CN101532249B - Method for weight-increasing and antimicrobial treatment of silk fiber - Google Patents
Method for weight-increasing and antimicrobial treatment of silk fiber Download PDFInfo
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- CN101532249B CN101532249B CN2009100976959A CN200910097695A CN101532249B CN 101532249 B CN101532249 B CN 101532249B CN 2009100976959 A CN2009100976959 A CN 2009100976959A CN 200910097695 A CN200910097695 A CN 200910097695A CN 101532249 B CN101532249 B CN 101532249B
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Abstract
The invention discloses a method for weight-increasing and antimicrobial treatment of silk fiber, comprising: the preparing of silk fiber, degumming, washing, weight increasing treatment, soaping, dyeing, antibacterial treatment and after-finishing, wherein the weight-increasing treatment is performed at high temperature and pressure, the high temperature is 85 to 90 DEG C, in the weight increasing treatment, a grafting solution is firstly prepared and contains methacrylate ester derivatives as grafting monomer, a initiator, a non-ion or anionic surfactant and degumming waste water. In the invention, the drained degumming waste water can be recycled, thus saving the resource, reducing the pollution, improving the efficiency, and according with the requirement of circular, economical and clean production. In the invention, the weight increasing treatment for the silk fiber is performed, at the same time, the antimicrobial treatment is also completed, thus the treated silk fiber has theideal weight-increasing effect and a certain of antimicrobial performance.
Description
Technical field
The present invention relates to the weightening finish modification arrangement of cocoon fiber, relate in particular to the method for a kind of cocoon fiber weightening finish and antibacterial treatment.
Background technology
The raw material of silk broadcloth is a silk, silk fiber mainly is made up of fibroin and two kinds of protein of silk gum, the dyeing processing of cocoon fiber all is to adopt the processing mode of removing silk gum earlier, but behind the concise silk gum of sloughing the cocoon fiber surface, the weight saving of silk fiber, fiber attenuates, make real silk fabric exist defectives such as wear-resisting wiping is poor, crease recovery is poor, wash and wear difference, and cocoon fiber is carried out grafting weight gaining when handling, can also suitably improve its antibiotic property, wrinkle resistance, stiffness and solid sense.
The processing method of weightening finish cocoon fiber mainly contains following two classes at present: a class is to carry out chemical graft on fibroin fiber, to reach the weight that increases fiber, improves the purpose of silk fiber wearability.Method commonly used is to introduce the polyvinyl copolymer with vinyl monomer on fiber; Another kind of method is the method for adhering sericin, by the polar group on sealing or the crosslinked silk gum fiber, increases the purpose of cocoon fiber weight to reach adhering sericin, and the main chemical reagent that uses has: the derivative of (1) aldehyde or aldehyde; (2) heavy metal salt; (3) tannin (tannic acid) class etc.
If cocoon fiber is removed the direct discharging of degumming waste water that silk gum produced through refining and not only environment is caused very big pollution, but also waste silk gum resource wherein, but when adopting chemical reagent in the above-mentioned adhering sericin scheme to come adhering sericin usually, generally need chemical agent concentration just can reach more satisfactory effect than higher, and the chemical reagent of high concentration has increased the difficulty of follow-up sewage disposal, therefore come the method for adhering sericin to have very big deficiency with chemical reagent, first kind processing method is still mainly adopted in cocoon fiber weightening finish at present, but aspect not only wanting to reach real silk weightening finish purpose but also wanting to recycle degumming waste water, also there is not effective solution at present, and real silk weight increasing method commonly used at present only is devoted to weightening finish research, make that the anti-microbial property of the cocoon fiber after increasing weight is generally relatively poor, limited the purposes of real silk fabric.
