CN112826286A - Washable silk quilt - Google Patents

Washable silk quilt Download PDF

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Publication number
CN112826286A
CN112826286A CN202110015364.7A CN202110015364A CN112826286A CN 112826286 A CN112826286 A CN 112826286A CN 202110015364 A CN202110015364 A CN 202110015364A CN 112826286 A CN112826286 A CN 112826286A
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silk
mass concentration
water
silkworm cocoons
degumming
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CN202110015364.7A
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CN112826286B (en
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倪冬栋
倪学林
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Zhejiang Canyuan Home Textile Co ltd
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Zhejiang Canyuan Home Textile Co ltd
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    • AHUMAN NECESSITIES
    • A47FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47GHOUSEHOLD OR TABLE EQUIPMENT
    • A47G9/00Bed-covers; Counterpanes; Travelling rugs; Sleeping rugs; Sleeping bags; Pillows
    • A47G9/02Bed linen; Blankets; Counterpanes
    • A47G9/0207Blankets; Duvets
    • 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
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/04Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres
    • D04H1/08Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres and hardened by felting; Felts or felted products
    • D04H1/09Silk
    • 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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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Animal Husbandry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a washable silk quilt, which is characterized in that according to the performance of sericin, the outermost layer of sericin is thoroughly removed by adopting a proper auxiliary agent and a degumming method, the middle layer of sericin is partially removed, the innermost layer of sericin is completely reserved, and the mixture of glutaraldehyde and polyamide formaldehyde is used as a glue fixing agent, so that the fluffiness and the acid and alkali resistance of the silk quilt are improved.

Description

Washable silk quilt
Technical Field
The invention relates to the technical field of home visits, in particular to a washable silk quilt.
Background
Silk is a natural filament fiber integrating softness, lightness and fineness in nature, has the reputation of 'second skin of human body' and is called 'fiber queen' in the industry. The components of the silk are most similar to those of human skin, contain various amino acids required by human body, and have the effects of removing dampness, preventing wind, calming the nerves, balancing and nourishing the human skin. The silk quilt manufactured by the traditional method has the unique excellent qualities of close-fitting heat preservation, fluffiness and softness, ventilation and health care, warm in winter and cool in summer and the like, but the silk quilt is not suitable for water washing, because the fibers are adhered and hardened to yellow after water washing, the fluffiness and the heat preservation of the silk quilt are reduced, and the excellent characteristics can be recovered only by turning over and detaching again, which brings great inconvenience to consumers.
Theoretically, the silk is composed of two parts of sericin and fibroin, wherein the sericin and the fibroin belong to proteins, and different physicochemical characteristics are formed due to the difference of molecular groups and structures. The silk fibroin is fibrous protein synthesized and secreted by a posterior silk gland, consists of amino acids such as alanine, alanine and serine, is formed by antiparallel folding chain conformation beta, can only absorb water, swell and expand under the condition of moist heat, is not easy to dissolve, has stable physicochemical properties, and is a main material of the silk quilt. Sericin is a natural water-soluble globulin secreted by silk glands of silkworms, is rich in amino acids with polar side chains such as serine, aspartic acid and glutamic acid, has good biological characteristics, but is easy to denature under the damp and hot conditions, and aqueous solution of the sericin is easy to gel, so that the phenomena of adhesion and hardening yellowing among fibers of silk quilt are caused. In addition, the existence of a large amount of sericin can influence the luster and hand feeling of silk fibers, and impurities such as wax, grease and the like on the surface of silk can bring certain difficulty to the silk making process. In the traditional production process of the silk quilt, in order to improve the softness of the silk quilt, a refining process is usually adopted to remove sericin.
