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WO2016058252A1 - Procédé pour le désencollage enzymatique du coton dans un fluide de dioxyde de carbone supercritique - Google Patents

Procédé pour le désencollage enzymatique du coton dans un fluide de dioxyde de carbone supercritique Download PDF

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Publication number
WO2016058252A1
WO2016058252A1 PCT/CN2014/093227 CN2014093227W WO2016058252A1 WO 2016058252 A1 WO2016058252 A1 WO 2016058252A1 CN 2014093227 W CN2014093227 W CN 2014093227W WO 2016058252 A1 WO2016058252 A1 WO 2016058252A1
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WIPO (PCT)
Prior art keywords
desizing
enzyme
cotton
carbon dioxide
supercritical carbon
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PCT/CN2014/093227
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English (en)
Chinese (zh)
Inventor
龙家杰
刘仕琪
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苏州大学
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Application filed by 苏州大学 filed Critical 苏州大学
Publication of WO2016058252A1 publication Critical patent/WO2016058252A1/fr

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Classifications

    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
    • D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
    • D06L1/02—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using organic solvents
    • D06L1/06—De-sizing
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic

Definitions

  • the invention belongs to the technical field of textile dyeing and finishing, and in particular relates to an enzyme desizing method for cotton in a supercritical carbon dioxide fluid.
  • the supercritical carbon dioxide fluid enzyme desizing technology has significant characteristics of clean production such as ecology, environmental protection, energy saving and emission reduction, and is of great significance for changing the status of high pollution and high energy consumption of traditional textile pretreatment processing.
  • biological enzymes have broad application prospects in dyeing and finishing. Because the enzyme preparation is a biological preparation, it is non-toxic and harmless, and its burst application conforms to the requirements of green processing and sustainable development.
  • the application of desizing enzymes is relatively mature and extensive, and has been increasingly accepted by printing and dyeing workers, and is used to remove impurities such as starch slurry on fabrics. Some of these enzymes have a synergistic effect in combination with hydrazine.
  • pectinase degrades the epidermal layer of the substrate, which can produce more sites of action for cellulase; and degradation of cellulase results in more epidermal layers. Pectin is exposed and interacts with pectinase.
  • pre-slurry treatment is an important processing process for the production of cotton products.
  • Traditional cotton products require a large amount of water, energy and chemicals to be produced before desizing, and produce a large amount of high-concentration wastewater. It poses a serious threat to resource protection and the ecological environment.
  • the technical problem to be solved by the present invention is to solve the problem that any method in the prior art can be conveniently operated to realize pre-treatment of cotton products in a supercritical carbon dioxide fluid, which is energy-saving and environmentally friendly.
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, comprising the following steps:
  • A a suitable amount of surfactant dissolved in a volume ratio of 1: 2: 5 alcohol and water in a mixed solution;
  • the desizing working fluid is placed in the desizing liquid storage tank of the enzyme desizing device, and the enzyme desizing device is placed in a supercritical carbon dioxide fluid processing system with a circulation device;
  • the surfactant is sodium diisooctyl succinate (AOT)
  • the concentration of the sodium diisooctyl succinate (AOT) is 2.5 g / L - 25 g / L.
  • the alcohol is ethanol.
  • the desizing enzyme is a composition of one of cellulase, pectinase, lipase, a-amylase or any ratio thereof.
  • the desizing enzyme is a composition composed of a cellulase, a pectinase, a lipase, and an ot-amylase in a ratio of 1:1:1:1.
  • the certain supercritical fluid condition is that the reaction temperature is 40 ° C, the pressure is 13 MPa, the treatment time is 1 h, and the inter-turn ratio of the fluid circulation and the static treatment is 1 : 10.
  • the present invention provides a method for enzymatic desizing of cotton in a supercritical carbon dioxide fluid, which comprises dissolving a desizing enzyme with an appropriate amount of a surfactant, an appropriate proportion of an alcohol and water into a desizing working liquid, and then containing the retreating
  • the desiccant working solution of the slurry enzyme forms a microemulsion in situ by using a hydrophobic supercritical carbon dioxide medium, and the microemulsion releases the active desizing enzyme with the fluid penetrating the cotton product, thereby realizing the cotton product pulp in the supercritical carbon dioxide medium.
  • Degradation treatment of the material The method of the invention has simple process and convenient operation.
