CN109400738B - Preparation of modified burdock polysaccharide and application of modified burdock polysaccharide in reactive dye dyeing - Google Patents
Preparation of modified burdock polysaccharide and application of modified burdock polysaccharide in reactive dye dyeing Download PDFInfo
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- 241000208843 Arctium Species 0.000 title claims abstract description 121
- 235000003130 Arctium lappa Nutrition 0.000 title claims abstract description 120
- 235000008078 Arctium minus Nutrition 0.000 title claims abstract description 120
- 150000004676 glycans Chemical class 0.000 title claims abstract description 95
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 95
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 95
- 238000004043 dyeing Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000985 reactive dye Substances 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000002244 precipitate Substances 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000006228 supernatant Substances 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000006266 etherification reaction Methods 0.000 claims abstract description 10
- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010298 pulverizing process Methods 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 49
- 239000004744 fabric Substances 0.000 claims description 40
- 229920000742 Cotton Polymers 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 230000001276 controlling effect Effects 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 2
- 239000000975 dye Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000835 fiber Substances 0.000 abstract description 5
- 238000004132 cross linking Methods 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000000643 oven drying Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- 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
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- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
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- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The invention relates to a preparation method of modified burdock polysaccharide and application of the modified burdock polysaccharide in reactive dye dyeing, belonging to the technical field of dyeing, wherein the preparation method of the modified burdock polysaccharide comprises the following steps: vacuum drying burdock, pulverizing into powder, extracting with sodium hydroxide in a reactor, regulating pH of the extracted supernatant to 3.0 with hydrochloric acid, centrifuging, collecting supernatant, concentrating the supernatant under reduced pressure, mixing with ethanol solution, precipitating precipitate, centrifuging the obtained supernatant, collecting precipitate, oven drying at 60 deg.C to constant weight to obtain burdock polysaccharide, and modifying burdock polysaccharide with 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to obtain modified burdock polysaccharide. According to the invention, the burdock polysaccharide is extracted from natural plant burdock, and then the burdock polysaccharide is subjected to etherification modification to prepare the modified burdock polysaccharide, so that the film forming property of the modified burdock polysaccharide is improved, and the modified burdock polysaccharide can generate a crosslinking effect with dye and fiber, thereby playing a good color fixing role.
Description
Technical Field
The invention relates to the technical field of dyeing, in particular to preparation of modified burdock polysaccharide and application of the modified burdock polysaccharide in reactive dye dyeing.
Background
Some water-soluble groups exist in the molecular structure of the reactive dye, the dyeing fastness, particularly the color fastness to washing, is often poor, and a color fixing mode is needed to improve the dyeing fastness. Most of the color fixing agents used in the printing and dyeing industry of China for a long time contain free formaldehyde, so that the color fixing agents not only have great harm to the environment, but also can cause harm to human health when being worn. In recent years, some novel color fixing agents such as cationic resin type color fixing agents, quaternary ammonium salt formaldehyde-free color fixing agents, quaternized reaction type formaldehyde-free color fixing agents and the like are developed, although the formaldehyde-free color fixing agents, the wet rubbing fastness of the reactive dye is still not ideal, and for the reactive dye, the requirements of excellent washing fastness and wet rubbing fastness of the reactive dye are not met. Therefore, there is a need for a new dye fixing agent, which not only can improve the color fastness of fabrics, but also has the characteristics of environmental protection and safety.
Disclosure of Invention
The technical problem to be solved is as follows:
aiming at the problems pointed out in the background art and the defects in the prior art, the invention aims to provide a preparation method of modified burdock polysaccharide and an application of the modified burdock polysaccharide in reactive dye dyeing.
The technical scheme is as follows:
the invention provides a preparation method of modified burdock polysaccharide, which comprises the following preparation steps:
(1) vacuum drying burdock, pulverizing with a pulverizer, sieving with 40 mesh sieve, and drying burdock powder;
(2) putting dried burdock powder into a reactor, adding a sodium hydroxide solution, controlling the material-liquid ratio, and carrying out extraction reaction;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution, standing at-4 deg.C for 12h, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving the burdock polysaccharide in isopropanol solution, adding sodium hydroxide and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction, cooling to room temperature after the reaction is finished, carrying out suction filtration to remove redundant liquid, washing the product for 4 times by using distilled water, and drying to obtain the modified burdock polysaccharide.
Preferably, the feed-liquid ratio in the step (2) is 1 (30-40), and the unit of the feed-liquid ratio is g/mL.
Preferably, the temperature of the extraction reaction in the step (2) is 60-90 ℃, and the extraction time is 4-8 h.
Preferably, the volume ratio of the concentrated solution to the 90 wt% ethanol solution in the step (4) is 1: 1.
Preferably, the weight ratio of the burdock polysaccharide, the sodium hydroxide and the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride in the step (6) is as follows: 1:(0.1-0.2): (0.05-0.15).
