CN101333769A - Silk weighting method for fixing sericin by sol-gel process - Google Patents
Silk weighting method for fixing sericin by sol-gel process Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 52
- 108010013296 Sericins Proteins 0.000 title claims abstract description 28
- 238000003980 solgel method Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- 239000004744 fabric Substances 0.000 claims description 29
- 239000000835 fiber Substances 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 238000004061 bleaching Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- VCMWDHLYGLMCCS-UHFFFAOYSA-N C(CC)[SiH3].[O] Chemical compound C(CC)[SiH3].[O] VCMWDHLYGLMCCS-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 10
- 230000037396 body weight Effects 0.000 description 6
- 235000019786 weight gain Nutrition 0.000 description 6
- 108010022355 Fibroins Proteins 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000000205 computational method Methods 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000006424 Flood reaction Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 238000007334 copolymerization reaction Methods 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical class ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
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- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
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- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- -1 salt metalloid ion Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a silk weight gaining method adopting a sol-gel method to fix sericin, which includes the following steps of: 1) impurity removal and clearing treatment of silk; 2) preparation of finishing liquid of sol; and 3) fixation and finishing of sericin: silk made by the step 2 is fixed and finished by finishing liquid of sol according to a secondary leaching and rolling method so that liquid carrying rate of silk can reach sixty percent to one hundred percent; then finished silk is aged for zero to twenty four hours at normal temperature; finally the silk is baked for ten to sixty minutes at a temperature between 120 and 180DEG C. The silk weight gaining method has the advantages of safety, environmental protection and effective fixation of silk.
Description
Technical field
The invention belongs to the textile chemistry technical field, specifically relate to a kind of silk weighting method that adopts the sol-gal process adhering sericin.
Background technology
In traditional Silk Industry, people mainly are the internal layer fibroin parts of utilizing silk fiber, and the outer sericin that accounts for silk raw silk weight about 25% is removed in the concise stage, and discharge with waste water; This sericin has higher biochemical oxygen demand (BOD) (BOD) in waste water, cause severe contamination to environment, and causes the waste of sericine resource.Silk gum has good skin-friendly and hygroscopicity, if can reduce the water-soluble of silk gum, and adhering sericin, can reduce the pollution of sericin on the one hand to environment; Can increase the weight of cocoon fiber on the other hand, improve the performance of cocoon fiber, thereby form the silk product of individual style.
For a long time, people after deliberation many methods increase the quality of cocoon fiber, wherein class methods are by carry out chemical modification on fibroin fiber, as weight increasing method (Rene Clavel.Processfor natural silk with pink salt metalloid ion processing real silk, US 1920063,1933.07.25), adopt the weight increasing method (CN1318685C of monomer-grafted copolymerization processing, a kind of method of plasma grafting weight gaining for silk fibre, 2007.5.30); But what the silk after pink salt processing can become is not durable, and when adopting the grafting method, if grafting is inhomogeneous, causes the inhomogeneous of silk fiber or squeeze quality easily.Another kind of is exactly silk weighting method by adhering sericin, as adopting derivative, heavy metallic salt, tannins, N-methylol compound and the adhering sericins such as Cyanuric Chloride class, rare earth of aldehyde or aldehyde.All there is environmental issue to some extent in the method for above-mentioned these adhering sericins.
And sol-gel process is occupied critical role as the important method of synthesizing inorganic compound or inorganic material under low temperature or the temperate condition in softening is synthetic; Obtain important application at aspects such as preparation glass, film, fiber, composites, more be widely used in the preparation nano particle.The chemical process of sol-gel process at first is that raw material is dispersed in the solvent, generates activated monomer through hydrolysis then, and activated monomer carries out polymerization, begins to become colloidal sol, and then generates the gel with certain space structure.The report that it is applied to textiles processing has: collosol and gel fixation (the collosol and gel color-fixing method of textiles, CN1170028C, 2004.10.6), the collosol and gel anion finishing of fabric, collosol and gel anti UV finishing (the collosol and gel anti UV finishing method of COTTON FABRIC of COTTON FABRIC, CN1282792C, 2006.11.01) etc.Yet, adopt the silk weighting method of sol-gal process adhering sericin not appear in the newspapers so far.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of safety and environmental protection and the effective silk weighting method of adhering sericin.
