CN114773878A - High-dispersity nano disperse dye and preparation method thereof - Google Patents
High-dispersity nano disperse dye and preparation method thereof Download PDFInfo
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- CN114773878A CN114773878A CN202210464858.8A CN202210464858A CN114773878A CN 114773878 A CN114773878 A CN 114773878A CN 202210464858 A CN202210464858 A CN 202210464858A CN 114773878 A CN114773878 A CN 114773878A
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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
- 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
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/008—Preparations of disperse dyes or solvent dyes
- C09B67/0082—Preparations of disperse dyes or solvent dyes in liquid form
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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
- 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
- C09B67/006—Preparation of organic pigments
- C09B67/0066—Aqueous dispersions of pigments containing only dispersing agents
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Abstract
The invention provides a high-dispersity nano disperse dye and a preparation method thereof, wherein the preparation method comprises the following steps: s1, pretreatment of the crude dye: adding organic solution of the crude dye into the aqueous solution under stirring for mixed precipitation reaction, and crushing and drying the generated precipitate to obtain pretreated crude dye powder; s2, preparation of a fiber carrier: after the cellulose fiber is cut, pulped and etched, the cellulose fiber is fished out, washed by water, drained until the water content of the cellulose short fiber is 40-80 percent, and subjected to freeze-drying treatment to obtain a fiber carrier; s3, preparing the high-dispersity nano disperse dye: the pretreated crude dye powder, the fiber carrier and the active calcium silicate are compounded together to obtain the high-dispersity nano disperse dye.
Description
Technical Field
The invention relates to the field of printing and dyeing materials, in particular to a high-dispersity nano disperse dye and a preparation method thereof.
Background
The disperse dye is mainly used for printing and dyeing of terylene and blended fabrics thereof, and can also be used for printing and dyeing of synthetic fibers such as acetate fibers, chinlon, polypropylene fibers, polyvinyl chloride fibers, acrylic fibers and the like. In recent years, with the wide application of polyester textiles, disperse dyes have been developed unprecedentedly, and become the dye supplies with the largest variety and the largest use amount.
In general, in order to rapidly disperse a disperse dye in water into a uniform and stable colloidal suspension, a commercial dye is prepared by subjecting a raw dye to post-treatment steps such as temperature-raising crystallization, sanding with a dispersant, and drying after synthesis. In the dyeing process, as a nonionic dye, the water solubility of a disperse dye is extremely low, the disperse dye is uniformly dispersed in a dye solution by virtue of a dispersing agent, then the fiber is bulked by virtue of the action of high temperature and the like, the gap inside the fiber is enlarged, so that the disperse dye molecules can enter the bulked and enlarged fiber gaps through diffusion, and finally the disperse dye molecules are fixed by virtue of intermolecular attraction and hydrogen bonds to realize dyeing.
Generally, when the particle diameter of the dye particles is more than 30um, defects such as spots, streaks and the like are easily generated on the surface of a dyed product; when the particle size of the dye particles is between 10 and 30 mu m, the surface of a dyed product is easy to have no luster; when the particle size of the dye particles is less than 5um, the use of common products can be met; however, for fibers with the monofilament diameter of 10-30 um and ultrathin films with the thickness of less than 10um, the particle size of the dye particles needs to be less than 1um, so that the comprehensive performances of the disperse dye, such as application range, coloring strength, luster, covering power and the like, can be effectively improved by reducing the particle size of the dye particles, and in addition, the capability of the dye particles entering the interior of the polyester material and the difficulty of the dyeing process can be improved by reducing the particle size of the dye particles. However, as the particle size of the dye particles decreases, for example, after the particle size of the dye particles reaches the nanometer level, the specific surface area of a single dye particle increases due to the particle size reduction of the dye particles, the surface energy of the dye particles increases, the particles with high surface energy meet each other, and energy is spontaneously released, the surface energy is reduced, so that the particles are in a stable state, and mutual aggregation among the dye particles is an effective way for reducing the surface energy, so that the nano dye particles and the particles are very easy to generate aggregation, the dispersibility is very poor, and particularly the nano dye particles in a liquid state are easy to re-aggregate into micron-sized dye particles after being dried, so that the nano disperse dye loses the excellent properties of the nano dye particles in the using process.
In addition, the content of the auxiliary agent in the existing disperse dye is generally high, and the use of a large amount of the auxiliary agent can cause the increase of the cost and the increase of the treatment difficulty of the production wastewater on one hand, and on the other hand, the use of a large amount of the auxiliary agent can increase the tendency of the migration phenomenon in the dyeing process.
Disclosure of Invention
The invention designs a high-dispersity nano disperse dye and a preparation method thereof, and aims to solve the technical problems of poor dispersity, easy agglomeration and high auxiliary agent content of the existing nano disperse dye.
In order to solve the problems, the invention discloses a preparation method of a high-dispersity nano disperse dye, which comprises the following steps:
s1, pretreatment of the raw dye: dissolving a crude dye in an organic solvent, adding the obtained organic solution into an aqueous solution under stirring for mixed precipitation reaction, and crushing and drying the generated precipitate to obtain pretreated crude dye powder;
s2, preparation of a fiber carrier: after the cellulose fiber is cut, pulped and etched, the cellulose fiber is fished out, washed by water and drained until the moisture content of the cellulose short fiber is 40-80 percent, and the moisture-containing cellulose short fiber is subjected to freeze-drying treatment to obtain a fiber carrier;
s3, preparing the high-dispersity nano disperse dye: compounding the pretreated crude dye powder, the fiber carrier and the active calcium silicate together to obtain the high-dispersity nano disperse dye.
Further, the step S1 includes the steps of:
s11, dissolving the crude dye obtained by the reaction in an organic solvent, and filtering to remove impurities to obtain an organic solution A;
s12, uniformly mixing water and the auxiliary agent to obtain a water solution B;
s13, placing the aqueous solution B in a heatable container, heating to 60-70 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuously stirring for 10-30 min, then placing the mixed solution in an ultrasonic cell crusher for ultrasonic crushing for 30-60min, and after ultrasonic crushing, removing water and organic solvent through spray drying to obtain the pretreated crude dye powder.
Further, in the step S12, the weight percentage of the auxiliary agent and the water is 0.5% to 3%, and the auxiliary agent includes, by weight:
further, the step S2 includes the steps of:
s21, cutting the cellulose fiber, mixing with water, placing in a pulping device for pulping, and obtaining pulp containing cellulose short fiber after pulping;
s22, adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers obtained in the step S21, uniformly stirring to obtain an alkaline treatment solution C containing the cellulose short fibers, heating the alkaline treatment solution C to 40-50 ℃, etching the cellulose short fibers in the alkaline treatment solution C at 40-50 ℃ for 0.2-3 h, fishing out, washing with water, and draining until the water content of the cellulose short fibers is 40% -80% for later use;
s23, freeze-drying the water-containing cellulose short fiber obtained in the step S22 in a freeze-drying device to obtain the fiber carrier.
Further, the cellulose fiber is one or more of cotton fiber, hemp fiber, modal fiber, bamboo fiber and kapok fiber.
Further, in step S22, the alkaline treatment liquid C contains: 0.2-3 g/L of sodium hydroxide, 0.5-5 g/L of organic silicon, 3-5 g/L of dispersing agent and 6-10 g/L of glycerol.
