CN113604890A - Combined production method of fibroin and white steam filature - Google Patents

Combined production method of fibroin and white steam filature Download PDF

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Publication number
CN113604890A
CN113604890A CN202110868677.7A CN202110868677A CN113604890A CN 113604890 A CN113604890 A CN 113604890A CN 202110868677 A CN202110868677 A CN 202110868677A CN 113604890 A CN113604890 A CN 113604890A
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fibroin
white steam
silkworm cocoons
steam filature
temperature
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CN202110868677.7A
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CN113604890B (en
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杨祖根
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Suzhou Jiahe Sericulture Biotechnology Co ltd
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Suzhou Jiahe Sericulture Biotechnology Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01CCHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
    • D01C3/00Treatment of animal material, e.g. chemical scouring of wool
    • D01C3/02De-gumming silk
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • D01F4/02Monocomponent artificial filaments or the like of proteins; Manufacture thereof from fibroin
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Animal Husbandry (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Peptides Or Proteins (AREA)

Abstract

The invention relates to a combined production method of fibroin and white steam filature, which comprises the steps of putting silkworm cocoons into a cocoon cooking machine filled with neutral solution, cooking at a first temperature, and then preserving heat at a second temperature to degum the silkworm cocoons. The neutral solution in the application is mild, the damage to silk fibers is small, and the silkworm cocoons after being boiled and degummed can be used as raw materials for reeling silk to be continuously processed and used, and are made into white steam filature (raw silk) through reeling silk, re-shaking, finishing and inspection; under the condition of not influencing the yield and the quality of the white steam filature silk, the waste solution in the degumming process of the silkworm cocoons is reused to extract the fibroin, so that the waste is changed into valuable; the fibroin prepared by the method has good quality, and although the yield is a little lower than that of fibroin prepared by dissolving silk, the cost is lower, and the method has higher economic and application values.

