CN111621995B - Preparation method of dye composition - Google Patents
Preparation method of dye composition Download PDFInfo
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- CN111621995B CN111621995B CN202010428880.8A CN202010428880A CN111621995B CN 111621995 B CN111621995 B CN 111621995B CN 202010428880 A CN202010428880 A CN 202010428880A CN 111621995 B CN111621995 B CN 111621995B
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- dyeing
- dye composition
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- leveling agent
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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
- D06P1/46—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 natural macromolecular substances or derivatives thereof
- D06P1/48—Derivatives of carbohydrates
-
- 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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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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
- D06P1/16—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 dispersed, e.g. acetate, dyestuffs
-
- 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
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
-
- 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
- D06P2001/0088—Aqueous dyeing characterised by a short bath ratio
- D06P2001/0092—Foam dyeing
Abstract
The invention relates to a preparation method of a dye composition, which comprises the steps of preparing a suspension from disperse dye, sodium dodecyl sulfate, glycerol, a dispersing agent and water, grinding the suspension until the particle size of the disperse dye is 30-50 nm, and then adding a leveling agent and acetic acid to prepare the dye composition. The dye composition is suitable for continuous pad dyeing and coating dyeing, and compared with dye vat dyeing under high temperature and high pressure, the dye composition can reduce energy consumption, improve dyeing efficiency, improve product quality, enable the color fastness and color uniformity of fabrics to reach the grade A specified by the national standard, and enable continuous dyeing under normal temperature and normal pressure to replace high temperature and high pressure dye vat dyeing to be possible.
Description
The invention relates to a leveling agent, a preparation method thereof and divisional application of the leveling agent, wherein the application date of the leveling agent is 2018, 3 and 2, the application number of the leveling agent is 2018101739413.
Technical Field
The invention belongs to the technical field of textile printing and dyeing, and particularly relates to a preparation method of a dye composition suitable for continuous pad-type or coating-type dyeing of polyester fabrics at normal temperature and normal pressure.
Background
The textile industry makes a great contribution to the economic development of China, and over 5000 thousands of workers in the textile printing and dyeing industry develop to the problems of very serious environmental pollution and energy shortage. The daily discharge amount of the printing and dyeing wastewater reaches 600 million tons, the components are complex and variable, the concentration is high, the chroma is deep, the COD value and the Cr value are large, and meanwhile, the printing and dyeing wastewater also contains various toxic and harmful substances, so that the great difficulty is brought to the wastewater treatment and the standard discharge. Meanwhile, the printing and dyeing industry is also a resource consumption type industry, and the average energy consumption per ton of fiber is 2.84 tons of standard coal. The energy consumption of water, electricity and steam of a printing and dyeing mill accounts for 40-60% of the total cost of printing and dyeing cloth, so that the reduction of the energy consumption is the key for improving the competitiveness of products, the energy conservation and emission reduction become basic policies for development in China, and the reduction of the emission of greenhouse gases also becomes the most important problem for economic development.
In order to realize energy conservation and emission reduction, all enterprises and scientific research institutions research textile dyeing technology with less water and no water, but the supercritical carbon dioxide technology has no wastewater discharge, but the production cost is dozens of times of the dyeing cost of a dye vat; although the organic solvent dyeing technology does not discharge waste water, once the organic solvent is leaked, the difficulty of pollution control and the risk of fire are increased; although the continuous dyeing method under normal temperature and normal pressure has the advantages of high production speed, low energy consumption and no wastewater discharge, the finished product can not reach the grade A specified in the national standard GB 18401-2010 because the contact time of the dye and the textile is very short and the uniformity and the color fastness of the coloring are very poor.
The polyester fiber has wide application field, accounts for more than 60 percent of the total amount of the synthetic fiber, but has strong hydrophobicity, lacks active groups capable of reacting with dye molecules in a molecular structure, has compact molecular arrangement, only has small gaps in the fiber, and is difficult to dye under the condition of normal temperature and normal pressure without proper auxiliary agents. Only when the movement of the fiber molecular chain is aggravated by long-time heating, enough gaps can be generated to enable the dye to enter the fiber and be attached, so that the energy consumption and the wastewater amount are both extremely large. In order to realize continuous and rapid dyeing at normal temperature and normal pressure so as to achieve the purposes of reducing wastewater discharge and reducing energy consumption, an auxiliary agent is required to be added into a dye bath to help disperse dye to be rapidly and uniformly attached to a fabric.
201710343323.4 discloses a chitosan derivative useful as a dispersant, the chitosan derivative having the formula:
m is alkali metal, and the relative molecular mass of the chitosan derivative is 5500-10000. And (3) soaking a piece of desized small fabric of 25 x 15cm into the dye composition added with the dispersing agent for 1min at normal temperature and normal pressure, rolling and drying to obtain a product, wherein the washing color fastness and the rubbing color fastness of the product reach 4-5 levels.
