product woven or be formed by weaving.
Experiment is composed as follows with silkworm feed:
Embodiment 3
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 20min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 4min, the power output of micro-wave oven is 850W, namely makes mixed feed after cooling; Wherein, the quality of water is 2.5 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 0.6% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.7%
2cO
3in the aqueous solution, boil 25min, then use washed with de-ionized water;
(3) repeat (2) step 2 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 400MPa, and elongation at break is 16%, and energy to failure is 32J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
Silk product is formed through braiding by high-performance silk.
Experiment is composed as follows with silkworm feed:
Embodiment 4
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 18min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 5min, the power output of micro-wave oven is 880W, namely makes mixed feed after cooling; Wherein, the quality of water is 2.5 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 1.5% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in described mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.7%
2cO
3in the aqueous solution, boil 25min, then use washed with de-ionized water;
(3) repeat (2) step 2 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 620MPa, and elongation at break is 23%, and energy to failure is 80J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
Silk product is formed through braiding by high-performance silk.
Experiment is composed as follows with silkworm feed:
Embodiment 5
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 18min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 5min, the power output of micro-wave oven is 950W, namely makes mixed feed after cooling; Wherein, the quality of water is 3 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 1% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in described mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.7%
2cO
3in the aqueous solution, boil 22min, then use washed with de-ionized water;
(3) repeat (2) step 3 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 550MPa, and elongation at break is 17%, and energy to failure is 58J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
Silk product is formed through braiding by high-performance silk.
Embodiment 6
The nano titanium oxide preparing high-performance silk freshens food and educates a silkworm method, first prepares mixed feed, is specially:
(1) be that the nano titanium oxide of 50 ~ 400nm is soluble in water by size range, make nanometer titanium dioxide titanium solution;
(2) first by ultrasonic for nanometer titanium dioxide titanium solution 18min, make nanoparticle dispersion even, then nanometer titanium dioxide titanium solution and silkworm feed are stirred, then put into micro-wave oven and heat 4min, the power output of micro-wave oven is 850W, namely makes mixed feed after cooling; Wherein, the quality of water is 2 times of silkworm feed;
Then in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorbing nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 1.8% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons, cocoon period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, in described mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
Add food by a kind of nano titanium oxide preparing high-performance silk above and educate the high-performance silk that silkworm method obtains, carried out removing silk gum by high-performance silk, the detailed process removing silk gum comprises the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.8%
2cO
3in the aqueous solution, boil 28min, then use washed with de-ionized water;
(3) repeat (2) step 3 times, the silk come unstuck is hung on Indoor Natural air-dry.The fracture strength of high-performance silk monofilament after removing silk gum is 580MPa, and elongation at break is 21%, and energy to failure is 72J/g.High-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
By high-performance silk through being formed by weaving silk product.
Claims (9)
1. the nano titanium oxide preparing high-performance silk freshens food and educates silkworm method, it is characterized in that: in silkworm artificial feed and silkworm feed, add nano titanium oxide and feed silkworm, absorb nano titanium oxide by silkworm and enter sericterium and final combination by nano titanium oxide in spinning process enters silk, namely obtain high-performance silk;
Be specially: silkworm an age to four age feeding do not add the silkworm feed of nano titanium oxide, start feeding five second day ages and with the addition of the mixed feed that mass percent is 0.5 ~ 2% nano titanium oxide, cocoon until be placed on small straw bundles to spin cocoons.
2. a kind of nano titanium oxide preparing high-performance silk according to claim 1 freshens food and educates silkworm method, it is characterized in that, described mixed feed refers to and in silkworm feed, is evenly mixed into a certain amount of nano titanium oxide and the feed heating shortening; The concrete preparation process of described mixed feed comprises the following steps:
(1) nano titanium oxide is soluble in water, make nanometer titanium dioxide titanium solution;
(2) nanometer titanium dioxide titanium solution and silkworm feed are stirred, then heat, after cooling, namely make mixed feed;
Wherein, the quality of water is 2 ~ 3 times of silkworm feed.
