CN108625169B - All-silk yarn-dyed warp knitting preparation process - Google Patents

All-silk yarn-dyed warp knitting preparation process Download PDF

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CN108625169B
CN108625169B CN201810497252.8A CN201810497252A CN108625169B CN 108625169 B CN108625169 B CN 108625169B CN 201810497252 A CN201810497252 A CN 201810497252A CN 108625169 B CN108625169 B CN 108625169B
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silk
parts
agent
sericin
soaking
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CN108625169A (en
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陈张仁
王逍清
周小娟
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Hangzhou Fuqiang Silk Co ltd
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Hangzhou Fuqiang Silk Co ltd
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Abstract

The invention discloses a full real silk yarn-dyed warp knitting preparation process, which belongs to the technical field of real silk textile, and the technical scheme is characterized by comprising the following steps: (1) selecting yarn, (2) pretreating, (3) refining, (4) twisting, (5) dyeing, (6) weaving, (7) finishing, and (8) finishing, wherein oleic acid polyoxyethylene ester, lauryl alcohol polyoxyethylene ether, sodium silicate and water are adopted to soak silk during pretreatment, so that sericin is swelled, permeation of a refining agent is facilitated, the sericin is fully reacted with the sericin, the dissolving time of the sericin is shortened, and the technical effect of reducing damage of the refining agent to silk fibroin is achieved.

Description

All-silk yarn-dyed warp knitting preparation process
Technical Field
The invention relates to the technical field of real silk textile, in particular to a full real silk yarn-dyed warp knitting preparation process.
Background
The silk is silk, including mulberry silk, tussah silk, castor-oil plant silk, cassava silk, etc., belonging to protein fiber, and the fibroin contains 18 amino acids beneficial to human body. The silk fiber is the only natural filament fiber which is practically applied and is formed by silkworm-changed mucus solidification. The silk fiber is divided into a plurality of types according to different feeding habits of silkworms, wherein the silk fiber is formed by eating mulberry leaves, the tussah silk fiber is formed by eating tussah leaves, and other wild silk fibers are formed by eating cassava leaves, coriaria sinica and castor bean leaves; the mulberry silk fiber and the tussah silk fiber can retain the form of the filament fiber in the filament yarn formed by bundling, and other wild silk fibers can only be reformed into short fibers for textile processing; among filament yarns formed by bundling mulberry silk fibers and tussah silk fibers, the mulberry silk fiber filament yarn is most important and occupies most of natural filament yarns.
The main components of the silk are sericin and silk fibroin, wherein the sericin accounts for about 25-30% of the weight of the silk, the sericin is wrapped on the outer layer of the silk fibroin and plays a role in protecting the silk fibroin, and the silk reeled by silkworm cocoons has sericin and impurity residues, so that the dyeing effect of silk fabrics can be influenced, and the luster, the hand feeling and the texture of the silk fabrics can be influenced, and therefore the residual sericin and the impurity on the surface of the silk must be removed before dyeing; the principle of separating silk fibroin and sericin is that silk fibroin is insoluble in water, and sericin has water solubility; the aim of removing sericin can be achieved under certain conditions by adopting acid, alkali, soap, high temperature and high pressure and enzyme treatment.
Prior art can refer to patent application publication No. CN106757384A, which discloses a production method of an elastic puffed silk quilt, comprising cocoon selection, cocoon cooking, degumming, pupa removal, lantern ring, silk sleeve, and wire drawing, and further comprising the following steps: A. soaking the cocoons in purified water at 50-70 deg.C for 3-5min before boiling, placing the cocoons and purified water in a vacuum container, adding alkaline swelling agent with pH of 9-10, and steaming at 90-100 deg.C for 5-10 min. B. Soaking silk in purified water at 70-80 deg.C for 3-5min, soaking in purified water containing acidic swelling agent at 20-30 deg.C for 2-4 min, and oven drying.
The principle of alkali refining silk is that an alkali agent acts on peptide bonds of sericin to hydrolyze the sericin, the reaction is nonspecific, and the main acting amino acids are cysteine, serine, threonine and arginine; after degumming with an alkaline agent, the average titer of the silk is reduced by about 7dtex, the breaking strength, the elongation at break and the initial modulus are all reduced, and the softness, whiteness, glossiness and handfeel of silk fabrics are all deteriorated due to the obvious reduction of the titer of the silk.