However, when the chitosan derivative dispersant is added into a dye to perform large-scale continuous dyeing at normal temperature and normal pressure, because the contact time between the dye and a fabric is very short, only 10-20 s, and the area of the fabric is enlarged, even if the disperse dye is ground to be within a nanometer range under the action of the dispersant, the dyeing uniformity still cannot be realized, and the difference of the front and back colors caused by migration in the drying and color development processes cannot be avoided.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a leveling agent suitable for large-scale continuous pad-type or coating-type dyeing of polyester fabrics at normal temperature and normal pressure, a preparation method of the leveling agent, a dye composition added with the leveling agent and a continuous pad-type or coating-type dyeing method.
In order to solve the technical problems, the invention adopts a technical scheme that:
one object of the present invention is to provide a leveling agent, which has the structural formula:
wherein n is a number between 5 and 10.
The invention also aims to provide a preparation method of the leveling agent, which comprises the following steps:
performing reflux reaction on oleic acid and hydrogen bromide in the presence of a solvent to obtain a product A, wherein the structural formula of the product A is as follows:
reacting chitosan with the product A in the presence of alkali and a solvent at 80-100 ℃ to obtain a product B, wherein the structural formula of the product B is as follows:
and (3) reacting glycerol and the product B at 140-150 ℃ in the presence of a catalyst and a water-carrying agent under the protection of nitrogen to obtain the leveling agent.
Preferably, in the step (1), the feeding mass ratio of the oleic acid to the hydrogen bromide is 1: 0.28-0.35.
Preferably, in the step (2), the feeding mass ratio of the chitosan to the product A is 1: 2.30-2.40.
Preferably, in the step (3), the feeding mass ratio of the glycerol to the product B is 1: 16.50-17.50.
Preferably, the solvent used in the step (1) is chloroform, and the mass ratio of the oleic acid to the chloroform is 1: 1.78-2.14.
Preferably, the alkali adopted in the step (2) is sodium hydroxide, the solvent adopted is carbon tetrachloride, and the mass ratio of the chitosan to the sodium hydroxide to the carbon tetrachloride is 1: 0.50-0.60: 5.00-6.00.
Preferably, the catalyst used in the step (3) is HND-33 solid super acidic catalyst, the water-carrying agent used is toluene, and the mass ratio of the glycerol to the catalyst to the water-carrying agent is 1: 0.07-0.09: 4.00-4.25.
Preferably, the chitosan adopted in the step (2) is water-soluble chitosan with the relative molecular mass of 1000-1200 and the deacetylation degree of more than 90%.
According to a preferred and specific embodiment, the preparation process is carried out in the following specific embodiment:
adding the oleic acid, the hydrogen bromide and the solvent into a reactor under the ice-water bath condition, refluxing by using a condensing tube, stirring for reaction for 30-50 min, washing the product to be neutral by using water, and distilling the solvent and the unreacted hydrogen bromide at 70-75 ℃ to obtain a product A;
adding the chitosan, the alkali and the product A into the solvent, stirring and reacting for 3-4 hours at 80-100 ℃, and then distilling under reduced pressure at 35-45 ℃ to obtain a product B;
and (3) adding the glycerol, the product B, the catalyst and the water-carrying agent into a reactor with a water separator, introducing nitrogen to protect the product B, controlling the reaction temperature to be 140-150 ℃, enabling water generated by the reaction to form an azeotrope along with the water-carrying agent to flow out of the water separator, cooling to 45-55 ℃ after reacting for 4-5 hours, extracting with water, crystallizing the extract at-15-5 ℃, and filtering to obtain the leveling agent.
The third purpose of the invention is to provide the application of the leveling agent in textile printing and dyeing.
In particular to the application of the leveling agent in continuous padding type or coating type dyeing.
The fourth purpose of the invention is to provide a dye composition suitable for continuous pad-dyeing, which comprises a dye solution, and the dye composition also comprises the leveling agent, wherein the feeding mass of the leveling agent is that 1-2 g of the leveling agent is added into 1L of the dye solution.
Preferably, the dye composition further comprises acetic acid for adjusting the pH value of the dye composition to 5.5-6.0.
Preferably, the dye solution comprises disperse dye accounting for 2-5% of the total mass of the dye solution.
Further preferably, the dye liquor further comprises sodium dodecyl sulfate accounting for 3-5% of the total mass of the dye liquor, glycerol accounting for 2-3% of the total mass of the dye liquor, a dispersing agent accounting for 1-2% of the total mass of the dye liquor and water.