In order to solve the problems of the technologies described above, the invention provides a kind of silk weighting method that adopts the sol-gel process adhering sericin, comprise the steps:
1), the removal of impurities of silk is cleaned and is handled;
2), the preparation of colloidal sol dressing liquid:
By following components in percentage by volume constitutive material: 10～40% tetraethyl orthosilicate, 0～30% silane coupler and 40～80% absolute ethyl alcohol, all the other are the aqueous solution that contains catalyst; The concentration of catalyst in raw material is 0.001～1molL
-1After the full and uniform mixing of described raw material, constant temperature hydrolysis 4～16h under 25～70 ℃ of temperature obtains the colloidal sol dressing liquid of homogeneous transparent;
3), the set of silk gum arrangement:
Adopt above-mentioned colloidal sol dressing liquid that two methods of rolling are soaked in the silk employing two of step 1) gained and carry out the set arrangement, the liquid carrying rate that makes silk is 60%～100%;
With ageing 0～24h under the silk normal temperature after the above-mentioned arrangement; Under 120～180 ℃, bake 10～60min at last.
Improvement as silk weighting method of the present invention: silane coupling agent is gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl silane or gamma-methyl allyl acyloxypropyl trimethoxysilane.
Further improvement as silk weighting method of the present invention: catalyst is HCL or HNO
3
Further improvement as silk weighting method of the present invention: the silk in the step 1) is boiled silk fiber not, part boiled silk fiber, not boiled silk fabric or part boiled silk fabric.
Further improvement as silk weighting method of the present invention: not boiled silk fiber, part boiled silk fiber, not boiled silk fabric or process soft finish earlier of part boiled silk fabric and/or bleaching processing.
In silk weighting method of the present invention, at first silk to be carried out in a conventional manner removal of impurities and clean processing, purpose is the impurity of removing in the silk, so that the silk after cleaning up can combine with the colloidal sol dressing liquid is effective.
The present invention adopts and can form the silk dressing liquid with Nano silica sol with the reagent of sericin molecule generation chemical bonding--silane coupler is one of raw material; Therefore, after arrangement, can form the firm network thin-film structure of one deck, thereby reach the purpose of adhering sericin and silk weighting on the surface of silk gum; And formed network thin-film structure can also prevent effectively that silk gum is water-soluble.The present invention has adopted quite ripe sol-gel technology, therefore can overcome the water-soluble high problem of silk gum, thereby silk gum is played good set effect, and can not produce pollution.The present invention also has following characteristics except above-mentioned advantage:
1, the gel film of Xing Chenging not only self can play effect of gain, and it can also adhering sericin, reaches dual gaining effect;
2, to become membrane matrix be silk fiber or fabric to gel, helps the firm bonding with film;
3, do not produce formaldehyde and heavy metal ion, harmless;
Feel was hard partially when 4, silk contained silk gum, and whiteness is lower; Therefore, in advance silk fiber or fabric are carried out soft finish or bleaching processing, can effectively address the above problem, and can the finishing effect of subsequent step not exerted an influence;
5, in the present invention, adopt the temperature more relatively low to bake, can not make the fibroin fiber sex change than conventional sol gel process; Effective energy savings.
In sum, adopt method of the present invention can form the silica-based cubic network film of one deck complexity on the silk fiber surface, thereby reduce the water-soluble of silk gum, and the silk gum on the silk played the set effect, reach the purpose of silk weighting, both improved the utilization rate of silk, reduced the pollution of silk gum again environment.Compare with weight increasing methods such as above-mentioned traditional aldehyde, heavy metallic salts, method of the present invention is compliance with environmental protection requirements more.
