CN101880335A - Method for preparing modified starch by oxidation and succinic anhydride esterification - Google Patents
Method for preparing modified starch by oxidation and succinic anhydride esterification Download PDFInfo
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- CN101880335A CN101880335A CN2010101182600A CN201010118260A CN101880335A CN 101880335 A CN101880335 A CN 101880335A CN 2010101182600 A CN2010101182600 A CN 2010101182600A CN 201010118260 A CN201010118260 A CN 201010118260A CN 101880335 A CN101880335 A CN 101880335A
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Abstract
The invention provides a method for preparing modified starch by oxidation and succinic anhydride esterification. The method comprises the following steps of: dissolving starch into water to form starch milk, performing oxidation reaction on sodium hypochlorite oxidant and starch to obtain oxidized starch, then removing chlorine, performing esterification reaction by adopting succinic anhydride, and finally dehydrating and drying the reaction product to obtain the modified starch. When the modified starch prepared by the method is used as starch size, the modified starch has the properties of good fluidity, low viscosity and high-concentration use of the oxidized starch; and because the succinic anhydride esterification solves the problem of poor thermal stability of the oxidized starch, the modified starch has the advantages that: adhesion of warps is remarkably improved; a size film has strong forming capability, good mechanical strength and extensibility; the paste has stable viscosity and good fluidity; the size has certain moisture absorption property; the modified starch has good co-solvency with a synthetic size; the film is easy to dissolve in water, and de-sizing is easy; and the paste has high thermal stability, is not affected by high-temperature melting and the like.
Description
Technical field
The application relates to a kind of preparation method of composite modified starch, more specifically, relates to a kind of preparation method who is used for the modified starch by oxidation and succinic anhydride esterification in spinning sizing agent field.
Background technology
In textile industry, the warp thread that fabric is used, be by regenerated fiber such as natural fiber such as cotton, hair, silk, fiber crops and viscose glue, cellulose acetate and synthon such as polypropylene is fine, nylon, polyester be spun into short fiber, union yarn, filament yarn and mix fine long filament etc.In weaving process, warp, weft yarn will be subjected to different mechanical effects.Every warp thread not only will have friction each other, also want successively contact with ten million root weft yarn, so it is very violent to rub.Simultaneously also because the opening of loom, throw a spear, beating motion, yarn with combine, friction between the reed, dropper etc. all can make the warp thread fluffing, so that break end.
The purpose of warp sizing is to improve the weavability of warp thread.For staple fibre, be exactly to paste the clothes filoplume, the serous coat that forms protectiveness in yam surface improves its wear resistance; Be exactly by increasing the cohesive force between monofilament for long filament, strengthen the boundling effect and improve its wear resistance.For the warp thread of undercapacity, can improve intensity by the adhesivity between the fortifying fibre.Therefore, be to have certain requirements to slurry, mainly contain following 7 points:
First: slurry must have certain clinging power, and yarn is bondd well, strengthens obvolvent, and filoplume is docile, increases yarn strength.In drying course the sizing drying cylinder is not adhered to behind the sizing, slurry can not come off too much in weaving process;
Second: it is strong that serous coat forms ability, and the serous coat of formation should have good physical strength and extensibility;
The 3rd: slurries should have suitable viscosity.Have enough perviousness, make slurry not only be overlayed on the surface of yarn but also porous, make the single thread line deadlocked mutually to the inside of yarn.So just make yam surface smooth, also increased brute force simultaneously.The slurry viscosity thermostability will be got well, and flowability will be got well, and the rate of sizing is even;
The the 4th: suitable water absorbability be arranged.In weaving environment, last sizing keeps suitable moisture, and flexibility is good, helps weaving.And for synthon, containing certain moisture also is a kind of anlistatig effective ways;
The 5th: joining the slurry composition with other will have certain mutual solubility;
The 6th: destarch is easy, brings detrimentally affect to the fabric aftertreatment is unlikely;
The 7th: slurries stability will be got well, and can not cause the yarn stain because of melted by heating.Should be difficult for going mouldy, be difficult for spuming, no stink;
At present, spinning sizing agent mainly contains polyvinyl alcohol, acrylic acid or the like and starch and modified starch three major types, wherein starch and modified starch with the resource abundance, cheap, be easy to decompose advantages such as being difficult for contaminate environment and occupied bigger slurry market.