According to a specific embodiment, the dye liquor comprises 2-5% of disperse dye, 3-5% of sodium dodecyl sulfate, 2-3% of glycerol, 1-2% of dispersing agent and water by mass fraction of 100%.
Preferably, the preparation method of the dye composition comprises the following steps: preparing the disperse dye, the sodium dodecyl sulfate, the glycerin, the dispersing agent and water into suspension, grinding the suspension until the particle size of the disperse dye is 30-50 nm, and then adding the leveling agent and the acetic acid to prepare the dye composition.
The fifth purpose of the invention is to provide a dye composition suitable for continuous coating type dyeing, which comprises a dye solution, and further comprises a leveling agent, a foaming agent and sodium alginate, wherein the feeding mass of the leveling agent is that 1-2 g of the leveling agent is added into each 1L of the dye solution, the feeding mass of the foaming agent is that 10-15 g of the foaming agent is added into each 1L of the dye solution, and the feeding mass of the sodium alginate is that 80-100 g of the sodium alginate is added into each 1L of the dye solution.
Preferably, the dye composition further comprises acetic acid for adjusting the pH value of the dye composition to 5.5-6.0.
Preferably, the dye solution comprises disperse dye accounting for 2-5% of the total mass of the dye solution.
Further preferably, the dye liquor further comprises sodium dodecyl sulfate accounting for 3-5% of the total mass of the dye liquor, glycerol accounting for 2-3% of the total mass of the dye liquor, a dispersing agent accounting for 1-2% of the total mass of the dye liquor and water.
According to a specific embodiment, the dye liquor comprises 2-5% of disperse dye, 3-5% of sodium dodecyl sulfate, 2-3% of glycerol, 1-2% of dispersing agent and water by mass fraction of 100%.
Preferably, the preparation method of the dye composition comprises the following steps: preparing the disperse dye, the sodium dodecyl sulfate, the glycerin, the dispersing agent and water into a suspension, grinding the suspension until the particle size of the disperse dye is 30-50 nm, adding the leveling agent, the foaming agent and the sodium alginate, and adding the acetic acid to adjust the pH value to obtain the dye composition.
The dye composition is added into a foaming agent before use to foam to obtain foamed slurry, and then the foamed slurry is coated on a fabric to be dyed.
The sixth purpose of the invention is to provide a continuous padding type dyeing method, which comprises the steps of guiding a desized fabric into a dye tank to contact the fabric with a dye composition, and then carrying out drying and color development treatment to complete dyeing, wherein the running speed of the fabric is controlled to be 50-100 m/min; the dye composition comprises a dye solution and a leveling agent, wherein the dye solution comprises a disperse dye accounting for 2-5% of the total mass of the dye solution, the feeding mass of the leveling agent is that 1-2 g of the leveling agent is added into every 1L of the dye solution, and the structural formula of the leveling agent is as follows:
wherein n is a number between 5 and 10.
Preferably, the fabric is made of terylene. Of course, fabrics made of other materials can also be dyed by the leveling agent, the dye composition and the dyeing method.
Preferably, the drying treatment is specifically performed by: and rolling the fabric contacted with the dye composition to dry by a padder, drying by an oven, and baking by a high-temperature baking oven to finish dyeing, wherein the pressure of the padder is controlled to be 0.3-0.4 MPa, the drying temperature of the oven is controlled to be 100-105 ℃, and the baking temperature of the high-temperature baking oven is controlled to be 180-185 ℃.
Further preferably, the travel of the fabric in the oven is 110-130 m, and the travel of the fabric in the high-temperature oven is 190-210 m.
Preferably, the dye composition further comprises acetic acid for adjusting the pH value of the dye composition to 5.5-6.0, and the dye liquor further comprises sodium dodecyl sulfate accounting for 3-5% of the total mass of the dye liquor, glycerol accounting for 2-3% of the total mass of the dye liquor, a dispersing agent accounting for 1-2% of the total mass of the dye liquor and water.
The seventh purpose of the invention is to provide a continuous coating type dyeing method, wherein the foamed dye composition is coated on the surface of the desized fabric, and then dyeing is completed through drying and color development treatment, wherein the running speed of the fabric is controlled to be 80-120 m/min, the coating speed of the dye composition is controlled to be 0.30-0.45m 3 /min；
The dye composition comprises a dye solution, a leveling agent, a foaming agent and sodium alginate, wherein the dye solution comprises a disperse dye accounting for 2-5% of the total mass of the dye solution, the feeding mass of the foaming agent is that 10-15 g of the foaming agent is added into every 1L of the dye solution, the feeding mass of the sodium alginate is that 80-100 g of the sodium alginate is added into every 1L of the dye solution, the feeding mass of the leveling agent is that 1-2 g of the leveling agent is added into every 1L of the dye solution, and the structural formula of the leveling agent is as follows:
wherein n is a number between 5 and 10.