Summary of the invention
Technical problem to be solved by this invention provides a kind of the realization can effectively reduce environmental pollution when cocoon fiber increases weight, and can suitably improve the cocoon fiber weightening finish of cocoon fiber antibiotic property, wrinkle resistance, stiffening sense and the method for antibacterial treatment, for this reason, the present invention is by the following technical solutions: it comprise cocoon fiber preparation, the processing of coming unstuck, wash, increase weight, soap, dyeing, antibacterial treatment and back arrangement step; Described weightening finish is handled and is carried out under high-temperature and high-pressure conditions, and described hot conditions is 85～90 ℃; Described weightening finish is handled needs preparation grafting liquid earlier, and described grafting liquid contains as the derivative of the methyl acrylic ester of grafted monomers, initator, nonionic or anion surfactant and degumming waste water; The addition of grafted monomers is by 20～66% of grafting weight gaining cocoon fiber weight, nonionic or anionic surfactant concentration are 0.8～2.0g/l, the pH value of grafting liquid is 3～4, and cocoon fiber is handled through carry out grafting weight gaining behind the grafting weight gaining in bath raio is 1: 15 grafting liquid.
The method of cocoon fiber weightening finish of the present invention and antibacterial treatment compared with prior art, remove can improve the pure silk products fugitive color effectively, easily contract, easy shortcoming such as wrinkle, and can obviously improve outside the flat deflection of real silk fabric, solid sense, hygroscopicity, the COLOR FASTNESS, also have following characteristics:
1. technical solutions according to the invention are recycled the former degumming waste water of wanting blowdown to go out, utilizing the hot conditions of full immersed type High Temperature High Pressure jet overflow dyeing machine (QR202A series) to make sericine in the degumming waste water be grafted to cocoon fiber again gets on, economize on resources, reduce and pollute, increase the benefit, meet recycling economy, the requirement of cleaner production.Owing to adopt technical scheme of the present invention, produce 1 ton of cocoon fiber, only need 0.8 ton of WHITE STEAM FILATURE YARNS, traditional handicraft then needs 1.33 tons of WHITE STEAM FILATURE YARNS, and the effect that visible present technique is saved the WHITE STEAM FILATURE YARNS resource is very significant; The condition of high voltage of full immersed type High Temperature High Pressure jet overflow dyeing machine can improve the conjugation of dyestuff and cocoon fiber, improves the defective of the cocoon fiber fugitive color in back arrangement step behind the weighting dyeing.
2. owing to adopt technical scheme of the present invention, full immersed type High Temperature High Pressure jet overflow dyeing machine handles, soaps for the preparation of cocoon fiber, the modification of coming unstuck, wash, increase weight and staining procedure provides an airtight environment, therefore largely block entering of external dust and bacterium, made pure silk products have the effect of certain inhibition golden staphylococci.
3. owing to adopt technical scheme of the present invention, also carried out antibacterial treatment when weightening finish is handled to cocoon fiber, made that the cocoon fiber after handling also has certain antibiotic (Escherichia coli and golden staphylococci) performance when reaching desirable gaining effect.
4. owing to adopt technical scheme of the present invention, weightening finish and staining procedure carry out in same full immersed type High Temperature High Pressure jet overflow dyeing machine, and the cocoon fiber of having avoided will increasing weight after handling moves into the loaded down with trivial details work that dye vat dyes again, has improved operating efficiency.
Description of drawings
Fig. 1 is the process chart of technical solution of the present invention embodiment.
The specific embodiment
Embodiment 1
Shown in accompanying drawing 1.The method of a kind of cocoon fiber weightening finish and antibacterial treatment comprises the steps: to prepare raw silk cheese material, and---coming unstuck with the real silk refining agent,------weightening finish is handled, and---soaping,---carrying out washing treatment dyes---fixation or---antibacterial treatment---back arrangement, oven dry---weightening finish (modification) product of soaping in processing.
In described preparation raw silk cheese material step, selecting silk fiber for use is example, respectively takes by weighing pure 100Kg silk fiber as pending material.
In the described treatment step that comes unstuck, with the real silk refining agent, technology is removed sericine routinely, adopts 100 ℃ of hot water wash together then, 70 ℃ of Warm Wash together, the normal temperature cold wash is together.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is respectively 20%, 50%, 66% of fabric weight; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; The pH value of regulating grafting liquid with formic acid and glacial acetic acid mixed liquor is 3～4; The weightening finish treatment step carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine, and treatment temperature is 85 ℃, 120 minutes time.