Further, the step S3 includes the steps of:
s31, firstly dispersing active calcium silicate and the pretreated crude dye powder prepared in the step S1 in water to obtain a mixed system D, then compounding the mixed system D on the fiber carrier prepared in the step S2, and draining the obtained composite material for later use;
and S32, spraying an acid solution on the composite material drained in the step S31, and drying to obtain the high-dispersity nano disperse dye.
Further, in the above step S31, the mixed system D is compounded on the fiber carrier by a compounding device, the compounding device including:
the outer shell is hollow inside;
a horizontal partition plate disposed in the outer case in a horizontal direction and dividing an inner space of the outer case into an upper cavity and a lower cavity;
the lower cavity is provided with an inlet and a liquid guide pipe, external air enters the lower cavity through the inlet, the mixed system D is arranged in the lower cavity, and the mixed system D in the lower cavity can enter the upper cavity through the liquid guide pipe under the pressure effect of the air input from the inlet;
and the upper cavity is filled with the fiber carrier, and the mixed system D entering the upper cavity is discharged through an outlet arranged on the upper cavity after passing through the fiber carrier.
Further, the compound device further comprises:
the gas homogenizing disc is positioned above the inlet, and the diameter of the gas homogenizing disc is 1.5-3 times of that of the inlet;
the annular inner wall is positioned in the outer shell and surrounds the periphery of the gas homogenizing disc, the lower end of the annular inner wall is connected with the lower bottom surface of the outer shell, the upper end of the annular inner wall is provided with an upper cover plate, the annular inner wall, the lower bottom surface of the outer shell and the upper cover plate enclose an inner cavity in the outer shell, the lower end of the annular inner wall is provided with a liquid discharging port, and the liquid discharging port is communicated with the inner cavity and the lower cavity;
the mounting connecting piece, the mounting connecting piece is inside hollow tubular structure, the upper end of mounting connecting piece is passed behind the upper cover plate, extend to the below of horizontal partition plate, just the upper end of mounting connecting piece with the clearance has between the horizontal partition plate, the lower extreme with even gas dish is connected set up the gas overflow hole on the mounting connecting piece, the gas overflow hole is located the below of upper cover plate.
The high-dispersity nano disperse dye is prepared by the preparation method of the high-dispersity nano disperse dye.
The high-dispersity nano disperse dye and the preparation method thereof have the following advantages: according to the application, the purified nano-raw dye particles are loaded on the fiber carrier, and the fiber carrier provides a supporting framework for the nano-dye particles, so that the nano-raw dye particles are not easy to agglomerate, good dispersibility can be realized during use, the advantages of the nano-dye particles are exerted, the use of an auxiliary agent is reduced, and the environment-friendly and efficient effects are achieved; in addition, through the addition of the active calcium silicate, a good bridging effect is achieved between the nano dye particles and the fiber carrier, so that the dye particles can be stably adsorbed on the fiber carrier; furthermore, the fiber carrier and the active calcium silicate can be removed by acidolysis in the dyeing process under the high-temperature and high-pressure environment during dyeing, without adversely affecting the dyeing process.
Drawings
FIG. 1 is a flow chart of the preparation method of the high-dispersibility nano disperse dye according to the invention;
FIG. 2 is a schematic perspective view of the composite device of the present invention;
FIG. 3 is a schematic top view of the composite device of the present invention;
FIG. 4 is a schematic cross-sectional view taken along the line A-A in FIG. 3;
FIG. 5 is a schematic perspective view of a cross-sectional structure along the direction A-A in FIG. 3;
FIG. 6 is a schematic front view of the composite device of the present invention;
FIG. 7 is a schematic cross-sectional view taken along the line C-C in FIG. 6;
FIG. 8 is a schematic view of another cross-sectional structure taken along the line A-A in FIG. 3;
FIG. 9 is a schematic cross-sectional view taken along the line B-B in FIG. 3;
FIG. 10 is a perspective view of another cross-sectional structure taken along the line A-A in FIG. 3;
FIG. 11 is a schematic view of another cross-sectional structure taken along the direction C-C in FIG. 6;
fig. 12 is a schematic cross-sectional view taken along the direction D-D in fig. 6.
Description of reference numerals:
1. an outer housing; 2. a horizontal partition plate; 3. an upper cavity; 301. an outlet; 302. a vertical partition; 303. filtering with a screen; 4. a lower cavity; 401. an inlet; 402. a catheter; 403. an air homogenizing disc; 404. installing a connecting piece; 405. an annular inner wall; 406. an upper cover plate; 407. an air overflow hole; 408. and a liquid discharge port.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
As shown in fig. 1, a method for preparing a high-dispersibility nano disperse dye includes the steps of:
s1, pretreatment of the crude dye: dissolving a crude dye in an organic solvent, adding the obtained organic solution into an aqueous solution under stirring for mixing and precipitation reaction, and crushing and drying the generated precipitate to obtain pretreated crude dye powder;
s2, preparation of a fiber carrier: after the cellulose fiber is cut, pulped and etched, fishing out, washing with water, draining until the water content of the cellulose short fiber is 40-80%, and freeze-drying the water-containing cellulose short fiber to obtain a fiber carrier;
s3, preparing the high-dispersity nano disperse dye: compounding the pretreated crude dye powder, the fiber carrier and the active calcium silicate together to obtain the high-dispersity nano disperse dye.
According to the preparation method of the disperse dye, the purified nano-raw dye particles are loaded on the fiber carrier, and the fiber carrier provides a supporting framework for the nano-dye particles, so that the nano-dye particles are not easy to agglomerate, good dispersibility can be realized during use, the advantages of the nano-dye particles are exerted, the use of an auxiliary agent is reduced, and the preparation method is more environment-friendly and efficient; in addition, through the addition of the active calcium silicate, a good bridging effect is achieved between the nano dye particles and the fiber carrier, so that the dye particles can be stably adsorbed on the fiber carrier; furthermore, the fiber carrier and the active calcium silicate can be removed by acidolysis in the dyeing process by utilizing the high-temperature and high-pressure environment during dyeing, and the dyeing process is not adversely affected.
Specifically, the step S1 includes the steps of:
s11, dissolving the crude dye obtained through the reaction in an organic solvent, and filtering to remove impurities to obtain an organic solution A;
s12, uniformly mixing water and the auxiliary agent to obtain a water solution B;
s13, placing the aqueous solution B in a heatable container, heating to 60-70 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuing stirring for 10-30 min, then placing the mixed solution in an ultrasonic cell crusher for ultrasonic crushing for 30-60min, and after ultrasonic crushing, removing water and organic solvent through spray drying to obtain the pretreated crude dye powder.
As some examples of the present application, in the step S11, the organic solvent may be one or more of ethanol, acetone, n-butanol, isobutanol, tetrahydrofuran, benzene, toluene, ethylbenzene, xylene, dichloromethane, dimethylformamide, chloroform, carbon tetrachloride.
Preferably, in the step S11, the weight percentage of the raw dye and the organic solvent is 10% to 30%.
As some examples of the present application, in the step S11, the raw dye may be one or more of azo type, anthraquinone type or heterocyclic type dyes, such as disperse red, disperse blue, etc.
