CN106468026A - For supercritical CO2The cotton fiber dyestuff of fluid dyeing and its colouring method - Google Patents
For supercritical CO2The cotton fiber dyestuff of fluid dyeing and its colouring method Download PDFInfo
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- CN106468026A CN106468026A CN201510505713.8A CN201510505713A CN106468026A CN 106468026 A CN106468026 A CN 106468026A CN 201510505713 A CN201510505713 A CN 201510505713A CN 106468026 A CN106468026 A CN 106468026A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B62/00—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
- C09B62/02—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group directly attached to a heterocyclic ring
- C09B62/04—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group directly attached to a heterocyclic ring to a triazine ring
- C09B62/08—Azo dyes
- C09B62/085—Monoazo dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/94—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in solvents which are in the supercritical state
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention proposes one kind and is used for supercritical CO2The cotton fiber dyestuff of fluid dyeing and its colouring method, described colouring method comprises the following steps：Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, and dyestuff kettle and dyeing caldron interconnect；Step S2, cotton fiber dyestuff is dissolved in fluid modified agent, then puts into together in dyestuff kettle, be then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized, make liquid carbon dioxide be converted into supercritical CO2Fluid, and make this supercritical CO2Fluid dissolves cotton fiber dyestuff；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, thus completing to dye.The cotton fiber dyestuff of the present invention has dye characteristic in outstanding absorption, additionally, the synthetic method craft process of the cotton fiber dyestuff of the present invention is simple.
Description
Technical field
The present invention relates to dye field, more particularly, to one kind are used for supercritical CO2The cotton fiber of fluid dyeing
Dyestuff and its colouring method.
Background technology
Supercritical CO2Fluid is the fluid media (medium) of a kind of color, environmental protection, replaces traditional water bath to fiber with it
Textile carries out Colour Difference, has the characteristics that environmental protection, clean manufacturing, and prominent energy-saving effect,
Have to changing the present situations such as traditional textile dyeing water resources consumption is high, blowdown flow rate is big, environmental pollution is serious
Significance.
Adopt disperse dyes in the majority to the research of the synthetic dyeings such as terylene at present, and part has been carried out work
Industry metaplasia is produced.But at present in supercritical CO2Disperse dyes are directly adopted to hydrophilic cotton, sheep in fluid
Hair and the natural fiber such as silkworm silk carry out dyeing and still can not reach commercialization requirement.Wherein, cotton fiber spins in the whole world
The market share in weaver's industry is up to 37%, is most important natural fiber, is also in supercritical CO2Fluid
In one of the most chromophobe natural fiber.At present, cotton fiber mainly adopts three kinds of dyeing approach：One is to change
Fluid polarity, but Color is undesirable；Two is to natural fiber modification poststaining, but reduces natural fibre
The performance of dimension otherwise superior；Three is using dissolving in supercritical CO2Introduce in the dye matrix structure of fluid
Active group, so that dyestuff can be with fiber-reactive and set, but its correlation report is very few.
Additionally, compared with traditional water bath coloring system, supercritical CO2Fluid belongs to hydrophobic medium；So,
(natural) filament expansion of easily realizing in conventional water-bath, the diffusion of dyestuff and promote fixation anti-using alkaline agent
Should wait in supercritical CO2It is difficult in fluid.Thus in supercritical CO2In fluid dyeing course, how
Open the hydrogen bond between fiber macromolecular chain, and how to improve dye activity base with fiber functional group anti-
Should, it is that natural cotton fiber is made in supercritical CO using reactive disperse dyes2Dye in fluid to obtain satisfied dye
The key of color effect.Therefore, in actual production, often need to adopt all kinds of solvents (generally to be contaminated in a large number
30%～50% of textile weight or more) or other moistening and puffing agent, fibre modifier etc. to hydrophilic sky
So fiber textile carries out pretreatment, to help swelling of fiber, to improve the upper dye of dyestuff, or fiber is carried out
Ammoniation modified, improve fixation rate on fiber for the dyestuff, which increase the complexity of dyeing course, and improve
Production cost.
