CN108978260B - Dyeing method of natural beet red pigment - Google Patents
Dyeing method of natural beet red pigment Download PDFInfo
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- CN108978260B CN108978260B CN201810625333.1A CN201810625333A CN108978260B CN 108978260 B CN108978260 B CN 108978260B CN 201810625333 A CN201810625333 A CN 201810625333A CN 108978260 B CN108978260 B CN 108978260B
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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
- 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
- D06P1/34—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 natural dyestuffs
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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
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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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
- 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
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
-
- 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
- D06P1/64—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 using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/642—Compounds containing nitrogen
- D06P1/645—Aliphatic, araliphatic or cycloaliphatic compounds containing amino groups
-
- 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
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coloring (AREA)
Abstract
The invention relates to a dyeing method of natural beet red pigment. Firstly, performing crude extraction on beet red pigment in beet by using ethanol-water, and then purifying by using a supramolecular solvent and a recrystallization technology to obtain natural beet red pigment; and then modifying the fabric in a modifier solution, dyeing in a natural beet red pigment dyeing solution, washing the fabric with water after dyeing is finished, soaping the fabric, and drying to obtain the natural beet red pigment dyed fabric. The fabric prepared by the method for dyeing the beet red dye provided by the invention has high fastness, does not contain artificial pigments and has high safety.
Description
Technical Field
The invention relates to the field of extraction and application of natural active ingredients, in particular to a dyeing method of natural beet red pigment.
Background
Natural pigments refer to dyes extracted from plants, animals or minerals with little or no chemical processing. Compared with synthetic dyes, most natural pigments are nontoxic and harmless, have the health-care functions of resisting bacteria, preventing diseases, preventing ultraviolet rays, diminishing inflammation and the like, and show great application prospects in the textile field.
The genus red beet belongs to the Li family, the genus beta, is one of the important vegetables in Europe and America. The two-year-old herbaceous plant has high yield, low price and high content of the chromosox, and is a good source of the water-soluble edible red pigment. The betalain is one of natural edible pigments, is safe and nontoxic, has high nutritive value, has a plurality of medical health care effects on human bodies, can be used for treating human body dysfunction related to peroxidation stress, has the effects of resisting cancer, resisting radiation, enhancing immunity, strengthening the body, improving liver function, promoting digestive absorption and the like, is one of the safe and nontoxic natural pigments which are universal in the world, and therefore, the betalain for textile dyeing is developed and has important significance when being applied to the field of textile dyeing.
With the higher and higher requirements of people on the safety of clothes, the safety of the artificially synthesized pigment is more and more questioned. Consumers prefer safe and nontoxic natural pigments with functions of resisting oxidation and the like, so that the demand of the textile printing and dyeing industry for the natural pigments is gradually increased. Most of the traditional natural pigment extraction methods are organic solvent extraction or ultrasonic-assisted extraction methods, and impurities such as lipid, protein, polysaccharide and the like contained in the obtained pigment extract are difficult to be directly applied to textile printing and dyeing.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a preparation method of a natural pigment which is prepared by using beet as a pigment raw material, extracting the pigment by using ethanol-water, and purifying by using a supramolecular solvent and recrystallization and can be directly used for textile printing and dyeing.
In order to achieve the purpose, the invention adopts the following technical scheme:
a dyeing method of natural beet red pigment is characterized by comprising the following steps:
(1) cleaning and drying beet, pulverizing to obtain beet powder, mixing beet powder with ethanol-water mixture, leaching at 40-60 deg.C for 10-12 hr, filtering, leaching residue for 2-3 times, mixing filtrates, and concentrating the filtrate under reduced pressure to obtain beet red pigment extract;
(2) adding 1 time of supramolecular solvent into the extract of the beet red pigment, performing vortex and centrifugal washing for 3 times, dissolving the extract of the beet red pigment in a hot organic solvent, standing, cooling, crystallizing, performing suction filtration by using a Buchner funnel, and freeze-drying crystals to obtain the natural beet red pigment;
(3) dissolving a modifier and caustic soda in water to prepare a modified solvent;
(4) dissolving natural beet red pigment and inorganic salt in water to prepare a dyeing solution;
(5) the fabric is treated in a modifying solvent at a temperature of 1: 15-25 of bath ratio, washing for 2-3 times after modification treatment for 1-2 hours at 30-50 ℃, putting the modified fabric into a dyeing solution, and reacting at a temperature of 1: dyeing for 1.5-2.5 hours at the temperature of 30-85 ℃ with the bath ratio of 35-50, and after dyeing is finished, washing the fabric with water, soaping and drying to obtain the natural beet red pigment dyed fabric.
