WO1999034038A1 - Matieres de soie modifiee et procede de production de celles-ci - Google Patents
Matieres de soie modifiee et procede de production de celles-ci Download PDFInfo
- Publication number
- WO1999034038A1 WO1999034038A1 PCT/JP1998/005784 JP9805784W WO9934038A1 WO 1999034038 A1 WO1999034038 A1 WO 1999034038A1 JP 9805784 W JP9805784 W JP 9805784W WO 9934038 A1 WO9934038 A1 WO 9934038A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silk
- modified
- silk material
- modified silk
- refined
- Prior art date
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01B—MECHANICAL TREATMENT OF NATURAL FIBROUS OR FILAMENTARY MATERIAL TO OBTAIN FIBRES OF FILAMENTS, e.g. FOR SPINNING
- D01B7/00—Obtaining silk fibres or filaments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
Definitions
- the present invention relates to a modified silk material useful for various uses, obtained by heat-treating silk in a gas stream.
- the modified silk material of the present invention can be used as a coating material for the human skin, such as a drug for the skin, a quasi-drug for the skin, or a material for cosmetics, etc. It can be used for applications such as filtration media and abrasives.
- organic materials are used as materials for coating materials for human skin such as eyebrows and gray hair dyeing by heating, and there are materials obtained by incompletely burning petroleum-based materials.
- adsorbent / filtration material a carbide obtained by heat-treating a plant is used.
- the heat treatment of the silk of the present invention is carried out at 600 to 2000 in an inert gas atmosphere.
- the heating temperature was set at 600 ° C. or higher to completely perform carbonization.
- carcinogenic substance (lenspirene) may be generated, and furthermore, tars may be formed due to the wax etc. in the silk material, and the product (carbide) may be in the form of fine particles or particles. It lacks usability because it does not happen.
- the upper limit of the heating temperature is set to 2000 ° C. because energy consumption is too large at 2000 ° C. or higher and it is difficult to industrially use it from a cost perspective.
- the degree of carbonization of the heat-treated one is extremely large, and therefore, the field of application is extremely limited.
- the present invention has been made under such a technical background.
- an object of the present invention is to further expand the application field utilizing the characteristics of silk carbide.
- the present inventors have conducted various studies on the conditions for heat-treating silk, and as a result, have been able to adjust the degree of carbonization of the heat-treated product in various ways, and to reduce the energy consumed by the heat treatment at low cost. Found a point that could be implemented industrially
- the present invention has been achieved based on this finding, and as described below, a method for producing a modified silk material comprising heat-treating silk under specific conditions, and a coating for human skin Materials that provide modified silk materials suitable for applications such as materials, medical materials, plant growth promoting materials, adsorbent materials, filtration materials, and abrasive materials.
- the present invention relates to (1) a method in which silk unrefined silk, silk semi-refined silk, refined silk, or a composite thereof is subjected to a gas pressure of 0.5 to 1.5 atm, a temperature of 150 to 5 atm. 0
- a method of producing a modified silk material which is subjected to heat treatment for a certain period of time in an atmosphere of a 0 U C airflow to obtain a modified silk material having various colors
- silk unrefined, silk semi-refined, silk refined, or a composite thereof is a film, powder, fiber, thread, fabric, braid, or in the method for producing a modified silk material according to any one of (1) and (4) above, which is in the form of these composites,
- the heat treatment time is in the range of several minutes to 20 hours in the modified silk material according to (7).
- (9) a method of converting unrefined silk, semi-refined silk, refined silk, or a composite thereof from nitrogen, helium, neon, argon, krypton, and xenon Gas pressure of active gas alone or a mixture thereof 0.5 to 1.5 atm, temperature 150 to 500. It exists in a denatured silk material with various colors obtained by heat treatment for a certain period of time in an atmosphere of C airflow.
- the heat treatment time is in the range of several minutes to 20 hours in the modified silk material of (9).
- the silk material which is the starting point of the modified silk material of the present invention is silk unscrutinized, silk semi-scrutinized, silk refined, or a composite thereof.