Content of the invention
The present invention is directed to the filament expansion easily realized in conventional water-bath, the diffusion of dyestuff and is promoted using alkaline agent
Enter fixation reaction etc. in supercritical CO2It is difficult in fluid, meanwhile, in actual production, often need
Adopt all kinds of solvents or other moistening and puffing agent, fibre modifier etc. in a large number to hydrophilic natural fiber textile
Carry out pretreatment, to help swelling of fiber, to improve the upper dye of dyestuff, or fiber is carried out ammoniation modified, carry
Fixation rate on fiber for the high dyestuff, which increases the complexity of dyeing course, and improves production cost
Problem is it is proposed that a kind of dyeing course is simply to supercritical CO2Fluid dyeing cotton fiber dyestuff and
Its colouring method.
The technical scheme that the present invention proposes to solve above-mentioned technical problem is as follows：
The present invention proposes one kind and is used for supercritical CO2The colouring method of the cotton fiber dyestuff of fluid dyeing,
Comprise the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；
Step S2, cotton fiber dyestuff is dissolved in fluid modified agent, then puts in dyestuff kettle together,
It is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2Fluid dissolves cotton fiber
Dyestuff；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that supercritical CO2
Fluid carries cotton fiber surface and the inside that cotton fiber dyestuff is diffused into fabric, and then completes to dye；
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
In the above-mentioned colouring method of the present invention, described coloring system is also included for preheating liquid carbon dioxide
Preheater, for injecting the booster pump of liquid carbon dioxide, be used for making supercritical CO2Fluid is in dyestuff kettle
Circulating pump with circulation in dyeing caldron.
In the above-mentioned colouring method of the present invention, described dyeing caldron has hollow and tube wall is covered with the dyeing of through hole
Axle；Described step S2 also includes：By fabric wrapping on this dyeing axle.
In the above-mentioned colouring method of the present invention, described step S3 also includes：When the temperature in coloring system and
When pressure reaches the temperature and pressure required for dyeing, close booster pump；Wherein, needed for dyeing
Temperature is 80 DEG C -100 DEG C, and desirable pressure is 20MPa-30MPa；
Then open circulating pump, make supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron.
In the above-mentioned colouring method of the present invention, supercritical CO2Circulation in dyestuff kettle and dyeing caldron for the fluid
Be forward circulation and recycled back alternately.
The invention allows for a kind of cotton fiber dyestuff using colouring method as above dyeing, have all
Triazine active group.
The cotton fiber dyestuff of the present invention, because of its s-triazine type active group, can occur bonding reaction with cotton fiber, from
And make dye fixing on cotton fiber, reach the effect of dyeing.The cotton fiber dyestuff of the present invention has outstanding
Characteristic is contaminated on absorption.Additionally, the synthetic method craft process of the cotton fiber dyestuff of the present invention is simple；Therefore,
The cotton fiber dyestuff for Supercritical carbon dioxide fluid dyeing of the present invention and its synthetic method have very
Wide application prospect.
Brief description
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing：
Fig. 1 is the synthetic route chart of yellow cotton fiber dyestuff；
Fig. 2 is the process chart of the yellow cotton fiber dyestuff shown in Fig. 1；
Fig. 3 is the supercritical CO of the yellow cotton fiber dyestuff of first embodiment of the invention2The work of fluid dyeing
Skill route map；
Fig. 4 is to carry out supercritical CO using SCF-Y1 dyestuff2First signal of the bafta of fluid dyeing
Figure；
Fig. 5 is to carry out supercritical CO using SCF-Y1 dyestuff2Second signal of the bafta of fluid dyeing
Figure；
Fig. 6 is to carry out supercritical CO using SCF-Y1 dyestuff23rd signal of the bafta of fluid dyeing
Figure；
Fig. 7 is to carry out supercritical CO using SCF-Y1 dyestuff24th signal of the bafta of fluid dyeing
Figure；
Fig. 8 is the synthetic route chart of blue cotton fiber dyestuff；
Fig. 9 is the process chart of the blue cotton fiber dyestuff shown in Fig. 8；
Figure 10 is the supercritical CO of the blue cotton fiber dyestuff of second embodiment of the invention2The work of fluid dyeing
Skill route map；
Figure 11 is to carry out supercritical CO using SCF-B1 dyestuff2Fluid dyes and passes through and irons dry and soap boiling work
The schematic diagram of the bafta of skill；
Figure 12 is to carry out supercritical CO using SCF-B1 dyestuff2Fluid dye and through ironing dry with acetone at
The schematic diagram of the bafta of reason；
Figure 13 is to carry out supercritical CO using SCF-B1 dyestuff2Fluid dyes and through soap boiling PROCESS FOR TREATMENT
Bafta schematic diagram；
Figure 14 is to carry out supercritical CO using SCF-B1 dyestuff2Fluid dyes and passes through and irons dry and fixation work
The schematic diagram of the bafta that skill is processed；
Figure 15 is the synthetic route chart of red cotton fiber dyestuff；
Figure 16 shows the process chart of the red cotton fiber dyestuff shown in Figure 15；
Figure 17 is the supercritical CO of the red cotton fiber dyestuff of third embodiment of the invention2The work of fluid dyeing
Skill route map；
Figure 18 is to carry out supercritical CO using SCF-R1 dyestuff2The schematic diagram of the bafta of fluid dyeing.