Preferably, the mass-to-volume ratio of the beet powder and the ethanol-water mixed solution in the step (1) is 1: 15-25; the volume fraction of the ethanol in the ethanol-water mixed solution is 25-40%.
Preferably, the density of the beet red pigment extract in the step (1) is not lower than 1.20 g/mL.
Preferably, the preparation method of the supramolecular solvent in the step (2) comprises the following steps: tetrahydrofuran, water and n-octanol are mixed according to the weight ratio of 35-50: 35-55: 30-45, and after vortex ultrasonic treatment, the centrifugal system is divided into two phases, and the upper phase is taken as the supermolecule solvent.
Preferably, the organic solvent in step (2) is: one of ethyl acetate, petroleum ether and propanol.
Preferably, the modifier in the step (3) is one of modifiers CR-2000, triethylene tetramine and Indosole E-50; the concentration of caustic soda in the modified solvent is 10-20g/L, and the concentration of the modifier is 65-100 g/L.
Preferably, the inorganic salt in the step (4) is Na2SO4、NaCl、Na2HPO4、K2SO4One kind of (1).
Preferably, the concentration of the beet red pigment in the dyeing solution in the step (4) is 0.5-2g/L, and the concentration of the inorganic salt is 80-120 g/L.
Preferably, the fabric in the step (5) is one of cotton fabric, hemp fabric, wool fabric and silk fabric.
Compared with the prior art, the dyeing method of the natural beet red pigment has the following beneficial effects that the beet red pigment with high natural pigment purity, which is prepared by extracting the pigment with water and then purifying the pigment with a supermolecular solvent and recrystallization, can be directly used as a dye for textile printing and dyeing; the dyeing method of the beet red dye provided by the invention adopts the modifier to treat the fabric, and the dyed fabric has high color fastness. The fabric prepared by the invention does not contain artificial pigment, and has high safety; in addition, the active ingredients contained in the beet red pigment enable the fabric to have the effects of enhancing immunity and building bodies.
Detailed Description
[ example 1 ]
A dyeing method of natural beet red pigment is characterized by comprising the following steps:
(1) washing beet completely, drying, pulverizing to obtain beet powder, mixing beet powder with 25% ethanol-water mixture at a ratio of 1: 10, leaching for 10 hours at 45 ℃, filtering, continuously leaching residues for 3 times, combining filtrates, and concentrating the filtrates under reduced pressure to obtain a beet red pigment extract;
(2) adding 1 time of supramolecular solvent into the extract of the beet red pigment, performing vortex and centrifugal washing for 3 times, dissolving the extract of the beet red pigment in hot ethyl acetate, standing, cooling, crystallizing, performing suction filtration by using a Buchner funnel, and freeze-drying crystals to obtain natural beet red pigment;
(3) dissolving CR-2000 and caustic soda in water to prepare a modified solvent containing 15g/L of caustic soda and 80 g/LCR-2000;
(4) mixing natural beet red pigment and Na2SO4Dissolving in water to obtain a solution containing betalain 0.8g/L and 100g/LNa2SO4The dyeing solution of (1);
(5) placing cotton fabric in a modified solvent, and performing reaction on the cotton fabric in a solvent of 1: and (3) after modification treatment for 1 hour at the temperature of 40 ℃ at the bath ratio of 20, washing with water for 3 times, placing the modified fabric into a dyeing solution, dyeing for 1.5 hours at the temperature of 65 ℃ at the bath ratio of 140, and after dyeing is finished, washing and soaping the fabric with water and drying to obtain the natural beet red pigment dyed cotton fabric.