Among other methods, the acid refining method has the advantages that the degumming rate is easy to control, partial degumming processing can be carried out, but the acid refining method cannot remove impurities such as grease on the silk, the requirement on processing equipment is high, and organic acid can be adsorbed by the silk fibroin fiber and is extremely difficult to remove, so that the utilization of the silk fiber is influenced; the soap refining method has the advantages that sericin on the silk can be dissociated, the sericin is prevented from being adhered to the silk again, emulsification and dispersion are achieved, the bulkiness, whiteness and glossiness of silk fabrics can be improved, and the soap consumption is large, the production cost is high, the degumming time is long, and the method is not suitable for uniform degumming; the high-temperature high-pressure method does not add chemical reagents, and sericin can be directly recovered from refining liquid for reuse, but the method needs high-temperature high-pressure equipment, so that the production cost is increased; the enzyme refining method has little pollution to the environment, the degumming has little damage to the limitation of the silk, but the conditions of the enzyme action are more complex, the culture cost of the enzyme-producing bacteria is large, and the production cost is high; various methods have advantages and disadvantages, so that the problem to be solved is how to remove sericin as much as possible in the silk refining process and reduce the damage to the silk cellulose during the degumming process as much as possible.
Disclosure of Invention
The invention aims to provide a full-real silk yarn-dyed weaving preparation process, which is characterized in that in the refining process, a soap-alkali refining method is adopted to carry out degumming treatment on silk, so that the damage of a pure alkali refining method to silk fibroin can be reduced, the degumming efficiency is improved, the soaking time is shortened, and the damage of a refining agent to the silk fibroin is reduced.
The technical purpose of the invention is realized by the following technical scheme:
a full-real silk yarn-dyed warp knitting preparation process comprises the following steps:
(1) selecting yarns: selecting complete white silkworm cocoons with plump shapes, and reeling silk on the selected silkworm cocoons;
(2) pretreatment: soaking silk in pretreatment solution at a bath ratio of 1:30 at 60-70 deg.C for 30-40 min;
(3) refining: then placing the silk into a refining agent, keeping the pH value at 9-10.5 at a degumming bath ratio of 1:60, soaking at 96-98 ℃ for 20-25min, then washing the silk with deionized water for 3-5min, then soaking the silk into the refining agent at a degumming bath ratio of 1:40, keeping the pH value at 9-10.5, soaking at 96-98 ℃ for 10-15min, washing with deionized water, and drying at 35-40 ℃ for 60-90min to obtain degummed silk;
(4) twisting: winding, combining and twisting the degummed silk to obtain silk threads;
(5) dyeing: immersing the silk thread into dye for dyeing for 45min, then fixing the color for 30min through soda ash, and then fully curing the pigment on the silk thread through water washing;
(6) weaving: warping and weaving the silk threads to obtain a full-real-silk fabric;
(7) and (3) after finishing: immersing the full-real-silk fabric into an antibacterial agent;
(8) and (3) finished product: drying at 35-40 deg.C for 60-90min to obtain the final product.
By adopting the scheme, before silk is refined, the silk is pretreated, and sericin absorbs moisture and swells at 60-70 ℃, so that the refining agent can permeate into the silk to fully react with the sericin, and the dissolving time of the sericin is shortened; the silk degumming agent is beneficial to dissolving sericin at the temperature of 96-98 ℃ during refining, silk fibroin can be damaged due to overhigh temperature, the temperature is too low, the dissolving effect of the sericin is poor, most of sericin on silk can be removed by first soaking, hydrolysis products attached to the surface of the silk can be removed by removing the silk with deionized water for washing, the residual sericin can be fully removed by the refining agent during second soaking, the soaking time of the silk in the refining agent is shortened, the damage of the refining agent to the silk fibroin can be reduced, and the degumming effect is better; after the silk is refined and degummed, the mass of the silk is reduced by about 25%, the fiber is thinned, the gaps among the silk are increased, and the fabric is thinned and softened, so that the single silk needs to be combined and twisted to obtain silk threads; then the silk thread is immersed in dye for dyeing, the dyed silk thread is woven into a yarn-dyed process, the coils formed by warp knitting are arranged along the vertical direction or the warp direction and are formed by mutually sleeving adjacent yarns, and the yarn-dyed silk fabric has the advantages of good longitudinal dimension stability, stiff and smooth fabric, small detachability, no curling, good air permeability and the like; since the silk is protein fiber and is easily polluted by bacteria to corrode and smell in the storage process, the antibacterial agent is added into the silk for antibacterial treatment, and then the full-silk fabric can be obtained through low-temperature drying.