Specific embodiment
The technical problem to be solved in the present invention is：Supercritical CO2Fluid belongs to hydrophobic medium；So,
(natural) filament expansion of easily realizing in conventional water-bath, the diffusion of dyestuff and promote fixation anti-using alkaline agent
Should wait in supercritical CO2It is difficult in fluid；Meanwhile, in actual production, often need to adopt in a large number
All kinds of solvents (30%～50% of generally contaminated textile weight or more) or other moistening and puffing agent, fibre
Dimension modifying agent etc. carries out pretreatment to hydrophilic natural fiber textile, to help swelling of fiber, to improve dyestuff
Upper dye, or fiber is carried out ammoniation modified, improves fixation rate on fiber for the dyestuff, which increase dyeing
The complexity of process, and improve production cost.The technical thought that the present invention solves this technical problem is：Adopt
With there is the reactive disperse dyes of s-triazine type active group in supercritical CO2In fluid, cotton fiber is contaminated
Color.Because reactive disperse dyes has s-triazine type active group, and in supercritical CO2Contaminated in fluid
During color, s-triazine type active group can occur bonding reaction with fiber, so that reactive disperse dyes fixation is in cotton
On fiber.
In the present invention, for supercritical CO2The cotton fiber dyestuff of fluid dyeing has s-triazine type activity
Base.
The synthetic method of this cotton fiber dyestuff comprises the following steps：
Step 1, with Cyanuric Chloride (TCT) as active group, and dye matrix and active group are all put into
So as to be completely dissolved in single or mixed solvent, thus obtaining reaction system；
Step 2, reaction system is placed in 0 DEG C～5 DEG C of ice bath, then to Deca trimerization in reaction system
Chlorine cyanogen solution and acid-capture agent, until the condensation reaction of reaction system terminates；
Step 3, the reaction system that condensation reaction terminates is diluted, scrubbed, filter, be dried to obtain
Cotton fiber dyestuff.
In above-mentioned synthetic method, dye matrix can be Isosorbide-5-Nitrae-diamino-anthraquinone, disperse orange 3 or disperse blue
35.When dye matrix is for Isosorbide-5-Nitrae-diamino-anthraquinone, cotton fiber dyestuff is redness, is designated as active dispersal red
SCF-R1；When dye matrix is for disperse orange 3, cotton fiber dyestuff is yellow, is designated as active dispersal yellow
SCF-Y1；When dye matrix is for disperse blue 35, cotton fiber dyestuff is blueness, is designated as active dispersal blue
SCF-B1；According to three primary colories color theory, by red, yellow, blue three-color cotton fiber dyestuff, just
The cotton fiber dyestuff of other shades of colours can be allotted.
In the present invention, the colouring method of above-mentioned cotton fiber dyestuff comprises the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；
In the present embodiment, coloring system also includes preheater for preheating liquid carbon dioxide, is used for noting
Enter the booster pump of liquid carbon dioxide, be used for making supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron
Circulating pump.
