CN104313891A - Starch slurry desizing method adopting supercritical carbon dioxide as medium - Google Patents
Starch slurry desizing method adopting supercritical carbon dioxide as medium Download PDFInfo
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Abstract
The invention discloses a starch slurry desizing method adopting supercritical carbon dioxide as a medium, which belongs to the technical field of textile dyeing processing, and solves the problem that the traditional desizing process is great in energy consumption and not environment-friendly. The desizing method comprises the following steps: A, dissolving succinic dioctyl sebacate sodium sulfonate in an ethanol and water mixed solution; B, adding desizing enzyme into the mixed solution, and stirring the mixed solution until the system is clear to obtain a desizing enzyme mixed solution; C, adding a buffer solution system, adjusting the pH value of the desizing enzyme mixed solution to 4 to 10 by virtue of a dilute alkaline solution to obtain a desizing working solution; and D, adding the desizing working solution into a supercritical carbon dioxide fluid processing system, and carrying out enzymatic treatment on the textile under a given condition. By adopting the method, the enzymatic treatment on the textile is realized; by adopting the buffer system applicable to the enzymatic reaction and environmental condition and method for forming a micro-emulsion under the supercritical carbon dioxide fluid condition, the desizing efficiency of the enzyme in the supercritical carbon dioxide medium is improved, and energy conservation and environmental protection can be realized.
Description
Technical field
The invention belongs to textile dyeing and finishing processing technique field, particularly relating to a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium.
Background technology
Supercritical carbon dioxide fluid enzyme desizing technology, has the feature of the cleanly production such as significant ecology, environmental protection and energy-saving and emission-reduction, significant to the present situation such as high pollution, high energy consumption changing traditional textile pre-treatment processing.At present, biology enzyme has broad application prospects in dyeing and finishing processing, because enzyme preparation is as a kind of biologic product, nontoxic, its Application and Development has complied with the requirement of green processing and sustainable development.Wherein the application of destarch enzyme is comparatively ripe and extensively, more and more accept by colourist, and be applied to the impurity such as the starch slurry removed on fabric.Wherein there is synergy during some enzyme conbined usage, such as, the epidermal area of pectase degraded substrate, can be cellulase and produces more multiaction site; And the degradation of cellulase can make the pectic substance in more multilist cortex expose, and with pectase effect.
But the enzyme desizing of textiles in supercritical carbon dioxide fluid, but wants complicated and much more difficult relatively.Its difficult point is how to make the high molecular protein compound-enzyme of polarity, enters in hydrophobic High-pressure supercritical CO 2 fluid medium, and can keep its greater activity.Secondly, applicable its is provided to carry out chemical environment and the condition of enzymic catalytic reaction how to the enzyme in High-pressure supercritical CO 2 medium.In addition, the most conventional slurry that textiles uses is all polarity macromolecular compound, at textile fiber table before and after film forming, all cannot carry out expansion and and then dissolve removal in hydrophobic supercritical carbon dioxide fluid.Therefore, for a long time, supercritical carbon dioxide fluid obtains more investigation and application as dyeing medium, but in the destarch pre-treatment of textiles, the investigation and application of especially enzyme desizing in supercritical carbon dioxide fluid, there is no people and set foot in viewed from existing document.But destarch pre-treatment is the important manufacturing procedure of textile production, traditional textiles destarch pre-treatment then needs to consume a large amount of water, energy and chemicals, and produces a large amount of high-concentration waste water, causes serious threat to protection of resources and ecological environment.
Therefore, research and develop textiles in supercritical carbon dioxide fluid medium, especially natural fabric carried out to the method for efficient destarch processing, to dyeing and finishing process technologies such as the anhydrous destarch pre-treatments of implementation textiles, thoroughly realize the cleaner production of textile printing and dyeing enterprises, have very important significance and wide market prospects.