Preferably, the fabric is made of terylene. Of course, fabrics made of other materials can also be dyed by the leveling agent, the dye composition and the dyeing method.
Preferably, the drying treatment is specifically performed by: and rolling the fabric coated with the dye composition to dry by a padder, drying by an oven, and baking by a high-temperature baking oven to finish dyeing, wherein the pressure of the padder is controlled to be 0.3-0.4 MPa, the drying temperature of the oven is controlled to be 100-105 ℃, and the baking temperature of the high-temperature baking oven is controlled to be 180-185 ℃.
Further preferably, the travel of the fabric in the oven is 110-130 m, and the travel of the fabric in the high-temperature oven is 190-210 m.
Preferably, the dye composition further comprises acetic acid for adjusting the pH value of the dye composition to 5.5-6.0, and the dye liquor further comprises sodium dodecyl sulfate accounting for 3-5% of the total mass of the dye liquor, glycerol accounting for 2-3% of the total mass of the dye liquor, a dispersing agent accounting for 1-2% of the total mass of the dye liquor and water.
In the present invention, the disperse dye can be any color.
Preferably, the dispersant of the present invention has the formula:
m is alkali metal, the relative molecular mass of the chitosan derivative is 5500-10000, and the preparation method of the dispersant is shown in example I in patent 201710343323.4.
According to the invention, chitosan with film-forming property is used as a raw material to prepare a leveling agent, an ester group is introduced into chitosan molecules by the leveling agent through modification to form an active site capable of being combined with a dye, and the crosslinking property among six-membered rings of chitosan is enhanced to enable the molecules to be crosslinked mutually, so that the film-forming property of chitosan is enhanced. The leveling agent is uniformly mixed with a dispersant, a nano dye and other auxiliary agents, the mixture is applied to the surface of a fabric in a padding or coating mode, a liquid film with uniform thickness is formed on the surface of the fabric by the leveling agent in a short time when the dye is contacted with the fabric, the liquid film is composed of a plurality of layers of monomolecular films formed by the leveling agent, the dye carried on the active site of the leveling agent is uniformly dispersed on the surface of the fabric, the dye permeates into the fiber after the dye is rolled and pressed by a uniform padder, the uniform distribution of the dye in the warp direction and the weft direction of the fabric is ensured, color spots, color stripes and color differences cannot occur, then the dye molecules are released by a low-temperature drying leveling agent, the moisture in a dyeing solution is evaporated to dryness, finally, the dye is firmly combined with the fabric through high temperature, a finished product can be obtained, and meanwhile, the migration and sublimation of the dye in the drying and color development processes are prevented by the films, the method prevents the color difference of the front side and the back side of the fabric, enables the dye to easily enter the fiber, has the color deepening effect, and can save the dye under the requirement of the same color depth. The leveling agent in the invention accelerates the production speed of padding dyeing and coating dyeing at normal temperature and normal pressure, widens the variety of applicable textiles, improves the quality of finished products, reaches the grade A specified by national standards, makes continuous dyeing at large scale and normal temperature and normal pressure possible to replace high-temperature dye vat dyeing, and makes contribution to the prevention of pollution and reduction of energy consumption in the textile industry.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
the leveling agent disclosed by the invention contains ester groups, has uniform active sites and good film-forming property, so that the leveling agent can be combined with dye through hydrogen bonds, further the dye can be uniformly carried on the fabric and forms a film, the dye is prevented from migrating and sublimating in the drying and color development processes, and the fabric is dark in color, good in color fastness and free of color difference.
The leveling agent is suitable for continuous pad dyeing and coating dyeing, so that the dyeing efficiency is improved, the product quality is improved, the product can reach the grade A specified by the national standard, the energy consumption is reduced, and the continuous dyeing at normal temperature and normal pressure can replace the high-temperature dye vat dyeing.
Detailed Description
Example 1:
the method comprises the following steps: preparation of halogenated crosslinkers
Respectively adding oleic acid, hydrogen bromide and chloroform into a three-neck flask according to a certain mass ratio under the condition of ice-water bath, refluxing by using a straight condensation pipe, stirring, reacting for 30-50 min, washing the product to be neutral by using water, adding the product into a distillation flask, and placing the distillation flask into a constant-temperature water bath kettle at 70-75 ℃ to distill out the chloroform solvent and unreacted hydrogen bromide to obtain a yellow product A.
Wherein the mass ratio of the oleic acid to the hydrogen bromide to the chloroform is as follows: 1: 0.28-0.35: 1.78-2.14.
