CN110670166B - Preparation method of sodium chloride high-temperature deep-dyed polyester fabric - Google Patents
Preparation method of sodium chloride high-temperature deep-dyed polyester fabric Download PDFInfo
- Publication number
- CN110670166B CN110670166B CN201910937413.5A CN201910937413A CN110670166B CN 110670166 B CN110670166 B CN 110670166B CN 201910937413 A CN201910937413 A CN 201910937413A CN 110670166 B CN110670166 B CN 110670166B
- Authority
- CN
- China
- Prior art keywords
- temperature
- sodium chloride
- dyeing
- deep
- spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
-
- 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
-
- 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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Coloring (AREA)
Abstract
The invention relates to the field of chemical fibers, and discloses a preparation method of a sodium chloride high-temperature deep-dyed polyester fabric. The invention can crystallize sodium chloride in the polyester to generate nano-scale crystals by adding sodium chloride in the polymerization process and controlling the adding mode and the adding time point of the sodium chloride. When dyeing is performed under high temperature and high pressure conditions, sodium chloride crystals are dissolved out, and nano-scale holes with uniform sizes can be formed on the surface of the fiber. The existence of the holes can effectively reduce the specular reflection on the surface of the fiber and increase the apparent color yield of the fiber, thereby obviously improving the dyeing depth of the fiber.
Description
Technical Field
The invention relates to the field of chemical fibers, in particular to a preparation method of a sodium chloride high-temperature deep-dyed polyester fabric.
Background
In recent decades, polyester productivity has increased rapidly, and the total energy of polyester fibers has increased from 516.5 ten thousand tons in the early 2000 to 4992 ten thousand tons in the end 2017. Dacron has become the synthetic fiber variety with the largest yield among chemical fibers, and is widely applied to various aspects such as clothing, decoration, household textiles, industrial textiles and the like. The polyester fiber has a series of excellent performances of high breaking strength, high elastic modulus, moderate rebound resilience, excellent heat setting, heat resistance, light resistance, acid resistance, corrosion resistance and the like, and the fabric has the advantages of crease resistance, non-ironing property, good stiffness and smoothness and the like, so the polyester fiber is widely applied to the fields of clothing, home textiles and the like.
On one hand, however, the macromolecular chains of the polyester fiber are arranged closely, so that dye molecules are difficult to diffuse into the fiber, and the polyester fiber is difficult to dye deep color; on the other hand, the polyester fiber has very smooth surface, regular round cross section, high light reflection and low apparent color yield, and the polyester cannot be dyed in deep color due to the two reasons. Meanwhile, the market demands deep-dyed polyester with excellent fastness, particularly for black-dyed polyester, the solution of the market is to use a deepening treatment in the dyeing and finishing post-treatment process to improve the depth of the polyester (i.e. to immerse the prepared fiber in a finishing liquid), but the problem of poor later-use fastness exists. Therefore, there is a great demand in the market for polyester that can be deeply dyed using a conventional high-temperature and high-pressure dyeing process.
The current commercial high-temperature high-pressure deep color cloth sample dyeing process has the problems of large dye consumption, poor deep dyeing effect, high production cost and deep residual liquid color.
For example, chinese patent application No. 201711322144.9 discloses a method for preparing deep-dyed polyester filament yarn at normal temperature and pressure, wherein the deep-dyed polyester is cationic low-temperature deep-dyed filament yarn, and deep dyeing can be realized by increasing the addition of three monomers. However, the dye used by the fiber is a cationic dye, the cost of the cationic dye is higher than that of the conventional dye, and the chromatographic and application range is not wide as that of a disperse dye. Meanwhile, the cationic low-temperature deep-dyed filaments of the type generally have the problem of poor light fastness.
Chinese patent with application number 201810609055.0 discloses extra dark polyester, wherein the polyester is cationic dyeable polyester, and deep dyeing is realized by cationic dye dyeing, disperse dyeing and deep treatment. The process can realize deep dyeing, but has the following problems: firstly, the dyeing process is relatively complex and the dyeing cost is relatively high; secondly, the durability of the subsequent deepening treatment is poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a sodium chloride high-temperature deep-dyed polyester fabric,
according to the invention, sodium chloride is added into the polyester chip in a specific manner, so that the dyeing depth of the polyester fiber can be 20% higher than that of the conventional polyester fiber after the polyester fiber is dyed at high temperature and high pressure. On one hand, the use cost of the dye can be reduced, and on the other hand, the added value of the product can be improved.