Description

Combined production method of fibroin and white steam filature
Technical Field
The invention relates to a combined production method of fibroin and white steam filature.
Background
The silk is mainly composed of silk fibroin and sericin wrapped on the outer layer of the silk fibroin. The silk can be degummed to separate sericin from the outer layer of fibroin, and sericin and fibroin can be obtained after further treatment.
The traditional degumming mode is mainly a water boiling method, the purpose of degumming is achieved by soaking the silkworm cocoons in boiling water and dissolving sericin by using the boiling water, the degumming mode has long degumming time and is easy to decompose the sericin, and the obtained sericin is low in quality and yield and is usually discarded as industrial waste. The alkali dissolving method is an improvement of the traditional method, and although the quality and yield of sericin can be improved to a certain extent by degumming the silkworm cocoons with alkali liquor, the alkali liquor can influence the luster and quality of degummed silk fibers, and the method has high requirements on equipment and is not environment-friendly.
Disclosure of Invention
The invention aims to solve the technical problem of providing a joint production method which can simultaneously give consideration to the quality of fibroin and white steam filature.
In order to achieve the purpose, the invention adopts the technical scheme that:
a combined production method of fibroin and white steam filature comprises the steps of putting silkworm cocoons into neutral solution, cooking at a first temperature, and then preserving heat at a second temperature to degum the silkworm cocoons, wherein the neutral solution is aqueous solution containing a surfactant, and the first temperature is higher than the second temperature.
Preferably, the extraction method comprises controlling the first temperature to be 98-100 ℃ under normal pressure.
Further preferably, the second temperature is controlled to be 95-97 ℃.
Preferably, the cooking time is controlled to be 20-40 min, and further 25-35 min.
Further preferably, the heat preservation time is controlled to be 1.5-2.5 hours, and further to be 1.8-2.2 hours.
Preferably, the surfactant comprises an anionic surfactant and/or a nonionic surfactant.
Further preferably, the anionic surfactant is a sulfonate and/or a sulfate salt.
Still further preferably, the anionic surfactant comprises one or more of sodium dioctyl sulfosuccinate, sodium dodecylbenzenesulfonate, sodium glycocholate, sodium lauryl sulfate, and sodium lauryl sulfate.
Further preferably, the nonionic surfactant is one or more of a polyoxyethylene type, a polyol type, an alkanolamide type, a polyether type, and an amine oxide type.
Still further preferably, the nonionic surfactant comprises one or more of alkyl glucoside, fatty acid glyceride, fatty acid sorbitan, polysorbate, polyoxyethylene polyoxypropylene.
According to some preferred embodiments, the surfactant comprises Pluronic F-127 and/or sodium glycocholate.
Preferably, the mass content of the surfactant in the neutral solution is 1.3-2%, further 1.4-1.8%, and further 1.4-1.6%.
Further preferably, the feeding mass ratio of the silkworm cocoons to the neutral solution is 1: (9-11), further 1: (9.5-10.5).
Preferably, the production method further comprises the step of cooling to 55-65 ℃ after degumming and decomposition of the silkworm cocoons so as to reeling the degummed silkworm cocoons to obtain the silk.
Further preferably, the silk reeling comprises the steps of silk reeling, re-shaking, finishing and checking.
The white steam filature silk in the invention is silk long fiber, is a high-grade textile material, has good strong elongation, soft luster and strong hygroscopicity, and can be used for weaving various silk fabrics with different organizational structures. For the silkworm cocoons with better quality, the silkworm cocoons are preferably used as raw materials, and are subjected to degumming decomposition and then reeling to obtain white steam filature with higher added value; for the silkworm cocoons with poor quality, the silkworm cocoons are preferably subjected to cocoon opening, degumming decomposition and silk drawing to obtain silk fibers which are used as raw materials for manufacturing the silk quilt.
Preferably, the production method further comprises the step of filtering and impurity removing, centrifuging and impurity removing, concentrating and freeze drying the processing liquid of the silkworm cocoons after the degumming of the silkworm cocoons so as to obtain the finished fibroin product.
According to some preferred embodiments, the production method comprises the steps of:
(1) placing the silkworm cocoons in a neutral solution, cooking at the temperature of 98-100 ℃, and then preserving heat at the temperature of 95-97 ℃ to degum the silkworm cocoons, wherein the cooking time is controlled to be 20-40 min, and the heat preservation time is controlled to be 1.5-2.5 h;
(2) cooling the system in the step (1) to 55-65 ℃, taking out the degummed silkworm cocoons, and reeling, re-shaking, finishing and inspecting the degummed silkworm cocoons to prepare the white steam filature;
(3) and filtering the treated liquid after the silkworm cocoons are taken out to remove impurities, centrifugally removing the impurities, concentrating and freeze-drying to obtain a finished fibroin product.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the neutral solution in the application is mild, the silk is slightly damaged, and the degummed and decomposed silk has the advantages of good fiber strength and good glossiness and can be used as a raw material for continuous reeling processing;
the method has the advantages of short degumming time and high preparation efficiency through the design of the degumming process, can effectively reduce the decomposition problem of the fibroin caused by degumming for too long time, and the prepared fibroin has good quality and low cost;