Step S2, cotton fiber dyestuff is dissolved in fluid modified agent, then puts in dyestuff kettle together,
It is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
In this step, dyeing caldron has hollow and tube wall is covered with the dyeing axle of through hole, usually, this dyeing
Axle is by stainless steel shaft it will be understood that dyeing axle can also be made up of other materials.Fabric is wound onto this dye
On colour axis.
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2Fluid dissolves cotton fiber
Dyestuff；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that supercritical CO2
Fluid carries cotton fiber surface and the inside that cotton fiber dyestuff is diffused into fabric, and then completes to dye；
In this step, temperature and the pressure required for dyeing is reached when the temperature and pressure in coloring system
During power, then can close booster pump, here, dyeing is temperature required to be 80 DEG C -100 DEG C, desirable pressure
For 20MPa-30MPa；Then open circulating pump, make supercritical CO2Fluid is in dyestuff kettle and dyeing caldron
Circulation.Here, supercritical CO2Circulation in dyestuff kettle and dyeing caldron for the fluid is forward circulation and reversely
Cycle alternation is carried out, to promote supercritical CO2The effect of fluid dyeing is more uniform.
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
In this step, by making coloring system lower the temperature and reducing pressure, can be by supercritical CO2Fluid separates
Reclaim.
In order that the technical purpose of the present invention, technical scheme and technique effect are clearer, below in conjunction with
The present invention will be further described in detail for drawings and the specific embodiments.
First embodiment
Present embodiments provide a kind of synthetic method of yellow cotton fiber dyestuff.
Specifically, with reference to Fig. 1, Fig. 1 is the synthetic route of yellow cotton fiber dyestuff it can be seen that this reality
Applying example adopts disperse orange 3 and Cyanuric Chloride as raw material, makes a Cl on Cyanuric Chloride replace disperse orange
A H on 3 amino, thus synthesize yellow cotton fiber dyestuff.
With reference to Fig. 2, Fig. 2 shows the process chart of the yellow cotton fiber dyestuff shown in Fig. 1.
The synthetic method of yellow cotton fiber dyestuff includes：
Step 1, using disperse orange 3 as dye matrix, and dye matrix is put into dioxane and water
So as to be completely dissolved in mixed solvent, thus obtaining reaction system；
In the mixed solvent with water for the dioxane, the mass ratio of Isosorbide-5-Nitrae-dioxane and distilled water is 2:1 or
1:(1～3)；
Further, disperse orange 3 adopts 0.001mol；Here, the mass ratio of disperse orange 3 and mixed solvent
Determine response speed, can be according to concrete test situation depending on；
Step 2, reaction system is placed in 0 DEG C～5 DEG C of ice bath, using Cyanuric Chloride (TCT) as living
Property base, then to Deca Cyanuric Chloride solution and acid-capture agent in reaction system, until the condensation of reaction system is anti-
Should terminate；
In the present embodiment, acid-capture agent adopts the sodium hydroxide of 0.1M.Cyanuric Chloride is rubbed with disperse orange 3
That ratio is 2:1.
This step also includes：To during Deca Cyanuric Chloride solution in reaction system and acid-capture agent, right
Reaction system carries out magnetic agitation；In the present embodiment, the time of magnetic agitation is 3h.
Step 3, the reaction system that condensation reaction terminates is diluted, scrubbed, filter, be dried to obtain
Yellow cotton fiber dyestuff.
Here, for the ease of the record of Color afterwards, yellow cotton fiber dyestuff is designated as SCF-Y1 dyestuff.
With reference to Fig. 3, Fig. 3 is the supercritical CO of the yellow cotton fiber dyestuff of first embodiment of the invention2Fluid
The process route chart of dyeing.
As shown in figure 3, the supercritical CO of yellow cotton fiber dyestuff2Fluid colouring method comprises the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；In the present embodiment, coloring system also includes the preheating for preheating liquid carbon dioxide
Device, for injecting the booster pump of liquid carbon dioxide, be used for making supercritical CO2Fluid is in dyestuff kettle and dye
The circulating pump of circulation in color kettle.