Further, in the step S12, the auxiliary agent includes, by weight:
preferably, the dispersant is one or more of lignosulfonate, a methyl naphthalene sulfonic acid formaldehyde condensate, fatty acid polyol ester polyoxyethylene ether and a benzyl naphthalene sulfonic acid formaldehyde condensate; the dispersing agent is a naphthalenesulfonic acid formaldehyde condensate; the emulsifier is one or a combination of more of Tween 60, sodium dodecyl sulfate, OP-10, SP-80 and isomeric tridecanol polyoxyethylene ether; the defoaming agent is an organic silicon defoaming agent; the surfactant is one or more of sodium dodecyl benzene sulfonate, sulfated castor oil, Dynol 607 and polyalcohol.
Further, in the step S12, the weight percentage of the auxiliary agent and the water is 0.5% to 3%.
Further, in the step S13, the weight percentage of the organic solution a and the aqueous solution B is 30 to 60%.
Preferably, in the step S13, the adding speed of the organic solution a is controlled to be substantially uniform, continuous and stable, and the amount of the organic solution a added to the aqueous solution B per minute should not exceed 10% of the total amount of the organic solution a.
More preferably, the adding speed of the organic solution A is reduced along with the increase of the weight percentage of the organic solution A and the aqueous solution B, and particularly, when the weight percentage of the organic solution A and the aqueous solution B is 30-40%, the adding amount of the organic solution A to the aqueous solution B per minute is not more than 10% of the total amount of the organic solution A; when the weight percentage of the organic solution A and the aqueous solution B is 40-60%, the amount of the organic solution A added into the aqueous solution B per minute should not exceed 5% of the total amount of the organic solution A.
Further, in the step S13, the ultrasonic frequency of the ultrasonic cell crusher is 20 to 60 KHz.
In the above step S1, the crude dye can be purified by dissolving it in an appropriate organic solvent to remove impurities such as inorganic salts in the crude dye by filtration; and then mixing an organic solvent of the crude dye with an aqueous solution, carrying out mixed precipitation reaction to separate out the crude dye, and simultaneously combining the control of the mixing rate and the dispersing, crushing and emulsifying effects of an ultrasonic cell crusher to realize the refining and uniform dispersion of the crude dye particles.
Further, the step S2 includes the steps of:
s21, cutting the cellulose fiber, mixing with a proper amount of water, placing in a pulping device for pulping, and obtaining pulp containing cellulose short fiber after pulping;
s22, adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers obtained in the step S21, uniformly stirring to obtain alkaline treatment liquid C containing the cellulose short fibers, heating the alkaline treatment liquid C to 40-50 ℃, etching the cellulose short fibers in the alkaline treatment liquid C at 40-50 ℃ for 0.2-3 h, fishing out, washing with water, and draining until the water content of the cellulose short fibers is 40-80% for later use;
s23, freeze-drying the water-containing cellulose short fiber obtained in the step S22 in a freeze-drying device to obtain the fiber carrier.
The moisture content of the cellulose staple fiber is (the current weight thereof-the weight when dried to a constant weight)/the weight when dried to a constant weight.
Preferably, in the step S21, after the cellulose fibers are cut to 10 to 30mm, the cellulose fibers and water are mixed in a weight ratio of 0.02:1 to 0.15:1, and then the mixture is added into a beating device for beating for 0.5 to 1 hour, and a pulp containing the cellulose staple fibers is obtained after beating.
More preferably, in the step S21, the amount of the cellulose fiber is 20 to 40% by weight of the pretreated crude dye powder obtained in the step S1.
As some examples herein, the cellulosic fibers may be one or more of cotton fibers, hemp fibers, modal fibers, bamboo fibers, kapok fibers, and the like.
Preferably, in step S22, the alkaline treatment solution C is an aqueous solution of sodium hydroxide.
More preferably, the alkaline treatment liquid C contains: 0.2-3 g/L of sodium hydroxide, 0.5-5 g/L of organic silicon, 3-5 g/L of dispersing agent and 6-10 g/L of glycerol.
Under the etching action of the alkaline component in the alkaline solution C in step S22, ester groups in the cellulose short fibers are broken and surface molecules fall off, so that a large number of pits can be etched and formed on the surface of the cellulose short fibers, and the specific surface area of the cellulose short fibers is increased, and simultaneously, the surface roughness of the cellulose short fibers can be improved, and the capability of the cellulose short fibers for adsorbing solid substances such as dye particles and the like is improved.
In addition, in common cellulose fibers such as cotton fibers, bamboo fibers, hemp fibers and the like, in addition to cellulose fiber components, impurities coexisting with the cellulose fibers such as pectin, wax and the like are present, during the treatment, these impurity components will form a film on the surface of the cellulose fiber, making it difficult for the dye particles to contact the surface of the cellulose fiber, resulting in a decrease in the adsorption capacity of the cellulose fiber, in the etching process of the alkaline solution C, the alkaline components can effectively remove impurities such as pectin, wax and the like in the cellulose fibers, so that molecular chains of the cellulose fibers are oxidized and broken, the strength and the length are reduced, meanwhile, the organosilicon can form an organosilicon film on the surface of the cellulose fiber by utilizing the telescopic silicon-oxygen bond in the organosilicon, so that the surface activity of the cellulose fiber and the cohesive force between the cellulose fiber and dye particles are increased; the addition of the dispersant and glycerin can improve the dispersion effect of the cellulose fibers in the alkaline treatment liquid C. The dispersant is one or more of polycarboxylate, lignosulfonate or sodium methylene dinaphthalene sulfonate.
Furthermore, under the etching action of the alkaline component in the alkaline solution C in step S22, the cellulose fiber can be swelled to some extent, which provides a good basis for proceeding the subsequent step S23. And the cellulose fiber can be rapidly decomposed in high-temperature acidic dye solution under the action of acid liquor sprayed on the surface of the cellulose fiber and acidic substances in the dye solution to generate carbide, so that the adverse effect on the dyeing process is avoided.
Preferably, in the step S23, the cellulose-containing short fiber needs to be placed in a freezing environment with a temperature of 60-100 ℃ and a pressure of 40-70 Pa, and is subjected to freezing sublimation treatment for 0.5-7 hours under the action of 10-20 KHz ultrasonic waves, and then is taken out, so as to obtain the fiber carrier.
In the step S23, the devillicate state of the beaten cellulose staple fiber can be maintained by the freeze-drying process, and meanwhile, in the freeze-drying process, liquid water molecules in the cellulose staple fiber are condensed into solid state and then spread out and occupy the space between the devillicate cellulose fibers by the ultra-low temperature freezing process, and in the subsequent sublimation process, solid water molecules in the cellulose are removed by sublimation, and a gap is formed in the space position occupied by the solid water molecules. Meanwhile, under the action of ultrasound, gaps with uniform distribution and size can be formed in the cellulose short fibers, and the specific surface area and the adsorption capacity of the cellulose short fibers are enhanced.
Further, the step S3 includes the steps of: and dispersing the pretreated crude dye powder, the fiber carrier and the active calcium silicate in water, compounding together, and drying to obtain the high-dispersity nano disperse dye.
Further, the step S3 includes the steps of:
s31, dispersing the pretreated crude dye powder prepared in the step S1, the fiber carrier prepared in the step S2 and the active calcium silicate in water, compounding together, and draining for later use;
and S32, spraying an acid solution on the composite material drained in the step S31, and drying to obtain the high-dispersity nano disperse dye.