- the silk material is in the form of powder, fiber, yarn, fabric (knit, woven, non-woven fabric, etc.), braid, or a composite thereof.
- cocoons are composed of five mouth proteins (about 70%) and sericin (about 28%), and sericin. Exists to wrap around the mouth
- the silk scoured material is obtained by treating silk with hot water containing a surfactant such as seggen or lazen power, or an alkaline substance such as sodium carbonate or sodium gayate (so-called “ Alkaline scouring), treated with warm water containing enzymes such as chymotrypsin, alcalase, and happine (so-called “enzyme scouring”), and treated with microorganisms (so-called “sap scouring”). ), Along with sericin.
- a surfactant such as seggen or lazen power
- an alkaline substance such as sodium carbonate or sodium gayate
- enzymes such as chymotrypsin, alcalase, and happine
- microorganisms sino-called “sap scouring”.
- the unscrutinized silk means silk that has not been scoured.
- silk semi-refined material refers to an intermediate between unrefined and refined materials, and usually contains less than 15% sericin.
- the heat treatment temperature is in the range of 150 to 50 (TC.
- the production method of the present invention has a relatively low temperature range for the heat treatment. Since it is carried out in an environment, energy consumption is kept low and it is extremely advantageous in industry.
- heat treatment can be performed without leaving impurities in the deformed silk material.
- the denatured silk material obtained by the heat treatment is dried, it is possible to easily obtain the denatured silk material in the form of fine particles or particles.
- the temperature of the raw silk material can be stably and efficiently raised.
- the raw silk material having a film-like or fabric-like shape has an extremely low tensile strength due to the heat treatment, it is easy to be mechanically pulverized. it can.
- the denatured silk material of the present invention changes to white, pale yellow, yellow, brown, dark brown, blue, purple, black brown, and then black depending on the degree of heat treatment. It can be used as a coating material for human skin, such as foundation, eyebrow dye, white hair dye, red lipstick, nail polish, lipstick, and eye shadow.
- the heat treatment can be quickly terminated at the stage of the target color to obtain the target denatured silk material of various colors.
- the modified silk material obtained in this way exhibits various colors according to the size of the uncarbonized portion (silk) that exists depending on the degree of carbonization, and partially has a biocompatibility function inherent to silk. Is what you are doing.
- the properties as a carbide and the inherent properties of silk can be positively combined, and the range of application is broadened, and it can be used for various purposes.
- it can be used for applications such as plant growth promoters, adsorbents, filtration materials and abrasives, as well as medical materials and coating materials for human skin that directly touch skin.
- the form of the silk material used as the raw material of the modified silk material includes various forms such as films, powders, fibers, yarns, fabrics (knitted fabrics, woven fabrics, non-woven fabrics), braids, and composites thereof. Can be taken.
- the form after heat treatment can be maintained in the form of the raw material, it can be directly used in that form.
- the fiber which is a characteristic of the fabric, is three-dimensionally entangled, resulting in a large surface area per unit volume. It is the best material.
- the modified silk material is mechanically pulverized, pulverize it to 0.01 to 10 micron.
- Fine particles of modified silk material smaller than 0.01 micron are expensive to manufacture, and in addition practically finer particles are not required.
- the crushed size is preferably between 0.01 mm and 20 mm:
- the present invention relates to a method for controlling the degree of carbonization by heat-treating silk under mild conditions (gas pressure: 0.5 to 1.5 atm, 150 to 50 (in a KC gas stream atmosphere)) to adjust the degree of carbonization. It is possible to obtain a modified silk material that is useful for various uses that has both the properties of silk and the inherent properties of silk.
- the heat treatment is performed under a gas stream of gas pressure of 0.5 to 1.5 atm.
- the gas stream does not carry volatile components generated by thermal decomposition out of the system, and does not produce the product which is like a conventional product in the form of a vitreous mixture.
- silk can be used even if it uses waste materials such as silk products.
