CN105568591B - The hydrogen peroxide desizing pretreatment process of cotton in a kind of supercritical carbon dioxide fluid - Google Patents
The hydrogen peroxide desizing pretreatment process of cotton in a kind of supercritical carbon dioxide fluid Download PDFInfo
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- CN105568591B CN105568591B CN201610045559.5A CN201610045559A CN105568591B CN 105568591 B CN105568591 B CN 105568591B CN 201610045559 A CN201610045559 A CN 201610045559A CN 105568591 B CN105568591 B CN 105568591B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
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- 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
- D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
- D06L1/14—De-sizing
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Abstract
The present invention provides a kind of hydrogen peroxide desizing pre-treating method of cotton in supercritical carbon dioxide fluid, and step A, surfactant is dissolved in into volume ratio is 1:2‑1:In 5 alcohols and water；B, hydrogen peroxide (unit mass green compact cotton products (g) correspondence 6 12ml) is added in alcohols and water, stirred to clarify；C, above-mentioned solution is placed in desizing reactor, forms hydrogen peroxide desizing device, green compact cotton products are placed in hydrogen peroxide desizing device, the hydrogen peroxide desizing device is placed in the supercritical carbon dioxide fluid processing system with EGR；D, closed processes system start EGR, in 60 90 DEG C of temperature, the 20Mpa of pressure 14, the 110min of processing time 50, fluid circulation and the time ratio 1 of static processing:Under 10, cotton products are carried out with oxidation desizing pre-treatment.The method technique is simple, and reaction is gentle, damage small to cotton products, it is to avoid a large amount of water, heat and high concentration alkali in traditional handicraft, with efficient, green, environmentally friendly, characteristics of energy saving.
Description
Technical field
The invention belongs to a kind of pair of cotton in textile dyeing and finishing processing technique field, more particularly to supercritical carbon dioxide fluid
Oxygen water desizing pretreatment process.
Background technology
Desizing is an indispensable step in fabric pretreatment technique.The slurry that it can will improve weaving efficiency and starching is gone
Remove, so as to be that fabric following process and printing and dyeing prepare.Traditional desizing method is carried out all in water, such as alkali desizing, oxidation
Agent desizing and sour desizing.Alkali desizing is swelled after being boiled for a long time in hot alkaline solution using conventional slurry, from gel
It is changed into collosol state, is fluffed with fiber bonding, then removed the slurry being swelled by washing.But generally consume a large amount of water and heat
Can, chemical oxygen consumption (COC) (COD) value of processed waste water is also very high, and environmental pollution is serious.One often used in oxidant desizing
A little oxidants such as NaBrO2、NaClO2And Na2S2O3Deng though slurry can be made to degrade, COD value is higher in the sewage after degraded, aggravates
Pollution to environment.Sour desizing generally can not be used alone, and damage big to fabric strength.
Supercritical carbon dioxide fluid technology is a kind of technology emerging in recent years, with environmental protection and energy-conservation the characteristics of.
Used carbon dioxide is safe and reliable, nontoxic, the features such as being also recycled recycling, its high efficiency and energy-conserving and environment-protective, standby
By favorable comment；Hydrogen peroxide is nontoxic, will not produce harmful toxic matter in processing procedure, and final catabolite is water and oxygen, right
Environmental nonpollution.In the prior art, in supercritical carbon dioxide fluid cotton hydrogen peroxide desizing pretreatment process nobody set foot in, due to
The particularity of supercritical carbon dioxide fluid, its hydrogen peroxide desizing technology in itself is different from the desizing in traditional water bath.
Therefore, cotton products are especially carried out before efficient desizing to natural cotton products in research and development supercritical carbon dioxide fluid medium
The method of processing, carries out the dyeing and finishing process technologies such as the anhydrous desizing pre-treatment of cotton products, thoroughly realizes textile printing and dyeing enterprises
Clean manufacturing, have very important significance and wide market prospects.
In view of above-mentioned defect, the design people is actively subject to research and innovation, to found a kind of supercritical carbon dioxide
The hydrogen peroxide desizing pre-treating method of cotton in fluid, makes it with more the value in industry.
The content of the invention
In order to solve the above technical problems, the purpose of the present invention is a kind of convenient operation of research and development, overcritical the two of energy-conserving and environment-protective
The hydrogen peroxide desizing pre-treating method of cotton in carbon oxide fluid.