Further, in the above step S31, the activated calcium silicate has a formula of CaO · mSiO2·nH2O, the particle size of the active calcium silicate is 0.1-10 um, and the specific surface area is 60-100 m2(ii) in terms of/g. The silicon-oxygen group, the silanol group and other groups on the surface of the active calcium silicate can be combined with hydrogen bonds and the like in cellulose fibers to generate stable chemical bond binding force, the active calcium silicate is firmly adsorbed on the surface of the cellulose fibers, meanwhile, the porous structure on the surface of the active calcium silicate can also adsorb disperse dye particles, a bridging effect is achieved between the cellulose fibers and the dye particles, and finally the adsorption force and the adsorption capacity of the cellulose fibers to the dye particles are improved. And the active calcium silicate is nontoxic and harmless white powder, is doped in dye particles, and cannot generate adverse effects on the dye particles and printing and dyeing fabrics. In addition, the active calcium silicate is a novel calcium silicate with high dispersibility, which is soluble in acid at high temperature, and thus, it can be dissolved by an acidic high-temperature dye solution during dyeing without adversely affecting the dyeing process.
Preferably, in step S31, the pretreated crude dye powder prepared in step S1 and activated calcium silicate are dispersed in water to obtain a mixed system D, and then the mixed system D is combined with the fibrous carrier prepared in step S2.
More preferably, in the step S31, the amount of the activated calcium silicate used is 4 to 18% by weight of the pretreated crude dye powder obtained in the step S1.
As some examples of the present application, in the step S32, the acidic solution may be an aqueous solution of an acidic substance such as an inorganic acid, an organic acid, and an acid salt, and the acidic solution contains 0.2% to 30% of the acidic substance by mass. The acidic substance may be hydrochloric acid, sulfuric acid, aluminum sulfate, carboxylic acid, etc., and the mass percentage of the acidic substance in the acidic solution may be adjusted as required due to the difference in acidity of different acidic substances, specifically, the acidic substance may completely decompose the cellulose fiber under the combined action of the acidic substance attached to the cellulose fiber and the acidic substance in the dyeing solution during printing and dyeing.
More preferably, in step S31, the mixed system D may be combined with the fibrous carrier prepared in step S2 by a combining device shown in fig. 2 to 12.
Specifically, as shown in fig. 2 to 12, the composite device includes:
an outer shell 1 which constitutes an outer wall of the composite device, the outer shell 1 being hollow inside;
a horizontal partition plate 2 which is provided in the outer case 1 in a horizontal direction and partitions an inner space of the outer case 1 into an upper cavity 3 and a lower cavity 4;
an inlet 401 and a liquid guide pipe 402 are arranged on the lower cavity 4, substances such as external gas can enter the lower cavity 4 through the inlet 401, the mixed system D is arranged in the lower cavity 4, and under the pressure effect of the gas input by the inlet 401, the mixed system D in the lower cavity 4 can enter the upper cavity 3 through the liquid guide pipe 402;
the upper cavity 3 is filled with the fiber carrier prepared in the step S2, and the mixed system D entering the upper cavity 3 passes through the fiber carrier and is then discharged through an outlet 301 provided in the upper cavity 3.
Furthermore, the lower end of the liquid guide pipe 402 is inserted into the bottom of the lower cavity 4, and the upper end of the liquid guide pipe 402 passes through the horizontal partition plate 2 and then is communicated with the upper cavity 3.
Further, the inlet 401 is located on the lower bottom surface of the lower cavity 4, a gas distribution disc 403 is arranged above the inlet 401, when gas is filled into the lower cavity 4 through the inlet 401, the gas sprayed out of the inlet 401 firstly impacts on the lower surface of the gas distribution disc 403, then the movement direction is changed, the gas moves downwards, and after the downward movement speed of the gas is reduced to zero, the gas moves upwards through a gap between the outer edge of the gas distribution disc 403 and the inner surface of the outer shell 1 under the buoyancy action of liquid in the lower cavity 4.
Preferably, the diameter of the gas homogenizing disc 403 is 1.5 to 3 times of the diameter of the inlet 401.
Preferably, the distance between the gas distribution disc 403 and the inlet 401 can be adjusted according to the pressure or flow rate of the gas filled into the inlet 401, so that the position where the downward movement speed of the gas sprayed from the inlet 401 after impacting the gas distribution disc 403 is reduced to zero is not lower than the lower bottom surface of the lower cavity 4.
As some embodiments of the present application, a mounting connector 404 is disposed in the lower cavity 4, an upper end of the mounting connector 404 is connected to the top surface of the lower cavity 4, a lower end of the mounting connector 404 is connected to the gas distribution plate 403, and the gas distribution plate 403 is suspended in the lower cavity 4 through the mounting connector 404. Preferably, the mounting connector 404 and the gas homogenizing plate 403 are both made of rigid materials.
The use method of the composite device comprises the following steps:
t1, filling a liquid fluid such as water or a water solution of pretreated crude dye powder or a water solution of activated calcium silicate into the lower cavity 4, and uniformly laying the fiber carrier in the upper cavity 3;
t2, opening the inlet 401 to inflate the lower cavity 4, the gas passing through the liquid fluid in the lower cavity 4 is gathered at the upper part of the lower cavity 4, meanwhile, the liquid fluid in the lower cavity 4 is pressed into the liquid guide tube 402 under the pressure of the gas inflated in the lower cavity 4, and the liquid level in the liquid guide tube 402 is continuously raised with the continuous inflation, and finally the liquid fluid in the lower cavity 4 is pressed into the upper cavity 3;
t3, the liquid fluid pressed into the upper cavity 3 mixes with the fibrous carrier in the upper cavity 3, passes through the fibrous carrier, and is discharged through the outlet 301.
As some examples of the present application, in the step T1, liquid fluid may be filled into the lower cavity 4 through a liquid inlet, a liquid inlet pipe, or the like, which is disposed on a side wall of the lower cavity.
As some examples of the present application, in the step T1, the pretreated crude dye powder prepared in the step S1 and the activated calcium silicate may be dispersed in water to obtain a mixed system D, and then the mixed system D may be directly filled into the lower cavity 4.
As other embodiments of the present application, in the step T1, deionized water may be filled in the lower cavity 4; and in the subsequent step T2, the gas filled into the lower cavity 4 through the inlet 401 fills the pretreated crude dye powder and the activated calcium silicate particles prepared in the step S1 into the deionized water in the lower cavity 4 to form a mixed system D.
As another example of the present application, in the step T1, one of the pretreated crude dye powder or the activated calcium silicate prepared in the step S1 may be directly dispersed in water, and the dispersion may be filled into the lower cavity 4; in the subsequent step T2, the other one of the pretreated nano-crude dye powder and the activated calcium silicate particles is filled into the deionized water in the lower cavity 4 by using the gas filled into the lower cavity 4 through the inlet 401, so as to form a mixed system D.
Preferably, in the step T1, the pretreated raw dye powder prepared in the step S1 is directly dispersed in water, and the dispersion liquid is filled into the lower cavity 4; and in the following step T2, the gas filled into the lower cavity 4 through the inlet 401 is used to fill the active calcium silicate particles into the deionized water in the lower cavity 4, so as to form a mixed system D. Tests show that when the compounding is carried out in this way, the amount of the residual dye powder in the water discharged from the outlet 301 is smaller, and the amount of the dye powder adsorbed by the fiber carrier is higher.