In order to prove the silk after the inventive method is handled, can realize effective weightening finish really, the inventor has done following contrast experiment:
Select for use not boiled silk fiber of the same race as experimental subjects, do not do any subsequent treatment for A, use the B that is that the inventive method handles, use the C that is that the pink salt silk weighting method of prior art handles.
Experimental result is as follows:
The rate of body weight gain of B is 21.5%; The rate of body weight gain of C is 18.7%.
The specific embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1, a kind of silk weighting method that adopts the sol-gel process adhering sericin, carry out following steps successively:
1), the removal of impurities of silk is cleaned and is handled;
Take by weighing silk raw silk 50g, part is come unstuck in 4% 2709 protein enzyme solutions, and residual silkgum content is 9%, takes out the back water and cleans up;
2), the preparation of colloidal sol dressing liquid:
The tetraethyl orthosilicate (TEOS) of 0.4L and the absolute ethyl alcohol of 0.5L are fully mixed, under magnetic stirrer, add the aqueous hydrochloric acid solution of 0.1L, contain the HCL of 0.1mol in this aqueous hydrochloric acid solution; The above-mentioned raw materials component at 60 ℃ of following constant temperature hydrolysis 6h, obtains the colloidal sol dressing liquid of homogeneous transparent after evenly mixing under stirring;
3), the set of silk gum arrangement:
The part boiled silk fiber of step 1) gained is put into above-mentioned colloidal sol dressing liquid, and employing two is soaked two methods of rolling and is carried out the set arrangement, and the liquid carrying rate that makes silk fiber is 60%;
With ageing 4h under the silk fiber normal temperature after the above-mentioned arrangement; Under 120 ℃, bake 60min at last.
The silk raw silk 50g of the same race that present embodiment is the selected processing of coming unstuck entirely in a conventional manner, thus know the weight of fibroin in this kind silk.
The weight of silk weighting rate=[weight of step 3) gained silk weight-fibroin]/fibroin.
According to the aforementioned calculation method, the silk fiber rate of body weight gain of present embodiment 1 gained is 15.6%.
Embodiment 2, a kind of silk weighting method that adopts the sol-gel process adhering sericin, carry out following steps successively:
1), the removal of impurities of silk is cleaned and is handled;
Take by weighing silk greig 100g, remove impurity and pigment with diluted alkaline, dipping is to soft in 3% softener KC again, and taking-up cleans up;
2), the preparation of colloidal sol dressing liquid:
The tetraethyl orthosilicate (TEOS) of 0.1L, the absolute ethyl alcohol of 0.8L and the gamma-aminopropyl-triethoxy-silane of 0.05L are fully mixed as coupling agent, under magnetic stirrer, add the aqueous solution of nitric acid of 0.05L, contain the HNO of 0.3mol in this aqueous solution of nitric acid
3The above-mentioned raw materials component at 25 ℃ of following constant temperature hydrolysis 16h, obtains the colloidal sol dressing liquid of homogeneous transparent after evenly mixing under stirring;
3), the set of silk gum arrangement:
Not boiled silk fabric after the soft finish of step 1) gained is put into above-mentioned colloidal sol dressing liquid, and employing two is soaked two methods of rolling and is carried out the set arrangement, and the liquid carrying rate that makes silk fabric is 70%;
With ageing 10h under the silk fabric normal temperature after the above-mentioned arrangement; Under 140 ℃, bake 30min at last.
According to the computational methods that are analogous to embodiment 1, the silk fabric rate of body weight gain of present embodiment 2 gained is 21.5%.
Measure the whiteness value behind folding 8 layers of the silk fabric of present embodiment 2 gained with WSD-3U type fluorescence whiteness test instrument, the result shows that whiteness value is 52.7.