The sizing performance of starch is based on its a large amount of hydroxyl, and they can form hydrogen bond with water molecules at the aqueous solution.Yarn absorbs starch solution, and in drying, water molecules is removed, and on the one hand in yarn inside, the hydroxyl in starch and the fiber molecule forms hydrogen bond, thereby fiber bonds together, and brute force is improved; On the other hand, form hydrogen bond between the fiber molecule on surface, thereby formed the slick epithelium of one deck, increased the wear resisting property of yarn in yam surface, the filoplume of yam surface also by docile and obedient on bar is done, help weaving.
Though the ative starch good film-forming property, serous coat is powerful high, and serous coat is crisp, and degree of stretching is little and hard, and pulping rear slurry viscosity height, poor stability influence starch finishing effect; Therefore the modified starch that has passed through denaturing treatment can overcome these shortcomings, for the research of modified starch starch size with use increasingly extensive.Be applied in Sumstar 190 slurry on the spinning sizing agent and have preferably flowability, the phenomenon of especially when low temperature, not congealing substantially, viscosity is low and stable, can use under high density.Because carboxyl has been introduced in oxidation on starch molecule, to the affinity increase of fiber; Along with the increase of oxidation depth, carboxyl-content increases, with the affinity increase of fiber, to the adhesivity raising of yarn.But serous coat, its poor heat stability cause the yarn stain easily when melted by heating.The suitability for industrialized production of Succinic anhydried modified starch starts from the fifties in last century, uses very extensively in paper industry, but rarely has application in spinning sizing agent.
In order to overcome natural ative starch and existing modified starch as the existing shortcoming of spinning sizing agent, the present invention is through discovering, natural ative starch is being carried out after oxidation obtains Sumstar 190, carry out succinic anhydride esterification again, thereby the modified starch by oxidation and succinic anhydride esterification slurry of producing has multiple advantage.
Summary of the invention
The invention provides a kind of preparation method of modified starch by oxidation and succinic anhydride esterification, it comprise at first with starch is soluble in water size mixing into starch milk after, adopt oxygenant clorox and starch generation oxidizing reaction again, obtain Sumstar 190, then, remove dechlorination, adopt Succinic anhydried to carry out esterification again, with acid pH value is neutralized to PH=6.0-6.5 afterwards, wash at last, dewater, dry, pulverize, sieve, pack and get final product.
In preparation method of the present invention, described starch can be selected from W-Gum, wheat starch, rye starch, oat starch, tapioca (flour), yam starch, glutinous rice starch, preferred yam starch.Because it is variant slightly on the native starch structure of different sources, the difference of these microcosmic has certain influence for sizing performance, the inventor finds through test of many times, adopt method of the present invention, adopting yam starch is that the advantage of the modified starch by oxidation and succinic anhydride esterification slurry that obtains of feedstock production is best, especially for guarantor's look effect of fabric, therefore, preferred especially yam starch.
In preparation method of the present invention, in oxidizing reaction, oxygenant clorox (in 100% hypochlorous acid) is the 0.3-1.0% based on starch weight, preferred 0.5-0.8%, more preferably 0.6%, in esterification, Succinic anhydried is the 0.2-0.8% based on starch weight, preferred 0.4-0.6%, more preferably 0.5%. The temperature of oxidizing reaction should be controlled at 40-42 ℃, and the reaction times can be 1.5-2.5 hour, preferred 2 hours; The temperature of esterification also should be controlled at 28-32 ℃, and the reaction times can be 15-40 minute, and preferred 20-35 minute, such as 20-30 minute.
In preparation method of the present invention,, before oxidizing reaction, adjusting PH is 8.0-8.5, in oxidizing reaction, PH is 8.5-9.5; After oxidizing reaction finishes, before the esterification, adopt the dechlorination of S-WAT or Sulfothiorine, its consumption is the 0.0015-0.005% based on starch weight; In esterification, PH is 8.0-9.0, preferred 8.5.
In a preparation method's of the present invention embodiment, in sizing mixing, can be with starch and water with suitable mixed, such as part by weight 1: 1; Before oxidizing reaction, can starch milk be warming up to 40-42 ℃ earlier, then regulate PH to PH 8.0-8.5 with alkali lye; In reaction process, regulate to make remaining on 8.5-9.5; After oxidizing reaction finishes, before the esterification, should adopt for example S-WAT or Sulfothiorine dechlorination, its consumption is the 0.0015-0.005% based on starch weight; Before esterification, make the temperature of starch milk be reduced to 28-32 ℃, preferred about 30 ℃.
