CN104313891B - A kind of starch slurry desizing method with supercritical carbon dioxide as medium - Google Patents
A kind of starch slurry desizing method with supercritical carbon dioxide as medium Download PDFInfo
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- CN104313891B CN104313891B CN201410554543.8A CN201410554543A CN104313891B CN 104313891 B CN104313891 B CN 104313891B CN 201410554543 A CN201410554543 A CN 201410554543A CN 104313891 B CN104313891 B CN 104313891B
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Abstract
The invention discloses a kind of starch slurry desizing method with supercritical carbon dioxide as medium, belong to textile dyeing and finishing processing technique field, design for solving the big problem such as the most not environmentally of tradition desizing power consumption.This desizing method comprises the following steps: A, be dissolved in by diisooctyl succinate sodium sulfonate in ethanol and water mixed solution;B, desizing enzyme is added in mixed solution, and stir and clarify to system, prepare desizing enzyme mixation;C, interpolation buffer solution system, by sig water regulation desizing enzyme mixation pH value to 4 10, obtain desizing working solution;D, desizing working solution is added in supercritical carbon dioxide fluid processing system, under certain condition textile is carried out enzymolysis processing.Present invention achieves the enzymolysis processing to textile, use and be suitable to the buffer system of enzyme reaction and under the conditions of supercritical carbon dioxide fluid, form environmental condition and the method for microemulsion, improve enzyme desizing efficiency in supercritical CO 2 medium, energy-conserving and environment-protective.
Description
Technical field
The invention belongs to textile dyeing and finishing processing technique field, particularly relate to a kind of with supercritical carbon dioxide for being situated between
The starch slurry desizing method of matter.
Background technology
Supercritical carbon dioxide fluid enzyme desizing technology, has significant ecology, environmental protection and energy-saving and emission-reduction etc. clear
The feature that clean produces, has weight to present situations such as changing the high pollution of traditional textile pre-treatment processing, high energy consumption
Want meaning.At present, enzyme has broad application prospects, because enzyme preparation is as one in dyeing and finishing is processed
Planting biological preparation, nontoxic, the requirement of green processing and sustainable development has been complied with in its exploitation application.
Wherein the application of desizing enzyme is more ripe and extensive, is the most increasingly accepted by colourist, and applies
In impurity such as the starch slurries removed on fabric.Synergism is there is in some of which enzyme when being used in combination, such as,
The epidermal area of pectase degraded substrate, can be that cellulase produces more action sites;And the fall of cellulase
Solution effect can make the pectic substance in more epidermal area expose, and with pectase effect.
But, the enzyme desizing of textile in supercritical carbon dioxide fluid, but relatively want complicated and much more difficult.
Its difficult point is how to make the high molecular protein compound-enzyme of polarity, enter hydrophobic High-pressure supercritical two
In carbon oxide fluid medium, and its greater activity can be kept.Secondly, how High-pressure supercritical carbon dioxide is given
Enzyme in medium provides and is suitable for its chemical environment carrying out enzymic catalytic reaction and condition.Additionally, make on textile
Most conventional slurry be all polarity macromolecular compound, at textile fiber table before and after film forming, all
Cannot carry out expanding and and then dissolving removal in hydrophobic supercritical carbon dioxide fluid.Therefore, for a long time
Since, supercritical carbon dioxide fluid has obtained more research and application as dyeing medium, but at textile
Desizing pre-treatment in, the especially research of enzyme desizing and application in supercritical carbon dioxide fluid, from existing
Document sees that there is no people sets foot in.But, desizing pre-treatment is the important manufacturing procedure of textile production, traditional
Textile desizing pre-treatment then needs to consume substantial amounts of water, energy and chemicals, and produces a large amount of high-concentration waste water,
Protection of resources and ecological environment are caused serious threat.
Therefore, research and develop textile in supercritical carbon dioxide fluid medium, especially natural fabric carried out height
The method of effect desizing processing, to carrying out the dyeing and finishing process technologies such as textile anhydrous desizing pre-treatment, thoroughly real
The cleaning of existing textile printing and dyeing enterprises produces, and has very important significance and wide market prospect.
Summary of the invention
The purpose of the present invention is to propose to a kind of enzymolysis processing realized textile spreading mass, improve enzyme and face super
Desizing efficiency in boundary's CO 2 medium, the starch with supercritical carbon dioxide as medium of energy-conservation environmental protection again
Slurry desizing method.