Summary of the invention
The object of the invention is to propose a kind of enzymolysis processing realized textiles spreading mass, improve the destarch efficiency of enzyme in supercritical CO 2 medium, energy-conservation environmental protection again take supercritical carbon dioxide as the starch slurry desizing method of medium.
For reaching this object, the present invention by the following technical solutions:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, comprises the following steps:
A, will to show in right amount and activating agent succinate sodium 2-ethylhexyl (AOT) is dissolved in the mixed solution of second alcohol and water;
B, appropriate destarch enzyme to be added in described mixed solution, and be stirred to system clarification, obtained destarch enzyme mixation;
C, interpolation buffer solution system, and regulate the pH value of described destarch enzyme mixation to 4-10 by sig water, obtain destarch working solution;
D, described destarch working solution to be added in supercritical carbon dioxide fluid treatment system, and utilize supercritical carbon dioxide fluid to form microemulsion under certain condition, destarch pre-treatment is carried out to pending textiles.
Further, in described steps A, the volume ratio of second alcohol and water is 1: 4.
Further, in described step B, described destarch enzyme is the composition of a kind of or its any ratio in cellulase, pectase, lipase, α-amylase.
Further, described destarch enzyme is the composition that cellulase, pectase, lipase and α-amylase form with 1: 1: 1: 1 ratio.
Further, in described step C, described buffer solution system is the cushioning liquid of citric acid and salt preparation thereof.
Further, in described step D, the temperature that described certain condition comprises supercritical CO 2 medium is 30 DEG C-95 DEG C, and pressure is 6Mpa-30Mpa.
Further, in described step D, described certain condition also comprises the circulation of CO 2 fluid and static process total time is 0.5h-24.0h, and the time ratio of fluid circulation and static process is 1: 20-10: 1.
Beneficial effect of the present invention is:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, by the destarch working solution containing destarch enzyme with citric acid and salting liquid thereof for buffer system, and pass through the pH value of sig water regulation system, after utilize hydrophobic supercritical CO 2 medium original position formed microemulsion, while microemulsion penetrates cotton products with fluid, discharge active destarch enzyme, thus realize the destarch pre-treatment to cotton products spreading mass.
Because the technology of the present invention have employed the buffer system being suitable for enzyme reaction and the environmental condition forming microemulsion under supercritical carbon dioxide fluid condition and method, improve the destarch efficiency of enzyme in supercritical CO 2 medium, and instrument and supplies is simple, easy to operate, destarch process is without the need at high temperature carrying out, avoid large water gaging in traditional desizing, heat and the application of high concentration alkali, and there is the features such as efficient, energy-conservation, green, environmental protection.
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, destarch still; 21, textiles wireline reel; 3, destarch working solution; 4, pending textiles; 5, circulation of fluid outlet; 6, fluid flow guiding cover; 7, filter; 8, jockey.
Detailed description of the invention
In conjunction with the accompanying drawings and embodiments, the specific embodiment of the present invention is described in further detail down.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment one
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and this enzyme desizing method adopts the supercritical carbon dioxide fluid desizing device of structure as shown in Figure 1 to realize.This desizing device comprises desizing liquid and stores still 1 and store by jockey 8 and desizing liquid the destarch still 2 that still 1 is tightly connected.
It is cylindrical shape kettle that desizing liquid stores still 1, desizing liquid stores the tubular fluid distributor 11 being provided with inversion " mountain " type in still 1, it is primarily of three the pipeline compositions be interconnected, the pipeline being positioned at center is circulation of fluid inlet tube 111, and the bottom of circulation of fluid inlet tube 111 is connected with the supercritical carbon dioxide fluid treatment system (not shown) of band circulating pump; Two pipelines being positioned at both sides are that the mouth of pipe of circulation of fluid outlet 112, two circulation of fluid outlets 112 bends towards below, and the open at one end of below all stretches into desizing liquid stores below the liquid level of the destarch working solution 3 in still 1.The top of destarch still 2 is provided with circulation of fluid outlet 5, and circulation of fluid outlet 5 is connected with supercritical carbon dioxide fluid treatment system.