Preferably, the pretreating agent in the step (2) comprises, by weight, 3-5 parts of polyoxyethylene oleate, 5-7 parts of polyoxyethylene lauryl ether, 10-15 parts of sodium silicate and 30-40 parts of water.
By adopting the scheme, the polyoxyethylene oleate is a nonionic surfactant, has the characteristics of low foam and good biodegradability, and is used for textile softeners and lubricants; the lauryl alcohol polyoxyethylene ether has excellent functions of washing, emulsifying, dispersing, wetting, solubilizing and the like, has strong foaming power, is easy to rinse, has excellent detergency, is one of the varieties with the lowest irritation to skin in the surfactant, can be compounded with the oleic acid polyoxyethylene ester surfactant to improve the performance of the product, and can be used as an emulsifier, a softener, a wetting agent, a foaming agent and the like; the sodium silicate can increase the alkalinity of the pretreating agent, so that the silk is in a weakly alkaline condition, and the swelling of sericin is facilitated; impurities such as grease in the silk can be removed through the pretreating agent, the binding force of sericin and fibroin is weakened, the soaking time of the silk in the refining agent can be shortened, and the damage of the refining agent to the fibroin is reduced.
Preferably, the refining agent in the step (3) comprises 30-40 parts by weight of sodium oleate, 10-20 parts by weight of lauric acid monoglyceride, 2-4 parts by weight of sodium silicate, 6-8 parts by weight of sodium carbonate, 2-3 parts by weight of sodium tripolyphosphate, 1-3 parts by weight of a fibroin protective agent, 2-3 parts by weight of sodium hydrosulfite and 70-90 parts by weight of water.
By adopting the scheme, the sodium oleate is a compound consisting of a hydrophobic group and a hydrophilic group, has excellent emulsifying power, penetrability and detergency, can generate hydrolysis in water to generate free alkali and fatty acid, the free alkali can promote the hydrolysis of sericin, the solubility of the sericin is improved, and the purpose of degumming is achieved; the lauric monoglyceride is synthesized by directly esterifying lauric acid and glycerol, is not only an excellent emulsifier, but also a safe, efficient and broad-spectrum antibacterial agent, and still has a good antibacterial effect under a neutral or slightly alkaline condition; the sodium silicate can increase the alkalinity of the refining agent, and simultaneously, silicic acid generated by hydrolysis of the sodium silicate has the capacity of protecting colloid, so that the fallen sericin, hydrolysate thereof and other impurities are prevented from being adhered to the fabric again, copper ions and iron ions can be adsorbed to prevent rust spots from being generated, and the whiteness of the fabric is improved; the sodium carbonate can supplement alkalinity in the refining agent and has the effect of softening water quality; the sodium tripolyphosphate is used as a washing product auxiliary agent, is used as a sodium oleate synergist, prevents grease of the sodium oleate from separating out and frosting, has strong emulsification effect on lubricating oil and fat, can be used for adjusting the pH value of a buffer refining agent, and can be used as a chelating agent to improve the dispersibility of sodium silicate; the fibroin protective agent can reduce the damage of alkaline substances in the refining agent to the fibroin and is beneficial to maintaining the mechanical property of the fibroin; sodium hyposulfite is used as deoxidant and bleaching agent, can prevent local oxidation of silk fibre from affecting fibre strength, and can be used for bleaching colouring dye and natural pigment on the fabric by means of reduction decomposition in alkaline solution.
Preferably, the dye in step (5) includes an acid dye and a reactive dye.
By adopting the scheme, the acid dye is also called as anionic dye, contains acid groups in dye molecules, can be combined with amino groups in protein fiber molecules by ionic bonds, and has the best dyeing effect on silk; the reactive dye has a chemical structure similar to that of an acid dye, has good dyeing performance, bright color, good color fastness and can be chemically combined with fibers, and the color fastness of the dye can be improved by dyeing silk yarns by adopting the acid dye and the reactive dye.
Preferably, the warping speed in the step (6) is 250-350m/min, the warping tension is 5-7cN, the temperature is 16-20 ℃, and the relative humidity is 65-70%.