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, including following step
Suddenly：
A, surfactant is dissolved in volume ratio is 1:2-1:In 5 alcohols and the mixed solution of water；
B, hydrogen peroxide is added in the mixed solution of the alcohols and water, the amount of wherein hydrogen peroxide is given birth to according to unit mass
The ratio addition of base cotton products (g) correspondence 6-12ml hydrogen peroxide, and stir to clarify, desizing working solution is made；
C, the desizing working solution described in step B is placed in desizing reactor, forms hydrogen peroxide desizing device, the life
Base cotton products are placed in hydrogen peroxide desizing device, and the hydrogen peroxide desizing device is placed in the overcritical titanium dioxide with EGR
In carbon fluid handling system；
D, the closed processing system, start EGR, and cotton products are carried out with oxidation desizing pre-treatment.
Further, reaction temperature be 60-90 DEG C, pressure be 14-20Mpa, processing time be 50-110min, fluid
The time ratio of circulation and static processing is 1:Under conditions of 10 cotton products are carried out with oxidation desizing pre-treatment.
Further, in the step A, it is 1 that surfactant, which is dissolved in volume ratio,:In 4 alcohols and the mixed solution of water.
Further, in the step B, the amount of hydrogen peroxide is double according to unit mass green compact cotton products (g) correspondence 10-12ml
The ratio addition of oxygen water.
Further, in the step D, reaction temperature is 75 DEG C, pressure be 16Mpa, processing time be 70min.
Further, in the step C, by hydrogen peroxide desizing device through circulation of fluid inlet tube and circulation of fluid outlet with
Supercritical carbon dioxide fluid processing system with EGR is connected.
Further, in the step A, the surfactant is diisooctyl succinate sodium sulfonate.
Further, the concentration of the surfactant is 2g/L.
Further, in the step A, the alcohols is ethanol.
Further, supercritical carbon dioxide fluid processing system is subtracted after desizing pre-treatment in the completion step D
Pressure, separation is with reclaiming desizing working solution and supercritical carbon dioxide fluid.
Beneficial effects of the present invention are：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, by hydrogen peroxide with
Proper amount of surfactant, the alcohols of proper proportion and water are made into desizing working solution, then by the desizing working solution containing hydrogen peroxide
Microemulsion is formed in situ using hydrophobic supercritical CO 2 medium, while microemulsion penetrates green compact cotton products with fluid,
Hydrogen peroxide is discharged, the degradation treatment in supercritical carbon dioxide fluid medium to impurity such as cotton products spreading masses is realized.
1st, the inventive method technique is simple, easy to operate, and reaction is gentle, and green compact cotton products are damaged in desizing processing procedure
Wound is small, it is to avoid the application of a large amount of water, heat and high concentration alkali in traditional desizing, with efficient, green, environmentally friendly, energy-conservation etc.
Feature；
2nd, the hydrogen peroxide desizing pretreatment process improves reactivity of the hydrogen peroxide to fiber spreading mass and impurity, improves
The desizing efficiency of cotton products slurry, is effectively realized in supercritical carbon dioxide fluid medium to the degraded of cotton products slurry
Reason；
3rd, hydrogen peroxide can also decompose a part of pigment oxidation, so as to effectively improve the whiteness of cotton products；
4th, the parameter such as pressure, temperature, processing time and dioxygen water consumption by controlling supercritical carbon dioxide fluid, it is real
The optimization of existing desizing.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention one supercritical carbon dioxide fluid in cotton desizing structure of reactor schematic diagram；
Fig. 2 is influence of the supercritical carbon dioxide fluid temperature to desizing pre-treatment cotton products capillary effect value；
Fig. 3 is influence of the supercritical carbon dioxide fluid temperature to desizing pre-treatment cotton products weight-loss ratio；
Fig. 4 is influence of the supercritical carbon dioxide fluid pressure to desizing pre-treatment cotton products capillary effect value；
Fig. 5 is influence of the supercritical carbon dioxide fluid pressure to desizing pre-treatment cotton products weight-loss ratio；
Fig. 6 is influence of the dioxygen water consumption to desizing pre-treatment cotton products capillary effect value；
Fig. 7 is influence of the dioxygen water consumption to desizing pre-treatment cotton products weight-loss ratio；
Fig. 8 is influence of the processing time to desizing pre-treatment cotton products capillary effect value；
Fig. 9 is the influence of processing time desizing pre-treatment cotton products weight-loss ratio.