  • the reaction is mild, the damage to the cloth is small, and the high temperature is not required, and the application of a large amount of water, heat and high concentration alkali in the traditional desizing process is avoided, and the method is efficient. , green, environmental protection and other characteristics.
  • optimization of the desizing process is achieved by controlling parameters such as the amount of water used in the desizing working fluid and the amount of desizing enzyme.
  • FIG. 1 is a schematic view showing the structure of an enzyme desizing device for cotton in a supercritical carbon dioxide fluid according to a first embodiment of the present invention
  • FIG. 2 is a graph showing the relationship between the weight loss rate of the cotton product treated by the enzyme desizing treatment and the water consumption amount of the desizing working liquid;
  • FIG. 3 is a graph showing the effect of the enzyme desizing treatment of the cotton product of the present invention and desizing.
  • FIG. 4 is a diagram showing the relationship between the weight loss rate of the cotton product treated by the enzyme desizing of the present invention and the desizing enzyme concentration of the desizing working fluid;
  • FIG. 5 is a graph showing the relationship between the hair effect value of the cotton desizing treatment of the enzyme and the desizing enzyme concentration of the desizing working fluid of the present invention.
  • a desizing liquid storage tank 11, a fluid distributor; 111, a circulating fluid inlet pipe; 112, a circulating fluid outlet pipe; 2, a desizing kettle; 21, a cotton product winding shaft; Slurry working fluid; 4, cotton products to be treated; 5, circulating fluid outlet; 6, fluid shroud; 7, filter; 8, connecting device.
  • Embodiment 1 provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, which is achieved by an enzyme desizing device for cotton in a supercritical carbon dioxide fluid having the structure shown in FIG.
  • the enzyme desizing apparatus includes a desizing stock storage tank 1 and a desizing kettle 2 which is sealingly connected to the desiccant storage tank 1 through a connection device 8.
  • the desizing liquid storage tank 1 is a cylindrical kettle body, and the desiccant storage tank 1 is provided with an inverted "mountain" type tubular fluid distributor 11 which is mainly composed of three pipes which are connected to each other, and the pipe located at the center
  • the bottom end of the circulating fluid inlet pipe 111 is connected to a supercritical carbon dioxide fluid treatment system (not shown) with a circulation pump; the two pipes on both sides are circulating fluid outlet pipes 112,
  • the nozzles of the two circulating fluid outlet tubes 112 are bent downward, and the lower end of the jaws extends below the level of the desizing working fluid 3 in the desizing liquid storage tank 1.
  • the top of the desizing kettle 2 is provided with a circulating fluid outlet 5, which is connected to a supercritical carbon dioxide fluid treatment system.
  • the desizing kettle 2 is also a cylindrical kettle body.
  • the desizing kettle 2 is equipped with an inner hollow cotton product winding shaft 21, and the cotton product winding shaft 21 is wound with a cotton product to be treated 4, cotton products.
  • the bottom end of the winding shaft 21 is closed at the top end, and a through hole is formed in the side wall of the shaft.
  • the bottom end of the cotton product winding shaft 21 adjacent to the connecting device 8 is connected to the horn-shaped fluid guide hood 6, and the filter 7 is disposed below the fluid guiding hood 6, which can effectively filter the desizing working fluid 3 and the circulating fluid mixture. Precipitated impurities contained in the liquid.
  • the filter 7 is preferably a single-layer or multi-layered plate material which is filled with 50-2000 mesh micropores.
  • the shaft body of the cotton product winding shaft 21 is made of Teflon or non-thermal conductive material, or the inner and outer surfaces thereof are made of Teflon or non-thermal conductive material, which prevents the winding axis of the cotton product from being fixed.
  • the temperature of the desizing working fluid and the circulating fluid mixture flow through to cause overheating damage, which prolongs the service life of the cotton product winding shaft.
  • the top of the desizing kettle 2 is provided with a circulating fluid outlet 5 which is connected to a supercritical carbon dioxide fluid treatment system with a circulation device.
  • the desizing stock storage tank 1 and the desizing tank 2 are connected to the supercritical carbon dioxide fluid treatment system through the above-mentioned circulating fluid inlet pipe 111 and circulating fluid outlet 5.
  • a method for applying an enzyme desizing device for cotton in a supercritical carbon dioxide fluid as described in the present embodiment includes the following steps:
  • AOT surfactant sodium diisooctyl succinate
  • [0035] B adding 2% of the desizing enzyme relative to the weight 4 of the cotton product to be treated to the above mixed solution system, and stirring until the system is clarified, to obtain a desizing working liquid 3; wherein, the cotton product to be treated
  • the weight of 4 is 2 g