By adopting the scheme, the warping is a technological process of winding a certain number of warps on a warp beam or a loom beam in parallel according to specified length and width, the warped warps are used for sizing and drawing, the warping requires that the tensions of all the warps are equal, the warps are uniformly distributed on the warp beam or the loom beam, the warping speed is 250-350m/min, the warping tension is 5-7cN, the temperature is 16-20 ℃, the relative humidity is 65-70%, and the warp-sizing agent is suitable for warping silk and can reduce the damage to silk yarns.
Preferably, the antibacterial agent in the step (7) comprises tannin, chitin and nano titanium dioxide; the mass ratio of the tannin to the chitin to the nano titanium dioxide is 3:1:1, the chitin and the nano titanium dioxide are added into the tannin according to the proportion, and the mixture is stirred for 20-30min at the speed of 100-140 r/min.
By adopting the scheme, the silk has stronger adsorption performance to tannin, so that the chitin, the nano titanium dioxide and the tannin are mixed, and the attachment of an antibacterial agent on the silk is facilitated; tannin can be used for weight increasing treatment of silk, can increase drapability of silk fabrics, endow the silk fabrics with soft and fluffy hand feeling, and improve wrinkle resistance, ultraviolet resistance, washing resistance and strength of the silk fabrics, because the tannin is plant weight gain, the tannin is milder than mineral weight gain, in addition, the tannin has obvious inhibiting effect on various bacteria, fungi and microorganisms, the growth and development of human cells can not be influenced under the same inhibiting concentration, the tannin has unique oxidation resistance, the tannin can effectively resist biological oxidation, and the tannin also has the function of scavenging active oxygen; chitin is a natural antibacterial agent, is easy to degrade, safe and nontoxic, but has limited antibacterial effect, so that the chitin needs to be used together with other antibacterial agents; the nanometer titanium dioxide is an inorganic antibacterial agent, has the performances of antibiosis, self-cleaning and ageing resistance, can prevent infection, deodorize and kill harmful bacteria, can absorb ultraviolet rays, can reflect and scatter the ultraviolet rays and can reduce the ageing of silk fabrics.
Preferably, the particle size of the nano titanium dioxide is 20-30 nm.
By adopting the scheme, the particle size of the nano titanium dioxide is 20-30nm, which is beneficial to the full mixing of the nano titanium dioxide and tannin.
Preferably, the fineness of the silk is 24/26D.
By adopting the scheme, the fineness is a unit representing fiber thickness, the larger the numerical value is, the thicker the silk is, and the fineness of the silk is 24/26D, so that the silk can maintain certain strength and good elasticity.
In conclusion, the invention has the following beneficial effects:
1. before silk is refined, the silk is pretreated, so that impurities such as grease and the like in the silk can be removed, the binding force between sericin and fibroin is weakened, the soaking time of the silk in a refining agent can be shortened, the sericin absorbs moisture and swells, the refining agent is favorably permeated and fully reacts with the sericin, the dissolving time of the sericin is shortened, and the damage of the refining agent to the fibroin is reduced; most sericin on the silk can be removed by primary soaking in refining, and hydrolysis products attached to the surface of the silk can be removed by removing the silk with deionized water for washing, so that the residual sericin can be sufficiently removed by the refining agent in secondary soaking, the soaking time of the silk in the refining agent is shortened, the damage of the refining agent to the fibroin can be reduced, and the degumming effect is better;
2. the polyoxyethylene oleate has the characteristics of low foam and good biodegradability, and is used for textile softeners and lubricants; the lauryl alcohol polyoxyethylene ether has excellent functions of washing, emulsifying, dispersing, wetting, solubilizing and the like, has strong foaming power, is easy to rinse, has excellent detergency, and is compounded with the oleic acid polyoxyethylene ester surfactant to improve the performance of the product; the sodium silicate can increase the alkalinity of the pretreating agent, so that the silk is in a weakly alkaline condition, and the swelling of sericin is facilitated;