Embodiment 3, a kind of silk weighting method that adopts the sol-gel process adhering sericin, carry out following steps successively:
1), the removal of impurities of silk is cleaned and is handled;
Take by weighing silk greig 100g, part is come unstuck in the solution of the soda ash that contains 1g/L 209 detergents and 1.2g/L earlier, and residual silkgum content is 11.5%; Reducing bleach in the bleaching liquid that contains auxiliary agents such as 2.5g/L thiourea dioxide and 2% penetrating agent JFC then takes out at last and cleans up;
2), the preparation of colloidal sol dressing liquid:
The tetraethyl orthosilicate (TEOS) of 0.3L, the absolute ethyl alcohol of 0.4L and γ-glycidyl ether oxygen propyl silane of 0.12L are fully mixed as coupling agent, the aqueous hydrochloric acid solution that adds 0.18L under magnetic stirrer contains the HCL of 0.5mol in this aqueous hydrochloric acid solution; The above-mentioned raw materials component at 70 ℃ of following constant temperature hydrolysis 4h, obtains the colloidal sol dressing liquid of homogeneous transparent after evenly mixing under stirring;
3), the set of silk gum arrangement:
Part boiled silk fabric after the bleaching processing of step 1) gained is put into above-mentioned colloidal sol dressing liquid, and employing two is soaked two methods of rolling and is carried out the set arrangement, and the liquid carrying rate that makes silk fabric is 80%;
With ageing 15h under the silk fabric normal temperature after the above-mentioned arrangement; Under 160 ℃, bake 20min at last.
According to the computational methods that are analogous to embodiment 1, the silk fabric rate of body weight gain of present embodiment 3 gained is 12.7%.
Measure the whiteness value behind folding 8 layers of the silk fabric of present embodiment 3 gained with WSD-3U type fluorescence whiteness test instrument, the result shows that whiteness value is 72.4.
Embodiment 4, a kind of silk weighting method that adopts the sol-gel process adhering sericin, carry out following steps successively:
1), the removal of impurities of silk is cleaned and is handled;
Take by weighing silk raw silk 50g, part is come unstuck in the solution of the soda ash that contains 1g/L 209 detergents and 1.2g/L, and residual silkgum content is 11.5%, and dipping is to soft in 3% softener KC then, and the taking-up washing is clean;
2), the preparation of colloidal sol dressing liquid:
The tetraethyl orthosilicate (TEOS) of 0.2L, the absolute ethyl alcohol of 0.6L and the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.16L are fully mixed as coupling agent, the aqueous solution of nitric acid that adds 0.04L under magnetic stirrer contains the HNO of 0.7mol in this aqueous solution of nitric acid
3The above-mentioned raw materials component at 55 ℃ of following constant temperature hydrolysis 8h, obtains the colloidal sol dressing liquid of homogeneous transparent after evenly mixing under stirring;
3), the set of silk gum arrangement:
Part boiled silk fiber after the soft finish of step 1) gained is put into above-mentioned colloidal sol dressing liquid, and employing two is soaked two methods of rolling and is carried out the set arrangement, and the liquid carrying rate that makes silk fiber is 90%;
With ageing 20h under the silk fiber normal temperature after the above-mentioned arrangement; Under 180 ℃, bake 10min at last.
According to the computational methods that are analogous to embodiment 1, the silk weighting rate of present embodiment 4 gained is 13.9%; And this silk fiber is soft.
Embodiment 5, a kind of silk weighting method that adopts the sol-gel process adhering sericin, carry out following steps successively:
1), the removal of impurities of silk is cleaned and is handled;
Take by weighing silk greig 100g, part is come unstuck in 4% 2709 protein enzyme solutions, and residual silkgum content is 9%; Reducing bleach in the bleaching liquid of 2.5g/L thiourea dioxide then floods in 3% softener KC to soft then, takes out at last to clean up;
2), the preparation of colloidal sol dressing liquid:
The tetraethyl orthosilicate (TEOS) of 0.1L, the absolute ethyl alcohol of 0.5L and γ-glycidyl ether oxygen propyl silane of 0.3L are fully mixed as coupling agent, under magnetic stirrer, add the aqueous hydrochloric acid solution of 0.1L, contain the HCL of 1mol in this aqueous hydrochloric acid solution; The above-mentioned raw materials component at 40 ℃ of following constant temperature hydrolysis 12h, obtains the colloidal sol dressing liquid of homogeneous transparent after evenly mixing under stirring;
3), the set of silk gum arrangement:
Above-mentioned colloidal sol dressing liquid is put in the bleaching processing of step 1) gained and the part boiled silk fabric after the soft finish, and employing two is soaked two methods of rolling and is carried out the set arrangement, and the liquid carrying rate that makes silk fabric is 100%;
With ageing 24h under the silk fabric normal temperature after the above-mentioned arrangement; Under 160 ℃, bake 15min at last.