[ example 2 ]
A dyeing method of natural beet red pigment is characterized by comprising the following steps:
(1) cleaning and drying beet, pulverizing to obtain beet powder, mixing beet powder with 30% ethanol-water mixture at a ratio of 1: 15, leaching for 10 hours at 45 ℃, filtering, continuously leaching residues for 2 times, combining filtrates, and concentrating the filtrates under reduced pressure to obtain a beet red pigment extract;
(2) adding 1 time of supramolecular solvent into the extract of the beet red pigment, performing vortex and centrifugal washing for 3 times, dissolving the extract of the beet red pigment in hot ethyl acetate, standing, cooling, crystallizing, performing suction filtration by using a Buchner funnel, and freeze-drying crystals to obtain natural beet red pigment;
(3) dissolving triethylene tetramine and caustic soda in water to prepare a modified solvent containing 20g/L of caustic soda and 70g/L of triethylene tetramine;
(4) dissolving natural beet red pigment and NaCl in water to prepare a dyeing solution containing 0.7g/L of beet red pigment and 110g/L of NaCl;
(5) the wool fabric is put in a modified solvent, and the weight ratio of 1: after a modification treatment at 45 ℃ for 2 hours at a bath ratio of 20, the fabric was washed 3 times with water, and the modified fabric was placed in a dyeing solution at a temperature of 1: dyeing for 2 hours at the temperature of 70 ℃ with the bath ratio of 45, and after dyeing is finished, washing the fabric with water, soaping and drying to obtain the natural beet red pigment dyed wool fabric.
[ example 3 ]
A dyeing method of natural beet red pigment is characterized by comprising the following steps:
(1) cleaning and drying beet, pulverizing to obtain beet powder, mixing beet powder with 35% ethanol-water mixture at a ratio of 1: 15, leaching for 10 hours at 40 ℃, filtering, continuously leaching residues for 2 times, combining filtrates, and concentrating the filtrates under reduced pressure to obtain a beet red pigment extract;
(2) adding 1 time of supramolecular solvent into the extract of the beet red pigment, performing vortex and centrifugal washing for 3 times, dissolving the extract of the beet red pigment in hot petroleum ether, standing, cooling, crystallizing, performing suction filtration by using a Buchner funnel, and freeze-drying crystals to obtain the natural beet red pigment;
(3) dissolving Indosole E-50 and caustic soda in water to prepare a modified solvent containing 15g/L of caustic soda and 65g/LIndosol E-50;
(4) dissolving natural beet red pigment and NaCl in water to prepare a dyeing solution containing 0.7g/L of the beet red pigment and 110g/L of LNaCl;
(5) placing the linen fabric in a modified solvent, and performing the following steps of 1: after a modification treatment at 50 ℃ for 2 hours at a bath ratio of 20, the fabric was washed 3 times with water, and the modified fabric was placed in a dyeing solution at a temperature of 1: dyeing for 2 hours at the temperature of 80 ℃ in a bath ratio of 45, and after dyeing is finished, washing the fabric with water, soaping and drying to obtain the natural beet red pigment dyed linen fabric.
And (3) testing color fastness:
the natural beet red vegetarian fabrics prepared in examples 1-3 were tested according to the following criteria and the results are shown in table 1:
the light fastness is tested according to GB/T8426-1998 light fastness and sunlight resistance of textile color fastness test.
The rubbing fastness is tested according to GB/T3920-2008 'color fastness to rubbing' test for textiles.
The soaping fastness is tested according to GB/T3921-2008 soaping fastness resistance color fastness of textile color fastness test.
TABLE 1 color fastness of the naturally beet red pigment dyed fabrics obtained in examples 1-3.
As can be seen from Table 1, after cotton fabrics, wool fabrics and linen fabrics are dyed by the dyeing method, the color fastness of the fabrics is all at level 4 or above, which shows that the dyeing method of the invention has good dyeing effect.
It is obvious to those skilled in the art that the present invention is not limited to the above embodiments, and it is within the scope of the present invention to adopt various insubstantial modifications of the method concept and technical scheme of the present invention, or to directly apply the concept and technical scheme of the present invention to other occasions without modification.