Preferably, the temperature of the etherification reaction in the step (6) is 50-70 ℃ and the time is 3-5 h.
The invention also provides an application method of the modified burdock polysaccharide in reactive dye dyeing, which comprises the following steps: dyeing the cotton fabric by using reactive black for 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water to obtain a modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, baking the dyed cotton fabric at 135 ℃ for 3min after drying, washing the dyed cotton fabric for 10min, and drying the dyed cotton fabric at 90 ℃.
Has the advantages that:
(1) according to the test results, the burdock polysaccharide is extracted from natural plants, the method is safe and environment-friendly, and the prepared modified burdock polysaccharide can be crosslinked on the surface of cotton fabric fibers to form a film and can generate a crosslinking effect with dyes and fibers, so that a good color fixing effect is achieved.
(2) The invention has the advantages of wide raw material source, low cost, no formaldehyde and other harmful substances, simple and easy operation of the preparation process, no environmental pollution and wide application prospect.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
(1) Vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:40, wherein the unit of the material-liquid ratio is g/mL, heating to 60 ℃, and extracting for 8 hours;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving 10g of burdock polysaccharide in 2L of 80 wt% isopropanol solution, adding 1g of sodium hydroxide and 1.5g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction for 5h at 50 ℃, then cooling to room temperature, carrying out suction filtration to remove redundant liquid, washing the product with distilled water for 4 times, and drying at 55 ℃ for 24h to obtain the modified burdock polysaccharide.
The application method of the modified burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Example 2
(1) Vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:30, wherein the unit of the material-liquid ratio is g/mL, heating to 90 ℃, and extracting for 4 hours;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving 10g of burdock polysaccharide in 2L of 80 wt% isopropanol solution, adding 2g of sodium hydroxide and 0.5g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction for 3h at 70 ℃, then cooling to room temperature, carrying out suction filtration to remove redundant liquid, washing the product with distilled water for 4 times, and drying at 55 ℃ for 24h to obtain the modified burdock polysaccharide.
The application method of the modified burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Example 3
(1) Vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:38, wherein the unit of the material-liquid ratio is g/mL, heating to 70 ℃, and extracting for 7 hours;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving 10g of burdock polysaccharide in 2L of 80 wt% isopropanol solution, adding 1.4g of sodium hydroxide and 1.2g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction for 4.5h at 55 ℃, then cooling to room temperature, carrying out suction filtration to remove redundant liquid, washing the product for 4 times with distilled water, and drying for 24h at 55 ℃ to obtain the modified burdock polysaccharide.
The application method of the modified burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Example 4
(1) Vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:32, wherein the unit of the material-liquid ratio is g/mL, heating to 80 ℃, and extracting for 5 hours;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving 10g of burdock polysaccharide in 2L of 80 wt% isopropanol solution, adding 1.6g of sodium hydroxide and 0.8g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction for 3.5h at 65 ℃, then cooling to room temperature, carrying out suction filtration to remove redundant liquid, washing the product for 4 times with distilled water, and drying for 24h at 55 ℃ to obtain the modified burdock polysaccharide.
The application method of the modified burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Example 5
(1) Vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:36, wherein the unit of the material-liquid ratio is g/mL, heating to 75 ℃, and extracting for 6 h;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving 10g of burdock polysaccharide in 2L of 80 wt% isopropanol solution, adding 1.5g of sodium hydroxide and 1g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction for 4h at 60 ℃, then cooling to room temperature, carrying out suction filtration to remove redundant liquid, washing the product with distilled water for 4 times, and drying at 55 ℃ for 24h to obtain the modified burdock polysaccharide.
The application method of the modified burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Comparative example 1
The comparative example differs from example 1 in that the burdock polysaccharide was not modified. Specifically, the method comprises the following steps:
(1) vacuum drying burdock at 70 deg.C for 4 hr, pulverizing with pulverizer to 40 mesh sieve, and drying burdock powder at 60 deg.C for 12 hr;
(2) putting dried burdock powder into a reactor, adding 1 wt% of sodium hydroxide solution, controlling the material-liquid ratio to be 1:40, wherein the unit of the material-liquid ratio is g/mL, heating to 60 ℃, and extracting for 8 hours;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant at 60 deg.C under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution at a ratio of 1:1, standing at-4 deg.C for 12 hr, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), centrifuging at 4000r/min for 20min, collecting the precipitate, and drying at 60 ℃ to constant weight to obtain the burdock polysaccharide.
The application method of the burdock polysaccharide comprises the following steps: dyeing cotton fabric by using active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, and drying the dyed cotton fabric for later use; dissolving burdock polysaccharide in deionized water, and uniformly mixing to obtain a 2 wt% burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, drying at 90 ℃, then baking at 135 ℃ for 3min, washing with water for 10min, and then drying at 90 ℃.