- crystalline silk powder similar to the crystalline silk powder described in the specification of Japanese Patent No. 2615440
- the glass tube was placed horizontally in an electric furnace (Shinyo Chemical Instruments Co., Ltd., Model KP-7). Nitrogen gas was applied from one end of the glass tube to the other end, and the gas pressure was set to 120.1 atm.
- the crystalline silk powder was heated from room temperature at a heating rate of 10 ° CZ while flowing so that Then, the color change of the crystalline silk powder during the heating process was visually observed.
- the same treatment as described above was performed with argon gas, and the color change of the crystalline silk powder during the heating process was similarly observed with the naked eye.
- the nitrogen gas and the argon gas have a slightly reddish color in the range of 240 ° C to 280 ° C, but the hue of both colors is Is the same.
- the raw silk is immersed in a 0.1% aqueous solution of sodium carbonate at a bath ratio of 1 to 50, boiled for 1 hour, renewed with an aqueous solution of sodium carbonate, boiled again for 1 hour, washed with water, dried, and dried with a silk thread. Fiber).
- Example 2 using the apparatus of Example 1, the conditions were set at a temperature of 280 ° C., a baking time of 3 minutes, and an argon gas flow of about 0.5 atm.
- the silk became semi-carbonized and a red-brown calcined material (modified silk material) was produced, partially retaining the properties of the silk protein.
- This modified silk material was pulverized by a micro-pulverizer (Hosokawa Miclon Co., Ltd.) and further classified to obtain particles of about 5 microns.
- a micro-pulverizer Hosokawa Miclon Co., Ltd.
- Example 2 The same experiment as in Example 1 was performed except that the pressure was changed to 1.6 atm in order to obtain a modified silk material under different firing conditions.
- Example 2 The same experiment as in Example 1 was performed except that the pressure was set to 0.4 atm. In these cases, stable heating of the crystalline silk powder in the glass tube was not possible.
- the silkworm silk obtained by boiling the silkworm silk with a 0.1% aqueous solution of sodium carbonate at a bath ratio of 50 times for 1 hour, washing with water and drying was used as a material.
- Modified silk of white (processing temperature of 25 ° C), light yellow (processing temperature of 220 ° C), and black tea (processing temperature of 300 ° C) obtained in the heat treatment of [Example 1].
- A, B, C, and D were prepared by mixing the ingredients with cosmetics for the care of skin prisoners as follows.
- Water (100 g) containing the modified silk material was given weekly to a grass whistle planted in a container about 20 cm wide, about 60 cm long and about 15 cm deep.
- the daily grass fed was 150 g.
- Example 4 2 g of the dark brown (see Table 4) crystalline silk powder obtained in the heat treatment of Example 3 was placed in a cotton cloth bag, and the bag was slightly turbid in 1 liter of fresh water (Lake Biwa). After 5 hours, it was less turbid and more transparent,
- Example 9 Example as an adsorbent (deodorant) for odors
- Polishing was performed using the white (processing temperature 100 ° C.) and brown (processing temperature 270 ° C.) crystalline silk powder obtained in the heat treatment of [Example 1]. Polishing, Mase containing alcohol cloth wipe eyeglasses glass and metal (copper) Menjo, good crystallinity silk powder white and brown every 5 0 cm 2 per Ri 2 g after wiping, dry thereon Glasses and a metal surface were polished for 1 hour with a load of 10 kg / cm 2 on which an eyeglass wipe and a plastic plate were placed. After that, the glass and metal surfaces were thoroughly wiped with alcohol wiped with a spectacle wipe. When the surface was observed while reflecting light on the glass and metal surfaces, the gloss was improved by polishing.
- Example 1 White (process temperature 100 ° C) obtained in the heat treatment of Using the crystalline silk powder (see Table 1), we conducted an experiment using it as a filter.
- Each of the white silk powders was sandwiched between flat plates, and was pressurized at a pressure of 20 kg / cm 2 and solidified to form a plate having a thickness of 2 mm.
- a plate made of this powder was sandwiched between filter papers to form a filter. Next, when suction filtration was performed using water from Lake Biwa at 0.5 atm, the degree of turbidity of the water after filtration was considerably reduced.