Processings of soaping of cocoon fiber after grafting weight gaining handled, the liquid of soaping soaps 209 with still, and consumption 2g/l soaps 10 minutes time, with the removal unreacted monomer; The temperature of soaping is 90 ℃, pressure 2Pa (from outside pressurising, to guarantee that weightening finish evenly).
Described staining procedure still carries out in described full immersed type High Temperature High Pressure jet overflow dyeing machine, full immersed type High Temperature High Pressure jet overflow dyeing machine model of the present invention is a QR202A series, weightening finish is handled and staining procedure all carries out in same full immersed type High Temperature High Pressure jet overflow dyeing machine, has avoided also cocoon fiber to be moved into the loaded down with trivial details work that dye vat dyes after the weightening finish step finishes in traditional real silk modified technique.
The nano titanium oxide (nanometer particle size is 10-50nm) that described antibacterial treatment is about to account for fabric weight 5% joins in the cocoon fiber after the dyeing, and the processing time is 30 minutes.
Steps such as follow-up back arrangement, oven dry adopt common process to get final product, and the cocoon fiber rate of body weight gain the results are shown in Table 1.
Table 1 cocoon fiber rate of body weight gain comparison sheet
| The addition of grafted monomers (accounting for the percentage of fabric weight) | 66％ | 50％ | 20％ |
| The gain in weight of cocoon fiber (Kg) | 50 | 37.5 | 15 |
| The rate of body weight gain of cocoon fiber (%) | 66.67 | 50.05 | 20.08 |
(annotating: obtain the contrast of 75Kg finished silk technology, rate of body weight gain=weightening finish quality/former finished silk quality) with original input 100Kg silk fiber
Embodiment 2
Shown in accompanying drawing 1.The method of a kind of cocoon fiber weightening finish and antibacterial treatment, step is with embodiment 1.
The described preparation raw silk cheese material and the step of coming unstuck are with embodiment 1.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is 66% of a fabric weight; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; Regulate the pH value 3～4 of grafting liquid with formic acid and acetate mixed liquor.The weightening finish treatment step carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine, and treatment temperature is respectively 75 ℃, 85 ℃, 90 ℃, 95 ℃, 120 minutes time.
Follow-up soap, steps such as dyeing, antibacterial treatment, back arrangement, oven dry are with embodiment 1, the cocoon fiber rate of body weight gain the results are shown in Table 2.
Table 2 cocoon fiber rate of body weight gain comparison sheet
| The temperature that weightening finish is handled | 75℃ | 85℃ | 90℃ | 95℃ |
| The gain in weight of cocoon fiber (Kg) | 45 | 49.5 | 51 | 47.3 |
| The rate of body weight gain of cocoon fiber | 60％ | 66％ | 68％ | 63.5％ |
Embodiment 3
Shown in accompanying drawing 1.A kind of cocoon fiber weightening finish and antibacterial modified method, step is with embodiment 1.
The described preparation raw silk cheese material and the step of coming unstuck are with embodiment 1.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is 66% of a fabric weight; And add respectively that to account for fabric weight be 10%, 20%, 30% degumming waste water; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; Regulate the pH value 3～4 of grafting liquid with formic acid and acetate mixed liquor.The weightening finish treatment step carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine, and treatment temperature is 85 ℃, 120 minutes time.
Follow-up soap, steps such as dyeing, antibacterial treatment, back arrangement, oven dry are with embodiment 1, the cocoon fiber rate of body weight gain the results are shown in Table 3.
Table 3 cocoon fiber rate of body weight gain comparison sheet
| The addition of degumming waste water (accounting for the percentage of 100Kg real silk weight) | 10％ | 20％ | 30％ |
| Save weighting agent (Kg) | 9 | 18 | 27 |
| Using water wisely (Kg) | 150 | 300 | 450 |
Table 3 is the result show, adds the weightening finish that degumming waste water is used for cocoon fiber and handles, can the conserve water resource, improve the utilization rate of silk gum in the degumming waste water, and reach the purpose of protection environment.