In preparation method of the present invention, regulate pH value and can be selected from dilute hydrochloric acid, dilute sulphuric acid, dilute acetic acid for acid used acid, the hydrochloric acid of preferred 6-12% concentration, regulate pH value and can be selected from sodium hydroxide solution, potassium hydroxide solution for the used alkali lye of alkalescence, the sodium hydroxide solution of preferred 2%-5% concentration, the sieve aperture that sieves is the 80-100 order.
In preparation method of the present invention, clorox can adopt noncorrosive pump to add; Whether the reaction that detects dechlorination if desired is complete, one 2% acetic acid solution can be dripped on the starch potassium iodide paper, dip in glass stick and to get starch milk and smear on it, test paper should no longer become blue getting final product in the place, insufficient if dechlorinate, can add suitable S-WAT again or Sulfothiorine further dechlorinates; In the preparation starch milk, rate of feeding should slowly at the uniform velocity to avoid producing agglomerate or gathering, in the starch milk temperature-rise period, can utilize interchanger that water is heated, and uses the temperature of heating in water bath starch milk again; In preparation method of the present invention, the adding speed of all ingredients should not be too fast, expands or gelatinization to prevent starch.
In an embodiment preferred of the present invention, a kind of preparation method of modified starch by oxidation and succinic anhydride esterification is provided, it comprises the steps:
1). starch and water are mixed, obtain uniform starch milk;
Wherein the consumption of water gets final product for the appropriate amount that starch can be modulated into starch milk, such as, in container, add entry earlier, start stirring, the ative starch of adding and water homogenous quantities such as potato ative starch are (promptly while stirring, the ratio of ative starch and water is 1: 1), until stirring to there not to be the uniform starch milk of block to get final product;
2). begin heating, make the starch milk temperature rise to 40-42 ℃, regulate pH value to 8.0-8.5 with the sodium hydroxide solution of 2%-5% concentration, slowly add the chlorine bleach liquor's (technical grade) who is equivalent to ative starch quality 0.3-1.0% (calculating) with 100% clorox, in the whole process of oxidizing reaction, keep pH value always, maintain the temperature at 40-42 ℃ simultaneously at 8.5-9.5; Oxidizing reaction should continue 1.5-2.5 hour;
In this step 2) in, adding the technical grade chlorine bleach liquor can add in 10-30 minute by flow with noncorrosive pump; After oxidizing reaction begins, can constantly regulate pH value, make it in the whole process of oxidizing reaction, remain on 8.5-9.5 always with the sodium hydroxide solution of 2%-5% concentration; The timing of oxidizing reaction adds from clorox;
3). after oxidizing reaction finishes, use S-WAT or Sulfothiorine dechlorination with respect to ative starch quality 0.0015-0.005%, can detect to the complete (method that can adopt: one 2% acetic acid solution is dripped on the starch potassium iodide paper of dechlorination with starch potassium iodide paper, dip in glass stick and to get starch milk and smear on it, this place of test paper no longer becomes indigo plant and is dechlorination fully);
4). after dechlorination finishes, stop heating, make the temperature of starch milk be reduced to 28-32 ℃, preferred 30 ℃;
5). the Succinic anhydried that will be equivalent to ative starch quality 0.2-0.8% from the starch milk top slowly joins the starch milk, keeps PH at 8.0-9.0 with alkali lye simultaneously; Esterification should continue 15-30 minute (beginning to calculate from adding Succinic anhydried);
6). after esterification finishes, with arriving 6.0-6.5 with starch milk to pH value in the hydrochloric acid soln of 6-12% concentration; Then starch milk is washed (such as placing the eddy flow machine to wash), dehydration (such as carrying out at water extracter), drying, pulverizes, sieves, packs, can obtain oxidation and succinic anhydride modified starch finished product, as potato oxidation and succinic anhydride modified starch finished product.