3. a kind of nano titanium oxide preparing high-performance silk according to claim 1 freshens food and educates silkworm method, it is characterized in that, described nanometer titanium dioxide titanium solution is before mixing with silkworm feed, and first ultrasonic 15 ~ 30min, makes nanoparticle dispersion even.
4. a kind of nano titanium oxide preparing high-performance silk according to claim 1 freshens food and educates silkworm method, it is characterized in that, described heating refers to puts into micro-wave oven heating 3 ~ 6min, and the power output of micro-wave oven is 800 ~ 1000W.
5. a kind of nano titanium oxide preparing high-performance silk according to claim 1 freshens food and educates silkworm method, and it is characterized in that, the size range of described nano titanium oxide is 50 ~ 400nm.
6. a kind of nano titanium oxide preparing high-performance silk according to claim 1 freshens food and educates silkworm method, it is characterized in that, cocoons period from second day five age to being placed on small straw bundles to spin cocoons with a collection of silkworm, and in described mixed feed, the food concentration of adding of nano titanium oxide remains unchanged.
7. a kind of nano titanium oxide preparing high-performance silk adds the high-performance silk eaten and educate silkworm method and obtain as claimed in claim 1, it is characterized in that: the fracture strength of described high-performance silk monofilament after removing silk gum is 340 ~ 620MPa, elongation at break is 15 ~ 23%, and energy to failure is 26 ~ 80J/g; Described high-performance silk remove after silk gum through light intensity be 1245 μ W/cm
2and wavelength is that after the UV-irradiation 3h of 390nm, fracture strength, without significantly sacrificing, is greater than 10.5mm to colibacillary inhibition zone.
8. high-performance silk according to claim 7, is characterized in that, described in remove silk gum detailed process comprise the following steps:
(1) silk cocoon is cut off the inner silkworm chrysalis of removing;
(2) silk cocoon is placed in the Na that mass percent is 0.5 ~ 1%
2cO
3in the aqueous solution, boil 20 ~ 30min, then use washed with de-ionized water;
(3) repeat (2) step 2 ~ 3 times, the silk come unstuck is hung on Indoor Natural air-dry.
9. a silk product, is characterized in that: by high-performance silk through braiding or be formed by weaving.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510214730.6A CN104878468A (en) | 2015-04-29 | 2015-04-29 | Nano-titanium dioxide-feeding silkworm rearing method for preparing high-performance silk and product prepared by nano-titanium dioxide-feeding silkworm rearing method |
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| CN106069992A (en) * | 2016-06-07 | 2016-11-09 | 东华大学 | A kind of nano-sized carbon preparing fluorescent natural silk is selected or graphene quantum dot freshens food and educates silkworm method and goods thereof |
| CN108354092A (en) * | 2018-03-09 | 2018-08-03 | 中科国思生物科技研究（广州）有限公司 | A kind of silkworm containing nano material adds food feed and preparation method |
| CN109122600A (en) * | 2018-07-13 | 2019-01-04 | 西安交通大学 | A kind of prepare freshens food from the nano tungsten trioxide of heat production silk and educates silkworm method and its product |
| CN110432407A (en) * | 2019-08-28 | 2019-11-12 | 苏州大学 | A kind of functionality silkworm artificial feed and the preparation method and application thereof |
| CN110552195A (en) * | 2019-09-23 | 2019-12-10 | 中国科学技术大学先进技术研究院 | Composite silk and preparation method thereof |
| WO2020225733A1 (en) * | 2019-05-06 | 2020-11-12 | The American University In Cairo | Electrical circuit components made from silkworm silk with silkworm-digested structured materials and methods for manufacturing same |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395861A (en) * | 2001-07-05 | 2003-02-12 | 华岛编织股份有限公司 | Silkworm feed containing functional particle and produced silk by silkworm feed with the feed and production using the silk |