3. the sodium oleate has excellent emulsifying power, penetrability and detergency, can generate hydrolysis in water to generate free alkali and fatty acid, the free alkali can promote the hydrolysis of sericin, the solubility of the sericin is improved, and the purpose of degumming is achieved; the lauric acid monoglyceride is an excellent emulsifier, is a safe, efficient and broad-spectrum antibacterial agent, and still has a good antibacterial effect under a neutral or slightly alkaline condition; the sodium silicate can increase the alkalinity of the refining agent, and simultaneously, silicic acid generated by hydrolysis of the sodium silicate has the capacity of protecting colloid, so that the fallen sericin, hydrolysate thereof and other impurities are prevented from being adhered to the fabric again, copper ions and iron ions can be adsorbed to prevent rust spots from being generated, and the whiteness of the fabric is improved; the sodium carbonate can supplement alkalinity in the refining agent and has the effect of softening water quality; the sodium tripolyphosphate is used for a sodium oleate synergist and preventing grease of the sodium oleate from separating out and frosting, has a strong emulsifying effect on lubricating oil and fat, can be used for adjusting the pH value of the buffer refining agent, and can be used as a chelating agent to improve the dispersibility of the sodium silicate; the fibroin protective agent can reduce the damage of alkaline substances in the refining agent to the fibroin and is beneficial to maintaining the mechanical property of the fibroin; sodium hydrosulfite is used as deoxidizer and bleaching agent, can prevent local oxidation of silk fiber from affecting fiber strength, and can play a role in bleaching with coloring dye and natural pigment on reduction decomposition fabric in alkaline solution;
4. the silk has stronger adsorption performance to tannin, so that the chitin, the nano titanium dioxide and the tannin are mixed, and the attachment of an antibacterial agent on the silk is facilitated; tannin can be used for weight increasing treatment of silk, can increase drapability of silk fabrics, endows the silk fabrics with soft and fluffy hand feeling, improves wrinkle resistance, ultraviolet resistance, washing resistance and strength of the silk fabrics, has obvious inhibition effect on various bacteria, fungi and microorganisms, has unique oxidation resistance, can effectively resist biological oxidation, and has the function of scavenging active oxygen; chitin is a natural antibacterial agent, is easy to degrade, safe and nontoxic; the nanometer titanium dioxide is an inorganic antibacterial agent, has the performances of antibiosis, self-cleaning and ageing resistance, can prevent infection, deodorize and kill harmful bacteria, can absorb ultraviolet rays, can reflect and scatter the ultraviolet rays and can reduce the ageing of silk fabrics.
Detailed Description
The present invention will be described in further detail below.
Examples 1 to 3
Example 1: the full-real silk yarn-dyed warp knitting is prepared by adopting the following process:
(1) selecting yarns: selecting complete white silkworm cocoons with full shapes, and then reeling the selected silkworm cocoons, wherein the titer of silk is 24/26D;
(2) pretreatment: soaking silk in pretreatment solution at a bath ratio of 1:30 at 65 deg.C for 35 min; the pretreatment agent comprises 4kg of oleic acid polyoxyethylene ester, 6kg of lauryl alcohol polyoxyethylene ether, 13kg of sodium silicate and 35kg of water;
(3) refining: then placing the silk into a refining agent, keeping the pH value at 9-10.5 at a degumming bath ratio of 1:60, soaking for 23min at the temperature of 97 ℃, then washing the silk with deionized water for 4min, then soaking the silk into the refining agent at a degumming bath ratio of 1:40, keeping the pH value at 9-10.5, soaking for 13min at the temperature of 97 ℃, washing with deionized water, and drying for 75min at the temperature of 38 ℃ to obtain degummed silk; the refining agent comprises 35kg of sodium oleate, 15kg of lauric acid monoglyceride, 3kg of sodium silicate, 7kg of sodium carbonate, 2.5kg of sodium tripolyphosphate, 2kg of fibroin protective agent, 2.5kg of sodium hydrosulfite and 80kg of water;
(4) twisting: winding, combining and twisting the degummed silk to obtain silk threads;
(5) dyeing: immersing the silk thread into dye for dyeing for 45min, then fixing the color for 30min through soda ash, and then fully curing the pigment on the silk thread through water washing;
(6) weaving: warping and weaving the silk threads to obtain a full-real-silk fabric; wherein the warping speed is 300m/min, the warping tension is 6cN, the temperature is 18 ℃, and the relative humidity is 68%;
(7) and (3) after finishing: immersing the full-real-silk fabric into an antibacterial agent; the antibacterial agent comprises tannin, chitin, and nanometer titanium dioxide, and is prepared by adding 10kg chitin and 10kg nanometer titanium dioxide with particle size of 20-30nm into 30kg tannin, and stirring at 120r/min for 25 min;
(8) and (3) finished product: drying at 38 deg.C for 75min to obtain the final product.