For reaching this purpose, the present invention by the following technical solutions:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, including following
Step:
A, by appropriate table, activating agent diisooctyl succinate sodium sulfonate (AOT) is dissolved in the mixing of second alcohol and water
In solution;
B, appropriate desizing enzyme is added in described mixed solution, and stir and clarify to system, prepare desizing enzyme
Mixed liquor;
C, add buffer solution system, and regulate the pH value of described desizing enzyme mixation to 4-10 by sig water,
Obtain desizing working solution;
D, described desizing working solution is added in supercritical carbon dioxide fluid processing system, and utilize supercritical
CO 2 fluid forms microemulsion under certain condition, and pending textile is carried out desizing pre-treatment.
Further, in described step A, the volume ratio of second alcohol and water is 1: 4.
Further, in described step B, described desizing enzyme be cellulase, pectase, lipase,
A kind of or the compositions of its any ratio in α-amylase.
Further, described desizing enzyme be cellulase, pectase, lipase and α-amylase with
The compositions of 1: 1: 1: 1 ratio composition.
Further, in described step C, described buffer solution system is the slow of citric acid and salt preparation thereof
Dissolved liquid.
Further, in described step D, described certain condition includes the temperature of supercritical CO 2 medium
Degree is 30 DEG C-95 DEG C, and pressure is 6Mpa-30Mpa.
Further, in described step D, described certain condition also includes the circulation of CO 2 fluid
Being 0.5h-24.0h with static process total time, the time ratio of fluid circulation and static process is 1: 20-10:
1。
The invention have the benefit that
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, will be containing moving back
The desizing working solution of slurry enzyme is with citric acid and saline solution thereof as buffer system, and by sig water regulation system
PH value, after utilize hydrophobic supercritical CO 2 medium to be formed in situ microemulsion, microemulsion penetrates with fluid
While cotton products, discharge activity desizing enzyme, thus realize the desizing pre-treatment to cotton products spreading mass.
It is suitable for the buffer system of enzyme reaction and at supercritical carbon dioxide fluid owing to the technology of the present invention have employed
Under the conditions of form environmental condition and the method for microemulsion, improve enzyme moving back in supercritical CO 2 medium
Slurry efficiency, and equipment and technique are simply, easy to operate, desizing processes without at high temperature carrying out, it is to avoid
A large amount of water, heat and the application of high concentration alkali in tradition desizing, and there is efficient, energy-conservation, green, ring
The features such as guarantor.
Accompanying drawing explanation
Fig. 1 is the structural representation of the desizing device of the supercritical carbon dioxide fluid of the embodiment of the present invention one.
In figure: 1, desizing liquid stores still;11, fluid distributor;111, circulation of fluid inlet tube;112、
Circulation of fluid outlet;2, desizing still;21, textile wireline reel;3, desizing working solution;4, pending
Textile;5, circulation of fluid outlet;6, fluid flow guiding cover;7, filter;8, attachment means.
Detailed description of the invention
Down and in conjunction with the accompanying drawings and embodiments, the detailed description of the invention of the present invention is described in further detail.With
Lower embodiment is used for illustrating the present invention, but is not limited to the scope of the present invention.
Embodiment one
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, this enzyme desizing
Method uses the supercritical carbon dioxide fluid desizing device of structure as shown in Figure 1 to realize.This desizing device
Store still 1 including desizing liquid and store, with desizing liquid, the desizing still 2 that still 1 is tightly connected by attachment means 8.
It is cylindrical shape kettle that desizing liquid stores still 1, and desizing liquid is provided with inversion " mountain " type in storing still 1
Tubular fluid distributor 11, it is mainly made up of three pipelines being interconnected, and is positioned at the pipeline at center for following
The stream of supercritical carbon dioxide of ring fluid inlet tube 111, the bottom of circulation of fluid inlet tube 111 and band circulating pump
Body processing system (not shown) is connected;Two pipelines being positioned at both sides are circulation of fluid outlet 112,
The mouth of pipe of two circulation of fluid outlets 112 bends towards lower section, and the open at one end of lower section all stretches into desizing liquid storage
Deposit below the liquid level of desizing working solution 3 in still 1.The top of desizing still 2 is provided with circulation of fluid outlet 5,
Circulation of fluid outlet 5 is connected with supercritical carbon dioxide fluid processing system.