The working principle of the compound device is as follows: when the lower cavity 4 is filled with gas, under the action of the gas distribution disc 403, the gas contents of different regions in the lower cavity 4 will be different, specifically, as shown in fig. 4, for convenience of description, the region between the gas distribution disc 403 and the inlet 401 is referred to as a K1 region, the region between the outer side of the gas distribution disc 403 and the outer shell 1 is referred to as a K2 region, the region above the gas distribution disc 403 is referred to as a K3 region, and the gas contents of the K1, K2 and K3 regions are gradually reduced under the influence of the movement, dissolution and precipitation of the gas and the gas diffusion path, and the change of the gas contents will generate a density difference between the fluids in the K1, K2 and K3 regions, and the density difference will further cause the relative movement of the fluids in the K1, K2 and K3 regions, and the relative movement enables the fluids in different regions to be mixed, thereby enabling the K1, K2 and K8625, The dye particles in the K2 and K3 regions and the active calcium silicate particles are always in a motion state, so that the dye particles are uniformly dispersed and are not easy to agglomerate; meanwhile, compared with the conventional mechanical strong stirring, the movement strength generated by the density difference is proper, and the active calcium silicate particles can be adsorbed and combined with the dye particles. Then, under the action of the air pressure in the lower cavity 4, the mixed system D in the lower cavity 4 overflows into the upper cavity 3 through the liquid guide pipe 402, and the overflow can make the mixed system D flow without too high flow speed, and this low-speed flow of the mixed system D can provide a proper contact speed and contact time for the fiber carrier to adsorb the particulate matters in the mixed system D.
As some embodiments of the present application, the composite device may be further optimized, specifically, as shown in fig. 8 to 12, a vertical partition plate 302 and a filter screen 303 are disposed in the upper cavity 3, the upper end of the liquid guide tube 402 is located on one side of the vertical partition plate 302, the outlet 301 is located on the other side of the vertical partition plate 302, the filter screen 303 is disposed on the vertical partition plate 302 along the horizontal direction, and the fiber carrier is located on the filter screen 303, so that the mixed system D discharged into the upper cavity 3 by the liquid guide tube 402 can flow to the other side of the vertical partition plate 302 and be discharged through the outlet 301 after having to pass through the filter screen 303 and the fiber carrier thereon.
Furthermore, the filter screen 303 has two specifications, and the aperture of the filter screen 303 on the side where the liquid guide tube 402 is located is far larger than the particle size of the particles in the mixing system D, and mainly plays a role of supporting a fiber carrier; the aperture of the filter screen 303 at the side of the outlet 301 is smaller than the particle size of the particles in the mixing system D, and can simultaneously play a role in supporting the fiber carrier and filtering. In this case, if necessary, a suction filtration device may be connected to the outlet 301 to increase the filtration rate. In fact, however, since a small amount of gas entering through the inlet 401 can enter the upper space 3 through the liquid guiding tube 402 and is enclosed by the filter net with smaller aperture and the cellulose thereon, a slightly positive pressure environment can be generated in the upper space 3 compared with the external atmospheric pressure during the use, which is beneficial for the filtration.
As some embodiments of the present application, the composite device may be further optimized, specifically, as shown in fig. 8 to 12, an annular inner wall 405 is disposed in the lower cavity 4, the annular inner wall 405 is located between the gas distribution disc 403 and the outer shell 1, specifically, the annular inner wall 405 is located inside the outer shell 1 and surrounds the periphery of the gas distribution disc 403, the lower end of the annular inner wall 405 is connected to the lower bottom surface of the outer shell 1, an upper cover plate 406 is disposed at the upper end of the annular inner wall 405, and an inner cavity may be defined in the outer shell 1 by the annular inner wall 405, the lower bottom surface of the outer shell 1 and the upper cover plate 406.
Furthermore, a liquid outlet 408 is arranged at the lower end of the annular inner wall 405, and the liquid outlet 408 is communicated with the inner cavity and the lower cavity 4.
Furthermore, the mounting connector 404 is a hollow cylindrical structure, the upper end of the mounting connector 404 passes through the upper cover plate 406 and extends to the lower part of the horizontal partition plate 2, and a gap is formed between the upper end of the mounting connector 404 and the horizontal partition plate 2, so that the upper end of the mounting connector 404 is communicated with the lower cavity 4; the lower end of the mounting connector 404 is hermetically connected with the gas distributing disc 403, an air overflow hole 407 is arranged on the mounting connector 404, and the air overflow hole 407 is located below the upper cover plate 406 and is close to the lower surface of the upper cover plate 406. At this time, the mounting connector 404 may be fixed by an upper cover plate 406.
Preferably, the open area of the air overflow hole 407 is smaller than the area of the inlet 401, and the exhaust rate of the air overflow hole 407 is smaller than the intake rate of the inlet 401.
At this time, the method of using the composite device includes the steps of:
t1', filling the inner cavity surrounded by the annular inner wall 405 with liquid fluid, and uniformly laying the fiber carrier on the filter screen 303 in the upper cavity 3;
t2', opening the inlet 401 to inflate the inner cavity, after the gas passes through the liquid fluid in the lower cavity 4, the gas is gathered at the upper part of the inner cavity, and the liquid in the inner cavity is discharged through the liquid outlet 408 under the pressure of the gas inflated in the inner cavity; meanwhile, part of the gas accumulated in the upper part of the inner cavity enters the mounting connector 404 through the overflow hole 407, and is discharged to the upper part of the lower cavity 4 through the opening at the upper end of the mounting connector 404, and finally accumulates in the upper part of the lower cavity 4, because the exhaust rate of the overflow hole 407 is smaller than the intake rate of the inlet 401, and the amount of the gas entering the upper cavity 3 is very small, the gas pressure P0 in the upper cavity 3 is smaller than the gas pressure P1 in the lower cavity 4 is smaller than the gas pressure P2 in the inner cavity, and under the action of the pressure difference, the liquid level in the liquid guide tube 402 continuously rises, and finally the liquid fluid in the lower cavity 4 is pressed into the upper cavity 3;
t3', the liquid pressed into the upper cavity 3 first enters the side of the vertical partition 302 close to the liquid guide tube 402, then flows through the filter screen 303 and the fiber carrier thereon by overflowing, flows to the side of the vertical partition 302 close to the outlet 301, and is discharged through the outlet 301.
In the composite device, the inner cavity divides the lower cavity 4 into two parts, and the fluid in the inner cavity can realize the relative motion similar to the areas K1, K2 and K3 under the direct action of the gas density difference; after the fluid is discharged out of the inner cavity body, the flow velocity is reduced, solid particles in the fluid can be adsorbed in the fluid with lower flow velocity between the annular inner wall 405 and the outer shell 1 for a relatively long time again, and finally good combination between the dye powder and the active calcium silicate is realized.