Embodiment 4
Shown in accompanying drawing 1.A kind of cocoon fiber weightening finish and antibacterial modified method, step is with embodiment 1.
The described preparation raw silk cheese material and the step of coming unstuck are with embodiment 1.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is 66% of a fabric weight; And add that to account for fabric weight be 30% degumming waste water; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; Regulate the pH value 3～4 of grafting liquid with formic acid and acetate mixed liquor.The weightening finish treatment step respectively in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine or with the container of extraneous open communication in carry out, treatment temperature is 85 ℃, 120 minutes time.
Follow-up soap, steps such as dyeing, antibacterial treatment, back arrangement, oven dry are with embodiment 1, the cocoon fiber bacteriostasis rate the results are shown in Table 4, bacteriostasis rate=[(the bacterial detection numbers after the bacterial detection before handling several is handled)/handle preceding bacterial detection number] * 100%.
Table 4 cocoon fiber bacteriostasis rate comparison sheet
| Mushroom | Full immersed type High Temperature High Pressure jet overflow dyeing machine | Container with extraneous open communication |
| Escherichia coli | 10.3％ | 0 |
| Golden staphylococci | 10.1％ | 0 |
Embodiment 5
Shown in accompanying drawing 1.A kind of cocoon fiber weightening finish and antibacterial modified method, step is with embodiment 1.
The described preparation raw silk cheese material and the step of coming unstuck are with embodiment 1.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is 66% of a fabric weight; And add that to account for fabric weight be 30% degumming waste water; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; Regulate the pH value 3～4 of grafting liquid with formic acid and acetate mixed liquor.The weightening finish treatment step carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine, and treatment temperature is 85 ℃, 120 minutes time.
Follow-up soap, steps such as dyeing, antibacterial treatment (or not carrying out this step), back arrangement, oven dry are with embodiment 1, the cocoon fiber rate of body weight gain the results are shown in Table 5.
Table 5 cocoon fiber bacteriostasis rate comparison sheet
| Mushroom | Add the antiseptic that contains titanium dioxide | Do not add the antiseptic that contains titanium dioxide |
| Escherichia coli | 28.3％ | 10.3％ |
| Golden staphylococci | 29.1％ | 10.1％ |
Embodiment 6
Shown in accompanying drawing 1.A kind of cocoon fiber weightening finish and antibacterial modified method, step is with embodiment 1.
The described preparation raw silk cheese material and the step of coming unstuck are with embodiment 1.
In described weightening finish treatment step, prepare grafting liquid earlier: grafted monomers adopts the derivative of methacrylate, as one or more the mixture in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate, its addition is 66% of a fabric weight; And add that to account for fabric weight be 30% degumming waste water; With the ammonium persulfate is initator; Non-ionic surface active agent adopts paregal O, and addition is 0.8g/l; Dispersant WA, addition is 1g/l; Solvent adopts soft water, and bath raio is 1: 15; Regulate the pH value 3～4 of grafting liquid with formic acid and acetate mixed liquor.The weightening finish treatment step carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine, and treatment temperature is 85 ℃, 120 minutes time.
Follow-up soap, steps such as dyeing, antibacterial treatment, back arrangement, oven dry are with embodiment 1, the cocoon fiber degree of staining the results are shown in Table 6.