Claims (3)
1. A dyeing method of natural beet red pigment is characterized by comprising the following steps:
(1) cleaning and drying beet, pulverizing to obtain beet powder, mixing beet powder with ethanol-water mixture, leaching at 40-60 deg.C for 10-12 hr, filtering, leaching residue for 2-3 times, mixing filtrates, and concentrating the filtrate under reduced pressure to obtain beet red pigment extract;
(2) adding 1 time of supramolecular solvent into the extract of the beet red pigment, performing vortex and centrifugal washing for 3 times, dissolving the extract of the beet red pigment in a hot organic solvent, standing, cooling, crystallizing, performing suction filtration by using a Buchner funnel, and freeze-drying crystals to obtain the natural beet red pigment;
(3) dissolving a modifier and caustic soda in water to prepare a modified solvent;
(4) dissolving natural beet red pigment and inorganic salt in water to prepare a dyeing solution;
(5) the fabric is treated in a modifying solvent at a temperature of 1: 15-25 of bath ratio, modified treatment is carried out for 1-2 hours at 40-50 ℃, then the fabric is washed for 2-3 times by water, and the modified fabric is placed in a dyeing solution, and the dyeing solution is mixed with water and the mixture is subjected to the following steps of 1: dyeing for 1.5-2.5 hours at 65-85 ℃ with a bath ratio of 35-50, washing the fabric with water and soaping after dyeing is finished, drying to obtain the natural beet red pigment dyed fabric,
wherein the mass-volume ratio of the beet powder in the step (1) to the ethanol-water mixed solution is 1: 15-25; the volume fraction of ethanol in the ethanol-water mixed solution is 25-40%;
the preparation method of the supramolecular solvent in the step (2) comprises the following steps: tetrahydrofuran, water and n-octanol are mixed according to the weight ratio of 35-50: 35-55: 30-45, performing vortex ultrasonic treatment, separating a centrifugal system into two phases, and taking the upper phase as the supramolecular solvent; the organic solvent is: one of ethyl acetate, petroleum ether and propanol;
the modifier in the step (3) is one of modifiers CR-2000, triethylene tetramine and Indosol E-50; the concentration of caustic soda in the modified solvent is 10-20g/L, and the concentration of the modifier is 65-100 g/L;
the inorganic salt in the step (4) is Na2SO4、NaCl、Na2HPO4、K2SO4One of (1); the dyeing is carried outThe concentration of the beet red pigment in the solution is 0.5-2g/L, and the concentration of the inorganic salt is 80-120 g/L.
2. The method for dyeing natural betalain pigment according to claim 1, wherein the density of the betalain extract in step (1) is not lower than 1.20 g/mL.
3. The method for dyeing natural betalain pigment according to claim 1, wherein the fabric in the step (5) is one of cotton fabric, hemp fabric, wool fabric and silk fabric.
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| CN201810625333.1A CN108978260B (en) | 2018-06-18 | 2018-06-18 | Dyeing method of natural beet red pigment |
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Citations (5)
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| CN102644204A (en) * | 2012-04-24 | 2012-08-22 | 大连工业大学 | Method for dyeing modified cellulose fabrics by green walnut epicarp pigment |
| CN102899930A (en) * | 2011-07-26 | 2013-01-30 | 李发勇 | Hematoxylon dyeing method applied on original bamboo fiber bedding |
| CN103614933A (en) * | 2013-12-12 | 2014-03-05 | 新疆大学 | Dyeing method for dyeing cellulose fiber by utilizing walnut green seedcase natural dye |
| CN105544239A (en) * | 2016-01-21 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Bamboo fiber dyeing method based on natural mangosteen dye |
| CN107130446A (en) * | 2017-06-06 | 2017-09-05 | 河南科恩生物科技有限公司 | Red pigments extracts and its to the method for textile dyeing in a kind of cape jasmine fruit |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163098B (en) * | 2017-06-28 | 2019-08-09 | 江苏优之食品有限公司 | A kind of extracting method of natural high-purity mogroside |
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- 2018-06-18 CN CN201810625333.1A patent/CN108978260B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899930A (en) * | 2011-07-26 | 2013-01-30 | 李发勇 | Hematoxylon dyeing method applied on original bamboo fiber bedding |
| CN102644204A (en) * | 2012-04-24 | 2012-08-22 | 大连工业大学 | Method for dyeing modified cellulose fabrics by green walnut epicarp pigment |
| CN103614933A (en) * | 2013-12-12 | 2014-03-05 | 新疆大学 | Dyeing method for dyeing cellulose fiber by utilizing walnut green seedcase natural dye |
| CN105544239A (en) * | 2016-01-21 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Bamboo fiber dyeing method based on natural mangosteen dye |
| CN107130446A (en) * | 2017-06-06 | 2017-09-05 | 河南科恩生物科技有限公司 | Red pigments extracts and its to the method for textile dyeing in a kind of cape jasmine fruit |
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