Clear water Zhende points out that sericin is divided into three different structures from outside to inside, the sericin on the outermost layer accounts for about 40% of the total mass of the sericin, can be dissolved in boiling water for 10min, is called sericin 1, the sericin on the second layer accounts for 40-50% of the total mass of the sericin, is difficult to dissolve, and needs to be boiled in boiling water for 2-3 hours, and is called sericin 2; the sericin in the innermost layer accounts for about 10-20% of the total sericin, takes 5-6 hours to dissolve, and is difficult to completely remove, namely sericin 3. Of the three sericins, sericin 1 is an amorphous substance, most soluble, hard and brittle. The sericin 2 has smooth surface, good luster and little hardness, can endow the fiber with rigidity and wrinkle resistance, and can reflect or absorb ultraviolet rays to slow down the yellowing and browning speed of the real silk fiber. Therefore, all or part of the sericin 2 is selectively reserved, and the performance of the silk fiber can be obviously improved. Sericin 2 and sericin 3 contain crystalline fractions, and sericin 3 shows that much wax is present, is most insoluble, and is difficult to remove.
The sericin residual rate of the silk quilt in the market is generally 3% -15%, even if the silk quilt is completely degummed, 2% -3% sericin remains, and the adoption of the complete degummed process wastes excellent sericin, and waste water discharged in the degummed process can cause rapid eutrophication of rivers and water pollution.
Besides improving the performance of the silk quilt after washing by adopting a degumming method, on the other hand, the proper cross-linking agent is selected to firmly fix the sericin on the fibroin, so that the sericin is protected while the water solubility of the sericin is changed. The sericin fixation adopts a physical or chemical method, so that a cross-linking agent enters sericin molecules to perform cross-linking reaction with amino acid side chain groups, and the sericin loses water solubility, has a stable structure and is fixed on the silk fibroin and is utilized as a part of silk fibers. The glue fixing method can lead silk fibers to obtain different surface effects, and the water solubility of the silk glue is changed and the wet and hot stability is improved by adopting the proper glue fixing method.
Glutaraldehyde (GA) is an excellent protein cross-linking agent, is cheap and easily available, is environment-friendly and nontoxic, and has a good cross-linking effect. However, the GA solid gum reported in the existing data has the defects that the silk is yellowed, and after being washed by water for many times, the compressibility and recovery rate of the silk quilt are obviously reduced. It is reported in the literature that addition of sodium bisulfite to the reaction mixture reduces the degree of yellowing, and addition of such an auxiliary reduces the degree of yellowing of silk, but the fastness to fixing also drops sharply. During degumming test, the refining rate is the same as that of the almost untreated sample, and the fixing effect is not ideal. It has also been reported that the degree of yellowing is reduced by using a very low concentration, but the fixing effect is also reduced by too low a concentration.
In the prior art, modified glutaraldehyde is also reported for glue fixation, for example, in qian xi huai, formaldehyde, methanol and glutaraldehyde are used for preparing modified glutaraldehyde in 'characterization of process conditions and product performance for silk glue fixation by using modified glutaraldehyde', and the modified glutaraldehyde is used as a cross-linking agent for fixing silk sericin. The cross-linking agent effectively reduces the yellowing degree of raw silk; the whiteness of the raw silk after glue fixation treatment by modified glutaraldehyde and optimized process conditions is not changed, and the basic performance of the silk fiber is maintained. In this scheme, all carry out the solid glue with the three layer construction of sericin, silk after this solid glue has kept the fibrous basic performance of silk, when being applied to production silk quilt, wax, grease etc. that exist in a large number in the sericin make the compliance and the warmth retention of silk quilt weaken to some extent.
Disclosure of Invention
The invention provides a washable silk quilt, which is characterized in that according to the performance of sericin, the outermost layer of sericin is thoroughly removed by adopting a proper auxiliary agent and a degumming method, the middle layer of sericin is partially removed, the innermost layer of sericin is completely reserved, and the mixture of glutaraldehyde and polyamide formaldehyde is used as a glue fixing agent, so that the fluffiness and the acid and alkali resistance of the silk quilt are improved.