The modified starch by oxidation and succinic anhydride esterification that the present invention also provides the preparation method according to modified starch by oxidation and succinic anhydride esterification slurry of the present invention to prepare.The Sumstar 190 slurry fluidity was good, the low character that can use under high density of viscosity so both had according to the prepared modified starch size of starch of the present invention, had been solved the problem of Sumstar 190 slurry poor heat stability again by succinic anhydride esterification.Adopt oxidative deformation and succinic anhydride esterification sex change simultaneously, also can obtain following advantage: the adhesivity to warp thread significantly improves, and has effectively increased yarn strength, and makes filoplume docile and obedient; Serous coat forms ability strong and difficult fragmentation and explosion; The paste fluid viscosity is stable, good fluidity, and the rate of sizing is even, and has enough perviousness to make yam surface smooth; Slurries have certain moisture, are beneficial to weave; Good with the synthetic slurry cosolvency; Film is soluble in water, and destarch is easy; Stick with paste liquid thermostability height, be not subject to the influence of high heat fusing etc.Compare the oxidative cationic starch size, operate more easyly, also have very strong price advantage.Simultaneously, have phosphate group and stick with paste the high yam starch of liquid transparency, fabric is protected look can play the best, obtain better slurry effect as raw material if use.
In addition, the present invention also provides described modified starch by oxidation and succinic anhydride esterification to be used in purposes in the spinning sizing agent.
Embodiment
Further elaborate the present invention with reference to embodiment below, but it will be appreciated by those skilled in the art that the present invention is not limited to the method for these embodiment and use.And those skilled in the art can carry out it is equal to replacement, combination, improvement or modification according to description of the invention to the present invention, but these all will comprise within the scope of the invention.
Embodiment 1 potato modified starch by oxidation and succinic anhydride esterification
Prepare potato oxidation and succinic anhydride esterification starch according to following steps:
1). with potato ative starch and water according to 1: 1 ratio furnishing starch milk of mass ratio;
2). begin heating, make the starch milk temperature rise to 40.0 ℃, sodium hydroxide solution with 2% concentration is regulated pH value to 8.0, slowly add the technical grade chlorine bleach liquor who is equivalent to ative starch quality 0.3% (calculating) with 100% clorox, remain on 8.5-9.5 in the whole process of oxidizing reaction always, maintain the temperature at 40-42 ℃ simultaneously; Add calculating from clorox, oxidizing reaction should continue 1.5 hours;
3). after oxidizing reaction finishes, use S-WAT dechlorination, can detect to dechlorinating fully with starch potassium iodide paper with respect to ative starch quality 0.005%;
4). stop heating, make the temperature of starch milk be reduced to 28 ℃;
5). the Succinic anhydried that will be equivalent to ative starch quality 0.2% from the starch milk top slowly joins the starch milk, and the sodium hydroxide solution with 2.8% concentration in the reaction process is regulated PH to 8.5, and esterification continues 15 minutes;
6). after esterification finishes, with in the hydrochloric acid soln of 6% concentration with starch milk to pH value to 6.21; Then to starch milk wash, dewater, dry, pulverize, sieve, pack, just obtained potato oxidation and succinic anhydride esterification finished product of starch.
Thermal stability data: first hour viscosity is 12.0cp, and second hour viscosity is 11.3cp, and viscosity was 10.7cp in the 3rd hour; Thermostability=10.7 ÷, 12.0 * 100%=89.17%
Embodiment 2 potato modified starch by oxidation and succinic anhydride esterification
Prepare potato oxidation and succinic anhydride esterification starch according to following steps:
1). with potato ative starch and water according to 1: 1 ratio furnishing starch milk of mass ratio;
2). begin heating, make the starch milk temperature rise to 42 ℃, sodium hydroxide solution with 4% concentration is regulated pH value to 8.5, slowly add the technical grade chlorine bleach liquor who is equivalent to ative starch quality 1.0% (calculating) with 100% clorox, remain on 9.0-9.2 in the whole process of oxidizing reaction always, maintain the temperature at 40-41 ℃ simultaneously; Add calculating from clorox, oxidizing reaction should continue 2 hours;
3). after oxidizing reaction finishes, use extremely complete with respect to the S-WAT dechlorination of ative starch quality 0.0015%;
4). stop heating, make the temperature of starch milk be reduced to 30 ℃;
5). the Succinic anhydried that will be equivalent to ative starch quality 0.8% from the starch milk top slowly joins the starch milk, and the sodium hydroxide solution with 4% concentration in the reaction process is regulated PH to 8.5, and esterification continues 25 minutes;
6). after esterification finishes, with in the hydrochloric acid soln of 12% concentration with starch milk to pH value to 6.5; Then to starch milk wash, dewater, dry, pulverize, sieve, pack, just obtained potato modified starch by oxidation and succinic anhydride esterification finished product.