Step S2, yellow cotton fiber dyestuff is dissolved in fluid modified agent, then puts into dyestuff kettle together
In, it is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
In this step, yellow cotton fiber dyestuff is active dispersal Huang SCF-Y1, and its addition content is 3%o.m.f；
Fluid modified agent is methanol, and its addition content is supercritical CO2The 10wt% of fluid.
In this step, dyeing caldron has hollow and tube wall is covered with the dyeing axle of through hole, usually, this dyeing
Axle is by stainless steel shaft it will be understood that dyeing axle can also be made up of other materials.Fabric is wound onto this dye
On colour axis.
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2Fluid dissolves yellow cotton
Fiber dyes；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that super face
Boundary CO2Fluid carries cotton fiber surface and the inside that yellow cotton fiber dyestuff is diffused into fabric, and then completes
Dyeing；
In this step, temperature and the pressure required for dyeing is reached when the temperature and pressure in coloring system
During power, then can close booster pump, here, dyeing is temperature required to be 100 DEG C, and desirable pressure is
28MPa；Then open circulating pump, make supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron.Here,
Supercritical CO2Circulation in dyestuff kettle and dyeing caldron for the fluid be forward circulation and recycled back alternately,
To promote supercritical CO2The effect of fluid dyeing is more uniform；Wherein, supercritical CO2Fluid is in dyestuff
In kettle and dyeing caldron, the circulation time of circulation is 90min.
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
As shown in figs. 4-7, Fig. 4-Fig. 7 is to carry out supercritical CO using different SCF-Y1 dyestuffs2Fluid contaminates
The schematic diagram of the bafta of color.
Here, in the synthetic method of SCF-Y1 dyestuff that Fig. 4 is adopted, Isosorbide-5-Nitrae-dioxane and distilled water
Mass ratio be 1:1；In the synthetic method of SCF-Y1 dyestuff that Fig. 5 is adopted, Isosorbide-5-Nitrae-dioxane and
The mass ratio of distilled water is 1:2；In the synthetic method of SCF-Y1 dyestuff that Fig. 6 is adopted, Isosorbide-5-Nitrae-dioxy
The mass ratio of six rings and distilled water is 1:3；In the synthetic method of SCF-Y1 dyestuff that Fig. 7 is adopted, Isosorbide-5-Nitrae-
The mass ratio of dioxane and distilled water is 3:1.
Second embodiment
Present embodiments provide a kind of synthetic method of blueness cotton fiber dyestuff.
Specifically, with reference to Fig. 8, Fig. 8 is the synthetic route of blue cotton fiber dyestuff it can be seen that this reality
Applying example adopts disperse blue 35 and Cyanuric Chloride as raw material, makes a Cl on Cyanuric Chloride replace disperse blue
A H on 35 hydroxyl, thus synthesize blue cotton fiber dyestuff.
With reference to Fig. 9, Fig. 9 shows the process chart of the blue cotton fiber dyestuff shown in Fig. 8.
The synthetic method of blue cotton fiber dyestuff includes：
Step 1, using disperse blue 35 as dye matrix, and dye matrix is put into oxolane and water
Mixed solvent in so as to be completely dissolved, thus obtaining reaction system；
In the mixed solvent with water for the oxolane, oxolane is 3 with the mass ratio of distilled water:1；
Further, disperse blue 35 adopts 0.001mol；Here, the ratio of disperse blue 35 and mixed solvent
Determine response speed, can be according to concrete test situation depending on；
Step 2, reaction system is placed in 0 DEG C～5 DEG C of ice bath, using Cyanuric Chloride (TCT) as living
Property base, then to Deca Cyanuric Chloride solution and acid-capture agent in reaction system, until the condensation of reaction system is anti-
Should terminate；
In the present embodiment, acid-capture agent adopts the sodium hydroxide of 0.1M.Cyanuric Chloride and disperse blue 35
Mol ratio is 2:1.
This step also includes：To during Deca Cyanuric Chloride solution in reaction system and acid-capture agent, right
Reaction system carries out magnetic agitation；In the present embodiment, the time of magnetic agitation is 3h.
Step 3, the reaction system that condensation reaction terminates is diluted, scrubbed, filter, be dried to obtain
Blue cotton fiber dyestuff.