The invention realizes the purpose through the following technical scheme:
(1) pretreatment of silkworm cocoon
The silkworm cocoons are soaked and pretreated by the compound penetrant, so that the silkworm cocoons are soft, the swelling of sericin is promoted, the penetration effect is improved, and preparation is provided for subsequent degumming and glue fixation.
The composition of the compound penetrant is as follows: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5-1.0%, a silk foaming agent ST-101 with the mass concentration of 1.0-2.0% and a silk foaming agent SW-102 with the mass concentration of 1.0-2.0% into purified water. The pretreatment process of the silkworm cocoon comprises the following steps: heating water to 50-80 ℃, immersing the silkworm cocoons in a penetrating agent at a bath ratio of 1: 10-20, pretreating the silkworm cocoons under normal pressure, pouring the silkworm cocoons into a vacuum penetration barrel in order to improve the penetration effect and prevent dry cocoons from floating, putting the silkworm cocoons into a cotton mesh bag, adding stones at the bottom of the mesh bag, sinking the silkworm cocoons to the bottom of the penetration barrel, starting a vacuum pump, wherein the vacuum degree is less than or equal to 70kPa, and keeping the time: 30-60 s/time; penetration times are as follows: 3-5 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons.
The silk soaking agent ST-101 is used for warp-wise soaking of silk, and the silk soaking agent SW-102 is used for warp-wise soaking of silk, so that the silk has excellent smoothness and better tensile strength.
(2) Degumming of silk
Washing the silkworm cocoon soaked by the penetrant with clear water for 1-2 times, treating the silkworm cocoon with degumming liquid, and removing
The glue solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5-1.0% into clear water, adding 3.0-8.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5-8.0 by using sodium bicarbonate at the bath ratio of 1: 20-30, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrant from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled. Washing the silkworm cocoons for 1-2 times by using clean water, obtaining fluffy and soft silk pieces by adopting a silk reeling process without passing through porcelain eyes and printing chiffon, and drying the obtained silk pieces by using infrared rays or hot air until no adhesion is generated between the silk pieces.
The degumming process can completely elute sericin on the outermost layer of the silk, 50-70% of the sericin on the middle layer and completely reserve the sericin on the inner layer. The silk softener Ultratex FSA is added into the degumming solution, so that silk can be softer and smoother on one hand, and on the other hand, the Ultratex FSA has very large molecular weight and hydroxyl end groups, so that the silk and the fabric can be further polymerized into a net structure under the action of the metal salt protonated ionic liquid, the sericin is removed in a layered manner, and the aims of retaining the sericin at the innermost layer, partially retaining the sericin at the middle layer and completely removing the sericin at the outermost layer are fulfilled by controlling degumming temperature and time.
In the silk, the silk mainly comprises 24-25 wt% of sericin and 75-76 wt% of fibroin, wherein the sericin is divided into three layers, the outermost layer of sericin accounts for about 40 wt% of the sericin, the second layer of sericin accounts for about 40-50 wt% of the sericin, the innermost layer of sericin accounts for about 10-20 wt% of the sericin, the degumming degree is obtained by weighing the weight of the silk before and after degumming, when the weight after degumming is 81.3-85.0 wt% of the silk before degumming, the outermost layer of sericin is completely eluted, the middle layer of sericin is eluted by 50-70 wt%, and the inner layer of sericin is completely reserved.
(3) Fixing glue for silk
And (3) carrying out sericin fixation treatment on the degummed silk slices by adopting a cross-linking agent. The cross-linking agent is a mixture of glutaraldehyde and polyamide formaldehyde, and the fixing process conditions are as follows: the bath ratio is 1: 30-50, the mass concentration of glutaraldehyde is 0.5-1.5%, the mass concentration of polyamide formaldehyde is 0.1-1.0%, the temperature is 40-50 ℃, and the soaking time is 1-2 h. The mixture of glutaraldehyde and polyamide formaldehyde is used as the glue fixing agent, so that sericin can be firmly coated outside the silk fibroin, silk is not adhered after washing, and after washing for multiple times, the silk can be kept soft and fluffy, and the heat retention of the silk quilt is kept.