According to the computational methods that are analogous to embodiment 1, the silk fabric rate of body weight gain of present embodiment 5 gained is 13.5%.
Measure the whiteness value behind folding 8 layers of the silk fabric of present embodiment 5 gained with WSD-3U type fluorescence whiteness test instrument, the result shows that whiteness value is 70.6, and this silk fabric is soft.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (5)
1, a kind of silk weighting method that adopts the sol-gel process adhering sericin is characterized in that comprising the steps:
1), the removal of impurities of silk is cleaned and is handled;
2), the preparation of colloidal sol dressing liquid:
By following components in percentage by volume constitutive material: 10～40% tetraethyl orthosilicate, 0～30% silane coupler and 40～80% absolute ethyl alcohol, all the other are the aqueous solution that contains catalyst; The concentration of described catalyst in raw material is 0.001～1molL
-1After the full and uniform mixing of described raw material, constant temperature hydrolysis 4～16h under 25～70 ℃ of temperature obtains the colloidal sol dressing liquid of homogeneous transparent;
3), the set of silk gum arrangement:
Adopt above-mentioned colloidal sol dressing liquid that two methods of rolling are soaked in the silk employing two of step 1) gained and carry out the set arrangement, the liquid carrying rate that makes silk is 60%～100%;
With ageing 0～24h under the silk normal temperature after the above-mentioned arrangement; Under 120～180 ℃, bake 10～60min at last.
2, the silk weighting method of employing sol-gel process adhering sericin according to claim 1 is characterized in that: described silane coupling agent is gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl silane or gamma-methyl allyl acyloxypropyl trimethoxysilane.
3, the silk weighting method of employing sol-gel process adhering sericin according to claim 2 is characterized in that: described catalyst is hydrochloric acid or nitric acid.
4, the silk weighting method of employing sol-gel process adhering sericin according to claim 3 is characterized in that: the silk in the described step 1) is boiled silk fiber not, part boiled silk fiber, not boiled silk fabric or part boiled silk fabric.
5, the silk weighting method of employing sol-gel process adhering sericin according to claim 4 is characterized in that: described not boiled silk fiber, part boiled silk fiber, not boiled silk fabric or process soft finish earlier of part boiled silk fabric and/or bleaching processing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677468A (en) * | 2012-03-01 | 2012-09-19 | 浙江理工大学 | Method for increasing weight and bulkiness of silk floss |
| CN113818248A (en) * | 2021-10-22 | 2021-12-21 | 浙江钱皇网络科技股份有限公司 | Fixing liquid and method for fixing silk floss by adopting same |
| CN114354440A (en) * | 2021-11-29 | 2022-04-15 | 南大光电半导体材料有限公司 | Device for detecting gasification characteristics of precursor material and using method |
| CN114504546A (en) * | 2020-11-16 | 2022-05-17 | 西南大学 | Preparation method of sericin nanogel |
-
2008
- 2008-08-05 CN CN2008100634548A patent/CN101333769B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677468A (en) * | 2012-03-01 | 2012-09-19 | 浙江理工大学 | Method for increasing weight and bulkiness of silk floss |
| CN114504546A (en) * | 2020-11-16 | 2022-05-17 | 西南大学 | Preparation method of sericin nanogel |
| CN114504546B (en) * | 2020-11-16 | 2024-02-02 | 西南大学 | Preparation method of sericin nanogel |
| CN113818248A (en) * | 2021-10-22 | 2021-12-21 | 浙江钱皇网络科技股份有限公司 | Fixing liquid and method for fixing silk floss by adopting same |
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