The equation for the reaction is:
step two: modification of chitosan
Adding chitosan, sodium hydroxide and the product A into carbon tetrachloride according to a certain proportion, stirring at 80-100 ℃, reacting for 3-4 hours, and distilling at 40 ℃ under reduced pressure to obtain a product B. Wherein the chitosan is water-soluble chitosan which is produced by Nantong Lvjingshen bioengineering limited company and has the relative molecular mass of 1000-1200 and the deacetylation degree of more than 90%.
Wherein the mass ratio of chitosan, sodium hydroxide, product A and carbon tetrachloride is as follows: 1: 0.50-0.60: 2.30-2.40: 5.00-6.00
The equation for the reaction is:
step three: cross-linking
Adding glycerol, the product B, a catalyst and toluene (water-carrying agent) into a closed reaction container with a water separator according to a certain proportion, introducing nitrogen to protect the product B, controlling the reaction temperature to be 140-150 ℃, heating, reacting for 4-5 hours, cooling to 50 ℃, extracting with water, crystallizing the extract in an ice water bath at-10 ℃, and filtering to obtain a product C, namely the leveling agent. Wherein the catalyst adopts HND-33 solid super acidic catalyst produced by south China general synthetic chemistry Limited company in Jiangyin city.
Wherein the mass ratio of the glycerol to the product B to the catalyst to the toluene is as follows: 1: 16.50-17.50: 0.07-0.09: 4.00-4.25
The equation for the reaction is:
step four: dyeing process
Dyeing method one (padding type):
adding water into disperse dye, sodium dodecyl sulfate, glycerol and a dispersing agent according to the mass fractions of 2-5 wt%, 3-5 wt%, 2-3 wt% and 1-2 wt% and stirring to prepare a suspension, adding a grinding machine to grind the suspension until the particle size of disperse dye particles is 30-50 nm, then adding a solid product C according to the mass ratio of 1-2 g/L, adding acetic acid to adjust the pH value to 5.5-6.0, and adding the solid product C into a dyeing tank of a padding type dyeing machine, wherein the dyeing machine comprises a cloth feeding device, a dye tank, a uniform roller, a low-temperature dryer, a high-temperature baking machine and a cloth collecting device. The disperse dye can be any one color, and the preparation method of the dispersant refers to example one in patent No. 201710343323.4.
Selecting a piece of desized polyester fabric with the length of 10 meters and the width of 1.6 meters in a whole breadth, adjusting the running speed of the fabric to be 50-100 m/min according to the thickness of the fabric, guiding the fabric into a dyeing tank through a fabric feeding device, guiding the fabric out by a fabric guide roller after contacting with the dyeing slurry, rolling and drying the fabric through a uniform padder with the pressure ranging from 0.3MPa to 0.4MPa, after the fabric is rolled and dried, feeding the fabric into an oven with the stroke of 120 meters, drying the fabric at the temperature of 100-105 ℃, and then feeding the fabric into a high-temperature baking oven with the stroke of 200 meters and baking the fabric at the temperature of 180-185 ℃ to obtain a finished product.
Dyeing mode two (coating mode):
adding 2-5 wt%, 3-5 wt%, 2-3 wt% and 1-2 wt% of disperse dye, sodium dodecyl sulfate, glycerol and a dispersing agent into water, stirring to prepare a suspension, adding a grinding machine, grinding until the particle size of disperse dye particles is 30-50 nm, then adding a solid product C according to a mass ratio of 1-2 g/L, adding a foaming agent according to a mass ratio of 10-15 g/L, adding sodium alginate according to a mass ratio of 80-100 g/L, and adding sodium alginateAdjusting the pH value to 5.5-6.0 by acetic acid, uniformly stirring, adding into a foaming machine for foaming, and dyeing the fabric by a coating type dyeing machine. The coating type dyeing machine comprises a cloth feeding device, a coating knife, a uniform roller, a low-temperature dryer, a high-temperature dryer and a cloth collecting device. The disperse dye can be any one color, wherein the preparation method of the dispersant refers to the example I in the patent with the patent number 201710343323.4, and the preparation method of the foaming agent refers to the chitosan-series composite macromolecular surfactant prepared in the step (1) and the step (2) in the example I in the patent with the patent number 201510237126.5. Selecting a piece of desized polyester fabric with the length of 10 meters and the width of 1.6 meters, adjusting the running speed of the fabric to be 80-120 m/min according to the thickness of the fabric, and simultaneously adjusting the running speed to be 0.30-0.45m 3 And applying the foamed dye slurry to the surface of the fabric through a coating knife at a speed of/min, uniformly coating the fabric, rolling and drying the fabric through a uniform padder, wherein the pressure range of the uniform padder is 0.3-0.4 MPa, after the fabric is rolled and dried, the fabric enters an oven with a stroke of 120 meters, and is dried at the temperature of 100-105 ℃, and then enters a high-temperature baking oven with a stroke of 200 meters and is baked at the temperature of 180-185 ℃ to obtain a finished product.