(4) Post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes to obtain a reusable liquid. Rinsing with clear water, bleaching and softening. Washing with water, drying, air drying (or oven drying), and drawing into silk floss quilt.
In the use process of the silk quilt, an environment system of a human body and the silk quilt contains two air types, namely static air and dead space air. Still air refers to air that is inactive and takes up some space. The air in the silk quilt comprises air between a human body and the silk quilt, air between the filler and the quilt cover and air between filler fiber layers. Researches show that the heat insulation value of the static air is increased along with the increase of the thickness, so that the filling power and the rebound resilience of the filler are increased, the increase of gaps among fibers is facilitated, the thickness of an air layer in the silk quilt is increased, and the heat insulation performance of the silk quilt is improved. With the use of the silk quilt, silk fibers absorb part of water vapor, the internal force among the fibers is gradually reduced and disappeared, the fluffiness is gradually reduced, the contained air amount is also gradually reduced, and if a very small amount of sericin is left on the fibroin, the silk fibers are gradually denatured and adhered in the moisture absorption process. When the fabric is wetted, the elasticity and bulkiness of the fabric are difficult to return to the original state due to the hardening of the sericin. Therefore, with the use of the silk quilt, the content of static air is gradually reduced, the fluffiness and the heat retention are obviously reduced, and the service life is greatly reduced. On the other hand, when the silk floss is washed by water, the air between the original silk floss is expelled, the silk and the silk are closely contacted, and sericin remained on the silk floss is mutually adhered; after drying, the silk floss becomes into cakes, the silk floss is long, the elasticity is limited, enough space force is not formed at all to restore the original shape, and the comforter batt becomes soft and uneven.
Therefore, the silk quilt keeps excellent heat retention for a long time, on one hand, the residual sericin needs to be insoluble in water, and the adhesion caused by gradual denaturation in the moisture absorption process of the sericin is prevented after the silk quilt is used for a long time; on the other hand, good compressibility and recovery are still required after multiple water washes.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the silk quilt obtained by the application, the water washing can be realized through the glue fixation of the cross-linking agent, and the softness, the fluffiness and the heat retention property of the silk quilt can be kept after multiple water systems.
2. By improving the degumming auxiliary agent and the degumming process, the silk glue layer is selectively removed, so that the residual of a wax layer caused by too much silk glue is avoided, the hardness of the silk quilt is increased, the silk glue layer can be remained to the maximum extent, the silk fibroin is protected, and the waste is also avoided.
3. The sericin fixation method adopted by the application ensures that the sericin is not dissolved in water, and also keeps the air permeability, the heat retention property and the flexibility of the silk,
Detailed Description
Example 1
(1) Pretreatment of silkworm cocoon
The composition of the compound penetrant is as follows: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5%, a silk foaming agent ST-101 with the mass concentration of 1.0% and a silk foaming agent SW-102 with the mass concentration of 1.0% into purified water. The pretreatment process of the silkworm cocoon comprises the following steps: heating water to 50-80 ℃, immersing the silkworm cocoons in a penetrant under the condition that the bath ratio is 1: 10, pouring the silkworm cocoons into a vacuum infiltration barrel, putting the silkworm cocoons into a cotton mesh bag in order to prevent the dry cocoons from floating upwards, adding stones into the bottom of the mesh bag, enabling the silkworm cocoons to sink to the bottom of the infiltration barrel, starting a vacuum pump, wherein the vacuum degree is 60-70 kPa, and the retention time is as follows: 30 s/time; penetration times are as follows: 3 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons.
(2) Degumming of silk
Washing silkworm cocoon soaked by penetrant with clear water for 2 times, and treating silkworm cocoon with degumming solution, wherein the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5% into clear water, adding 3.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5 by using sodium bicarbonate at the bath ratio of 1: 20, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrating agent from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled. Washing the silkworm cocoons for 1-2 times by using clean water, obtaining fluffy and soft silk pieces by adopting a silk reeling process without passing through porcelain eyes and printing chiffon, and drying the obtained silk pieces by using infrared rays or hot air until no adhesion is generated between the silk pieces.