In figure：1st, desizing liquid storage still；2nd, desizing kettle；3rd, fluid distributor；4th, filter；5th, fluid flow guiding cover；6th, it is raw
Base cotton products；7th, circulation of fluid is exported.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment one
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, the hydrogen peroxide is moved back
Slurry pretreatment process is realized using desizing reactor in the supercritical carbon dioxide fluid of structure as shown in Figure 1.The desizing is reacted
Device includes desizing liquid storage still 1 and the desizing kettle 2 being tightly connected by attachment means and desizing liquid storage still 1.Desizing liquid is stored
Kettle 1 is cylindrical shape kettle, is inside provided with the tubular fluid distributor 3 of inversion " mountain " type, and it is mainly managed by three be interconnected
Road constitute, positioned at center pipeline be circulation of fluid inlet tube, the bottom of circulation of fluid inlet tube with the overcritical of circulating pump
CO 2 fluid processing system (not shown) is connected；Two pipelines positioned at both sides are circulation of fluid outlet, two
The mouth of pipe of individual circulation of fluid outlet bends towards lower section, and the desizing work that stretches into desizing liquid storage still 1 of open at one end of lower section
Make below the liquid level of liquid.The top of desizing kettle 2 is provided with circulation of fluid outlet 7, circulation of fluid outlet 7 and supercritical carbon dioxide
Fluid handling system is connected.
Desizing kettle 2 is similarly the cotton products wireline reel that inner hollow is provided with cylindrical shape kettle, desizing kettle 2, cotton
It is wound with green compact cotton products 6, the bottom end opening top closure of cotton products wireline reel, and its axle side wall and offers on product wireline reel
Through hole.Bottom close to the cotton products wireline reel of attachment means is connected with tubaeform fluid flow guiding cover 5, fluid flow guiding cover 5
Lower section is provided with filter 4, can effectively filter the precipitated impurities contained in desizing working solution and circulation of fluid mixed liquor.At this
In embodiment, filter 4 is preferably the single or multiple lift board-like material for being covered with 50-2000 mesh micropores.
The axle body of cotton products wireline reel is made using Teflon or non heat conductivity material, or its surfaces externally and internally is using special
Fluorine dragon or non heat conductivity material are made, it is therefore prevented that cotton products wireline reel is mixed because of the desizing working solution and circulation of fluid of certain temperature
Liquid flows through and produced the phenomenon of cause thermal damage, extends the service life of cotton products wireline reel.
The top of desizing kettle 2 is provided with circulation of fluid outlet 7, circulation of fluid outlet 7 and overcritical two with EGR
Carbon oxide fluid processing system is connected.Desizing liquid storage still 1 and desizing kettle 2 pass through above-mentioned circulation of fluid inlet tube and circulation
Fluid issuing 7 realizes the connection with supercritical carbon dioxide fluid processing system.
During processing, desizing working solution is added in desizing liquid storage still 1, two circulation of fluids of fluid distributor 3 go out
The mouth of pipe of mouthful pipe is placed in desizing working solution, green compact cotton products 6 then in loose formula state entirely on cotton products wireline reel,
And the seamless netted infantees of last layer is covered in the outermost layer of winding cotton products, then it is placed in desizing kettle 2, and roll up cotton products
Well connected with fluid flow guiding cover 5 downwards around the openend of axle.