Table 6 cocoon fiber degree of staining comparison sheet
| Pressure conditions | Normal temperature and pressure 1Pa | High Temperature High Pressure 2Pa |
| Cocoon fiber degree of staining (level) | 3 | 4 |
Claims (5)
1. the method for cocoon fiber weightening finish and antibacterial treatment, it is characterized in that it comprise cocoon fiber preparation, the processing of coming unstuck, wash, increase weight, soap, dyeing, antibacterial treatment and afterwards put step in order; Described weightening finish is handled and is carried out under high-temperature and high-pressure conditions, and described hot conditions is 85～90 ℃; Described weightening finish is handled needs preparation grafting liquid earlier, described grafting liquid contains grafted monomers, initator, nonionic or anion surfactant and degumming waste water, and described grafted monomers is a kind of in methyl methacrylate, ethyl methacrylate, propyl methacrylate or the butyl methacrylate or greater than a kind of mixture; The addition of grafted monomers is by 20～66% of grafting weight gaining cocoon fiber weight, and non-, anionic surfactant concentration is 0.8～2.0g/l, and the pH value of grafting liquid is 3～4, and cocoon fiber carries out grafting weight gaining in bath raio is 1: 15 grafting liquid handles.
2. the method for a kind of cocoon fiber weightening finish as claimed in claim 1 and antibacterial treatment, the addition that it is characterized in that the degumming waste water in the described grafting liquid is by 10～30% of grafting weight gaining real silk weight.
3. the method for a kind of cocoon fiber weightening finish as claimed in claim 1 and antibacterial treatment, it is characterized in that described cocoon fiber preparation, the processing of coming unstuck, wash, increase weight, soap and staining procedure carries out in airtight full immersed type High Temperature High Pressure jet overflow dyeing machine.
4. the method for a kind of cocoon fiber weightening finish as claimed in claim 1 and antibacterial treatment is characterized in that described antibacterial treatment is to use nano titanium oxide that cocoon fiber is handled.
5. the method for a kind of cocoon fiber weightening finish as claimed in claim 1 and antibacterial treatment is characterized in that described initator is a kind of in potassium peroxydisulfate, persulfuric acid magnesium, the ammonium persulfate or greater than a kind of mixture.
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| JP6998847B2 (en) | 2018-09-11 | 2022-01-18 | 東洋紡Ｓｔｃ株式会社 | Antibacterial fiber |
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| CN102277731B (en) * | 2011-06-07 | 2013-03-06 | 东华大学 | Friction-increasing and weighting agent and its preparation method and use in improvement of kapok fiber spinning performances |
| CN102517894B (en) * | 2011-12-08 | 2013-06-12 | 浙江理工大学 | Method for regulating and controlling silk graft copolymerization reaction on basis of hydrophobic and hydrophilic performance of free radicals |
| CN103132156B (en) * | 2013-02-22 | 2016-04-13 | 广西立盛茧丝绸有限公司 | A kind of silk reparation method |
| CN103451935A (en) * | 2013-07-22 | 2013-12-18 | 苏州三和开泰花线织造有限公司 | Grafting and weight increasing method for real silk fibers |
| CN108625169B (en) * | 2018-05-22 | 2020-10-27 | 杭州富强丝绸有限公司 | All-silk yarn-dyed warp knitting preparation process |
| CN111945417B (en) * | 2020-08-19 | 2022-09-27 | 武汉纺织大学 | Preparation method of uvioresistant nano titanium dioxide loaded silk film |
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| CN1431357A (en) * | 2003-01-23 | 2003-07-23 | 苏州大学 | Manufacturing method for weighting cocoon fiber |
| CN1693574A (en) * | 2005-06-21 | 2005-11-09 | 苏州大学 | Method of plasma grafting weight gaining for silk fibre |
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Cited By (1)
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| JP6998847B2 (en) | 2018-09-11 | 2022-01-18 | 東洋紡Ｓｔｃ株式会社 | Antibacterial fiber |
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Effective date of registration: 20201021 Address after: No. 188, Haoyunlai Road, Shanhu street, Shengzhou City, Shaoxing City, Zhejiang Province Patentee after: Shengzhou Haoyunlai printing and dyeing Co.,Ltd. Address before: 312400 Zhejiang province north of the city of Shengzhou City Industrial Zone, Road No. 188. Patentee before: ZHEJIANG HAOYUNLAI DIGITAL TEXTILE Co.,Ltd. |