The present invention is further illustrated by the following examples.
The overall idea of example 2 was followed as in example 1, with the following specific parameters:
and (3) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.28: 1.78, distilling at 70 ℃ to obtain a product A, and determining the mass ratio of the chitosan, the sodium hydroxide, the product A and the carbon tetrachloride in the second step as follows: 1: 0.50: 2.30: 5.00, reacting for 3 hours at 80 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the third step as follows: 1: 16.50: 0.07: 4.00, and reacting at 140 ℃ for 4 hours to obtain a product C.
In the fourth step, grinding disperse red 3B, sodium dodecyl sulfate, glycerol and a dispersing agent according to the mass fractions of 2 wt%, 3 wt%, 2 wt% and 1 wt% to prepare a nano dye, adding a product C according to the amount of 1.0g/L, adding acetic acid to adjust the pH value of the dyeing slurry to 5.5, and selecting 190T, 58g/m 2 The polyester taffeta sets the fabric according to the first dyeing mode of the step fourDyeing is carried out at the running speed of 100m/min, the uniform padder pressure is set to be 0.3MPa, the drying temperature is set to be 100 ℃, the color development temperature is set to be 180 ℃, and a No. 1 sample is obtained after the fabric is taken out of the baking machine.
The overall idea of example 3 was followed as in example 1, with the following specific parameters:
and (3) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.31: 2.00, distilling at 73 ℃ to obtain a product A, and determining the mass ratio of the chitosan, the sodium hydroxide, the product A and the carbon tetrachloride in the second step as follows: 1: 0.55: 2.35: 5.50, reacting for 3.5 hours at 90 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the step III as follows: 1: 17.00: 0.08: 4.10, and reacting at 145 ℃ for 4.5 hours to obtain a product C.
In the fourth step, the disperse yellow G, the sodium dodecyl sulfate, the glycerol and the dispersant are ground according to the mass fractions of 3.5 wt%, 4 wt%, 2.5 wt% and 1.5 wt% to prepare the nano dye, then the solid C is added according to the amount of 1.5G/L, the pH value of the dyeing slurry is adjusted to 6.0 by adding acetic acid, and then 300T, 63G/m are selected 2 According to the first dyeing mode of the step four, the fabric is dyed at the running speed of 90m/min, the uniform padder pressure is set to be 0.35MPa, the drying temperature is set to be 100 ℃, the color development temperature is set to be 180 ℃, and a No. 2 sample is obtained after the fabric is taken out of the baking machine.
The overall concept of example 4 was followed as in example 1, with the following specific parameters:
and (2) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.35: 2.14, distilling at 75 ℃ to obtain a product A, and determining the mass ratio of chitosan, sodium hydroxide, the product A and carbon tetrachloride in the second step as follows: 1: 0.60: 2.40: 6.00, reacting for 4 hours at 100 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the third step as follows: 1: 17.50: 0.09: 4.25, and reacting at 150 ℃ for 5 hours to obtain a product C.
In the fourth step, the disperse blue G, the sodium dodecyl sulfate, the glycerol and the dispersant are ground according to the mass fractions of 5wt percent, 3wt percent and 2wt percent to prepare the nano dye, then the solid C is added according to the amount of 2.0G/L, and the acetic acid is added for regulationAfter the pH value of the dyeing slurry is 5.5, 400 Dx300D, 203g/m is selected 2 According to the first dyeing mode of the fourth step, the running speed of the fabric is set to be 60m/min for dyeing, the uniform padder pressure is set to be 0.4MPa, the drying temperature is set to be 105 ℃, the color development temperature is set to be 185 ℃, and the fabric is taken out of the baking machine to obtain a No. 3 sample.
The overall concept of example 5 was followed as in example 1, with the following specific parameters:
and (2) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.28: 1.78, distilling at 70 ℃ to obtain a product A, and determining the mass ratio of chitosan, sodium hydroxide, the product A and carbon tetrachloride in the second step as follows: 1: 0.50: 2.30: 5.00, reacting for 3 hours at 80 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the third step as follows: 1: 16.50: 0.07: 4.00, and reacting at 140 ℃ for 4 hours to obtain a product C.
