CN104372598B - Supercritical carbon dioxide fluid desizing method by use of combined enzyme - Google Patents
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Abstract
The invention discloses a supercritical carbon dioxide fluid desizing method by use of combined enzyme, which belongs to the technical field of dyeing and finishing processing of the textiles, and is designed for solving the serious problem of ecological environment caused by the traditional desizing process. The enzyme desizing method comprises the following steps: A. dissolving appropriate amount of bis(2-ethylhexyl)sulfosuccinate sodium salt into mixed solution of ethyl alcohol and water according to volume ratio of 1:2-1:5; B. mixing cellulase, pectinase, lipase and alpha-amylase according to mass ratio of 1:1-1:10 of each two enzymes, and dissolving appropriate amount of mixed enzyme into a mixed solution system to prepare desizing working solution; C. arranging the desizing working solution into a desizing device, and arranging the desizing device into a supercritical carbon dioxide fluid treatment system; and D. carrying out enzymolysis on the textile slurry by the desizing working solution under certain conditions. According to the supercritical carbon dioxide fluid desizing method, the sizing slurry of the textiles is subjected to enzymolysis, the enzyme desizing efficiency of the textiles is high, energy-saving and environment-friendly effects are realized, and the optimization of the combined enzyme desizing process can be realized.
Description
Technical field
The invention belongs to textile dyeing and finishing processing technique field, particularly relate to a kind of supercritical two using combination enzyme
Carbon oxide fluid desizing method.
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, before and after textile fiber surface filming, 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 easy to operate, it is achieved the enzymolysis processing to textile spreading mass, energy-conservation
Environmental protection, it is achieved the supercritical carbon dioxide fluid desizing of the optimized employing combination enzyme of combination enzyme desizing technique
Method.
For reaching this purpose, the present invention by the following technical solutions:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, including following
Step:
A, proper amount of surfactant diisooctyl succinate sodium sulfonate (AOT) is dissolved in volume ratio is 1:2-1:5
Second alcohol and water mixed solution in;
B, by cellulase, pectase, lipase and α-amylase with between every two kinds of enzymes according to 1:1-1:
The mass ratio of 10 uniformly mixes, and takes appropriate mixed enzyme and be dissolved in described mixed solution system, and stirs extremely
System is clarified, and prepares desizing working solution;
C, the desizing liquid that described desizing working solution is placed in desizing device store in still, and by described desizing device
It is placed in the supercritical carbon dioxide fluid processing system of band circulating device;
Described circulating device is started after D, closed system, under certain supercritical fluid conditions, described desizing work
Make liquid and the slurry of pending textile is carried out enzymolysis processing.
Further, in described step A, the concentration of diisooctyl succinate sodium sulfonate (AOT) is
2.5g/L-25g/L。
Further, in described step A, the quality of diisooctyl succinate sodium sulfonate (AOT) is 0.6g.
Further, in described step B, the matter of cellulase, pectase, lipase and α-amylase
Amount ratio is 1:1:1:1 or 1:2:2:2 or 1:3:3:3 or 2:1:3:2 or 2:2:1:3
Or 2:3:2:1 or 3:1:2:3 or 3:2:3:1 or 3:3:1:2.
Further, in described step C, described desizing working solution is 3 with the volume ratio of circulation of fluid:
100-1∶5。
Further, in described step D, described certain supercritical fluid conditions be reaction temperature be 30 DEG C
-95 DEG C, pressure is 6MPa-30MPa, and the desizing process time is 0.5h-24.0h, uses stream in course of reaction
The time ratio of body circulation and static process is for 1:20-10:1.
The invention have the benefit that
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, will be containing fine
The desizing working solution of the combination desizing enzyme of dimension element enzyme, pectase, lipase and α-amylase composition utilizes hydrophobic
Property supercritical CO 2 medium is formed in situ microemulsion, while microemulsion penetrates cotton products with fluid, releases
Release activity desizing enzyme, it is achieved degradation treatment to textile slurry in supercritical CO 2 medium, should
Enzyme desizing method is easy to operate, improves textile enzyme desizing efficiency in supercritical carbon dioxide fluid,
Reaction gentleness, little to cloth damage, it is not necessary at high temperature to carry out, it is to avoid a large amount of water in traditional desizing,
Heat and the application of high concentration alkali, have the features such as efficient, green, environmental protection.