Comparative example 2
This comparative example differs from example 1 in that no modified burdock polysaccharide treatment was used. Specifically, the method comprises the following steps:
dyeing cotton fabric with active black W-NNHC, wherein the dye consumption is 5% (o.m.f), the bath ratio is 1:20, the dyeing time is 30s, drying the dyed cotton fabric, baking the cotton fabric at 135 ℃ for 3min, washing the cotton fabric with water for 10min, and drying the cotton fabric at 90 ℃.
The treated cotton fabrics of examples 1-5 and comparative examples 1-2 were subjected to performance tests: the color fastness to washing is determined according to GB/T3921-4-1997, the rubbing fastness is determined according to GB/T3920-1997, and the test results are shown in the following table:
according to the test results, the burdock polysaccharide is extracted from natural plants, the method is safe and environment-friendly, and the prepared modified burdock polysaccharide can be crosslinked on the surface of cotton fabric fibers to form a film and can generate a crosslinking effect with dyes and fibers, so that a good color fixing effect is achieved. The modified burdock polysaccharide prepared by the preparation process in the example 5 has the best color fixing effect, and the cotton fabric treated by the burdock polysaccharide in the example 5 has the color fastness to washing of 4 grades, the color fastness to dry rubbing of 5 grades and the color fastness to wet rubbing of 4-5 grades. In the comparative example 2, the modified burdock polysaccharide is not adopted for treatment, the color fastness to washing is 1-2 grade, the dry rubbing fastness is 2 grade, and the wet rubbing fastness is 1-2 grade, so that the modified burdock polysaccharide is proved to be an effective color fixing agent in the invention. Compared with the comparative example 2, the performance of the treatment of the unmodified burdock polysaccharide in the comparative example 1 is improved, but the color fixing effect is not as good as that of the example 1, which shows that the unmodified burdock polysaccharide can play a certain color fixing role.
Claims (7)
1. The preparation method of the modified burdock polysaccharide is characterized by comprising the following preparation steps:
(1) vacuum drying burdock, pulverizing with a pulverizer, sieving with 40 mesh sieve, and drying burdock powder;
(2) putting dried burdock powder into a reactor, adding a sodium hydroxide solution, controlling the material-liquid ratio, and carrying out extraction reaction;
(3) filtering the extracting solution in the step (2), taking supernate, regulating the pH value of the supernate to 3.0 by using hydrochloric acid, centrifuging the supernate for 20min at 4000r/min, and collecting the supernate;
(4) concentrating the supernatant under reduced pressure to half of the original volume, mixing the concentrated solution with 90 wt% ethanol solution, standing at-4 deg.C for 12h, and separating out precipitate;
(5) centrifuging the supernatant of the precipitate separated out in the step (4), collecting the precipitate, and drying at 60 ℃ to constant weight to obtain burdock polysaccharide;
(6) dissolving the burdock polysaccharide in isopropanol solution, adding sodium hydroxide and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, carrying out etherification reaction, cooling to room temperature after the reaction is finished, carrying out suction filtration to remove redundant liquid, washing the product for 4 times by using distilled water, and drying to obtain the modified burdock polysaccharide.
2. The preparation method of the modified burdock polysaccharide according to claim 1, wherein the feed-liquid ratio in the step (2) is 1 (30-40), and the unit of the feed-liquid ratio is g/mL.
3. The preparation method of the modified burdock polysaccharide according to claim 1, wherein the extraction reaction in the step (2) is carried out at the temperature of 60-90 ℃ for 4-8 h.
4. The preparation method of the modified burdock polysaccharide as claimed in claim 1, wherein the volume ratio of the concentrated solution to the 90 wt% ethanol solution in the step (4) is 1: 1.
5. The preparation method of the modified burdock polysaccharide according to claim 1, wherein the weight ratio of the burdock polysaccharide, the sodium hydroxide and the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride in the step (6) is as follows: 1:(0.1-0.2): (0.05-0.15).
6. The preparation method of the modified burdock polysaccharide as claimed in claim 1, wherein the temperature of the etherification reaction in the step (6) is 50-70 ℃ and the time is 3-5 hours.
7. The application of the modified burdock polysaccharide prepared by the preparation method of the modified burdock polysaccharide in reactive dye dyeing according to claim 1 is characterized by comprising the following steps: dyeing the cotton fabric by using reactive black for 30s, and drying the dyed cotton fabric for later use; dissolving the modified burdock polysaccharide in deionized water to obtain a modified burdock polysaccharide solution; soaking the dyed cotton fabric in the modified burdock polysaccharide solution for two times and two times, wherein the rolling residual rate is 75%, baking the dyed cotton fabric at 135 ℃ for 3min after drying, washing the dyed cotton fabric for 10min, and drying the dyed cotton fabric at 90 ℃.
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