The specific technical scheme of the invention is as follows: a preparation method of a sodium chloride high-temperature deep-dyed polyester fabric comprises the following steps: 1) polyester synthesis: adding part of ethylene glycol into a reaction container, adding a dissolved sodium chloride aqueous solution, adding the rest ethylene glycol containing a catalyst and terephthalic acid, pulping, and reacting to obtain the sodium chloride deep-dyed polyester chip.
2) Spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing to obtain pre-drawn yarns with uniform yarn levelness, and drawing and texturing to obtain drawn textured yarns.
3) Dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
By adopting the technical scheme, sodium chloride is added in the polymerization process, and the adding mode and the adding time point of the sodium chloride are controlled, so that the sodium chloride can be crystallized in the polyester to generate nano-scale crystals. When dyeing is performed under high temperature and high pressure conditions, sodium chloride crystals are dissolved out, and nano-scale holes with uniform sizes can be formed on the surface of the fiber. The existence of the holes can effectively reduce the specular reflection on the surface of the fiber and increase the apparent color yield of the fiber, thereby obviously improving the dyeing depth of the fiber. Meanwhile, the sodium chloride added by the method of the invention has good control performance on the dispersibility in the polyester, and has good spinning condition and no blockage of the filter in the spinning process.
Preferably, in the step 1), the mass of the sodium chloride is 0.5-2% of the mass of the sodium chloride deep-dyed polyester chip.
Preferably, in step 1), the sodium chloride is pretreated by: dispersing isobutyl triethoxy silane in distilled water to make its concentration be 2.3-2.5wt%, heating in 65-75 deg.C water for 15-25 min; then adding the obtained solution into a prepared sodium chloride solution, and simultaneously adding chitosan with the mass of 8-12% of the sodium chloride to control the crystallization of the sodium chloride.
The principle of the pretreatment is that the combination of sodium chloride and polyester is promoted by the modification of isobutyl triethoxy silane, and the crystallization of the sodium chloride can be promoted by adding chitosan, so that the crystal quantity is increased.
Preferably, in step 1), the molar ratio of ethylene glycol to terephthalic acid is 1.15-1.35: 1; the catalyst is an Sb catalyst; the addition amount of the catalyst is 0.02-0.06% of the mass of the terephthalic acid.
Preferably, in the step 1), the reaction conditions are specifically: in the step 1), the reaction conditions are specifically as follows: firstly, carrying out esterification reaction, controlling the temperature to slowly rise at the temperature rise speed of 1.5-2.5 ℃, ensuring the esterification temperature not to exceed 240 ℃, raising the temperature to 255 ℃ after the esterification is finished, and vacuumizing for 50-60min until the vacuum degree is 1800-; carrying out a polycondensation reaction: heating to above 270 deg.C, vacuumizing to 60-80pa, polycondensation temperature not exceeding 282 deg.C, and melt viscosity controlled at 0.75-0.78 dl/g.
Preferably, in step 2), the drying conditions are: crystallization temperature of 135-
Preferably, in step 2), the spinning assembly used is: the size of the filter screen is 200 meshes and 250 meshes.
Preferably, the spinning process is as follows: the screw temperature (the temperature of the first zone of the screw is 285-.
The invention optimizes and improves the spinning process according to the characteristics of the deep-dyed polyester chips. For example, the sodium chloride is dispersed by the mesh number of the filter screen, and on the other hand, the filament is formed by controlling the spinning temperature.
Preferably, in the step 3), dyeing is carried out under the conditions that dyeing is started from 25-35 ℃, the temperature is raised to 85-95 ℃ at the temperature raising rate of 1.5-2.5 ℃/min, then the temperature is raised to 125-135 ℃ at the temperature raising rate of 0.5-1.5 ℃/min, the temperature is kept for 35-45min, and the dyeing pressure is 0.3-0.5 MPa.
Preferably, in the step 3), the dye is used in an amount of 3-7% o.w.f, the bath ratio is 1:45-55, the oil removing agent is used in an amount of 0.8-1.2g/L, and the pH value of the dye solution is 4-5.
Preferably, in the step 3), the reduction cleaning specifically comprises: adding 1.5-2.5g/L NaOH and 1.5-2.5g/L sodium hydrosulfite, at 75-85 deg.C for 20-40 min.