The hydrogen peroxide desizing pre-treating method of cotton in supercritical carbon dioxide fluid, wherein, the quality of pending cotton products 6
For 2g, comprise the following steps that：
A, by 0.1g surfactants diisooctyl succinate sodium sulfonate (A0T), be dissolved in volume ratio for 1:4 10mL ethanol
In the mixed solution of 40mL water, i.e., the concentration of diisooctyl succinate sodium sulfonate (A0T) is 2g/L；
B, 20ml hydrogen peroxide is added in the mixed solution of alcohols and water, the amount of wherein hydrogen peroxide is given birth to according to unit mass
The ratio addition of base cotton products (g) correspondence 10ml hydrogen peroxide, and stir to clarify, desizing working solution is made；
C, desizing working solution 2 is placed in the desizing liquid storage still 1 of desizing reactor, by green compact cotton products 6 wound on cotton
On product wireline reel, it is placed in the desizing kettle 2 of desizing reactor, desizing liquid storage still 1 and desizing kettle 2 are tightly connected to form double
Oxygen water desizing device, hydrogen peroxide desizing device is placed in the supercritical carbon dioxide fluid device with EGR, or will be double
Oxygen water desizing device is exported at 7 and the supercritical carbon dioxide fluid with EGR through circulation of fluid inlet tube and circulation of fluid
Reason system is connected；Hydrogen peroxide desizing device ensures that the open at one end of cotton products wireline reel and desizing working solution liquid level keep 45cm
Distance, with prevent because fluid distributor 3 stirring and fluid entrainment effect desizing working solution is occurred with green compact cotton products 6
Directly contact；
D, the closed processing system, start EGR, are 90 DEG C in reaction temperature, pressure is 16Mpa, processing time
For 70min, the time ratio of fluid circulation and static processing is 1：Under 10 treatment conditions, oxidation is carried out to green compact cotton products 6 and moved back
Starch pre-treatment.
Supercritical carbon dioxide fluid is circulated to work by the tubular fluid distributor 3 in desizing liquid storage still 1 and desizing
Liquid is sufficiently mixed, and microemulsion is formed in the presence of surfactant, and hydrogen peroxide is transferred into hydrophobic fluid, and and then
Flow into cotton products wireline reel, had an effect by through hole with the green compact cotton products 6 on cotton products wireline reel, complete to move back
Slurry processing.
After the completion of hydrogen peroxide desizing, fluid stops circulation, and supercritical carbon dioxide fluid processing system is depressurized,
Desizing working solution and circulation of fluid are separated and reclaimed using external separation and recovery system.Connection dress is opened in decompression after terminating
Put, take out the cotton products after being handled through hydrogen peroxide desizing.The mixed solution of residual may be recovered in desizing liquid storage still 1, or
Continuous use is carried out after adding component.
The weight-loss ratio and capillary effect value of the cotton products of hydrogen peroxide desizing pre-treatment are tested, weight-loss ratio and capillary effect value are to move back
Starch the important criterion of effect.It is many that weight-loss ratio intuitively represents that slurry is removed by the loss of quality before and after fabric desizing
It is few；Capillary effect value can represent the water absorbing capacity of fabric, and it is more thorough that pending cotton products spreading mass is removed, and the water absorbing capacity of fabric is got over
By force, capillary effect value is also bigger.
Wherein weight-loss ratio and capillary effect value method of testing is as follows：
Weight-loss ratio is tested：Cotton products sample is taken out after the completion of desizing pre-treatment, after being cleaned 2-3 times with water, cotton products are put
In temperature be to dry 120min under conditions of 105 DEG C in drying box, be subsequently placed in drier balance more than 24h, weighing its
Weight；The cotton products without desizing pre-treatment of formed objects are taken to handle in an identical manner, by contrasting before desizing pre-treatment
The weight of cotton products, obtains the weight-loss ratio of cotton products afterwards.
Capillary effect value is tested：Carried out with reference to textile industry standard FZ/T 01071-2008 cotton products capillary effects test method
Determine, take the cotton products after desizing pre-treatment, tested on ZBW04019 type capillary effect testers, the time is 30min.
Result, the weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment are obtained after tested
For：Weight-loss ratio is 3.9%, and capillary effect value is 12.8cm.
Embodiment two
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment surpasses
The temperature of critical carbon dioxide fluid is 75 DEG C.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 4.7%,
Capillary effect value is 14.4cm.
Embodiment three：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment surpasses
The temperature of critical carbon dioxide fluid is 60 DEG C.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 2.7%,
Capillary effect value is 11.3cm.
Example IV：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment surpasses
The pressure of critical carbon dioxide fluid is 14MPa.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 2.4%,
Capillary effect value is 6.3cm.
Embodiment five：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment surpasses
The pressure of critical carbon dioxide fluid is 18MPa.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 4.8%,
Capillary effect value is 12.4cm.
Embodiment six：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment surpasses
The pressure of critical carbon dioxide fluid is 20MPa.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 2.4%,
Capillary effect value is 8.9cm.