Desizing still 2 is cylindrical shape kettle too, be provided with in desizing still 2 fabric roll of inner hollow around
Axle 21, textile wireline reel 21 is wound with pending textile 4, and the bottom of textile wireline reel 21 is opened
Through hole is offered in mouth top closure, and its axle sidewall.The textile wireline reel 21 of close attachment means 8
Bottom is connected with tubaeform fluid flow guiding cover 6, and the lower section of fluid flow guiding cover 6 is provided with filter 7, it is possible to
Effectively filter the precipitated impurities contained in desizing working solution 3 and circulation of fluid mixed liquor.In the present embodiment,
Filter 7 is preferably covered with the single or multiple lift board-like material of 50-2000 mesh micropore.
The axle body of textile wireline reel 21 uses Teflon or non heat conductivity material to be made, or appearance in it
Face uses Teflon or non heat conductivity material to make, it is therefore prevented that textile wireline reel is because of the desizing work of uniform temperature
Make liquid and circulation of fluid mixed liquor flows through and produced the phenomenon of cause thermal damage, extend making of textile wireline reel
Use the life-span.
The top of desizing still 2 is provided with circulation of fluid outlet 5, and circulation of fluid outlet 5 is super with band circulating device
Critical carbon dioxide fluid handling system is connected.Desizing liquid stores still 1 and desizing still 2 by above-mentioned following
Ring fluid inlet tube 111 and circulation of fluid outlet 5 realize the company with supercritical carbon dioxide fluid processing system
Connect.
Add man-hour, desizing working solution 3 is added to desizing liquid and stores in still 1, two of fluid distributor 11
The mouth of pipe of circulation of fluid outlet 112 is placed in desizing working solution 3, and pending textile 4 is then in Song Shizhuan
State is entirely wound on textile wireline reel 21, and at the outermost layer set seamless net of last layer of winding up textile product
Shape infantees, is then placed in desizing still 2, and makes the opening of textile wireline reel 21 downwards and fluid
Kuppe 6 well connects.
The present embodiment provide a kind of starch slurry desizing method with supercritical carbon dioxide as medium, including with
Lower step:
A, by 0.6g surfactant diisooctyl succinate sodium sulfonate (AOT), to be dissolved in volume ratio be 1: 4
10mL ethanol and 40mL water mixed solution in.
B, by cellulase, pectase, lipase and α-amylase with 1: 1: 1: 1 mass ratio uniform
Mixing, and take appropriate mixed enzyme and be dissolved in above-mentioned mixed solution system, and stir and clarify to system, prepare
Desizing enzyme mixation;Wherein, the weight of pending textile 4 is 2g, and desizing enzyme is each 0.01g cellulose
The compositions of enzyme, pectase, lipase and α-amylase.
C, interpolation citric acid and the buffer solution system of salt preparation thereof, and mixed by sig water regulation desizing enzyme
The pH value of liquid, to 4.0, obtains desizing working solution 3, desizing working solution 3 is placed in desizing liquid and stores in still 1,
Being placed in desizing still 2 by the pending textile 4 being wound on textile wireline reel 21, desizing liquid stores still
1 and desizing still 2 be tightly connected formation desizing device, it is ensured that the open at one end of textile wireline reel 21 and desizing
Working solution 3 liquid level keeps the distance of 45cm, to prevent from carrying effect secretly because of the stirring of fluid distributor and fluid
Desizing working solution is made to occur directly to contact with textile.
D, desizing device is placed in the supercritical carbon dioxide fluid device of band circulating device, after closed system
Starting circulating device, under certain supercritical fluid conditions, desizing working solution forms microemulsion, spins pending
The slurry of fabric 4 carries out desizing pre-treatment.
Concrete, desizing device is exported 5 and band circulating pump through circulation of fluid inlet tube 111 and circulation of fluid
Supercritical carbon dioxide fluid processing system be connected, or desizing device is placed in the supercritical of band circulating pump
In CO 2 fluid processing means, again by predetermined desizing flow process and parameter (reaction after closed system
Temperature is 40 DEG C, and pressure is 13Mpa, and the desizing process time is 1h, uses fluid circulation and static process
Time ratio be 1: 10 pending textile 4 to be carried out desizing process), start external supercritical carbon dioxide
Circulating pump in fluid handling system, makes circulation of fluid pass through the tubular fluid distribution that desizing liquid stores in still 1
Device 11 mixes with desizing working solution 3 and is fully contacted, and forms microemulsion under the effect of surfactant, moves back
Slurry enzyme is transferred in entrance hydrophobic fluid, and and then flows in textile wireline reel 21, by through hole and volume
The pending textile 4 being wound on textile wireline reel 21 is had an effect, and completes desizing and processes.