Preferably, the heat-setting conditions are 165-.
Compared with the prior art, the invention has the beneficial effects that:
(1) by the polyester polymerization process, the particle size of sodium chloride crystals in the polyester is well controlled, and cavities with uniform sizes can be formed on the surface of the fiber after high-temperature and high-pressure dyeing. The existence of the holes effectively reduces the specular reflection on the surface of the polyester fiber, thereby endowing the deep-dyed polyester with remarkable deep-dyeing effect, and the dyeing depth of the deep-dyed polyester is 20 percent higher than that of the conventional polyester under the conditions of high temperature and high pressure.
(2) The sodium chloride added by the method of the invention has good control performance on the dispersibility in the polyester, and has good spinning condition and no blockage of the filter in the spinning process.
(3) In order to promote the crystallization of the sodium chloride, the invention carries out pretreatment on the sodium chloride.
(4) The invention optimizes and improves the spinning process according to the characteristics of the deep-dyed polyester chips.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A preparation method of a sodium chloride high-temperature deep-dyed polyester fabric comprises the following steps:
1) polyester synthesis: adding part of ethylene glycol into a reaction container, adding a dissolved sodium chloride aqueous solution, adding the rest ethylene glycol containing Sb catalyst and terephthalic acid, pulping, and reacting to obtain the sodium chloride deep-dyed polyester chip. Wherein the mass of the sodium chloride is 0.5-2% of that of the sodium chloride deep-dyed polyester chips. The molar ratio of the ethylene glycol to the terephthalic acid is 1.15-1.35: 1; the addition amount of the catalyst is 0.02-0.06% of the mass of the terephthalic acid.
The reaction conditions are specifically as follows: firstly, carrying out esterification reaction, controlling the temperature to slowly rise at the temperature rise speed of 1.5-2.5 ℃, ensuring the esterification temperature not to exceed 240 ℃, raising the temperature to 255 ℃ after the esterification is finished, and vacuumizing for 50-60min until the vacuum degree is 1800-; carrying out a polycondensation reaction: heating to above 270 deg.C, vacuumizing to 60-80pa, polycondensation temperature not exceeding 282 deg.C, and melt viscosity controlled at 0.75-0.78 dl/g.
2) Spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing to obtain pre-drawn yarns with uniform yarn levelness, and drawing and texturing to obtain drawn textured yarns.
Wherein, the drying conditions are as follows: the crystallization temperature is 135-.
The spinning components used were: the size of the filter screen is 30-40 holes, 150 meshes and 250 meshes, and the hole diameter is 0.2-0.4 mm.
The spinning process comprises the following steps: the screw temperature (the temperature of the first zone of the screw is 285-.
3) Dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
Wherein the dyeing condition is that dyeing is started from 25-35 ℃, the temperature is raised to 85-95 ℃ at the heating rate of 1.5-2.5 ℃/min, then the temperature is raised to 125-135 ℃ at the heating rate of 0.5-1.5 ℃/min, the temperature is kept for 35-45min, and the dyeing pressure is 0.3-0.5 MPa. The dye dosage is 3-7% o.w.f, the bath ratio is 1:45-55, the oil removing agent dosage is 0.8-1.2g/L, and the pH value of the dye liquor is 4-5. The reduction cleaning specifically comprises the following steps: adding 1.5-2.5g/L NaOH and 1.5-2.5g/L sodium hydrosulfite, at 75-85 deg.C for 20-40 min. The heat setting condition is 165-175 ℃ multiplied by 0.5-1.5 min.
Preferably, in step 1), the sodium chloride needs to be pretreated, and the pretreatment method comprises the following steps: isobutyl triethoxysilane was dispersed in distilled water at a mass ratio of 2.4% to distilled water, and then heated in 70 ℃ water for 20 min. This solution was then slowly added to the prepared sodium chloride solution. Meanwhile, chitosan with the mass ratio of sodium chloride of 10 percent is added to control the crystallization of the sodium chloride.
Example 1
A preparation method of a sodium chloride high-temperature deep-dyed polyester fabric comprises the following steps:
1) polyester synthesis: 387.62g of ethylene glycol is added into a reaction vessel, then dissolved sodium chloride aqueous solution is added, then 0.367g of Sb catalyst and 830g of terephthalic acid are added, and reaction is carried out after beating to obtain sodium chloride deep-dyed polyester chips.