Here, for the ease of the record of Color afterwards, blue cotton fiber dyestuff is designated as SCF-B1 dyestuff.
With reference to Figure 10, Figure 10 is the supercritical CO of the blue cotton fiber dyestuff of second embodiment of the invention2
The process route chart of fluid dyeing.
As shown in Figure 10, the supercritical CO of blue cotton fiber dyestuff2Fluid colouring method comprises the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；In the present embodiment, coloring system also includes the preheating for preheating liquid carbon dioxide
Device, for injecting the booster pump of liquid carbon dioxide, be used for making supercritical CO2Fluid is in dyestuff kettle and dye
The circulating pump of circulation in color kettle.
Step S2, blue cotton fiber dyestuff is dissolved in fluid modified agent, then puts into dyestuff kettle together
In, it is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
In this step, blue cotton fiber dyestuff is active dispersal indigo plant SCF-B1, and its addition content is 2%o.m.f；
Fluid modified agent is methanol, and its addition content is supercritical CO2The 10wt% of fluid.
In this step, dyeing caldron has hollow and tube wall is covered with the dyeing axle of through hole, usually, this dyeing
Axle is by stainless steel shaft it will be understood that dyeing axle can also be made up of other materials.Fabric is wound onto this dye
On colour axis.
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2The blue cotton of fluid dissolving
Fiber dyes；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that super face
Boundary CO2Fluid carries cotton fiber surface and the inside that blue cotton fiber dyestuff is diffused into fabric, and then completes
Dyeing；
In this step, temperature and the pressure required for dyeing is reached when the temperature and pressure in coloring system
During power, then can close booster pump, here, dyeing is temperature required to be 100 DEG C, and desirable pressure is
30MPa；Then open circulating pump, make supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron.Here,
Supercritical CO2Circulation in dyestuff kettle and dyeing caldron for the fluid be forward circulation and recycled back alternately,
To promote supercritical CO2The effect of fluid dyeing is more uniform；Wherein, supercritical CO2Fluid is in dyestuff
In kettle and dyeing caldron, the circulation time of circulation is 120min.
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
As illustrated in figs. 11-14, Figure 11-14 is to carry out supercritical CO using SCF-B1 dyestuff2Fluid dyes
And the schematic diagram of the bafta through over cleaning loose colour technique.
Here, the bafta shown in Figure 11 employs and irons dry and soap boiling PROCESS FOR TREATMENT, and the cotton shown in Figure 12 is knitted
Thing employs and irons dry and acetone treatment；Bafta shown in Figure 13 use only soap boiling PROCESS FOR TREATMENT, Figure 14
Shown bafta employs to iron dry and processes with color fixing process；
3rd embodiment
Present embodiments provide a kind of synthetic method of redness cotton fiber dyestuff.
Specifically, with reference to Figure 15, Figure 15 be red cotton fiber dyestuff synthetic route it can be seen that this
Embodiment adopts Isosorbide-5-Nitrae-diamino-anthraquinone and Cyanuric Chloride as raw material, so that on Cyanuric Chloride Cl is taken
For the H on an amino of Isosorbide-5-Nitrae-diamino-anthraquinone, or the Cl on two Cyanuric Chlorides is made to replace respectively
The H of two amino of Isosorbide-5-Nitrae-diamino-anthraquinone, thus synthesize red cotton fiber dyestuff.
With reference to Figure 16, Figure 16 shows the process chart of the red cotton fiber dyestuff shown in Figure 15.
The synthetic method of red cotton fiber dyestuff includes：
Step 1, using Isosorbide-5-Nitrae-diamino-anthraquinone (i.e. disperse violet 1) as dye matrix, and by dye matrix
Put in Isosorbide-5-Nitrae-dioxane and the mixed solvent of water so as to be completely dissolved, thus obtaining reaction system；
In the mixed solvent with water for the Isosorbide-5-Nitrae-dioxane, Isosorbide-5-Nitrae-dioxane with the mass ratio of distilled water is
4:1；
Further, Isosorbide-5-Nitrae-diamino-anthraquinone adopts 0.001mol；Here, Isosorbide-5-Nitrae-diamino-anthraquinone with mix
The ratio of solvent determines response speed, can be according to concrete test situation depending on；
Step 2, reaction system is placed in 0 DEG C～5 DEG C of ice bath, using Cyanuric Chloride (TCT) as living
Property base, then to Deca Cyanuric Chloride solution and acid-capture agent in reaction system, until the condensation of reaction system is anti-
Should terminate；
In the present embodiment, acid-capture agent adopts the sodium hydroxide of 0.1M.Cyanuric Chloride and 1,4- diaminoanthraquinone-
The mol ratio of quinone is 1:3.