(3) Fixing glue for silk
And (3) carrying out sericin fixation treatment on the degummed silk slices by adopting a cross-linking agent. The cross-linking agent is a mixture of glutaraldehyde and polyamide formaldehyde, and the fixing process conditions are as follows: the bath ratio is 1:30, the mass concentration of glutaraldehyde is 0.5%, the mass concentration of polyamide formaldehyde is 0.1%, the temperature is 40-50 ℃, and the soaking time is 2 hours.
(4) Post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes to obtain a reusable liquid. Rinsing with clear water, bleaching and softening. Washing with water, drying, air drying (or oven drying), and drawing into silk floss quilt.
Example 2
In the cocoon pretreatment step of this example, the cocoon was immersed in the penetrant at normal temperature, and the operation method and raw materials of the other steps were the same as those of example 1.
Example 3
In the degumming step of silk in this example, the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.3% into clear water, and then adding 1% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 4
In the degumming step of silk in this example, the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5% into clear water, and then adding 3% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 5
In the degumming step of silk in this example, the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.7% into clear water, and then adding 5% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 6
In the degumming step of silk in this example, the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.8% into clear water, and then adding 6% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 7
In the degumming step of silk in this example, the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.9% into clear water, and then adding 7% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 8
In the degumming step of silk in this example, the degumming solution comprises the following components: adding 1.0 mass percent of silk softening agent Ultratex FSA into clear water, and then adding 8 mass percent of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 9
In the degumming step of silk in this example, the degumming solution comprises the following components: adding 1.1% of silk softening agent Ultratex FSA in mass concentration into clear water, and then adding 9% of methoxypropylamine silver nitrate protonated ionic liquid, wherein the operation methods and raw materials of other steps are the same as those in example 1.
Example 10
In the step of fixing the silk glue, the cross-linking agent comprises the following components: the glutaraldehyde mass concentration was 0.8%, the polyamide-formaldehyde mass concentration was 0.3%, and the operation methods and raw materials of the other steps were the same as those of example 1.
Example 11
In the step of fixing the silk glue, the cross-linking agent comprises the following components: the glutaraldehyde mass concentration was 1.0%, the polyamide formaldehyde mass concentration was 0.5%, and the operation methods and raw materials of the other steps were the same as those of example 1.
Example 12
In the step of fixing the silk glue, the cross-linking agent comprises the following components: the glutaraldehyde mass concentration was 1.2%, the polyamide formaldehyde mass concentration was 0.7%, and the operation methods and raw materials of the other steps were the same as those of example 1.
Example 13
In the step of fixing the silk glue, the cross-linking agent comprises the following components: the glutaraldehyde mass concentration was 1.5%, the polyamide formaldehyde mass concentration was 0.9%, and the operation methods and raw materials of the other steps were the same as those of example 1.
Example 14
In the step of fixing the silk glue, the cross-linking agent comprises the following components: the glutaraldehyde mass concentration was 1.7%, the polyamide formaldehyde mass concentration was 1.0%, and the operation methods and raw materials of the other steps were the same as those of example 1.
Example 15
(1) Pretreatment of silkworm cocoon
The composition of the compound penetrant is as follows: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.8%, a silk foaming agent ST-101 with the mass concentration of 1.5% and a silk foaming agent SW-102 with the mass concentration of 1.5% into purified water. The pretreatment process of the silkworm cocoon comprises the following steps: heating water to 50-80 ℃, immersing the silkworm cocoons in a penetrant under the condition that the bath ratio is 1: 10, pouring the silkworm cocoons into a vacuum infiltration barrel, putting the silkworm cocoons into a cotton mesh bag in order to prevent the dry cocoons from floating upwards, adding stones into the bottom of the mesh bag, enabling the silkworm cocoons to sink to the bottom of the infiltration barrel, starting a vacuum pump, wherein the vacuum degree is 60-70 kPa, and the retention time is as follows: 30 s/time; penetration times are as follows: 3 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons.