Example 2: the full-real silk yarn-dyed warp knitting is prepared by adopting the following process:
(1) selecting yarns: selecting complete white silkworm cocoons with full shapes, and then reeling the selected silkworm cocoons, wherein the titer of silk is 24/26D;
(2) pretreatment: soaking silk in pretreatment solution at a bath ratio of 1:30 at 60 deg.C for 40 min; the pretreatment agent comprises 3kg of oleic acid polyoxyethylene ester, 5kg of lauryl alcohol polyoxyethylene ether, 10kg of sodium silicate and 30kg of water;
(3) refining: then placing the silk into a refining agent, keeping the pH value at 9-10.5 at a degumming bath ratio of 1:60, soaking for 25min at 96 ℃, then washing the silk with deionized water for 3min, then soaking the silk into the refining agent at a degumming bath ratio of 1:40, keeping the pH value at 9-10.5, soaking for 15min at 96 ℃, then washing with deionized water, and drying for 90min at 35 ℃ to obtain degummed silk; the refining agent comprises 30kg of sodium oleate, 10kg of lauric acid monoglyceride, 2kg of sodium silicate, 6kg of sodium carbonate, 2kg of sodium tripolyphosphate, 1kg of fibroin protective agent, 2kg of sodium hydrosulfite and 70kg of water;
(4) twisting: winding, combining and twisting the degummed silk to obtain silk threads;
(5) dyeing: immersing the silk thread into dye for dyeing for 45min, then fixing the color for 30min through soda ash, and then fully curing the pigment on the silk thread through water washing;
(6) weaving: warping and weaving the silk threads to obtain a full-real-silk fabric; wherein the warping speed is 250m/min, the warping tension is 5cN, the temperature is 16 ℃, and the relative humidity is 65%;
(7) and (3) after finishing: immersing the full-real-silk fabric into an antibacterial agent; the antibacterial agent comprises tannin, chitin, and nanometer titanium dioxide, and is prepared by adding 10kg chitin and 10kg nanometer titanium dioxide with particle size of 20-30nm into 30kg tannin, and stirring at 100r/min for 30 min;
(8) and (3) finished product: drying at 35 deg.C for 90min to obtain the final product.
Example 3: the full-real silk yarn-dyed warp knitting is prepared by adopting the following process:
(1) selecting yarns: selecting complete white silkworm cocoons with full shapes, and then reeling the selected silkworm cocoons, wherein the titer of silk is 24/26D;
(2) pretreatment: soaking silk in pretreatment solution at a bath ratio of 1:30 at 70 deg.C for 30 min; the pretreatment agent comprises 5kg of oleic acid polyoxyethylene ester, 7kg of lauryl alcohol polyoxyethylene ether, 15kg of sodium silicate and 40kg of water;
(3) refining: then placing the silk into a refining agent, keeping the pH value at 9-10.5 at a degumming bath ratio of 1:60, soaking for 20min at the temperature of 98 ℃, then washing the silk with deionized water for 5min, then soaking the silk into the refining agent at a degumming bath ratio of 1:40, keeping the pH value at 9-10.5, soaking for 10min at the temperature of 98 ℃, then washing with deionized water, and drying for 60min at the temperature of 40 ℃ to obtain degummed silk; the refining agent comprises 40kg of sodium oleate, 20kg of lauric acid monoglyceride, 4kg of sodium silicate, 8kg of sodium carbonate, 3kg of sodium tripolyphosphate, 3kg of fibroin protective agent, 3kg of sodium hydrosulfite and 90kg of water;
(4) twisting: winding, combining and twisting the degummed silk to obtain silk threads;
(5) dyeing: immersing the silk thread into dye for dyeing for 45min, then fixing the color for 30min through soda ash, and then fully curing the pigment on the silk thread through water washing;
(6) weaving: warping and weaving the silk threads to obtain a full-real-silk fabric; wherein the warping speed is 350m/min, the warping tension is 7cN, the temperature is 20 ℃, and the relative humidity is 70%;
(7) and (3) after finishing: immersing the full-real-silk fabric into an antibacterial agent; the antibacterial agent comprises tannin, chitin and nanometer titanium dioxide, 10kg chitin and 10kg nanometer titanium dioxide with particle size of 20-30nm are added into 30kg tannin, and stirred at the speed of 140r/min for 20 min;
(8) and (3) finished product: drying at 40 deg.C for 60min to obtain the final product.