  • the desizing enzyme is a combination of each O.Olg cellulase, pectinase, lipase, and ot-amylase.
  • the desizing working fluid 3 is placed in the desizing liquid storage tank 1, the cotton product 4 to be processed wound on the cotton product winding shaft 21 is placed in the desizing kettle 2, the desizing liquid storage tank 1 Sealed and connected with the desizing kettle 2 to form an enzyme desizing device, ensuring that the mouth of the cotton product winding shaft 21 is kept at a distance of 45 cm from the liquid level of the desizing working fluid 3, so as to prevent the agitation of the fluid distributor and the entrainment of the fluid.
  • the desizing working fluid is brought into direct contact with the cotton product; and the enzyme desizing device is placed in a supercritical carbon dioxide fluid device with a circulation device.
  • the enzyme desizing device is connected to the supercritical carbon dioxide fluid treatment system with a circulation pump through the circulating fluid inlet pipe 111 and the circulating fluid outlet 5, or the enzyme desizing device is placed in a supercritical state with a circulation pump.
  • the carbon dioxide fluid treatment device after the closed system, the predetermined desizing process and parameters are followed (the reaction temperature is 40 ° C, the pressure is 13 MPa, and the desizing treatment is 1 h, and the inter-turn ratio of fluid circulation and static treatment is adopted.
  • the circulation pump in the external supercritical carbon dioxide fluid treatment system is started, and the circulating fluid is passed through the tubular fluid distributor 11 and the desizing working fluid in the desizing liquid storage tank 1
  • the mixture is fully contacted, and a microemulsion is formed under the action of the surfactant, and the desizing enzyme is transferred into the hydrophobic fluid, and then flows into the winding shaft 21 of the cotton product, and is wound around the cotton product through the through hole and the winding.
  • the cotton product 4 to be treated on the shaft 21 acts to complete the desizing treatment.
  • the enzyme desizing method improves the reactivity of the desizing enzyme on the slurry and impurities on the fiber, improves the desizing efficiency of the cotton product slurry, and effectively realizes the cotton product slurry in the supercritical carbon dioxide fluid medium. Degradation treatment.
  • the fluid stops circulating and depressurizes the supercritical carbon dioxide fluid treatment system.
  • the desizing working fluid 3 and the circulating fluid are separated and recovered by an external separation and recovery system.
  • the connecting device 8 is opened, and the cotton product after the enzyme desizing treatment is taken out.
  • the mixed solution remaining in the desizing liquid storage tank 1 can be recovered or replenished after the components are added.
  • Weight loss rate test After the desizing is completed, the swatch sample is taken out, and after washing 2-3 times with water, the cotton product is placed in an electric blast drying oven and baked at a temperature of 105 ° C for 120 min, using a sealed bag. Seal the sample, balance it in the dryer for more than 24 hours, and weigh the weight. The cotton product before desizing is treated in the same manner, and the weight loss rate of the cotton product is obtained by comparing the weight of the cotton product before and after the desizing treatment.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the first embodiment, and details are not described herein again.
  • the desizing working fluid component of the present embodiment is a mixed solution of 10 mL of ethanol and 30 mL of water in a volume ratio of 1:3.
  • the weight loss rate and the gross effect value of the cotton products subjected to desizing treatment in this example are: the weight loss rate is 5.8%, and the gross effect value is 5.7 cm.
  • Embodiment 3 is a diagrammatic representation of Embodiment 3
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the first embodiment, and details are not described herein again.
  • the desizing working fluid component of the present embodiment is a mixed solution of 10 mL of ethanol and 40 mL of water in a volume ratio of 1:4.
  • the weight loss rate and the gross effect value of the cotton product subjected to desizing treatment in this example are: the weight loss rate is 8.2%, and the gross effect value is 7.5 cm. [0055]
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the first embodiment, and details are not described herein again.
  • the desizing working fluid component of the present embodiment is a mixed solution of 10 mL of ethanol and 50 mL of water in a volume ratio of 1:5.
  • the weight loss rate and the gross effect value of the cotton products subjected to desizing treatment in this example are: the weight loss rate is 6.9%, and the gross effect value is 6.8 cm.
  • Embodiment 5 is a diagrammatic representation of Embodiment 5
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the third embodiment, and details are not described herein again.
  • the desizing enzyme of the present embodiment is a combination of 0.004 g of cellulase, pectinase, lipase and ot-amylase, that is, the weight of the desizing enzyme is the weight of the cotton product to be treated. 0.8%.