The preparation method of the high-dispersibility nano-disperse dye is illustrated by the following specific examples:
example 1
Weighing 100g of disperse blue BGL crude dye obtained through reaction, dissolving the disperse blue BGL crude dye in 1kg of ethanol solution, and filtering to remove impurities to obtain an organic solution A; uniformly mixing 3kg of water and 15g of auxiliary agent to obtain a water solution B; wherein the auxiliary agent comprises 30 parts by weight of lignosulfonate, 5 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 3 parts by weight of SP-80, 1 part by weight of silicone defoamer and 0.5 part by weight of sodium dodecyl benzene sulfonate; and (2) placing the aqueous solution B in a heatable container, heating to 60 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, completely adding the organic solution A into the aqueous solution B, continuing stirring for 10min, placing the mixed solution in an ultrasonic cell crusher, performing ultrasonic crushing for 30min at 20KHz, and removing water and an organic solvent through spray drying after ultrasonic crushing to obtain the pretreated crude dye powder.
Weighing natural cotton fibers accounting for 20% of the weight of the pretreated crude dye powder, cutting the natural cotton fibers to about 10mm, mixing the natural cotton fibers and water according to the weight ratio of 0.02:1, adding the mixture into a pulping device, pulping for 0.5 hour, and pulping to obtain pulp containing cellulose short fibers; and then adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers, and uniformly stirring to obtain an alkaline treatment liquid C containing the cellulose short fibers, wherein the alkaline treatment liquid C contains: 0.2g/L of sodium hydroxide, 0.5g/L of organic silicon, 3g/L of dispersing agent and 6g/L of glycerol; heating the alkaline treatment liquid C to 40 ℃, etching the cellulose short fibers in the alkaline treatment liquid C at 40 ℃ for 0.2h, taking out the cellulose short fibers, washing the cellulose short fibers with water, draining the cellulose short fibers until the water content of the cellulose short fibers is 40%, putting the water-containing cellulose short fibers into a freeze-drying device, and freeze-drying the cellulose short fibers for 0.2h under the action of 10KHz ultrasonic waves in a freezing environment at-60 ℃ and 40Pa to obtain the fiber carrier.
Weighing active calcium silicate accounting for 5% of the weight of the pretreated crude dye powder, placing the active calcium silicate, the pretreated crude dye powder and the fiber carrier obtained in the previous steps into the composite device to form a composite material, draining the composite material, spraying a hydrochloric acid solution accounting for 10% of the mass percentage of the drained composite material, and drying to obtain the high-dispersity nano disperse dye.
Example 2
Weighing 100g of disperse red 3B crude dye obtained through reaction, dissolving the disperse red 3B crude dye in 600g of ethanol solution, and filtering to remove impurities to obtain an organic solution A; uniformly mixing 1500g of water and 8g of auxiliary agent to obtain an aqueous solution B; wherein the auxiliary agent comprises 40 parts by weight of lignosulfonate, 6 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 4 parts by weight of tween 60, 1.5 parts by weight of silicone defoamer and 0.8 part by weight of Dynol 607; and (2) placing the aqueous solution B in a heatable container, heating to 68 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuously stirring for 25min, then placing the mixed solution in an ultrasonic cell crusher, carrying out ultrasonic crushing for 50min at 30KHz, and after ultrasonic crushing, removing water and an organic solvent through spray drying to obtain the pretreated crude dye powder.
Weighing natural cotton fibers accounting for 28% of the weight of the pretreated crude dye powder, cutting the natural cotton fibers to about 20mm, mixing the natural cotton fibers and water according to the weight ratio of 0.1:1, adding the mixture into a pulping device, pulping for 0.6h, and pulping to obtain pulp containing cellulose short fibers; and then adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers, and uniformly stirring to obtain an alkaline treatment liquid C containing the cellulose short fibers, wherein the alkaline treatment liquid C contains: 1g/L of sodium hydroxide, 2.5g/L of organic silicon, 3.5g/L of dispersing agent and 8g/L of glycerol; and heating the alkaline treatment liquid C to 47 ℃, etching the cellulose short fibers in the alkaline treatment liquid C at 47 ℃ for 1h, taking out and washing the cellulose short fibers, draining the cellulose short fibers until the water content of the cellulose short fibers is 70%, putting the water-containing cellulose short fibers into a freeze-drying device, and freeze-drying the water-containing cellulose short fibers for 5h under the action of 15KHz ultrasonic waves in a freezing environment with the temperature of 90 ℃ below zero and the pressure of 60Pa to obtain the fiber carrier.
Weighing active calcium silicate which accounts for 10% of the weight of the pretreated crude dye powder, placing the active calcium silicate, the pretreated crude dye powder and the fiber carrier which are obtained in the previous steps into the composite device to form a composite material, draining the composite material, spraying an aluminum sulfate solution which accounts for 20% of the mass of the drained composite material, and drying to obtain the high-dispersity nano disperse dye.
Example 3
Weighing 50g of disperse blue BGL crude dye obtained through reaction and 50g of disperse yellow 3GL crude dye obtained through reaction, dissolving the disperse blue BGL crude dye and the disperse yellow 3GL crude dye in 320g of ethanol solution, and filtering to remove impurities to obtain an organic solution A; uniformly mixing 530g of water and 15g of auxiliary agent to obtain an aqueous solution B; wherein the auxiliary agent comprises 50 parts by weight of lignosulfonate, 10 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 5 parts by weight of tween 60, 2 parts by weight of organosilicon antifoaming agent and 1 part by weight of Dynol 607; and (2) placing the aqueous solution B in a heatable container, heating to 70 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuously stirring for 30min, then placing the mixed solution in an ultrasonic cell crusher, carrying out ultrasonic crushing for 60min at 60KHz, and after ultrasonic crushing, removing water and an organic solvent through spray drying to obtain the pretreated crude dye powder.
Weighing natural bamboo fibers accounting for 40% of the weight of the pretreated crude dye powder, cutting the natural bamboo fibers to about 30mm, mixing the natural bamboo fibers and water according to the weight ratio of 0.15:1, adding the mixture into a pulping device, pulping for 1 hour, and pulping to obtain pulp containing cellulose short fibers; and then adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers, and uniformly stirring to obtain alkaline treatment liquid C containing the cellulose short fibers, wherein the alkaline treatment liquid C contains: 3g/L of sodium hydroxide, 5g/L of organic silicon, 5g/L of dispersing agent and 10g/L of glycerol; heating the alkaline treatment liquid C to 50 ℃, etching the cellulose short fibers in the alkaline treatment liquid C at 50 ℃ for 3h, taking out the cellulose short fibers, washing the cellulose short fibers with water, draining the cellulose short fibers until the water content of the cellulose short fibers is 80%, putting the cellulose short fibers containing water into a freeze-drying device, and freeze-drying the cellulose short fibers in a freezing environment at 100 ℃ below zero and 70Pa for 7h under the action of 20KHz ultrasonic waves to obtain the fiber carrier.
Weighing active calcium silicate accounting for 18% of the weight of the pretreated crude dye powder, placing the active calcium silicate, the pretreated crude dye powder and the fiber carrier obtained in the previous steps into the composite device to form a composite material, draining the composite material, spraying a hydrochloric acid solution accounting for 10% of the mass percentage of the drained composite material, and drying to obtain the high-dispersity nano disperse dye.
Comparative example 1
Weighing 100g of disperse red 3B crude dye obtained by reaction, dissolving the crude dye in 600g of ethanol solution, and filtering to remove impurities to obtain an organic solution A; uniformly mixing 1500g of water and 8g of auxiliary agent to obtain an aqueous solution B; wherein the auxiliary agent comprises 40 parts by weight of lignosulfonate, 6 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 4 parts by weight of tween 60, 1.5 parts by weight of silicone defoamer and 0.8 part by weight of Dynol 607; and (2) placing the aqueous solution B in a heatable container, heating to 68 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, completely adding the organic solution A into the aqueous solution B, continuing stirring for 25min, placing the mixed solution in an ultrasonic cell crusher, performing ultrasonic crushing for 50min at 30KHz, and removing water and an organic solvent through spray drying after ultrasonic crushing to obtain the pretreated crude dye powder.