This desizing method improves desizing enzyme to fiber spreading mass and the reactivity of impurity, improves textile
The desizing efficiency of slurry, effectively achieves and moves back textile slurry in supercritical carbon dioxide fluid medium
Slurry pre-treatment.
After desizing completes, fluid stops circulation, and supercritical carbon dioxide fluid processing system is carried out pressure release,
External separation and recovery system is utilized desizing working solution 3 and circulation of fluid to be separated and reclaims.Pressure release terminates
Rear unlatching attachment means 8, and take out the textile after enzyme desizing processes.Desizing liquid remains in storing still 1
Mixed solution may be recovered, or carries out continuous use after adding component.
Weight-loss ratio and the capillary effect value of the textile after processing desizing are tested, wherein weight-loss ratio and capillary effect value
Method of testing is as follows:
Weight-loss ratio is tested: desizing takes out cloth specimen after completing, and after cleaning 2-3 time with water, textile is placed in electricity
Hot blast drying baker bakes and banks up with earth 120min under conditions of temperature is 105 DEG C, seals sample with sealing bag,
Exsiccator balances more than 24h, its weight of weighing.Textile before desizing processes in an identical manner, logical
Cross the weight of textile before and after contrast desizing processes, obtain the weight-loss ratio of textile.
Capillary effect value is tested: with reference to textile industry standard FZ/T 01071-2008 textile capillary effect test side
Method is measured, and takes the fabric after desizing processes, and tests 15min on ZBW04019 type capillary effect tester.
Obtaining result after tested, the textile weight-loss ratio processed through desizing is 7.1%, and capillary effect value is 5.7cm.
Embodiment two:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is taken charge of mutually with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 5.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
7.8%, capillary effect value is 5.8cm.
Embodiment three:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is essentially identical with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 6.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
8.1%, capillary effect value is 6.2cm.
Embodiment four:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is essentially identical with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 7.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
8.3%, capillary effect value is 7.0cm.
Embodiment five:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is essentially identical with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 8.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
8.7%, capillary effect value is 7.2cm.
Embodiment six:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is taken charge of mutually with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 9.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
8.0%, capillary effect value is 5.9cm.
Embodiment seven:
The invention provides a kind of starch slurry desizing method with supercritical carbon dioxide as medium, its enzyme desizing
Method is essentially identical with the desizing method described in embodiment one, does not repeats them here.
It is in place of difference: the pH value of the present embodiment desizing working solution is 10.0.
Weight-loss ratio and the capillary effect value test result of the textile that the present embodiment processes through desizing be: weight-loss ratio is
7.4%, capillary effect value is 4.9cm.
The relation table of the pH value of the weight-loss ratio of table 1 textile and capillary effect value and desizing working solution
By embodiment one to embodiment seven and table 1 it can be seen that general enzyme reaction is the most sensitive to pH value,
After optimum pH scope, enzyme the most easily shows as activity decrease, even inactivates.But, supercritical titanium dioxide
Carbon fluid and the application of microemulsion, to a certain extent can be with protective enzyme not easy in inactivation, and therefore the present invention is relatively
In wide pH scope (4-10), this desizing method all has preferable desizing effect, has in actual production
Well adapting to property and application.
In desizing working solution of the present invention, the volume ratio of ethanol and water mixed solution can be controlled in 1: the scope of 2-1: 5.
It addition, the reaction temperature processed by conservative control desizing is the scope of 30 DEG C-95 DEG C, pressure exists
The scope of 6Mpa-30Mpa, desizing processes the time scope at 0.5h-24.0h, and stream of supercritical carbon dioxide
The time ratio of body circulation and static process is 1: the scope of 20-10: 1, the desizing of textile can be processed effect
Fruit is cooked optimization further.
The method that the present invention provides is to textile, the especially stream of supercritical carbon dioxide of starch starching cotton products
Body anhydrous enzyme desizing processing has preferable practicality, little to cloth damage, reaction gentleness, it is not necessary at high temperature
Carry out, it is to avoid a large amount of water, heat and the application of high concentration alkali, supercritical process during department in traditional desizing
Easily controllable and carry out, and there is the features such as efficient, green, environmental protection, thus application prospect is the most wide.