Grinding disperse red 3B, sodium dodecyl sulfate, glycerol and a dispersing agent by mass fractions of 2 wt%, 3 wt%, 2 wt% and 1 wt% to prepare a nano dye, adding solid C by 1.0g/L, adding a foaming agent by 10g/L, adding sodium alginate by 80g/L, adding acetic acid to adjust the pH value of the dyeing slurry to 5.5, and selecting 190T and 58g/m 2 According to the second dyeing mode of the step four, setting the running speed of the fabric to be 120m/min for dyeing, and adjusting the slurry application speed to be 0.3m 3 And/min, setting the uniform padder pressure to be 0.3MPa, setting the drying temperature to be 100 ℃, setting the color development temperature to be 180 ℃, and obtaining a No. 4 sample after the fabric is taken out of the baking machine.
The overall concept of example 6 was followed as in example 1, with the following specific parameters:
and (2) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.31: 2.00, distilling at 73 ℃ to obtain a product A, and determining the mass ratio of the chitosan, the sodium hydroxide, the product A and the carbon tetrachloride in the second step as follows: 1: 0.55: 2.35: 5.50, reacting for 3.5 hours at 90 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the third step as follows: 1: 17.00: 0.08: 4.10, reacting for 4.5 hours at 145 ℃ to obtain a product C.
In the fourth step, grinding the disperse yellow G, the sodium dodecyl sulfate, the glycerol and the dispersing agent by the mass fractions of 3.5 wt%, 4 wt%, 2.5 wt% and 1.5 wt% to prepare the nano dye, adding the solid C in an amount of 1.5G/L, adding the foaming agent in an amount of 13G/L, adding the sodium alginate in an amount of 90G/L, adding the acetic acid to adjust the pH value of the dyeing slurry to 6.0, and selecting 300T and 63G/m 2 According to the second dyeing mode of the step four, setting the running speed of the fabric to be 100m/min for dyeing, and adjusting the slurry application speed to be 0.38m 3 And/min, setting the uniform padder pressure to be 0.35MPa, setting the drying temperature to be 100 ℃, setting the color development temperature to be 180 ℃, and obtaining a No. 5 sample after the fabric is taken out of the baking machine.
The overall concept of example 7 was followed as in example 1, with the following specific parameters:
and (2) determining the mass ratio of the oleic acid, the hydrogen bromide and the chloroform in the step one as follows: 1: 0.35: 2.14, distilling at 75 ℃ to obtain a product A, and determining the mass ratio of chitosan, sodium hydroxide, the product A and carbon tetrachloride in the second step as follows: 1: 0.60: 2.40: 6.00, reacting for 4 hours at 100 ℃ to obtain a product B, and determining the mass ratio of the glycerol, the product B, the catalyst and the toluene in the step three as follows: 1: 17.50: 0.09: 4.25, and reacting at 150 ℃ for 5 hours to obtain a product C.
In the fourth step, grinding disperse blue G, sodium dodecyl sulfate, glycerol and a dispersing agent by the mass fractions of 5 wt%, 3 wt% and 2 wt% to prepare a nano dye, adding solid C in an amount of 2.0G/L, adding a foaming agent in an amount of 15G/L, adding sodium alginate in an amount of 100G/L, adding acetic acid to adjust the pH value of the dyeing slurry to 5.5, and selecting 400 Dx 300D, 203G/m 2 The oxford fabric is dyed according to the second dyeing mode of the step four, the running speed of the fabric is set to be 80m/min, and the application speed of the sizing agent is adjusted to be 0.45m 3 And/min, setting the uniform padder pressure to be 0.4MPa, setting the drying temperature to be 105 ℃, setting the color development temperature to be 185 ℃, and obtaining a No. 6 sample after the fabric is taken out of the baking machine.
Comparative example 1
Grinding disperse blue G, sodium dodecyl sulfate, glycerol and dispersant by mass fractions of 5 wt%, 3 wt% and 2 wt%Grinding to prepare nano dye, adding acetic acid to adjust the pH value of the dyeing slurry to 5.5, and selecting 400 Dx300D, 203g/m 2 The oxford fabric is dyed according to the first dyeing mode of the fourth step in the example 1, the running speed of the fabric is set to be 60m/min, the uniform padder pressure is set to be 0.4MPa, the drying temperature is set to be 105 ℃, the color development temperature is set to be 185 ℃, and a 7# sample is obtained after the fabric is taken out of the baking machine. Wherein the dispersant is according to example one of patent No. 201710343323.4.