This step also includes：To during Deca Cyanuric Chloride solution in reaction system and acid-capture agent, right
Reaction system carries out magnetic agitation；In the present embodiment, the time of magnetic agitation is 2.5h.
Step 3, the reaction system that condensation reaction terminates is diluted, scrubbed, filter, be dried to obtain
Red cotton fiber dyestuff.
Here, for the ease of the record of Color afterwards, red cotton fiber dyestuff is designated as SCF-R1 dyestuff.
With reference to Figure 17, Figure 17 is the supercritical CO of the red cotton fiber dyestuff of third embodiment of the invention2
The process route chart of fluid dyeing.
As shown in figure 17, the supercritical CO of red cotton fiber dyestuff2Fluid colouring method comprises the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；In the present embodiment, coloring system also includes the preheating for preheating liquid carbon dioxide
Device, for injecting the booster pump of liquid carbon dioxide, be used for making supercritical CO2Fluid is in dyestuff kettle and dye
The circulating pump of circulation in color kettle.
Step S2, red cotton fiber dyestuff is dissolved in fluid modified agent, then puts into dyestuff kettle together
In, it is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
In this step, red cotton fiber dyestuff is the red SCF-R1 of active dispersal, and its addition content is 3%o.m.f；
Fluid modified agent is methanol, and its addition content is supercritical CO2The 10wt% of fluid.
In this step, dyeing caldron has hollow and tube wall is covered with the dyeing axle of through hole, usually, this dyeing
Axle is by stainless steel shaft it will be understood that dyeing axle can also be made up of other materials.Fabric is wound onto this dye
On colour axis.
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2The red cotton of fluid dissolving
Fiber dyes；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that super face
Boundary CO2Fluid carries cotton fiber surface and the inside that red cotton fiber dyestuff is diffused into fabric, and then completes
Dyeing；
In this step, temperature and the pressure required for dyeing is reached when the temperature and pressure in coloring system
During power, then can close booster pump, here, dyeing is temperature required to be 120 DEG C, and desirable pressure is
28MPa；Then open circulating pump, make supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron.Here,
Supercritical CO2Circulation in dyestuff kettle and dyeing caldron for the fluid be forward circulation and recycled back alternately,
To promote supercritical CO2The effect of fluid dyeing is more uniform；Wherein, supercritical CO2Fluid is in dyestuff
In kettle and dyeing caldron, the circulation time of circulation is 120min.
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
As shown in figure 18, Figure 18 is to carry out supercritical CO using SCF-R1 dyestuff2The cotton of fluid dyeing is knitted
The schematic diagram of thing.
From Fig. 4-7,11-14,18 can see, by SCF-Y1 dyestuff, SCF-B1 dyestuff and SCF-R1
Application is in supercritical CO2It is feasible in fluid dyeing；And SCF-Y1 dyestuff, SCF-B1 contaminate
Material and SCF-R1 dyestuff are in supercritical CO2In fluid, cotton fiber is shown with dye in very outstanding absorption
Characteristic, and the upper dye to cotton fiber and reaction set can be realized under 80 DEG C of lower temperature conditions.
The cotton fiber dyestuff of the present invention, because of its s-triazine type active group, can occur bonding reaction with cotton fiber, from
And make dye fixing on cotton fiber, reach the effect of dyeing.The cotton fiber dyestuff of the present invention has outstanding
Characteristic is contaminated on absorption.Additionally, the synthetic method craft process of the cotton fiber dyestuff of the present invention is simple；Therefore,
The cotton fiber dyestuff for Supercritical carbon dioxide fluid dyeing of the present invention and its synthetic method have very
Wide application prospect.