Weighing natural cotton fibers which are 28% of the weight of the pretreated crude dye powder, cutting the natural cotton fibers to about 20mm, mixing the natural cotton fibers and water according to the weight ratio of 0.1:1, adding the mixture into a pulping device, pulping for 0.6h, and pulping to obtain pulp containing cellulose short fibers; the cellulose short fiber is taken out by filtering, washed by water and drained until the water content of the cellulose short fiber is 70 percent, the water-containing cellulose short fiber is placed in freeze-drying equipment, and is freeze-dried for 5 hours under the action of 15KHz ultrasonic waves in a freezing environment with the temperature of 90 ℃ below zero and the pressure of 60Pa, and the fiber carrier is obtained.
Weighing active calcium silicate accounting for 10% of the weight of the pretreated crude dye powder, placing the active calcium silicate, the pretreated crude dye powder and the fiber carrier which are obtained in the previous steps into the composite device to form a composite material, draining the composite material, spraying an aluminum sulfate solution accounting for 20% of the mass percentage of the aluminum sulfate solution onto the drained composite material, and drying to obtain the nano disperse dye.
Comparative example 2
Weighing 100g of disperse red 3B crude dye obtained through reaction, dissolving the disperse red 3B crude dye in 600g of ethanol solution, and filtering to remove impurities to obtain an organic solution A; mixing 1500g of water and 8g of auxiliary agent uniformly to obtain a water solution B; wherein the auxiliary agent comprises 40 parts by weight of lignosulfonate, 6 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 4 parts by weight of tween 60, 1.5 parts by weight of silicone defoaming agent and 0.8 part by weight of Dynol 607; and (2) placing the aqueous solution B in a heatable container, heating to 68 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuously stirring for 25min, then placing the mixed solution in an ultrasonic cell crusher, carrying out ultrasonic crushing for 50min at 30KHz, and after ultrasonic crushing, removing water and an organic solvent through spray drying to obtain the pretreated crude dye powder.
Weighing natural cotton fibers accounting for 28% of the weight of the pretreated crude dye powder, cutting the natural cotton fibers to about 20mm, mixing the natural cotton fibers and water according to the weight ratio of 0.1:1, adding the mixture into a pulping device, pulping for 0.6h, and pulping to obtain pulp containing cellulose short fibers; and (3) fishing out the cellulose short fibers by filtering, washing with water, and draining to constant weight to obtain the fiber carrier.
Weighing active calcium silicate accounting for 10% of the weight of the pretreated crude dye powder, placing the active calcium silicate, the pretreated crude dye powder and the fiber carrier obtained in the previous steps into the composite device to form a composite material, draining the composite material, spraying an aluminum sulfate solution accounting for 20% of the mass percentage of the drained composite material, and drying to obtain the nano disperse dye.
Comparative example 3
Weighing 100g of disperse red 3B crude dye obtained by reaction, dissolving the crude dye in 600g of ethanol solution, and filtering to remove impurities to obtain an organic solution A; uniformly mixing 1500g of water and 8g of auxiliary agent to obtain an aqueous solution B; wherein the auxiliary agent comprises 40 parts by weight of lignosulfonate, 6 parts by weight of naphthalene sulfonic acid formaldehyde condensate, 4 parts by weight of tween 60, 1.5 parts by weight of silicone defoaming agent and 0.8 part by weight of Dynol 607; and (2) placing the aqueous solution B in a heatable container, heating to 68 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, completely adding the organic solution A into the aqueous solution B, continuing stirring for 25min, placing the mixed solution in an ultrasonic cell crusher, performing ultrasonic crushing for 50min at 30KHz, and removing water and an organic solvent through spray drying after ultrasonic crushing to obtain the pretreated crude dye powder.
Weighing natural cotton fibers which are 28% of the weight of the pretreated crude dye powder, cutting the natural cotton fibers to about 20mm, mixing the natural cotton fibers and water according to the weight ratio of 0.1:1, adding the mixture into a pulping device, pulping for 0.6h, and pulping to obtain pulp containing cellulose short fibers; and then adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers, and uniformly stirring to obtain alkaline treatment liquid C containing the cellulose short fibers, wherein the alkaline treatment liquid C contains: 1g/L of sodium hydroxide, 2.5g/L of organic silicon, 3.5g/L of dispersing agent and 8g/L of glycerol; and heating the alkaline treatment liquid C to 47 ℃, etching the cellulose short fibers in the alkaline treatment liquid C at 47 ℃ for 1h, taking out and washing the cellulose short fibers, draining the cellulose short fibers until the water content of the cellulose short fibers is 70%, putting the water-containing cellulose short fibers into a freeze-drying device, and freeze-drying the water-containing cellulose short fibers for 5h under the action of 15KHz ultrasonic waves in a freezing environment with the temperature of 90 ℃ below zero and the pressure of 60Pa to obtain the fiber carrier.
And (2) placing the pretreated crude dye powder and the fiber carrier obtained in the previous step into the composite device to form a composite material, draining the composite material, spraying an aluminum sulfate solution with the mass percentage of 20% onto the drained composite material, and drying to obtain the nano disperse dye.
Test example 1
Respectively dissolving the disperse dyes prepared in the embodiments 1-3 in water to prepare a dye solution, wherein the dye solution contains 0.2g/L of the disperse dyes and 0.05g/L of an auxiliary agent MF0.05g/L, adjusting the pH value of the dye solution to 5 by using a buffer solution, taking 100ml of the dye solution, heating to 70 ℃, and adding 2g of polyester fiber fabric at 2.02 x 105pa, heating the temperature of a dye solution to 130 ℃ within 30min, keeping the temperature at 130 ℃ for 30min, cooling to 90 ℃ to obtain a dyed fabric, and sampling and detecting, wherein the method specifically comprises the following steps:
the method comprises the following steps of detecting the color fastness to washing of dyed fabrics according to GB/T3921-2008, detecting the sublimation color fastness of the dyed fabrics according to AATCC117, detecting the friction color fastness of the dyed fabrics according to AATCC8, determining the COD value of the dyeing raffinate by adopting a GB11914-89 chemical oxygen demand-dichromate method according to the chromatic value of the dyeing raffinate under the wavelength of 380-750 mm by adopting an ultraviolet visible spectrophotometer, and obtaining the detection result shown in the following Table 1:
TABLE 1 dyeing Properties test values
| Detecting items | Example 1 | Example 2 | Example 3 |
| Color fastness to washing | Grade 4-5 | Grade 4-5 | 4 to 5 grades |
| Color fastness to |
4 to 5 |
4 to 5 grades | Grade 5 |
| Colour fastness to rubbing (Dry) | 4 to 5 |
4 to 5 |
4 to 5 grades |
| Colorimetric value (ads value) | 65.4 | 70.2 | 69.3 |
| COD value (mg/L) | 924 | 876 | 983 |
In addition, the dye solution before dyeing corresponding to the above examples 1 to 3 is taken as a dye solution sample, and meanwhile, in order to prevent the thread scraps falling off from the dyed fabric from interfering with the test result, another dye solution before dyeing corresponding to the above examples 1 to 3 is taken, and the dye solution before dyeing is respectively subjected to heating and pressurizing treatment according to the high-temperature and high-pressure process in the dyeing process, but no polyester fiber fabric is added, and after the dye solution is treated according to the dyeing process, the dye solution sample before dyeing and the dye residual liquid sample are compared, and the following results are found: after the high-temperature and high-pressure dyeing treatment process, compared with a dye liquor sample before dyeing, the content of active calcium silicate particles in dyeing residual liquid is reduced to 1.07-0.2% of the initial content, and the content of cellulose fibers in the dyeing residual liquid is reduced to 3-0.6% of the initial content, which shows that the active calcium silicate particles and the cellulose fibers can be dissolved, acidolyzed, hydrolyzed or carbonized in the dyeing process.