(2) Degumming of silk
Washing silkworm cocoon soaked by penetrant with clear water for 2 times, and treating silkworm cocoon with degumming solution, wherein the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.8% into clear water, adding 5.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5 by using sodium bicarbonate at the bath ratio of 1: 20, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrating agent from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled. Washing the silkworm cocoons for 1-2 times by using clean water, obtaining fluffy and soft silk pieces by adopting a silk reeling process without passing through porcelain eyes and printing chiffon, and drying the obtained silk pieces by using infrared rays or hot air until no adhesion is generated between the silk pieces.
(3) Fixing glue for silk
And (3) carrying out sericin fixation treatment on the degummed silk slices by adopting a cross-linking agent. The cross-linking agent is a mixture of glutaraldehyde and polyamide formaldehyde, and the fixing process conditions are as follows: the bath ratio is 1:30, the mass concentration of glutaraldehyde is 1.0%, the mass concentration of polyamide formaldehyde is 0.5%, the temperature is 40-50 ℃, and the soaking time is 2 hours.
(4) Post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes to obtain a reusable liquid. Rinsing with clear water, bleaching and softening. Washing with water, drying, air drying (or oven drying), and drawing into silk floss quilt.
Example 16
(1) Pretreatment of silkworm cocoon
The composition of the compound penetrant is as follows: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5%, a silk foaming agent ST-101 with the mass concentration of 2.0% and a silk foaming agent SW-102 with the mass concentration of 2.0% into purified water. The pretreatment process of the silkworm cocoon comprises the following steps: heating water to 50-80 ℃, immersing the silkworm cocoons in a penetrant under the condition that the bath ratio is 1: 10, pouring the silkworm cocoons into a vacuum infiltration barrel, putting the silkworm cocoons into a cotton mesh bag in order to prevent the dry cocoons from floating upwards, adding stones into the bottom of the mesh bag, enabling the silkworm cocoons to sink to the bottom of the infiltration barrel, starting a vacuum pump, wherein the vacuum degree is 60-70 kPa, and the retention time is as follows: 30 s/time; penetration times are as follows: 3 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons.
(2) Degumming of silk
Washing silkworm cocoon soaked by penetrant with clear water for 2 times, and treating silkworm cocoon with degumming solution, wherein the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 1.0% into clear water, adding 8.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5 by using sodium bicarbonate at the bath ratio of 1: 20, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrating agent from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled. Washing the silkworm cocoons for 1-2 times by using clean water, obtaining fluffy and soft silk pieces by adopting a silk reeling process without passing through porcelain eyes and printing chiffon, and drying the obtained silk pieces by using infrared rays or hot air until no adhesion is generated between the silk pieces.
(3) Fixing glue for silk
And (3) carrying out sericin fixation treatment on the degummed silk slices by adopting a cross-linking agent. The cross-linking agent is glutaraldehyde, and the fixing process conditions are as follows: the bath ratio is 1:30, the mass concentration of glutaraldehyde is 1.5%, the temperature is 40-50 ℃, and the soaking time is 2 hours.
(4) Post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes to obtain a reusable liquid. Rinsing with clear water, bleaching and softening. Washing with water, drying, air drying (or oven drying), and drawing into silk floss quilt.
Example 17
The crosslinking agent for the solid adhesive in this example was a polyamide formaldehyde concentration of 1.5% by mass, and the operation and raw materials in the other steps were the same as those in example 16.