Embodiment seven：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment pair
The dioxygen water volume of unit mass fabric (g) is 12ml, uses hydrogen peroxide (hydrogenperoxide steam generator of mass fraction 30%) volume
For 24ml.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 4.8%,
Capillary effect value is 10.8cm.
Embodiment eight：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment pair
The dioxygen water volume of unit mass fabric (g) is 8ml, is using hydrogen peroxide (hydrogenperoxide steam generator of mass fraction 30%) volume
16ml。
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 3.8%,
Capillary effect value is 9.9cm.
Embodiment nine：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment pair
The dioxygen water volume of unit mass fabric (g) is 6ml, is using hydrogen peroxide (hydrogenperoxide steam generator of mass fraction 30%) volume
12ml。
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 3.8%,
Capillary effect value is 7.3cm.
Embodiment ten：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment
Processing time is 50min.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 3.6%,
Capillary effect value is 1.2cm.
Embodiment 11：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment
Processing time is 90min.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 4.8%,
Capillary effect value is 11.6cm.
Embodiment 12：
The invention provides a kind of hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid, its hydrogen peroxide is moved back
Starch pretreatment process identical with the hydrogen peroxide desizing pretreatment process step described in embodiment one, difference part is：The present embodiment
Processing time is 110min.
The weight-loss ratio and capillary effect value test result of cotton products of the present embodiment through desizing pre-treatment be：Weight-loss ratio is 3.1%,
Capillary effect value is 5.4cm.
It can be seen that by embodiment one to three, Fig. 2 and Fig. 3, the processing in supercritical carbon dioxide fluid during hydrogen peroxide desizing
Temperature can directly influence the oxidation Decomposition speed of hydrogen peroxide.Between 70 DEG C~90 DEG C, due to suitably increasing temperature, improve
The decomposition rate of hydrogen peroxide, while supercritical carbon dioxide fluid flow faster, formation and the motion of microemulsion system are accelerated；
At 75 DEG C or so preferably, this temperature may be considered the optimal place of hydrogen peroxide desizing in supercritical carbon dioxide fluid to desizing effect
Manage temperature.
It can be seen that by example IV to six and embodiment one, Fig. 4 and Fig. 5, the pressure change of supercritical carbon dioxide fluid
There is considerable influence to the property of system fluid, the formation of microemulsion system is also affected.In the selected experiment pressure of this experiment
Under power (14MPa~20MPa), the desizing of supercritical carbon dioxide fluid hydrogen peroxide all achieves preferable desizing effect.With pressure
Power gradually increases, and microemulsion is more readily formed in the increase of Fluid pressure.With the circulation stirring of fluid, microemulsion forms more
Plus it is uniform, and hydrogen peroxide in interfibrous flowing can preferably reach the surface of cotton grey cloth with fluid.In processing pressure
During 16MPa, the capillary effect value of the fabric after processing reaches maximum, and weight-loss ratio value is larger, it is believed that this processing pressure is optimal
Pressure.
It can be seen that by embodiment seven to nine and embodiment one, Fig. 6 and Fig. 7, the consumption of hydrogen peroxide has larger to desizing effect
Influence.The consumption of appropriate increase hydrogen peroxide, so that the more slurries of oxidation Decomposition, can improve desizing effect.But cross highly concentrated
The hydrogen peroxide of degree can also be such that fabric is necessarily damaged.
It can be seen that supercritical carbon dioxide fluid hydrogen peroxide is moved back by embodiment ten to 12 and embodiment one, Fig. 8 and Fig. 9
Slurry is before certain reaction time is reached, with the increase of processing time, and corresponding agitation cycle number of times increases, formation it is micro-
Emulsion is also more, and evenly hydrogen peroxide obtains more abundant with slurry contact, and desizing effect is also become better and better.And reached in processing time
To after 70min, capillary effect value does not have occurs obvious increase as the continuation of processing time increases.This explanation is in processing
Between 70min or so, the desizing processing of supercritical carbon dioxide fluid hydrogen peroxide is substantially by the slurry removal on fabric surface.