- the modified silk material of the present invention can be used as a coating material for the human skin, such as a drug for the skin, a quasi-drug for the skin, or a material for cosmetics, etc. It can be used for applications such as filtration media and abrasives, but also has many potential uses, such as for material paints and clothing dyeing.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Animal Husbandry (AREA)
- Molecular Biology (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Cosmetics (AREA)
- Materials For Medical Uses (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE69821916T DE69821916T2 (de) | 1997-12-25 | 1998-12-21 | Modifizierte seidenmaterialen und herstellungsverfahren |
KR10-1999-7007681A KR100393831B1 (ko) | 1997-12-25 | 1998-12-21 | 변성견소재, 그 제조방법 |
EP98961455A EP0964085B1 (en) | 1997-12-25 | 1998-12-21 | Modified silk materials and process for the production thereof |
BR9807604A BR9807604A (pt) | 1997-12-25 | 1998-12-21 | Material de seda desnaturado e método para preparar o mesmo |
HK00103414A HK1024272A1 (en) | 1997-12-25 | 2000-06-07 | Denatured silk material or various colors and method for preparing same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP36739597 | 1997-12-25 | ||
JP9/367395 | 1997-12-25 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1999034038A1 true WO1999034038A1 (fr) | 1999-07-08 |
Family
ID=18489211
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP1998/005784 WO1999034038A1 (fr) | 1997-12-25 | 1998-12-21 | Matieres de soie modifiee et procede de production de celles-ci |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP0964085B1 (ja) |
KR (1) | KR100393831B1 (ja) |
CN (1) | CN1123656C (ja) |
BR (1) | BR9807604A (ja) |
DE (1) | DE69821916T2 (ja) |
HK (1) | HK1024272A1 (ja) |
WO (1) | WO1999034038A1 (ja) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4171491B2 (ja) * | 2003-07-16 | 2008-10-22 | シナノケンシ株式会社 | 絹焼成体の製造方法および絹焼成体からなる抗菌材の製造方法 |
EP1659218A1 (en) * | 2004-11-19 | 2006-05-24 | The Procter & Gamble Company | A tissue paper with silk fibers |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6115896A (ja) * | 1984-07-02 | 1986-01-23 | Jiro Asahina | ▲おん▼度変化式▲きぬ▼粉体の製造方法 |
JPH04174763A (ja) * | 1990-10-31 | 1992-06-22 | Kanebo Ltd | 絹繊維構造物の改質方法 |
JP2950729B2 (ja) * | 1994-08-18 | 1999-09-20 | 上谷 昇一 | 絹素材の処理方法 |
JPH10266010A (ja) * | 1997-03-25 | 1998-10-06 | Kawamura:Kk | 絹材料の炭化処理粉末、炭化処理物並びにそれらの製造方法 |
KR100402051B1 (ko) * | 2000-10-18 | 2003-10-17 | 한국과학기술연구원 | 질소산화물 저감용 선택적 무촉매 환원제 |
-
1998
- 1998-12-21 BR BR9807604A patent/BR9807604A/pt active Search and Examination
- 1998-12-21 CN CN98803385A patent/CN1123656C/zh not_active Expired - Fee Related
- 1998-12-21 DE DE69821916T patent/DE69821916T2/de not_active Expired - Fee Related
- 1998-12-21 WO PCT/JP1998/005784 patent/WO1999034038A1/ja active IP Right Grant
- 1998-12-21 KR KR10-1999-7007681A patent/KR100393831B1/ko not_active IP Right Cessation
- 1998-12-21 EP EP98961455A patent/EP0964085B1/en not_active Expired - Lifetime
-
2000
- 2000-06-07 HK HK00103414A patent/HK1024272A1/xx not_active IP Right Cessation
Non-Patent Citations (1)