Destarch still 2 is cylindrical shape kettle too, is provided with the textiles wireline reel 21 of inner hollow in destarch still 2, textiles wireline reel 21 is wound with pending textiles 4, the bottom end opening top closure of textiles wireline reel 21, and its axle sidewall offers through hole.Be connected with tubaeform fluid flow guiding cover 6 near the bottom of the textiles wireline reel 21 of jockey 8, the below of fluid flow guiding cover 6 is provided with filter 7, effectively can filter the precipitated impurities contained in destarch 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 order micropore.
The axle body of textiles wireline reel 21 adopts Teflon or non heat conductivity material to be made, or its surfaces externally and internally adopts Teflon or non heat conductivity material to make, prevent textiles wireline reel to flow through because of the destarch working solution of uniform temperature and circulation of fluid mixed liquor and produced the phenomenon of cause thermal damage, extend the service life of textiles wireline reel.
The top of destarch still 2 is provided with circulation of fluid outlet 5, and circulation of fluid outlet 5 is connected with the supercritical carbon dioxide fluid treatment system of band circulating device.Desizing liquid stores still 1 and destarch still 2 realizes the connection with supercritical carbon dioxide fluid treatment system by above-mentioned circulation of fluid inlet tube 111 and circulation of fluid outlet 5.
Add man-hour, destarch working solution 3 being added to desizing liquid stores in still 1, the mouth of pipe of two circulation of fluid outlets 112 of fluid distributor 11 is placed in destarch working solution 3, pending textiles 4 is entirely wound on textiles wireline reel 21 in loose formula state, and overlap the seamless netted infantees of last layer at the outermost layer of winding up textile product, then be placed in destarch still 2, and the openend of textiles wireline reel 21 is well communicated with fluid flow guiding cover 6 downwards.
The present embodiment provide a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, comprise the following steps:
A, by 0.6g surfactant succinate sodium 2-ethylhexyl (AOT), 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 quality than Homogeneous phase mixing, and get appropriate mixed enzyme and be dissolved in above-mentioned mixed solution system, and be stirred to system clarification, obtained destarch enzyme mixation; Wherein, the weight of pending textiles 4 is 2g, and destarch enzyme is the composition of each 0.01g cellulase, pectase, lipase and α-amylase.
C, add the buffer solution system of citric acid and salt preparation thereof, and the pH value to 4.0 of destarch enzyme mixation is regulated by sig water, obtain destarch working solution 3, destarch working solution 3 being placed in desizing liquid stores in still 1, the pending textiles 4 be wound on textiles wireline reel 21 is placed in destarch still 2, desizing liquid stores still 1 and destarch still 2 and to be tightly connected formation desizing device, the open at one end of guarantee textiles wireline reel 21 and destarch working solution 3 liquid level keep the distance of 45cm, to prevent because the stirring of fluid distributor and the effect of carrying secretly of fluid make destarch working solution and textiles occur directly to contact.
D, desizing device is placed in the supercritical carbon dioxide fluid device of band circulating device, start circulating device after closed system, under certain supercritical fluid conditions, destarch working solution forms microemulsion, carries out destarch pre-treatment to the slurry of pending textiles 4.
Concrete, desizing device is connected with the supercritical carbon dioxide fluid treatment system of circulation of fluid outlet 5 with band circulating pump through circulation of fluid inlet tube 111, or desizing device is placed in the supercritical carbon dioxide fluid treating apparatus of band circulating pump, after closed system, by predetermined desizing flow process and parameter, (reaction temperature is 40 DEG C again, pressure is 13Mpa, and the destarch processing time is 1h, fluid circulation and the time ratio of static process is adopted to be to pending textiles 4 carry out destarch process at 1: 10), start the circulating pump in external supercritical carbon dioxide fluid treatment system, make circulation of fluid store tubular fluid distributor 11 in still 1 by desizing liquid to mix with destarch working solution 3 and fully contact, and microemulsion is formed under the effect of surfactant, destarch enzyme is transferred and enters in hydrophobic fluid, and and then flow in textiles wireline reel 21, had an effect by through hole and the pending textiles 4 be wound on textiles wireline reel 21, complete destarch process.