It addition, by changing the proportioning of each component in combination desizing enzyme, it is achieved that combination enzyme desizing technique is
Optimize.
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
Below in conjunction with the accompanying drawings and embodiment, 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 supercritical carbon dioxide fluid desizing method using combination enzyme, 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 use combination enzyme supercritical carbon dioxide fluid desizing method, 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, i.e. the concentration of diisooctyl succinate sodium sulfonate (AOT)
For 12g/L.
B, cellulase, pectase, lipase and α-amylase is uniform with the mass ratio of 1:1:1:1
Mixing, and take appropriate mixed enzyme and be dissolved in above-mentioned mixed solution system, and stir and clarify to system, prepare
Desizing working solution;Wherein, the weight of pending textile 4 is 2g, desizing enzyme be each 0.01g cellulase,
The compositions of pectase, lipase and α-amylase.
C, desizing working solution 3 is placed in desizing liquid stores in still 1, will be wound on textile wireline reel 21
Pending textile 4 be placed in desizing still 2, desizing liquid stores still 1 and desizing still 2 and is tightly connected formation
Desizing device, it is ensured that the open at one end of textile wireline reel 21 keeps 45cm's with desizing working solution 3 liquid level
Distance, to prevent because the stirring of fluid distributor and the effect of carrying secretly of fluid make desizing working solution send out with textile
Raw directly contact;And desizing device is placed in the supercritical carbon dioxide fluid device of band circulating device.
Starting circulating device after D, closed system, under certain supercritical fluid conditions, desizing working solution treats place
The slurry of reason textile 4 carries out enzymolysis processing.
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 than for 1:10, pending textile 4 is 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 the fall to textile slurry in supercritical carbon dioxide fluid medium
Solution processes.
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 6.3%, and capillary effect value is 4.6cm.
Embodiment two:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.01g, pectase is 0.02g, fat
Fat enzyme is 0.02g, and α-amylase is 0.02g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 1:2:2:2.
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
6.6%, capillary effect value is 4.9cm.
Embodiment three:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.01g, pectase is 0.03g, fat
Fat enzyme is 0.03g, and α-amylase is 0.03g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 1:3:3:3.
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
7.6%, capillary effect value is 6.4cm.
Embodiment four:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.02g, pectase is 0.01g, fat
Fat enzyme is 0.03g, and α-amylase is 0.02g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 2:1:3:2.
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
7.2%, capillary effect value is 6.1cm.
Embodiment five:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.02g, pectase is 0.03g, fat
Fat enzyme is 0.02g, and α-amylase is 0.01g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 2:3:2:1.
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
7.1%, capillary effect value is 5.8cm.
Embodiment six:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.03g, pectase is 0.01g, fat
Fat enzyme is 0.02g, and α-amylase is 0.03g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 3:1:2:3.
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
9.1%, capillary effect value is 7.1cm.
Embodiment seven:
The invention provides a kind of supercritical carbon dioxide fluid desizing method using combination enzyme, 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 present embodiment desizing enzyme cellulase is 0.03g, pectase is 0.03g, fat
Fat enzyme is 0.01g, and α-amylase is 0.02g, i.e. cellulase, pectase, lipase and α-amylase
Mass ratio be 3:3:1:2.
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
8.4%, capillary effect value is 6.6cm.
Combination enzyme as shown in table 1 is obtained to desizing effect by embodiment one to embodiment seven and other experiment
Orthogonal test, the quality being index evaluation desizing effect with weight-loss ratio, as can be seen from Table 1, desizing enzyme
In the number of various component enzymes consumptions, directly affects the quality of textile desizing effect.Various component enzymes
Extreme difference R size order is: R (cellulase) > R (α-amylase) > R (lipase) > R (pectin
Enzyme), secondary factors is cellulase, α-amylase, lipase, pectase.Wherein, cellulase master
Will be to the cellulose on textile and hemicellulose generation effect;α-amylase primarily serves and carries out starch slurry
The effect of hydrolysis, for the cotton products of textile, α-amylase is most important enzyme in desizing;
Pectase can break ring textile constructions makes more cellulose and starch come out, and is the water of other enzymes
Solving and provide more binding site, lipase can improve hydrophilic with the waxiness on hydrolysis fiber surface.To sum up
Described, cellulase serves the effect of the most key property to the desizing effect of textile.Move back by changing combination
The proportioning of each component in slurry enzyme, it is achieved that the optimization of combination enzyme desizing technique.