Title |
---|
See also references of EP0964085A4 * |
Also Published As
Publication number | Publication date |
---|---|
BR9807604A (pt) | 2000-03-21 |
EP0964085B1 (en) | 2004-02-25 |
KR100393831B1 (ko) | 2003-08-06 |
DE69821916D1 (de) | 2004-04-01 |
DE69821916T2 (de) | 2004-12-23 |
KR20000075618A (ko) | 2000-12-26 |
CN1123656C (zh) | 2003-10-08 |
EP0964085A4 (en) | 2002-03-06 |
CN1250492A (zh) | 2000-04-12 |
HK1024272A1 (en) | 2000-10-05 |
EP0964085A1 (en) | 1999-12-15 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR100393832B1 (ko) | 결정성 견 초미세분말의 제조방법 | |
JP3066434B2 (ja) | 変性絹素材、その製造方法 | |
WO1999034038A1 (fr) | Matieres de soie modifiee et procede de production de celles-ci | |
CN105908302B (zh) | 一种复合雪纺面料的制备方法 | |
JPH101820A (ja) | 人造繊維およびその製品 | |
JP3505677B2 (ja) | 結晶性絹超微粉末を含有する化粧料 | |
CN104233508A (zh) | 一种高弹性膨化蚕丝复合纤维及其制作方法 | |
KR19990038571A (ko) | 황토분을 이용한 섬유의 염색방법 | |
CN1826359A (zh) | 氨基酸衍生物缓释性聚合物、含有该聚合物的化妆品及纤维结构物与这些的制造法及再生处理法 | |
KR100352240B1 (ko) | 쑥을 이용한 섬유 염색방법 및 그 제품 | |
CN107502981A (zh) | 一种羽绒服用抗菌防潮羽绒的加工工艺 | |
CN106637909A (zh) | 一种热稳定性保暖胶原蛋白羊绒复合面料及其制作方法 | |
CN106637974A (zh) | 一种悬垂性好的胶原蛋白羊绒复合面料及其制作方法 | |
JPH10266010A (ja) | 絹材料の炭化処理粉末、炭化処理物並びにそれらの製造方法 | |
JPH03220267A (ja) | 黒色着色材の製造方法およびその応用 | |
JP3851928B2 (ja) | 細胞生育性に優れた改質絹粉末、その製造方法及びその利用 | |
CN107595033A (zh) | 茉莉花香桑蚕丝靠枕 | |
KR102659626B1 (ko) | 분무건조 공정을 이용한 구형 탄산칼슘-셀룰로오스 복합입자의 제조방법 | |
KR100431669B1 (ko) | 누에고치로부터 제조된 분말, 그 제조방법 및 용도 | |
JP4624710B2 (ja) | 着色絹粒子、油性物質含有絹粒子の製造方法 | |
TW200808169A (en) | Method and nano-composition for producing colored silkworm cocoons | |
KR960020846A (ko) | 자연산 악세사리 및 그 가공방법 | |
Sathish | A Study on Silk Fabric Applied with Eco-Friendlycolorants for the Enhancement of Textile Properties | |
CN115075000A (zh) | 一种真丝织物持续天然凉感印制整理方法 | |
KR20090131765A (ko) | 쪽염색 분말을 포함하는 화장료 조성물 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 98803385.2 Country of ref document: CN |
|
AK | Designated states |
Kind code of ref document: A1 Designated state(s): BR CN IN KR US VN |
|
AL | Designated countries for regional patents |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE |
|
WWE | Wipo information: entry into national phase |
Ref document number: 1998961455 Country of ref document: EP Ref document number: 1019997007681 Country of ref document: KR |
|
WWE | Wipo information: entry into national phase |
Ref document number: IN/PCT/1999/19/KOL Country of ref document: IN Ref document number: 1199900695 Country of ref document: VN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application | ||
WWE | Wipo information: entry into national phase |
Ref document number: 09380252 Country of ref document: US |
|
WWP | Wipo information: published in national office |
Ref document number: 1998961455 Country of ref document: EP |
|
WWP | Wipo information: published in national office |
Ref document number: 1019997007681 Country of ref document: KR |
|
WWG | Wipo information: grant in national office |
Ref document number: 1019997007681 Country of ref document: KR |
|
WWG | Wipo information: grant in national office |
Ref document number: 1998961455 Country of ref document: EP |