This desizing method improves the reactivity of destarch enzyme to fiber spreading mass and impurity, improves the destarch efficiency of textiles slurry, effectively achieves the destarch pre-treatment to textiles slurry in supercritical carbon dioxide fluid medium.
After destarch completes, fluid stops circulation, and carries out pressure release to supercritical carbon dioxide fluid treatment system, utilizes external separation and recovery system carry out being separated to destarch working solution 3 and circulation of fluid and reclaim.Pressure release terminates rear unlatching jockey 8, and takes out the textiles after enzyme desizing process.Desizing liquid stores mixed solution residual in still 1 and can reclaim, or after adding component, carry out continuous using.
The weight-loss ratio of the textiles after destarch process and capillary effect value are tested, wherein weight-loss ratio and capillary effect value method of testing as follows:
Weight-loss ratio is tested: taking-up cloth specimen after destarch completes, and after water cleaning 2-3 time, textiles being placed in electric drying oven with forced convection is bake and bank up with earth 120min under the condition of 105 DEG C in temperature, uses sealing bag seal sample, in drier, balances more than 24h, its weight of weighing.Textiles before destarch processes in an identical manner, by the weight of textiles before and after contrast destarch process, obtains the weight-loss ratio of textiles.
Capillary effect value is tested: measure with reference to textile industry standard FZ/T 01071-2008 textiles capillary effect test method, get the fabric after destarch process, 15min tested by ZBW04019 type capillary effect tester.
Obtain result after tested, the textiles weight-loss ratio through destarch process is 7.1%, and capillary effect value is 5.7cm.
Embodiment two:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is taken charge of substantially mutually with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 5.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 7.8%, and capillary effect value is 5.8cm.
Embodiment three:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is substantially identical with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 6.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 8.1%, and capillary effect value is 6.2cm.
Embodiment four:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is substantially identical with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 7.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 8.3%, and capillary effect value is 7.0cm.
Embodiment five:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is substantially identical with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 8.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 8.7%, and capillary effect value is 7.2cm.
Embodiment six:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is taken charge of substantially mutually with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 9.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 8.0%, and capillary effect value is 5.9cm.
Embodiment seven:
The invention provides a kind of take supercritical carbon dioxide as the starch slurry desizing method of medium, and its enzyme desizing method is substantially identical with the desizing method described in embodiment one, does not repeat them here.
Difference part is: the pH value of the present embodiment destarch working solution is 10.0.
The present embodiment through the weight-loss ratio of the textiles of destarch process and capillary effect value test result is: weight-loss ratio is 7.4%, and capillary effect value is 4.9cm.
The relation table of the weight-loss ratio of table 1 textiles and the pH value of capillary effect value and destarch working solution
Can be found out by embodiment one to embodiment seven and table 1, general enzyme reaction is all comparatively responsive to pH value, and after exceeding optimal pH scope, enzyme all easily shows as activity decrease, even inactivation.But; the application of supercritical carbon dioxide fluid and microemulsion, to a certain extent can protective enzyme not easy in inactivation, and therefore the present invention is in wider pH scope (4-10); this desizing method all has good destarch effect, has good adaptability and application in actual production.
In destarch 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.In addition, by the reaction temperature of the conservative control destarch process scope at 30 DEG C-95 DEG C, pressure is in the scope of 6Mpa-30Mpa, the destarch processing time is in the scope of 0.5h-24.0h, and the time ratio of supercritical carbon dioxide fluid circulation and static process is in the scope of 1: 20-10: 1, can do further optimization to the destarch treatment effect of textiles.