according to the method, under the condition of ensuring the yield and the quality of the white steam filature, the original waste solution in the cocoon cooking process is reused, waste is changed into valuable, and the fibroin is prepared through filtering, centrifuging and concentrating, so that the method has high application and economic values.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not mentioned are conventional conditions in the industry. The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
The following examples and comparative examples were carried out under normal pressure unless otherwise specified.
Example 1
(1) Taking high-quality silkworm cocoons, and stripping the cocoon shells to obtain the silkworm cocoons for later use, which are referred to as light cocoons hereinafter;
(2) placing cocoons (100 g) in 1000g of neutral aqueous solution, heating to 100 ℃, keeping the temperature of 100 ℃, boiling for 30min, then cooling to 96 ℃, and preserving heat for 2 hours to ensure that the fibroin is degummed and decomposed on the cocoons; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;
(3) cooling to 60 ℃, taking out the smooth cocoons, using the smooth cocoons as a reeling raw material for later use, and preparing white filature (raw silk) through reeling, re-shaking, finishing and checking; filtering the neutral water solution of the cooked cocoons, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.
In the embodiment, when silk reeling is performed, silk reeling is smooth, the silk reeling end breakage rate is low, wherein 1.8g of fibroin and 33g of white filature are obtained in the embodiment, and the white filature meets the 4A-level standard of the GBT1797-2008 raw silk standard.
Example 2
(1) Taking high-quality silkworm cocoons, and stripping the cocoon shells to obtain the silkworm cocoons for later use, which are referred to as light cocoons hereinafter;
(2) placing cocoons (100 g) in 1000g of neutral aqueous solution, heating to 100 ℃, keeping the temperature of 100 ℃, boiling for 30min, then cooling to 96 ℃, and preserving heat for 2 hours to ensure that the fibroin is degummed and decomposed on the cocoons; wherein the neutral aqueous solution is prepared by dissolving 15g of sodium glycocholate surfactant in 985g of water;
(3) cooling to 60 ℃, taking out the smooth cocoons, using the smooth cocoons as a reeling raw material for later use, and preparing white filature (raw silk) through reeling, re-shaking, finishing and checking; filtering the neutral water solution of the cooked cocoons, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.
In the embodiment, when silk reeling is performed, silk reeling is smooth, the silk reeling end breakage rate is low, wherein 1.5g of fibroin and 32g of white filature are obtained in the embodiment, and the white filature meets the 4A-level standard of the GBT1797-2008 raw silk standard.
Comparative example 1
(1) Taking high-quality silkworm cocoons, and stripping the cocoon shells to obtain the silkworm cocoons for later use, which are referred to as light cocoons hereinafter;
(2) placing cocoons (100 g) in 1000g of aqueous alkali, heating to 100 ℃, keeping the temperature of 100 ℃, boiling for 30min, cooling to 96 ℃, and keeping the temperature for 2 hours to ensure that the fibroin is degummed and decomposed on the cocoons; wherein the alkali solution is prepared by dissolving 15g of sodium carbonate in 985g of water;
(3) cooling to 60 ℃, taking out the smooth cocoons, using the smooth cocoons as a reeling raw material for later use, and preparing white filature (raw silk) through reeling, re-shaking, finishing and checking; filtering the alkali solution of the boiled cocoons, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain the fibroin.
In this embodiment, when reeling, reeling is unsmooth, and the reeling end breakage rate is high, wherein 1.7g of fibroin and 32g of white filature are obtained in this embodiment, and the white filature is GBT1797-2008 raw silk standard level 2A standard.
Comparative example 2
(1) Taking high-quality silkworm cocoons, and stripping the cocoon shells to obtain the silkworm cocoons for later use, which are referred to as light cocoons hereinafter;
(2) placing cocoons (100 g) in 1000g of neutral aqueous solution, heating to 100 ℃, keeping the temperature at 100 ℃, boiling for 30min, and then preserving the temperature at 100 ℃ for 2 hours to ensure that the fibroin is degummed and decomposed on the cocoons; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;
(3) cooling to 60 ℃, taking out the smooth cocoons, using the smooth cocoons as a reeling raw material for later use, and preparing white filature (raw silk) through reeling, re-shaking, finishing and checking; filtering the solution of cooked cocoon, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain fibroin.
In the embodiment, when silk reeling is performed, the silk reeling is unsmooth, and the silk reeling end breakage rate is high, wherein 1.7g of fibroin and 28g of white filature are obtained in the embodiment, and the white filature is GBT1797-2008 raw silk standard 3A-grade standard.
Comparative example 3
(1) Taking high-quality silkworm cocoons, and stripping the cocoon shells to obtain the silkworm cocoons for later use, which are referred to as light cocoons hereinafter;
(2) placing a light cocoon (100 g) in 1000g of neutral aqueous solution, heating to 96 ℃, and preserving heat for 2.5 hours to ensure that the fibroin is degummed and decomposed on the light cocoon; wherein the neutral aqueous solution is prepared by dissolving 15g of Pluronic F-127 surfactant in 985g of water;
(3) cooling to 60 ℃, taking out the smooth cocoons, using the smooth cocoons as a reeling raw material for later use, and preparing white filature (raw silk) through reeling, re-shaking, finishing and checking; filtering the solution of cooked cocoon, centrifuging by a centrifuge to remove impurities, concentrating the centrifuged supernatant, and freeze-drying to obtain fibroin.
In the embodiment, when silk reeling is performed, silk reeling is unsmooth, silk is sticky and easy to wind, and the silk reeling end breakage rate is high, wherein 1.3g of fibroin and 32g of white filature are obtained in the embodiment, and the white filature is GBT1797-2008 raw silk standard level 2A standard.
The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.