Thermal stability data: first hour viscosity is 14.9cp, and second hour viscosity is 14.0cp, and viscosity was 13.5cp in the 3rd hour; Thermostability=13.5 ÷, 14.9 * 100%=90.60%
Embodiment 3 potato modified starch by oxidation and succinic anhydride esterification
Prepare potato oxidation and succinic anhydride esterification starch according to following steps:
1). with potato ative starch and water according to 1: 1 ratio furnishing starch milk of mass ratio;
2). begin heating, make the starch milk temperature rise to 41.0 ℃, sodium hydroxide solution with 3% concentration is regulated pH value to 8.35, slowly add the technical grade chlorine bleach liquor who is equivalent to ative starch quality 0.7% (calculating) with 100% clorox, remain on 9.1-9.2 in the whole process of oxidizing reaction always, maintain the temperature at 41-42 ℃ simultaneously; Add calculating from clorox, oxidizing reaction should continue 2.5 hours;
3). after oxidizing reaction finishes, use S-WAT dechlorination with respect to ative starch quality 0.008%;
4). stop heating, make the temperature of starch milk be reduced to 30 ℃;
5). the Succinic anhydried that will be equivalent to ative starch quality 0.5% from the starch milk top slowly joins the starch milk, and the sodium hydroxide solution with 4% concentration in the reaction process is regulated PH to 8.6, and esterification continues 35 minutes;
6). after esterification finishes, with in the hydrochloric acid soln of 10% concentration with starch milk to pH value to 6.09; Then to starch milk wash, dewater, dry, pulverize, sieve, pack, just obtained potato modified starch by oxidation and succinic anhydride esterification finished product.
Thermal stability data: first hour viscosity is 8.1cp, and second hour viscosity is 7.9cp, and viscosity was 7.5cp in the 3rd hour; Thermostability=7.5 ÷, 8.1 * 100%=92.59%
Attached: the measuring method of thermostability
A. calculate sample weighting amount:
M=300 * beat and stick with paste concentration %/(1-moisture %-beats and sticks with paste concentration %)
Amount of water: 300ml
Annotate: beating paste concentration and be the requirements set according to the client, generally is 6%-10%; Starch moisture is directly measured with Moisture Meter)
B. in water-bath, add the water of q.s, be warming up to 60 ℃.The three-necked bottle of having prepared is put into water-bath, plug, funnel, thermometer and stirring rake are connected with three-necked bottle, prepare 300ml distilled water.
C. an off-the-shelf 100ml beaker is placed on the balance, peeling is heavy, take by weighing the sample size of having calculated, add a small amount of distilled water and break into starch milk, along funnel with starch milk to going in the three-necked bottle, with residue distilled water flushing beaker, glass stick and funnel, all change in the three-necked bottle then until 300ml distilled water.
D. open stirring rake,, open thermostat water bath simultaneously, be warming up to 100 ℃ warming-in-water to 100 ℃, stirring can be soon before the starch ungelatinized, after starch begins gelatinization, when temperature rises to 60-70 ℃, calculate with stopwatch, number stirring rake revolution, about 160 rev/mins get final product.
E. continue to heat up, begin to clock during temperature to 95 ℃, measure viscosity number for the first time after one hour, measured viscosity number for the second time, and measured viscosity number for the third time after three hours in two hours.
F. measure: earlier the NDJ-7 viscometer is made zero, be connected with water bath with thermostatic control with suitable test cup, required rotor is put into test cup endoporus, open the water bath with thermostatic control circulation, when treating that the viscometer temperature rises to 95 ℃, draw an amount of liquid of sticking with paste with syringe, add in the test cup, will test the cup endoporus and fill with, liquid level is concordant with the inclined-plane lower rim, rotor is hung on the viscometer, and temperature begins when arriving 95 ℃ to measure, and rotor hangs iron wire and wants vertical, rotate with one heart, do not allow to depart from the center double swerve, treat that reading is stable after, multiply by the rotor coefficient with the viscometer reading and be and record viscosity number.Wash test cup and rotor with clear water, blot water with filter paper then.