The silk quilts of examples 1-17, which were obtained with the same weight and area, were tested for thickness, compressibility and recovery after multiple water washes, and the results are shown in table 1 below:
TABLE 1 Water-washable performance of silk obtained in examples of the present application
Figure BDA0002886604770000091
Figure BDA0002886604770000101
From the above table, it can be seen that the silk is washed with water for several times, and the thickness, compression ratio and recovery rate of the silk are reduced, but the reduction degree is obviously different by adopting different processes. Particularly for the glue-fixing agent, the thickness, the compression ratio and the recovery rate of the single glutaraldehyde or polyamide formaldehyde for oil extraction after twice water washing are obviously reduced, and the heat retention property and the comfort of the silk quilt are obviously reduced. The performance of the silk quilt is reduced after being washed by water for many times by adopting the mixture of glutaraldehyde or polyamide formaldehyde as a cross-linking agent. Meanwhile, the preparation process of the silk quilt and the content of each component have obvious influence on the performance, and the performance of the silk quilt obtained in example 15 is optimal.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.

Claims (5)

1. The washable silk quilt is characterized by comprising the following preparation processes:
(1) pretreatment of silkworm cocoon
Carrying out soaking pretreatment on the silkworm cocoons by using a compound penetrant, wherein the compound penetrant comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5-1.0%, a silk foaming agent ST-101 with the mass concentration of 1.0-2.0% and a silk foaming agent SW-102 with the mass concentration of 1.0-2.0% into purified water; the pretreatment process of the silkworm cocoon comprises the following steps: heating the water to 50-80 ℃, and immersing the silkworm cocoons in the penetrating agent at a bath ratio of 1: 10-20;
(2) degumming of silk
Washing the silkworm cocoons soaked by the penetrant with clear water for 1-2 times, and treating the silkworm cocoons with degumming liquid, wherein the degumming liquid comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.5-1.0% into clear water, adding 3.0-8.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5-8.0 by using sodium bicarbonate at the bath ratio of 1: 20-30, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrant from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled;
(3) fixing glue for silk
The degumming silk slice is processed by silk glue fixation by adopting a cross-linking agent, the cross-linking agent is a mixture of glutaraldehyde and polyamide formaldehyde, and the fixation process conditions are as follows: the bath ratio is 1: 30-50, the mass concentration of glutaraldehyde is 0.5-1.5%, the mass concentration of polyamide formaldehyde is 0.1-1.0%, the temperature is 40-50 ℃, and the soaking time is 1-2 h;
(4) post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes, rinsing with clear water, bleaching, softening, washing with water, spin-drying, airing (or drying), and drawing into the silk wadding quilt.
2. The silk quilt capable of being washed by water as claimed in claim 1, wherein the pretreatment of the silkworm cocoons adopts a vacuum infiltration mode, the silkworm cocoons are poured into a vacuum infiltration barrel, a vacuum pump is started, the vacuum degree is less than or equal to 70kPa, and the retention time is as follows: 30-60 s/time; penetration times are as follows: 3-5 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons.
3. The water-washable silk quilt according to claim 1, characterized in that in the degumming solution, the mass concentration of a silk softener Ultratex FSA is 0.6-0.8%, and the mass concentration of a 3-methoxypropylamine silver nitrate protonated ionic liquid is 4.0-6.0%.
4. The washable silk quilt as recited in claim 1, wherein the cross-linking agent is glutaraldehyde with a mass concentration of 0.8-1.2%, and the polyamide formaldehyde with a mass concentration of 0.4-0.8%.