The invention of right described and claimed herein is not limited to the model of the specific embodiments disclosed in this
Enclose, because these embodiments are served only for the explanation of the several aspect of the present invention.Any embodiment of equal value is equal
To be within the scope of the invention.Really, those skilled in the art are appreciated that in this paper institute from previously described
Show with described embodiment outside can have various modifications.These modifications are also in the scope of the appended claims
Interior.
Claims (6)
1. one kind is used for supercritical CO2Fluid dyeing cotton fiber dyestuff colouring method it is characterised in that
Comprise the following steps：
Step S1, offer coloring system, this coloring system includes dyestuff kettle and dyeing caldron, dyestuff kettle and dye
Color kettle interconnects；
Step S2, cotton fiber dyestuff is dissolved in fluid modified agent, then puts in dyestuff kettle together,
It is then shut off dyestuff kettle；Fabric is put in dyeing caldron, turns off dyeing caldron；
Step S3, liquid carbon dioxide is injected in coloring system, then make coloring system rise gentle be pressurized,
Liquid carbon dioxide is made to be converted into supercritical CO2Fluid, and make this supercritical CO2Fluid dissolves cotton fiber
Dyestuff；Then make supercritical CO again2Fluid circulates in dyestuff kettle, dyeing caldron, so that supercritical CO2
Fluid carries cotton fiber surface and the inside that cotton fiber dyestuff is diffused into fabric, and then completes to dye；
Step S4, complete dyeing after, clean loose colour；Make coloring system cooling again and reduce pressure, finally, beat
Open dyeing caldron, take out the fabric after dyeing.
2. colouring method according to claim 1 is it is characterised in that described coloring system also includes
For the preheater of preheating liquid carbon dioxide, for injecting the booster pump of liquid carbon dioxide, being used for making
Supercritical CO2The circulating pump that fluid circulates in dyestuff kettle and dyeing caldron.
3. colouring method according to claim 1 is it is characterised in that described dyeing caldron has hollow
And tube wall is covered with the dyeing axle of through hole；Described step S2 also includes：By fabric wrapping on this dyeing axle.
4. colouring method according to claim 2 is it is characterised in that described step S3 also includes：
When reaching the temperature and pressure required for dyeing when the temperature and pressure in coloring system, close supercharging
Pump；Wherein, dyeing is temperature required is 80 DEG C -100 DEG C, and desirable pressure is 20MPa-30MPa；
Then open circulating pump, make supercritical CO2Fluid circulates in dyestuff kettle and dyeing caldron.
5. colouring method according to claim 4 is it is characterised in that supercritical CO2Fluid is in dye
Circulation in material kettle and dyeing caldron be forward circulation and recycled back alternately.
6. a kind of cotton fiber dyestuff using the colouring method dyeing as claim 1-5 any one, its
It is characterised by that there is s-triazine type active group.
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| CN201510505713.8A CN106468026A (en) | 2015-08-18 | 2015-08-18 | For supercritical CO2The cotton fiber dyestuff of fluid dyeing and its colouring method |
| PCT/CN2015/087662 WO2017028306A1 (en) | 2015-08-18 | 2015-08-20 | Cotton fiber dye for supercritical co2 fluid dyeing, and dyeing method thereof |
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| CN201510505713.8A CN106468026A (en) | 2015-08-18 | 2015-08-18 | For supercritical CO2The cotton fiber dyestuff of fluid dyeing and its colouring method |
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| CN109295768A (en) * | 2018-10-16 | 2019-02-01 | 苏州大学 | The anhydrous fine dyeing method of one kind of cotton |
| CN109355929A (en) * | 2018-10-16 | 2019-02-19 | 苏州大学 | It is a kind of using supercritical carbon dioxide fluid as the anhydrous fine dyeing method of medium |
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| CN109295768A (en) * | 2018-10-16 | 2019-02-01 | 苏州大学 | The anhydrous fine dyeing method of one kind of cotton |
| CN109355929A (en) * | 2018-10-16 | 2019-02-19 | 苏州大学 | It is a kind of using supercritical carbon dioxide fluid as the anhydrous fine dyeing method of medium |
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