Claims (10)

1. A joint production method of fibroin and white steam filature is characterized in that: the production method comprises the steps of putting the silkworm cocoons into a neutral solution, cooking at a first temperature, and then preserving heat at a second temperature to degum the silkworm cocoons, wherein the neutral solution is an aqueous solution containing a surfactant, and the first temperature is higher than the second temperature.
2. The process for the co-production of fibroin and white steam filature according to claim 1, characterized in that: the production method comprises the step of controlling the first temperature to be 98-100 ℃ and/or controlling the second temperature to be 95-97 ℃ under normal pressure.
3. A process for the co-production of fibroin and white steam filature according to claim 1 or 2, characterized in that: and controlling the cooking time to be 20-40 min and/or controlling the heat preservation time to be 1.5-2.5 h.
4. The process for the co-production of fibroin and white steam filature according to claim 1, characterized in that: the surfactant includes an anionic surfactant and/or a nonionic surfactant.
5. The process for the co-production of fibroin and white steam filature according to claim 4, characterized in that: the anionic surfactant comprises one or more of dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate, sodium glycocholate, sodium lauryl sulfate and sodium dodecyl sulfate; and/or the nonionic surfactant comprises one or more of alkyl glucoside, fatty glyceride, sorbitan fatty acid, polysorbate, polyoxyethylene polyoxypropylene.
6. Process for the co-production of fibroin and white steam filature according to any one of claims 1, 4, and 5, characterized in that: the surfactant includes Pluronic F-127 and/or sodium glycocholate.
7. The process for the co-production of fibroin and white steam filature according to claim 1, characterized in that: the mass content of the surfactant in the neutral solution is 1.3-2%, and/or the mass ratio of the silkworm cocoon to the neutral solution is 1: (9-11).
8. The process for the co-production of fibroin and white steam filature according to claim 1, characterized in that: the production method further comprises the step of cooling to 55-65 ℃ after degumming and decomposition of the silkworm cocoons so as to reeling the degummed silkworm cocoons to obtain white steam filature.
9. Process for the joint production of fibroin and white steam filature according to claim 1 or 8, characterized in that: the production method also comprises the step of filtering, removing impurities, centrifuging, removing impurities, concentrating and freeze-drying the silkworm cocoon treatment solution after degumming the silkworm cocoon to obtain a finished fibroin product.
10. The process for the co-production of fibroin and white steam filature according to claim 1, characterized in that: the production method comprises the following steps:
(1) placing the silkworm cocoons in a neutral solution, cooking at the temperature of 98-100 ℃, and then preserving heat at the temperature of 95-97 ℃ to degum the silkworm cocoons, wherein the cooking time is controlled to be 20-40 min, and the heat preservation time is controlled to be 1.5-2.5 h;
(2) cooling the system in the step (1) to 55-65 ℃, taking out the degummed silkworm cocoons, and reeling, re-shaking, finishing and inspecting the degummed silkworm cocoons to prepare the white steam filature;
(3) and filtering the treated liquid after the silkworm cocoons are taken out to remove impurities, centrifugally removing the impurities, concentrating and freeze-drying to obtain a finished fibroin product.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103205885A (en) * 2012-11-28 2013-07-17 苏州大学 Silk degumming/scouring agent and applications thereof
CN106012040A (en) * 2016-07-18 2016-10-12 上林县中兴丝业有限公司 Production process of white steam filature yarns
CN106435765A (en) * 2016-12-12 2017-02-22 广西江缘茧丝绸有限公司 Silk degumming method
CN106676642A (en) * 2016-12-12 2017-05-17 苏州大学 Silk degumming/scouring agent, application and treatment method for degumming waste liquid
CN111101207A (en) * 2020-01-07 2020-05-05 圣凯科技产业(辽宁)有限公司 Degumming agent and preparation method thereof, silkworm cocoon degumming method and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103205885A (en) * 2012-11-28 2013-07-17 苏州大学 Silk degumming/scouring agent and applications thereof
CN106012040A (en) * 2016-07-18 2016-10-12 上林县中兴丝业有限公司 Production process of white steam filature yarns
CN106435765A (en) * 2016-12-12 2017-02-22 广西江缘茧丝绸有限公司 Silk degumming method
CN106676642A (en) * 2016-12-12 2017-05-17 苏州大学 Silk degumming/scouring agent, application and treatment method for degumming waste liquid
CN111101207A (en) * 2020-01-07 2020-05-05 圣凯科技产业(辽宁)有限公司 Degumming agent and preparation method thereof, silkworm cocoon degumming method and application

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Title
沈淦清: "染整工艺 第二册 蛋白质纤维、合成纤维及其混纺制品的染整", vol. 1, 高等教育出版社, pages: 48 - 52 *

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