The know-why of the present invention is described above in association with specific embodiment.These describe and are intended merely to explain this
The principle of invention, and limiting the scope of the invention can not be construed to by any way.Based on herein
Explaining, those skilled in the art need not pay performing creative labour can associate other tool of the present invention
Body embodiment, within these modes fall within protection scope of the present invention.
Claims (2)
1. the starch slurry desizing method with supercritical carbon dioxide as medium, it is characterised in that: include with
Lower step:
A, proper amount of surfactant diisooctyl succinate sodium sulfonate (AOT) is dissolved in the mixing of second alcohol and water
In solution, the volume ratio of second alcohol and water is 1:4;
B, the combination that cellulase, pectase, lipase, α-amylase are formed with 1:1:1:1 ratio
Thing adds in described mixed solution, and stirs to system clarification, prepares desizing enzyme mixation;
C, interpolation buffer solution system, and regulate the pH value of described desizing enzyme mixation extremely by sig water
4-10, obtains desizing working solution;
D, described desizing working solution is added in supercritical carbon dioxide fluid processing system, and utilize supercritical
CO 2 fluid temperature be 30 DEG C-95 DEG C, pressure be the circulation of 6MPa-30MPa, CO 2 fluid
With static process total time be 0.5h-24.0h, the time ratio of fluid circulation and static process is for 1:20-10:
Form microemulsion under conditions of 1, pending textile is carried out desizing pre-treatment.
Starch slurry desizing method with supercritical carbon dioxide as medium the most according to claim 1, its
Being characterised by: in described step C, described buffer solution system is that the buffering of citric acid and salt preparation thereof is molten
Liquid.
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CN104631134A (en) * | 2015-02-09 | 2015-05-20 | 苏州陈恒织造有限公司 | Method for preparing viscose fiber fabric by carbon dioxide desizing process |
CN104674431A (en) * | 2015-03-19 | 2015-06-03 | 苏州陈恒织造有限公司 | Manufacturing method for carbon dioxide desized mucilage glue/copper ammonia fiber blended yarn weaved fabric |
CN105651719B (en) * | 2016-01-21 | 2018-08-21 | 苏州大学 | A kind for the treatment of with supercritical fluid method improving pectinase activity and stability |
CN105568591B (en) * | 2016-01-25 | 2017-10-13 | 苏州大学 | The hydrogen peroxide desizing pretreatment process of cotton in a kind of supercritical carbon dioxide fluid |
CN106843308A (en) * | 2017-04-21 | 2017-06-13 | 安庆华茂佰斯特纺织科技有限公司 | Impregnator pH value device for automatically regulating |
CN106996034A (en) * | 2017-05-22 | 2017-08-01 | 苏州凯邦生物技术有限公司 | A kind of cotton desizing method based on supercritical carbon dioxide with alkaline biology enzyme |
CN110747625A (en) * | 2019-11-01 | 2020-02-04 | 苏州大学 | Method for cleaning animal fiber by using supercritical fluid |
CN113550137B (en) * | 2021-07-12 | 2022-04-22 | 武汉纺织大学 | Method for preparing non-woven fabric through multi-effect composite bleaching |
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CN1587491A (en) * | 2004-10-12 | 2005-03-02 | 成都纺织高等专科学校 | Method for treating ramie fabric by super critical CO2 fluid |
WO2006065579A2 (en) * | 2004-12-02 | 2006-06-22 | Novozymes North America, Inc. | Desizing process |
CN1718912A (en) * | 2005-07-14 | 2006-01-11 | 沙洲职业工学院 | Immersion method bioenzyme pretreatment technology of hemp and its cospinned fabric |
CN1955346A (en) * | 2005-10-24 | 2007-05-02 | 中国农业科学院麻类研究所 | Method for extracting ramie from supercritical CO2 media by enzyme method |
CN103255609B (en) * | 2013-06-08 | 2015-06-17 | 武汉纺织大学 | Pretreatment method of cotton fabric |
CN104018336B (en) * | 2014-06-25 | 2016-01-20 | 江苏联发纺织股份有限公司 | A kind of desizing method of textile yarn-dyed fabric |
CN104018337B (en) * | 2014-06-25 | 2015-12-02 | 江苏联发纺织股份有限公司 | With the desizing method of the textile yarn-dyed fabric of starch and the starching of PVA mixed slurry |
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