5. The water-washable silk quilt according to claim 1, characterized in that the preparation process of the silk quilt is as follows:
(1) pretreatment of silkworm cocoon
The composition of the compound penetrant is as follows: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.8%, a silk soaking agent ST-101 with the mass concentration of 1.5% and a silk soaking agent SW-102 with the mass concentration of 1.5% into purified water, wherein the pretreatment process of the silkworm cocoons comprises the following steps: heating water to 50-80 ℃, immersing the silkworm cocoons in a penetrant at a bath ratio of 1: 10, pouring the silkworm cocoons into a vacuum infiltration barrel, putting the silkworm cocoons into a cotton mesh bag, adding stones into the bottom of the mesh bag to enable the silkworm cocoons to sink to the bottom of the infiltration barrel, starting a vacuum pump, ensuring the vacuum degree to be 60-70 kPa, and keeping the vacuum degree for: 30 s/time; penetration times are as follows: 3 times, ensuring that the penetrant uniformly permeates into the silkworm cocoons;
(2) degumming of silk
Washing silkworm cocoon soaked by penetrant with clear water for 2 times, and treating silkworm cocoon with degumming solution, wherein the degumming solution comprises the following components: adding a real silk softening agent Ultratex FSA with the mass concentration of 0.8% into clear water, adding 5.0% of 3-methoxypropylamine silver nitrate protonated ionic liquid, adjusting the pH value of the solution to 7.5 by using sodium bicarbonate at the bath ratio of 1: 20, keeping the temperature at 70-80 ℃ for 20-30 min, raising the temperature to 80-100 ℃ for 30-50 min, and separating a penetrating agent from silkworm cocoons by using a filtering mode, wherein the obtained liquid can be recycled; washing the silkworm cocoons for 1-2 times by using clean water, obtaining fluffy and soft silk pieces by adopting a silk reeling process without passing through porcelain eyes and printing chiffon, and drying the obtained silk pieces by using infrared rays or hot air until no adhesion is generated among the silk pieces;
(3) fixing glue for silk
The degumming silk slice is processed by silk glue fixation by adopting a cross-linking agent, the cross-linking agent is a mixture of glutaraldehyde and polyamide formaldehyde, and the fixation process conditions are as follows: the bath ratio is 1:30, the mass concentration of glutaraldehyde is 1.0%, the mass concentration of polyamide formaldehyde is 0.5%, the temperature is 40-50 ℃, and the soaking time is 2 h;
(4) post-treatment
And (3) dehydrating the silk subjected to glue fixation in a centrifugal machine for 1-2 minutes, rinsing with clear water, bleaching, softening, washing with water, spin-drying, airing (or drying), and drawing into the silk wadding quilt.
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JPH0995865A (en) * 1995-09-27 1997-04-08 Heian Yushi Kagaku Kogyo Kk Sericin-set cocoon and sericin-set yarn
CN1923090A (en) * 2006-09-11 2007-03-07 潘新平 Manufacturing method of washable mulberry silk quilt
CN202287407U (en) * 2011-08-25 2012-07-04 浙江神神丝绸家纺有限公司 Washable silk quilt
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CN106676642A (en) * 2016-12-12 2017-05-17 苏州大学 Silk degumming/scouring agent, application and treatment method for degumming waste liquid
CN109183402A (en) * 2018-08-28 2019-01-11 江苏鑫缘丝绸科技有限公司 A kind of expansion silk wadding quilt and preparation method thereof
CN110387586A (en) * 2019-06-17 2019-10-29 浙江蚕缘家纺有限公司 A kind of solidifying degumming of silk technique of silk
CN110592938A (en) * 2019-09-18 2019-12-20 界首市双鑫纺织有限公司 Antibacterial modified silk fiber and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0995865A (en) * 1995-09-27 1997-04-08 Heian Yushi Kagaku Kogyo Kk Sericin-set cocoon and sericin-set yarn
CN1923090A (en) * 2006-09-11 2007-03-07 潘新平 Manufacturing method of washable mulberry silk quilt
CN202287407U (en) * 2011-08-25 2012-07-04 浙江神神丝绸家纺有限公司 Washable silk quilt
CN102605438A (en) * 2012-04-05 2012-07-25 常德诺雅蚕丝制品有限公司 Manufacture method of washable mulberry silkworm long silk floss with high sericin content
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CN106676642A (en) * 2016-12-12 2017-05-17 苏州大学 Silk degumming/scouring agent, application and treatment method for degumming waste liquid
CN109183402A (en) * 2018-08-28 2019-01-11 江苏鑫缘丝绸科技有限公司 A kind of expansion silk wadding quilt and preparation method thereof
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