Method provided by the invention is to textiles, especially the supercritical carbon dioxide fluid of starch starching cotton products anhydrous enzyme desizing processing has good practicality, little to cloth damage, reaction temperature and, without the need at high temperature carrying out, avoid large water gaging in traditional desizing, the application of heat and high concentration alkali, during department, supercritical process is easy to control and carry out, and has the features such as efficient, green, environmental protection, and thus application prospect is very wide.
Below know-why of the present invention is described in conjunction with specific embodiments.These describe just in order to explain principle of the present invention, and can not be interpreted as limiting the scope of the invention by any way.Based on explanation herein, those skilled in the art does not need to pay performing creative labour can associate other detailed description of the invention of the present invention, and these modes all will fall within protection scope of the present invention.
Claims (7)
1. be a starch slurry desizing method for medium with supercritical carbon dioxide, it is characterized in that: comprise the following steps:
A, proper amount of surfactant succinate sodium 2-ethylhexyl (AOT) is dissolved in the mixed solution of second alcohol and water;
B, appropriate destarch enzyme to be added in described mixed solution, and be stirred to system clarification, obtained destarch enzyme mixation;
C, interpolation buffer solution system, and regulate the pH value of described destarch enzyme mixation to 4-10 by sig water, obtain destarch working solution;
D, described destarch working solution to be added in supercritical carbon dioxide fluid treatment system, and utilize supercritical carbon dioxide fluid to form microemulsion under certain condition, destarch pre-treatment is carried out to pending textiles.
2. according to claim 1 take supercritical carbon dioxide as the starch slurry desizing method of medium, and it is characterized in that: in described steps A, the volume ratio of second alcohol and water is 1: 4.
3. according to claim 1 take supercritical carbon dioxide as the starch slurry desizing method of medium, it is characterized in that: in described step B, described destarch enzyme is the composition of a kind of or its any ratio in cellulase, pectase, lipase, α-amylase.
4. according to claim 3 take supercritical carbon dioxide as the starch slurry desizing method of medium, it is characterized in that: described destarch enzyme is the composition that cellulase, pectase, lipase and α-amylase form with 1: 1: 1: 1 ratio.
5. according to claim 1 take supercritical carbon dioxide as the starch slurry desizing method of medium, it is characterized in that: in described step C, and described buffer solution system is the cushioning liquid of citric acid and salt preparation thereof.
6. according to claim 1 take supercritical carbon dioxide as the starch slurry desizing method of medium, and it is characterized in that: in described step D, the temperature that described certain condition comprises supercritical CO 2 medium is 30 DEG C-95 DEG C, and pressure is 6Mpa-30Mpa.
7. according to claim 6 take supercritical carbon dioxide as the starch slurry desizing method of medium, it is characterized in that: in described step D, described certain condition also comprises the circulation of CO 2 fluid and static process total time is 0.5h-24.0h, and the time ratio of fluid circulation and static process is 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 |
| CN105568591A (en) * | 2016-01-25 | 2016-05-11 | 苏州大学 | Hydrogen peroxide desizing pretreatment method for cotton in supercritical carbon dioxide fluid |
| CN105651719A (en) * | 2016-01-21 | 2016-06-08 | 苏州大学 | Supercritical fluid processing method for improving activity and stability of pectinase |
| 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 |
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| CN113550137A (en) * | 2021-07-12 | 2021-10-26 | 武汉纺织大学 | Method for preparing non-woven fabric through multi-effect composite bleaching |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN105651719A (en) * | 2016-01-21 | 2016-06-08 | 苏州大学 | Supercritical fluid processing method for improving activity and stability of pectinase |
| CN105568591A (en) * | 2016-01-25 | 2016-05-11 | 苏州大学 | Hydrogen peroxide desizing pretreatment method for cotton in supercritical carbon dioxide fluid |
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| 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 |
| CN113550137A (en) * | 2021-07-12 | 2021-10-26 | 武汉纺织大学 | Method for preparing non-woven fabric through multi-effect composite bleaching |
| 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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