The method of the present invention is to cotton, and the anhydrous hydrogen peroxide desizing of supercritical carbon dioxide fluid of especially starch starching cotton adds
Instrument has preferable practicality, damage small to cloth, reaction is gentle, without carrying out at high temperature, it is to avoid in traditional desizing
The application of a large amount of water, heat and high concentration alkali, while supercritical process is easily controllable and carries out, and with efficient, green, environmental protection etc.
Feature, thus have a extensive future.
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and
Modification, these improvement and modification also should be regarded as protection scope of the present invention.
Claims (6)
1. the hydrogen peroxide desizing pretreatment process of cotton in a kind of supercritical carbon dioxide fluid, it is characterised in that comprise the following steps：
A, surfactant is dissolved in volume ratio is 1:2-1:In 5 alcohols and the mixed solution of water；The surfactant is
Diisooctyl succinate sodium sulfonate；The concentration of the diisooctyl succinate sodium sulfonate is 2g/L；The alcohols is ethanol；
B, hydrogen peroxide is added in the mixed solution of the alcohols and water, wherein the amount of hydrogen peroxide is according to unit mass gram green compact
The ratio addition of cotton products correspondence 6-12ml hydrogen peroxide, and stir to clarify, desizing working solution is made；
C, the desizing working solution described in step B is placed in desizing reactor, forms hydrogen peroxide desizing device, the green compact cotton
Product is placed in hydrogen peroxide desizing device, and the hydrogen peroxide desizing device is placed in into the stream of supercritical carbon dioxide with EGR
In body processing system；
D, the closed processing system, start EGR, and cotton products are carried out with oxidation desizing pre-treatment；Wherein, in reaction temperature
The time ratio that degree is 60-90 DEG C, pressure is 14-20Mpa, processing time is 50-110min, fluid circulation and static processing is 1:
Under conditions of 10 cotton products are carried out with oxidation desizing pre-treatment.
2. the hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid according to claim 1, its feature exists
In：In the step A, it is 1 that surfactant, which is dissolved in volume ratio,:In 4 alcohols and the mixed solution of water.
3. the hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid according to claim 1, its feature exists
In：In the step B, the amount of hydrogen peroxide is added according to the ratio of unit mass gram green compact cotton products correspondence 10-12ml hydrogen peroxide.
4. the hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid according to claim 1, its feature exists
In：In the step D, reaction temperature is 75 DEG C, pressure be 16Mpa, processing time be 70min.
5. the hydrogen peroxide desizing pre-treatment of cotton in the supercritical carbon dioxide fluid according to any one of claim 1-4
Method, it is characterised in that：In the step C, by hydrogen peroxide desizing device through circulation of fluid inlet tube and circulation of fluid outlet and band
The supercritical carbon dioxide fluid processing system of EGR is connected.
6. the hydrogen peroxide desizing pretreatment process of cotton in supercritical carbon dioxide fluid according to claim 1, its feature exists
In：Complete in the step D after desizing pre-treatment, supercritical carbon dioxide fluid processing system is depressurized, separation is moved back with recovery
Starch working solution and supercritical carbon dioxide fluid.
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| CN107099995B (en) * | 2017-03-24 | 2019-11-12 | 苏州大学 | The supercritical fluid phase transfer catalysis (PTC) desizing method of textile |
| 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 |
| CN109281088A (en) * | 2018-11-14 | 2019-01-29 | 苏州大学 | A kind of supercritical carbon dioxide fluid mercerization finish method of wool spinning product |
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| CN104313891A (en) * | 2014-10-17 | 2015-01-28 | 苏州大学 | Starch slurry desizing method adopting supercritical carbon dioxide as medium |
| CN104389153A (en) * | 2014-10-17 | 2015-03-04 | 苏州大学 | Method for enzymatic desizing of cotton in supercritical carbon dioxide fluid |
| CN104452319A (en) * | 2014-10-17 | 2015-03-25 | 苏州大学 | Desizing pretreatment method of textile |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104313891A (en) * | 2014-10-17 | 2015-01-28 | 苏州大学 | Starch slurry desizing method adopting supercritical carbon dioxide as medium |
| CN104389153A (en) * | 2014-10-17 | 2015-03-04 | 苏州大学 | Method for enzymatic desizing of cotton in supercritical carbon dioxide fluid |
| CN104452319A (en) * | 2014-10-17 | 2015-03-25 | 苏州大学 | Desizing pretreatment method of textile |
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