The result calculates: viscosity number * 100% that the viscosity number ÷ of thermostability=3rd hour mensuration measured in first hour.
Claims (9)
1. the preparation method of a modified starch by oxidation and succinic anhydride esterification, it comprise at first with starch is soluble in water size mixing into starch milk after, adopt oxygenant clorox and starch generation oxidizing reaction again, obtain Sumstar 190, then, remove dechlorination, adopt Succinic anhydried to carry out esterification again, with acid pH value is neutralized to PH=6.0-6.5 afterwards, wash at last, dewater, dry, pulverize, sieve, pack and get final product.
2. according to the preparation method of claim 1, wherein said starch is selected from W-Gum, wheat starch, rye starch, oat starch, tapioca (flour), yam starch, glutinous rice starch, preferred yam starch.
3. according to the preparation method of claim 1, wherein in oxidizing reaction, oxygenant clorox (in 100% pure hypochlorous acid) is the 0.3-1.0% based on starch weight, preferred 0.5-0.8%, more preferably 0.6%; In esterification, Succinic anhydried is the 0.2-0.8% based on starch weight, preferred 0.4-0.6%, more preferably 0.5%.
4. according to the preparation method of claim 1, wherein the temperature of oxidizing reaction should be controlled at 40-42 ℃, and the reaction times can be 1.5-2.5 hour; The temperature of esterification also should be controlled at 28-32 ℃, and the reaction times can be 15-40 minute.
5. according to the preparation method of claim 1, before oxidizing reaction, adjusting PH is 8.0-8.5, and in oxidizing reaction, PH is 8.5-9.5; After oxidizing reaction finishes, before the esterification, adopt the dechlorination of S-WAT or Sulfothiorine, its consumption is the 0.0015-0.005% based on starch weight; In esterification, PH is 8.0-9.0, preferred 8.5.
6. according to the preparation method of claim 5, wherein regulate pH value and be selected from dilute hydrochloric acid, dilute sulphuric acid, dilute acetic acid for acid used acid, the hydrochloric acid of preferred 6-12% concentration, regulate pH value and be selected from sodium hydroxide solution, potassium hydroxide solution for the used alkali lye of alkalescence, the sodium hydroxide solution of preferred 2%-5% concentration, the sieve aperture that sieves is the 80-100 order.
7. the preparation method of a modified starch by oxidation and succinic anhydride esterification, it comprises the steps:
1). starch and water are mixed, obtain uniform starch milk;
2). begin heating, make the starch milk temperature rise to 40-42 ℃, regulate pH value to 8.0-8.5 with the sodium hydroxide solution of 2%-5% concentration, slowly add the technical grade chlorine bleach liquor who is equivalent to ative starch quality 0.3-1.0%, in the whole process of oxidizing reaction, keep pH value always, maintain the temperature at 40-42 ℃ simultaneously at 8.5-9.5; Oxidizing reaction should continue 1.5-2.5 hour;
3). after oxidizing reaction finishes, use S-WAT or Sulfothiorine dechlorination, can detect to dechlorinating fully with starch potassium iodide paper with respect to ative starch quality 0.0015-0.005%;
4). after dechlorination finishes, stop heating, make the temperature of starch milk be reduced to 28-32 ℃, preferred 30 ℃;
5). the Succinic anhydried that will be equivalent to ative starch quality 0.2-0.8% slowly joins in the starch milk, keeps PH at 8.0-9.0 with alkali lye simultaneously; Esterification should continue 15-40 minute;
6). after esterification finishes, with arriving 6.0-6.5 with starch milk to pH value in the hydrochloric acid soln of 6-12% concentration; Then to starch milk wash, dewater, dry, pulverize, sieve, pack, promptly obtain finished product.
8. the modified starch by oxidation and succinic anhydride esterification for preparing according to each preparation method in the claim 1 to 7 is used for slurry.
9. the modified starch by oxidation and succinic anhydride esterification of claim 8 is used for the purposes of pulp preparation.
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| CN113463391A (en) * | 2021-07-20 | 2021-10-01 | 广东汇美淀粉科技有限公司 | Novel warp sizing material for spandex filament core-spun yarn and preparation method thereof |
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