Comparative example 2
Grinding disperse blue G, sodium dodecyl sulfate, glycerol and a dispersing agent by mass fractions of 5 wt%, 3 wt% and 2 wt% to prepare a nano dye, adding a foaming agent by the amount of 15G/L, adding sodium alginate by the amount of 100G/L, adding acetic acid to adjust the pH value of the dyeing slurry to 5.5, and selecting 400 Dx300D, 203G/m 2 The oxford fabric is dyed according to the second dyeing mode of the fourth step in the embodiment 1, the running speed of the fabric is set to be 80m/min, and the application speed of the sizing agent is adjusted to be 0.45m 3 And/min, setting the uniform padder pressure to be 0.4MPa, setting the drying temperature to be 105 ℃, setting the color development temperature to be 185 ℃, and obtaining an 8# sample after the fabric is taken out of the baking machine. Wherein, the preparation method of the dispersant refers to the first example in the patent with the patent number 201710343323.4, and the preparation method of the foaming agent refers to the chitosan-based composite polymer surfactant prepared in the step (1) and the step (2) in the first example in the patent with the patent number 201510237126.5.
The sample detection method and the detection result are as follows:
the color fastness to rubbing is detected according to GB/T3920-.
| Test items | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# |
| Colour fastness to rubbing (grade) | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 2-3 | 2-3 |
| Fastness to washing (grade) | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 2-3 | 2-3 |
| Fastness to soaping (grade) | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 2-3 | 2 |
| Colour fastness to perspiration (grade) | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 4-5 | 2-3 | 2-3 |
| Colour fastness to light (grade) | 4 | 4 | 4 | 4 | 4 | 4 | 2 | 2 |
| Warp direction color difference (NBS) | 0.02 | 0.01 | 0.03 | 0.01 | 0.02 | 0.01 | 0.53 | 0.65 |
| Latitudinal chromatic aberration (NBS) | 0.01 | 0.02 | 0.01 | 0.02 | 0.01 | 0.02 | 0.28 | 0.36 |
| Front and back color difference (NBS) | 0.03 | 0.02 | 0.03 | 0.02 | 0.03 | 0.01 | 1.17 | 1.23 |
| Color difference between # 7 and # 3 (NBS) | 1.56 | |||||||
| Color difference between 8# and 6# (NBS) | 1.61 |
Remarking: 1NBS corresponds to 5 times the human visual threshold, and human vision below 0.2NBS is considered to be achromatic.
The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.
Claims (10)
1. A method of preparing a dye composition, comprising: preparing a suspension from disperse dye, sodium dodecyl sulfate, glycerol, a dispersing agent and water, grinding the suspension until the particle size of the disperse dye is 30-50 nm, and then adding a leveling agent and acetic acid to prepare the dye composition, wherein the leveling agent has a structural formula as follows:
wherein n is a number between 5 and 10.
2. The method for preparing the dye composition according to claim 1, wherein: the mass percent of the disperse dye is 2-5%, the mass percent of the sodium dodecyl sulfate is 3-5%, the mass percent of the glycerol is 2-3%, the mass percent of the dispersant is 1-2% and the balance of water is calculated according to 100% of the suspension.
3. The method for preparing a dye composition according to claim 1, characterized in that: the feeding mass of the leveling agent is that 1-2 g of the leveling agent is added into every 1L of the suspension.
4. The method for preparing a dye composition according to claim 1, characterized in that: the addition amount of the acetic acid is to adjust the pH value of the dye composition to 5.5-6.0.
5. The method for preparing the dye composition according to claim 1, wherein: the structural formula of the dispersant is as follows:
m is alkali metal, and the relative molecular mass of the dispersing agent is 5500-10000.
6. A method of preparing a dye composition, comprising: preparing a suspension from disperse dye, sodium dodecyl sulfate, glycerol, a dispersing agent and water, grinding the suspension until the particle size of the disperse dye is 30-50 nm, adding a leveling agent, a foaming agent and sodium alginate, and adding acetic acid to adjust the pH value to obtain the dye composition, wherein the leveling agent has a structural formula as follows:
wherein n is a number between 5 and 10.
7. The method for preparing a dye composition according to claim 6, characterized in that: the mass percent of the disperse dye is 2-5%, the mass percent of the sodium dodecyl sulfate is 3-5%, the mass percent of the glycerol is 2-3%, the mass percent of the dispersant is 1-2% and the balance of water is calculated according to 100% of the suspension.
8. The method for preparing the dye composition according to claim 6, wherein: the leveling agent is characterized in that 1-2 g of the leveling agent is added into every 1L of turbid liquid, 10-15 g of the foaming agent is added into every 1L of turbid liquid, and 80-100 g of sodium alginate is added into every 1L of turbid liquid.
9. The method for preparing the dye composition according to claim 6, wherein: the addition amount of the acetic acid is to adjust the pH value of the dye composition to 5.5-6.0.
10. The method for preparing a dye composition according to claim 6, characterized in that: the structural formula of the dispersant is as follows:
m is alkali metal, and the relative molecular mass of the dispersing agent is 5500-10000.
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