Table 1 combines the impact on desizing effect of the enzyme each component
In desizing working solution of the present invention, the volume ratio of ethanol and water mixed solution can be controlled in the scope of 1:2-1:5,
Desizing enzyme relative to pending textile Weight control in the scope of 0.1%-20%.Succinic acid di-isooctyl sulfonic acid
The concentration of sodium (AOT) can be controlled in the scope of 2.5g/L-25g/L.It addition, by conservative control desizing
The reaction temperature of reason processes the time at the scope of 30 DEG C-95 DEG C, pressure in the scope of 6MPa-30MPa, desizing
In the scope of 0.5h-24.0h, the desizing treatment effect of textile can be done optimization further.
The present invention provide use combination enzyme supercritical carbon dioxide fluid desizing method to textile, especially
Starch starching textile has preferable practicality, little to cloth damage, reaction gentleness, it is not necessary at high temperature enter
OK, it is to avoid a large amount of water, heat and the application of high concentration alkali in traditional desizing, supercritical process is easy simultaneously
In controlling and carrying 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 (6)
1. one kind use combination enzyme supercritical carbon dioxide fluid desizing method, it is characterised in that: include with
Lower step:
A, proper amount of surfactant diisooctyl succinate sodium sulfonate (AOT) is dissolved in volume ratio is 1:2-1:5
Second alcohol and water mixed solution in;
B, by cellulase, pectase, lipase and α-amylase with between every two kinds of enzymes according to 1:1-1:
The mass ratio of 10 uniformly mixes, and takes appropriate mixed enzyme and be dissolved in described mixed solution system, and stirs extremely
System is clarified, and prepares desizing working solution;
C, the desizing liquid that described desizing working solution is placed in desizing device store in still, and by described desizing device
It is placed in the supercritical carbon dioxide fluid processing system of band circulating device;
Described circulating device is started after D, closed system, under certain supercritical fluid conditions, described desizing work
Make liquid and the slurry of pending textile is carried out enzymolysis processing.
The supercritical carbon dioxide fluid desizing method using combination enzyme the most according to claim 1, its
Being characterised by: in described step A, the concentration of diisooctyl succinate sodium sulfonate (AOT) is
2.5g/L-25g/L。
The supercritical carbon dioxide fluid desizing method using combination enzyme the most according to claim 1, its
Being characterised by: in described step A, the quality of diisooctyl succinate sodium sulfonate (AOT) is 0.6g.
The supercritical carbon dioxide fluid desizing method using combination enzyme the most according to claim 1, its
It is characterised by: in described step B, the mass ratio of cellulase, pectase, lipase and α-amylase
For 1:1:1:1 or 1:2:2:2 or 1:3:3:3 or 2:1:3:2 or 2:2:1:3 or 2:
3:2:1 or 3:1:2:3 or 3:2:3:1 or 3:3:1:2.
The supercritical carbon dioxide fluid desizing method using combination enzyme the most according to claim 1, its
Being characterised by: in described step C, described desizing working solution is 3 with the volume ratio of circulation of fluid:
100-1∶5。
The supercritical carbon dioxide fluid desizing method using combination enzyme the most according to claim 1, its
Be characterised by: in described step D, described certain supercritical fluid conditions be reaction temperature be 30 DEG C-95 DEG C,
Pressure is 6MPa-30MPa, desizing process the time be 0.5h-24.0h, in course of reaction use fluid circulation and
The time of static process is than for 1:20-10:1.
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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 |
CN106978713A (en) * | 2017-05-22 | 2017-07-25 | 苏州凯邦生物技术有限公司 | A kind of desizing agent and its preparation and application for viscose glue sill matter carbon fiber |
CN110747625A (en) * | 2019-11-01 | 2020-02-04 | 苏州大学 | Method for cleaning animal fiber by using supercritical fluid |
CN113529401B (en) * | 2021-07-12 | 2022-06-24 | 武汉纺织大学 | Green and pollution-free cold-batch method for pure cotton spunlace non-woven fabric |
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