  • the weight loss rate and the gross effect value of the cotton products subjected to desizing treatment in this example are: the weight loss rate is 4.1%, and the gross effect value is 6.0 cm.
  • the present invention provides an enzyme desizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the third embodiment, and details are not described herein again.
  • the desizing enzyme of the present embodiment is a combination of each of 0.008 g of cellulase, pectinase, lipase and ot-amylase, that is, the weight of the desizing enzyme is the weight of the cotton product to be treated. 1.6%.
  • the weight loss rate and the gross effect value of the cotton products subjected to desizing treatment in this example are: the weight loss rate is 6.9%, and the gross effect value is 7.0 cm.
  • Embodiment 7 is a diagrammatic representation of Embodiment 7
  • the present invention provides an enzyme de-sizing method for cotton in a supercritical carbon dioxide fluid, and the enzyme desizing method is substantially the same as the enzyme desizing method described in the third embodiment, and details are not described herein again.
  • the desizing enzyme of the present embodiment is a combination of 0.012g of cellulase, pectinase, lipase and ot-amylase, that is, the weight of the desizing enzyme is the weight of the cotton product to be treated. 2.4%.
  • the weight loss rate and the gross effect value of the cotton products subjected to desizing treatment in this example are as follows: the weight loss rate is 7.1%, and the gross effect value is 7.7 cm.
  • the amount of water used in the desizing working fluid directly affects the desizing effect of the cotton product.
  • the amount of ethanol is 10 mL
  • the amount of water is 20 mL, that is, the volume ratio of ethanol to water is 1:2 (as in Example 1)
  • the weight loss rate of the cotton product is 4.6%.
  • the hair effect value is 4.6cm, the desizing effect is not ideal; and as the water dosage increases, that is, the volume ratio of ethanol to water increases, and the water consumption is 40mL (as in the third embodiment), the weight loss rate of cotton products It reaches 8.2%, the gross effect value is 7.5cm, and the desizing effect is optimal. As the water dosage continues to increase, too much water can not form a micro-emulsion well, resulting in a decrease in desizing effect.
  • Example 5 From Example 3, Example 5 to Example 7, Figure 4 and Figure 5, it can be seen that the concentration of desizing enzyme in the desizing working fluid also has a great influence on the desizing effect of the cotton product.
  • concentration of desizing enzyme is between 0-0.8g/L, the higher the desizing enzyme concentration, the better the desizing effect of cotton products, the weight loss rate increases from 1% to 7.5%, and the effect value is also from 5.5.
  • cm to 7.8cm indicates that the desizing effect is good and the hydrophilicity of cotton products is enhanced.
  • the concentration of desizing enzymes retreats with the concentration of desizing enzymes continuing to increase. The effect of the slurry effect is reduced, and even because the concentration of the desizing enzyme is too high, the activity is inhibited and the desizing effect is lowered.
  • the volume ratio of the mixed solution of ethanol and water in the desizing working fluid of the present invention can be controlled in the range of 1:2-1:5, and the weight of the desizing enzyme is controlled to be 0.1%-20 ⁇ 3 ⁇ 4 with respect to the weight of the cotton product to be treated. range.
  • the concentration of sodium diisooctyl succinate (AOT) can be controlled in the range of 2.5 g/L to 25 g/L.
  • AOT sodium diisooctyl succinate
  • the desizing treatment reaction temperature in the range of 30 ° C -95 ° C
  • the pressure in the range of 6Mpa-30Mpa, desizing treatment in the range of 0.5h-24. Oh can be used for cotton products
  • the desizing treatment effect is further optimized.
  • the surfactant in the present invention is not limited to sodium diisooctyl succinate (AOT), but also may be dodecyl polyoxyethylene ether (C12E4), lecithin, cetyltrimethyl One of ammonium bromide or sodium diisooctyl succinate (AOT), dodecyl polyoxyethylene ether (C12E4), lecithin and cetyltrimethylammonium bromide mixture.
  • Alcohols are not limited to ethanol, but may also be methanol or other C1-C1 0 fatty alcohol.
  • the desizing enzyme is not limited to a mixture of equal amounts of cellulase, pectinase, lipase and ot-amylase, and may also be one of cellulase, pectinase, lipase and alpha-amylase. Or a composition of any ratio thereof.
  • the method of the invention has good practicability for supercritical carbon dioxide fluid anhydrous enzyme desizing processing of cotton, especially starch sizing cotton, has small damage to cloth, mild reaction, and does not need to be carried out at high temperature, avoiding the tradition
  • the application of a large amount of water, heat and high-concentration alkali in the desizing process is easy to control and carry out with the supercritical process, and has the characteristics of high efficiency, greenness and environmental protection, so the application prospect is broad.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Enzymes And Modification Thereof (AREA)