Test example 2
1g of the disperse dyes prepared in the above examples 1 to 3 and comparative examples 1 to 3 were respectively taken, 1000mL of water was added and stirred until the disperse dyes were uniformly dispersed, the mixture was allowed to stand at room temperature, whether the agglomeration phenomenon occurred or not was observed by using a high power microscope every 15min, and the time for the occurrence of the precipitation delamination was observed by naked eyes, and the results are shown in Table 2 below:
TABLE 2 Dispersion Performance test results
Although the present invention is disclosed above, the present invention is not limited thereto. In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Various changes and modifications may be effected by one skilled in the art without departing from the spirit and scope of the invention, as defined in the appended claims.
Claims (10)
1. A preparation method of high-dispersity nano disperse dye is characterized by comprising the following steps:
s1, pretreatment of the raw dye: dissolving a crude dye in an organic solvent, adding the obtained organic solution into an aqueous solution under stirring for mixed precipitation reaction, and crushing and drying the generated precipitate to obtain pretreated crude dye powder;
s2, preparation of a fiber carrier: after the cellulose fiber is cut, pulped and etched, fishing out, washing with water, draining until the water content of the cellulose short fiber is 40-80%, and freeze-drying the water-containing cellulose short fiber to obtain a fiber carrier;
s3, preparing the high-dispersity nano disperse dye: compounding the pretreated crude dye powder, the fiber carrier and the active calcium silicate together to obtain the high-dispersity nano disperse dye.
2. A method for preparing a disperse dye according to claim 1, wherein the step S1 includes the steps of:
s11, dissolving the crude dye obtained through the reaction in an organic solvent, and filtering to remove impurities to obtain an organic solution A;
s12, uniformly mixing water and the auxiliary agent to obtain a water solution B;
s13, placing the aqueous solution B in a heatable container, heating to 60-70 ℃, slowly adding the organic solution A into the aqueous solution B under stirring for mixing and precipitation reaction, after completely adding the organic solution A into the aqueous solution B, continuing stirring for 10-30 min, then placing the mixed solution in an ultrasonic cell crusher for ultrasonic crushing for 30-60min, and after ultrasonic crushing, removing water and organic solvent through spray drying to obtain the pretreated crude dye powder.
3. The method for preparing a disperse dye according to claim 2, wherein in the step S12, the weight percentage of the auxiliary agent and the water is 0.5% to 3%, and the auxiliary agent comprises:
4. the method for preparing a disperse dye according to claim 1, wherein the step S2 comprises the steps of:
s21, cutting the cellulose fiber, mixing with water, placing in a pulping device for pulping, and obtaining pulp containing cellulose short fiber after pulping;
s22, adding an alkaline substance and an etching assistant into the slurry containing the cellulose short fibers obtained in the step S21, uniformly stirring to obtain an alkaline treatment solution C containing the cellulose short fibers, heating the alkaline treatment solution C to 40-50 ℃, etching the cellulose short fibers in the alkaline treatment solution C at 40-50 ℃ for 0.2-3 h, fishing out, washing with water, and draining until the water content of the cellulose short fibers is 40% -80% for later use;
s23, freeze-drying the water-containing cellulose short fiber obtained in the step S22 in a freeze-drying device to obtain the fiber carrier.
5. The method for preparing the disperse dye according to claim 1 or 4, wherein the cellulose fiber is one or more of cotton fiber, hemp fiber, modal fiber, bamboo fiber and kapok fiber.
6. The method for producing a disperse dye according to claim 4, wherein in the step S22, the alkali treatment liquid C contains: 0.2-3 g/L of sodium hydroxide, 0.5-5 g/L of organic silicon, 3-5 g/L of dispersing agent and 6-10 g/L of glycerol.
7. The method for preparing a disperse dye according to claim 1, wherein the step S3 comprises the steps of:
s31, firstly dispersing active calcium silicate and the pretreated crude dye powder prepared in the step S1 in water to obtain a mixed system D, then compounding the mixed system D on the fiber carrier prepared in the step S2, and draining the obtained composite material for later use;
and S32, spraying an acid solution on the composite material drained in the step S31, and drying to obtain the high-dispersity nano disperse dye.
8. The method for producing a disperse dye according to claim 7, wherein in the step S31, the mixed system D is compounded on the fiber support by a compounding device comprising:
the outer shell (1), the inside of the outer shell (1) is hollow;
a horizontal partition plate (2) which is arranged in the outer shell (1) along the horizontal direction and divides the inner space of the outer shell (1) into an upper cavity (3) and a lower cavity (4);
an inlet (401) and a liquid guide pipe (402) are arranged on the lower cavity (4), external air enters the lower cavity (4) through the inlet (401), the mixing system D is arranged in the lower cavity (4), and under the pressure effect of the air input by the inlet (401), the mixing system D in the lower cavity (4) can enter the upper cavity (3) through the liquid guide pipe (402);
the upper cavity (3) is filled with the fiber carrier, and a mixed system D entering the upper cavity (3) is discharged through an outlet (301) formed in the upper cavity (3) after passing through the fiber carrier.
9. The method for preparing a disperse dye according to claim 8, wherein the compounding device further comprises:
the gas homogenizing disc (403) is positioned above the inlet (401), and the diameter of the gas homogenizing disc (403) is 1.5-3 times that of the inlet (401);
the annular inner wall (405) is located inside the outer shell (1) and surrounds the periphery of the gas homogenizing disc (403), the lower end of the annular inner wall (405) is connected with the lower bottom surface of the outer shell (1), an upper cover plate (406) is arranged at the upper end of the annular inner wall (405), the lower bottom surface of the outer shell (1) and the upper cover plate (406) form an inner cavity in the outer shell (1), a liquid discharging port (408) is arranged at the lower end of the annular inner wall (405), and the liquid discharging port (408) is communicated with the inner cavity and the lower cavity (4);
the mounting connecting piece (404), the mounting connecting piece (404) is inside hollow tubular structure, pass the upper cover plate (406) back, extend to the below of horizontal partition board (2) the upper end of mounting connecting piece (404) just the upper end of mounting connecting piece (404) with have the clearance between horizontal partition board (2), the lower extreme with even gas dish (403) are connected set up air overflow hole (407) on mounting connecting piece (404), air overflow hole (407) are located the below of upper cover plate (406).
10. A high-dispersibility nano disperse dye, which is prepared by the preparation method of any one of claims 1 to 9.
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