| JP3560825B2 (en) * | 1998-09-01 | 2004-09-02 | 華島ニット株式会社 | Silk feed with ceramics and silk produced by feeding the feed |
| JP2007110905A (en) * | 2005-10-18 | 2007-05-10 | Unitika Ltd | Nano composite silk product and method for producing the same |
| CN103564196A (en) * | 2013-11-15 | 2014-02-12 | 苏州大学 | Additive for improving bombyx mori yield |
| CN103952774A (en) * | 2014-04-24 | 2014-07-30 | 苏州大学 | Method for preparing mulberry silk containing nanometer TiO2 |
-
2015
- 2015-04-29 CN CN201510214730.6A patent/CN104878468A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3560825B2 (en) * | 1998-09-01 | 2004-09-02 | 華島ニット株式会社 | Silk feed with ceramics and silk produced by feeding the feed |
| CN1395861A (en) * | 2001-07-05 | 2003-02-12 | 华岛编织股份有限公司 | Silkworm feed containing functional particle and produced silk by silkworm feed with the feed and production using the silk |
| JP2007110905A (en) * | 2005-10-18 | 2007-05-10 | Unitika Ltd | Nano composite silk product and method for producing the same |
| CN103564196A (en) * | 2013-11-15 | 2014-02-12 | 苏州大学 | Additive for improving bombyx mori yield |
| CN103952774A (en) * | 2014-04-24 | 2014-07-30 | 苏州大学 | Method for preparing mulberry silk containing nanometer TiO2 |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106069992A (en) * | 2016-06-07 | 2016-11-09 | 东华大学 | A kind of nano-sized carbon preparing fluorescent natural silk is selected or graphene quantum dot freshens food and educates silkworm method and goods thereof |
| CN108354092A (en) * | 2018-03-09 | 2018-08-03 | 中科国思生物科技研究（广州）有限公司 | A kind of silkworm containing nano material adds food feed and preparation method |
| CN109122600A (en) * | 2018-07-13 | 2019-01-04 | 西安交通大学 | A kind of prepare freshens food from the nano tungsten trioxide of heat production silk and educates silkworm method and its product |
| WO2020225733A1 (en) * | 2019-05-06 | 2020-11-12 | The American University In Cairo | Electrical circuit components made from silkworm silk with silkworm-digested structured materials and methods for manufacturing same |
| EP3955749A4 (en) * | 2019-05-06 | 2023-08-16 | The American University in Cairo | Electrical circuit components made from silkworm silk with silkworm-digested structured materials and methods for manufacturing same |
| WO2021037180A1 (en) * | 2019-08-28 | 2021-03-04 | 苏州大学 | Functional artificial feed for silkworms, preparation method and application thereof |
| CN110432407A (en) * | 2019-08-28 | 2019-11-12 | 苏州大学 | A kind of functionality silkworm artificial feed and the preparation method and application thereof |
| CN110552195A (en) * | 2019-09-23 | 2019-12-10 | 中国科学技术大学先进技术研究院 | Composite silk and preparation method thereof |
| CN113826590A (en) * | 2021-09-23 | 2021-12-24 | 苏州大学 | Method for improving strength of silkworm cocoon silk |
| CN114128681A (en) * | 2021-11-12 | 2022-03-04 | 西南大学 | Preparation method of nano enhanced functional flat wire composite material |
| CN114128681B (en) * | 2021-11-12 | 2023-08-04 | 西南大学 | Preparation method of nano enhanced functional flat wire composite material |
| CN114164509A (en) * | 2021-12-16 | 2022-03-11 | 中国科学院电工研究所 | Silk fiber with ultraviolet and near-infrared shielding performance and preparation method and application thereof |
| CN114164509B (en) * | 2021-12-16 | 2024-02-02 | 中国科学院电工研究所 | Silk fiber with ultraviolet and near infrared shielding performance and preparation method and application thereof |
| CN114351458A (en) * | 2022-02-10 | 2022-04-15 | 江苏欣鑫纺织科技有限公司 | Health-care silk fabric and preparation method thereof |
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