Abstract

L'invention concerne un procédé pour le désencollage enzymatique du coton dans un fluide de dioxyde de carbone supercritique, appartenant au domaine technique de la coloration et de la finition textiles, et conçu de manière à résoudre les problèmes des procédés de désencollage classiques, tels qu'une consommation d'énergie élevée et la nocivité pour l'environnement. Le procédé de désencollage enzymatique comprend les étapes suivantes : A. une quantité appropriée de tensio-actif est dissoute dans une solution mixte d'alcool et d'eau ayant un rapport en volume de 1:2 à 1:5 ; B. une enzyme de désencollage ayant un poids de 0,1 % à 20 % du poids du produit de coton devant être traité est ajoutée à la solution mixte, qui est agitée jusqu'à ce que le système soit clarifié, de manière à obtenir une solution de travail de désencollage ; C. la solution de travail de désencollage est placée dans une bouilloire de stockage de liquide de désencollage d'un appareil de désencollage enzymatique, et l'appareil de désencollage enzymatique est placé dans un système de manipulation de fluide de dioxyde de carbone supercritique ayant un appareil de circulation ; D. après fermeture du système, l'appareil de circulation est activé ; dans les conditions d'un certain fluide supercritique, la solution de travail de désencollage traite par voie enzymatique la boue du produit de coton à traiter. La présente invention permet d'obtenir un prétraitement de désencollage enzymatique d'un produit de coton dans un fluide de dioxyde de carbone supercritique, et est économe en énergie et respectueuse de l'environnement.
PCT/CN2014/093227 2014-10-17 2014-12-08 Procédé pour le désencollage enzymatique du coton dans un fluide de dioxyde de carbone supercritique WO2016058252A1 (fr)

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CN201410553202.9A CN104389153B (zh) 2014-10-17 2014-10-17 一种超临界二氧化碳流体中棉的酶退浆方法
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WO2016058257A1 (fr) * 2014-10-17 2016-04-21 苏州大学 Procédé de prétraitement pour le désencollage textile
CN104674431A (zh) * 2015-03-19 2015-06-03 苏州陈恒织造有限公司 一种二氧化碳退浆粘胶/铜氨纤维混纺面料的制作方法
CN105651719B (zh) * 2016-01-21 2018-08-21 苏州大学 一种提高果胶酶活性及稳定性的超临界流体处理方法
CN105568591B (zh) * 2016-01-25 2017-10-13 苏州大学 一种超临界二氧化碳流体中棉的双氧水退浆前处理法
CN106996034A (zh) * 2017-05-22 2017-08-01 苏州凯邦生物技术有限公司 一种基于超临界二氧化碳与碱性生物酶的棉退浆方法
CN109281088A (zh) * 2018-11-14 2019-01-29 苏州大学 毛纺品的一种超临界二氧化碳流体丝光处理方法
CN110747625A (zh) * 2019-11-01 2020-02-04 苏州大学 利用超临界流体清洗动物纤维的方法
JP7133125B2 (ja) * 2021-05-19 2022-09-08 伊澤タオル株式会社 糊剤を繊維品に付与する方法、糊剤付き繊維品の製造方法、糊剤付き繊維品から糊剤を除去する方法、及び糊剤付き繊維品から繊維品を製造する方法
CN114292437A (zh) * 2021-12-31 2022-04-08 石狮市中纺学服装及配饰产业研究院 一种超临界二氧化碳萃取浆料中pva的方法

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