Second, comparative examples 1 to 3
Comparative example 1: adopt application publication No. CN 106757384A's patent application file, it discloses a production method of elasticity popped silk quilt, including selecting the cocoon, boiling the cocoon, come unstuck, remove pupa, lantern ring, silk braid, wire drawing, still includes following step: A. soaking the cocoons in purified water at 50-70 deg.C for 3-5min before boiling, placing the cocoons and purified water in a vacuum container, adding alkaline swelling agent with pH of 9-10, and steaming at 90-100 deg.C for 5-10 min. B. Soaking silk in purified water at 70-80 deg.C for 3-5min, soaking in purified water containing acidic swelling agent at 20-30 deg.C for 2-4 min, and oven drying.
Comparative example 2: adopting patent application publication No. CN102660781A, it discloses a mulberry silk cone dyeing method, which comprises the following steps: preparing mulberry silk skein raw materials, pretreating the mulberry silk skein, soaking and degumming the mulberry silk skein, refining and degumming mulberry silk, drying, spooling and dyeing; during soaking degumming, the degumming auxiliary agent adopted consists of 0.3 to 0.5 percent of sodium carbonate, 0.5 to 1.8 percent of sodium hexametaphosphate, 0.4 to 0.5 percent of sodium oleate and 30 percent of proteolytic enzyme, wherein the percentages are weight percentages relative to the soaking solution; the following degumming auxiliary agents are adopted during refining degumming: 0.2 to 0.6 percent of alkaline endoprotease, 0.8 percent of soda ash and 0.8 percent of non-ionic penetrant, wherein the percentages are weight percentages relative to the refining liquid; after refining degumming, the degumming rate of the silk thread is 23-25%.
Comparative example 3: the invention discloses a silk making process which is implemented by the following process steps of silk drawing, soaking, cleaning, softening and drying, and specifically comprises the steps of spraying silk-debonding liquid on silkworm cocoons while spinning, preparing sheet-shaped silk with degreased sericin still adhered to the silk by a silk drawing machine, soaking the sheet-shaped silk with the degreased sericin still adhered to the silk by cleaning liquid, cleaning and soaking by clear water to obtain the degreased silk with sericin separated from the adhered silk, soaking by softening liquid, and finally dehydrating and drying the softened silk.
Thirdly, the performance of the silk fabrics prepared in examples 1 to 3 and comparative examples 1 to 3 was tested.
1. Raw silk glue degumming degree test
Qualitatively judging the degumming degree of different degumming methods in examples 1-3 and comparative examples 1-3 by using picric acid carmine, dissolving 1g of carmine in 10mL of 25% ammonia water, adding 20mL of deionized water, stirring, mixing and heating; after cooling, adding 45mL of saturated picric acid solution, adding water to 100mL, adjusting the pH value to 8-9 by using hydrochloric acid solution to form a picric acid carmine color developing reagent, and using the reagent to check whether degumming is complete. The principle is as follows: under the alkalescent condition, the silk fibroin is dyed yellow by picric acid, and the action of the silk fibroin and carmine is insensitive and insecure and is immediately removed after being washed by water. When the sericin is not removed completely, the carmine dyes the sericin into red, the yellow color of picric acid is covered, and after degumming, if the sericin is removed completely, a sample is tested by a color reagent and then dyed into yellow.
Percent degumming ratio (%) - (W)0-W1)/W0100％
In the formula: w0Dry weight before degumming of raw silk; w1Dry weight after degumming of raw silk.
TABLE 1 comparative table of degumming rates of raw silk in examples 1 to 3 and comparative examples 1 to 3
Test items Example 1 Example 2 EXAMPLE 3 Comparative example 1 Comparative example 2 Comparative example 3
Degumming Rate (%) 25.13 25.12 25.21 25.17 24.00 24.75
The data show that the degumming rate of the sericin of the raw silk is similar to that of the sericin of the traditional method, and the sericin has better degumming effect by the method.
2. Mechanical property detection
The silk fabrics prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for their tensile properties in the machine direction (parallel to the arrangement direction of the silk fibers) and in the transverse direction (perpendicular to the arrangement direction of the silk fibers) at room temperature and 50% relative humidity using a universal material testing machine; the distance between the clamps is 20 mm; the tensile rates were 2mm/min (transverse direction) and 0.2mm/min (transverse direction), respectively, and the tensile strength and breaking strength of all the specimens were averaged over ten test results.
Table 2 table for testing properties of silk fabrics of examples 1 to 3 and comparative examples 1 to 3
Detecting items Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3
Tensile strength, MPa 31.13 31.27 31.22 20.02 22.31 19.87
Elongation at break, based on 1.8 1.9 1.8 1.3 1.4 1.1
From the data, the tensile strength and the elongation at break of the silk fabric prepared by the method are obviously higher than those of the silk fabric prepared by the traditional method, which shows that the silk fabric prepared by the method has less damage to the silk cellulose during the process of refining and degumming the silk.
In conclusion, the silk prepared by the method has good degumming effect, less damage to silk cellulose fibers in the degumming process, and better mechanical property of silk fabrics; due to the addition of the post-finishing process, the added tannin can play a role in weight increment of the silk, increase the drapability of the silk and improve the anti-wrinkle ability of the silk; in addition, tannin, chitin and nano titanium dioxide have antibacterial effect, and can reduce the damage of microorganisms to silk fabrics.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.

Claims (7)

1. A full-real silk yarn-dyed warp knitting preparation process is characterized in that: the method comprises the following steps:
(1) selecting yarns: selecting complete white silkworm cocoons with plump shapes, and reeling silk on the selected silkworm cocoons;
(2) pretreatment: soaking silk in pretreatment solution at a bath ratio of 1:30 at 60-70 deg.C for 30-40 min;
(3) refining: then placing the silk into a refining agent, keeping the pH value at 9-10.5 at a degumming bath ratio of 1:60, soaking at 96-98 ℃ for 20-25min, then washing the silk with deionized water for 3-5min, then soaking the silk into the refining agent again, keeping the pH value at 1:40 at a degumming bath ratio of 9-10.5, soaking at 96-98 ℃ for 10-15min, washing with deionized water, and drying at 35-40 ℃ for 60-90min to obtain degummed silk;
(4) twisting: winding, combining and twisting the degummed silk to obtain silk threads;
(5) dyeing: immersing the silk thread into dye for dyeing for 45min, fixing the color for 30min by soda ash, and washing to obtain the pigment
Fully solidifying on the silk thread;
(6) weaving: warping and weaving the silk threads to obtain a full-real-silk fabric;
(7) and (3) after finishing: immersing the full-real-silk fabric into an antibacterial agent;
(8) and (3) finished product: drying at 35-40 deg.C for 60-90min to obtain the final product;
the pretreating agent in the step (2) comprises, by weight, 3-5 parts of oleic acid polyoxyethylene ester, 5-7 parts of lauryl alcohol polyoxyethylene ether, 10-15 parts of sodium silicate and 30-40 parts of water.
2. The process according to claim 1, wherein the process comprises the steps of: the refining agent in the step (3) comprises, by weight, 30-40 parts of sodium oleate, 10-20 parts of lauric acid monoglyceride, 2-4 parts of sodium silicate, 6-8 parts of sodium carbonate, 2-3 parts of sodium tripolyphosphate, 1-3 parts of a fibroin protective agent, 2-3 parts of sodium hydrosulfite and 70-90 parts of water.
3. The process according to claim 1, wherein the process comprises the steps of: the dye in the step (5) comprises an acid dye and a reactive dye.
4. The process according to claim 1, wherein the process comprises the steps of: the warping speed in the step (6) is 250-350m/min, the warping tension is 5-7cN, the temperature is 16-20 ℃, and the relative humidity is 65-70%.
5. The process according to claim 1, wherein the process comprises the steps of: the antibacterial agent in the step (7) comprises tannin, chitin and nano titanium dioxide; the mass ratio of the tannin to the chitin to the nano titanium dioxide is 3:1:1, the chitin and the nano titanium dioxide are added into the tannin according to the proportion, and the mixture is stirred for 20-30min at the speed of 100-140 r/min.
6. The process according to claim 5, wherein the yarn-dyed warp knitting process comprises the following steps: the particle size of the nano titanium dioxide is 20-30 nm.
7. The process according to claim 1, wherein the process comprises the steps of: the titer of the silk is 24/26D.
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