The reaction conditions are specifically as follows: firstly, carrying out esterification reaction, controlling the temperature to slowly rise (the temperature rise speed is 2 ℃/min), controlling the esterification temperature not to exceed 240 ℃, raising the temperature to 250 ℃ after the esterification is finished, and vacuumizing for 55min to 2000 pa; carrying out a polycondensation reaction: heating to 270 deg.C, vacuumizing to 70pa, and controlling the melt viscosity at 0.75-0.78dl/g while the temp is not higher than 282 deg.C. The intrinsic viscosity obtained was 0.75dl/g and the diethylene glycol content was 1.64%.
2) Spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing, and heating by a hot roller to obtain fully drawn yarns.
Wherein the drying conditions of the slices are as follows: crystallization temperature 140 ℃ 15min, drying temperature 150 ℃ 9 h.
The spinning components used were: the size of the filter screen is 200 meshes.
The spinning process comprises the following steps: the screw temperature (screw first zone temperature: 290 ℃, second zone temperature: 293 ℃, third zone temperature: 296 ℃, fourth zone temperature: 299 ℃, fifth zone temperature: 302 ℃, sixth zone temperature: 305 ℃), the filter (mesh number: 40 mu), the box (spinning box temperature: 285 ℃), the side blowing (wind speed: 0.4m/s, nozzle: cluster oiling) -pre-network device (0.08MPa), the first hot roll (90 ℃), the second hot roll (125 ℃), the main network device (0.35MPa) -winding molding (4800 m/min).
3) Dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
Wherein, the dyeing condition is that dyeing is started from 30 ℃, the temperature is raised to 90 ℃ at the heating rate of 2 ℃/min, and then the temperature is raised to 130 ℃ at the heating rate of 1 ℃/min, and the temperature is kept for 40min (high-temperature high-pressure dyeing is adopted, and the pressure is 0.4 MPa). The ECO dosage of the dye dispersed black is 5% o.w.f, the bath ratio is 1: 50, the dosage of the degreasing agent is 1g/L, and the pH value of the dye solution is 4-5. The reduction cleaning specifically comprises the following steps: adding 2g/L NaOH and 2g/L sodium hydrosulfite, and keeping the temperature at 80 ℃ for 30 min. The heat setting condition is 170 ℃ multiplied by 1 min.
Example 2
Example 2 differs from example 1 in that the sodium chloride is pretreated: dispersing isobutyl triethoxysilane in distilled water to a concentration of 2.4 wt%, and heating in 70 deg.C water for 20 min; the resulting solution was then added to a prepared sodium chloride solution, while chitosan, 10% by mass of sodium chloride, was added to control crystallization of sodium chloride.
Example 3
A preparation method of a sodium chloride high-temperature deep-dyed polyester fabric comprises the following steps:
1) polyester synthesis: 37.36kg of ethylene glycol is added into a reaction vessel, then the pretreated sodium chloride aqueous solution is added, then the catalyst containing 35.36g of Sb and 80kg of terephthalic acid are added, and the reaction is carried out after pulping to obtain the sodium chloride deep-dyed polyester chip.
The reaction conditions are specifically as follows: firstly, carrying out esterification reaction, controlling the temperature to slowly rise (the temperature rise speed is 2 ℃/min), controlling the esterification temperature not to exceed 240 ℃, raising the temperature to 245 ℃ after the esterification is finished, and vacuumizing for 60min to 2000 pa; carrying out a polycondensation reaction: heating to above 270 deg.C, vacuumizing to 30pa, and controlling the melt viscosity at 0.75-0.78dl/g by controlling the discharge power, wherein the polycondensation temperature is not more than 282 deg.C.
2) Spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing, and heating by a hot roller to obtain fully drawn yarns.
Wherein the drying conditions of the slices are as follows: crystallization temperature 140 ℃ 20min, drying temperature 150 ℃ 9 h.
The spinning components used were: the size of the filter screen is 200 meshes.
The spinning process comprises the following steps: the screw temperature (screw first zone temperature: 290 ℃, second zone temperature: 293 ℃, third zone temperature: 296 ℃, fourth zone temperature: 299 ℃, fifth zone temperature: 302 ℃, sixth zone temperature: 305 ℃), the filter (mesh number: 40 mu), the box (spinning box temperature: 285 ℃), the side blowing (wind speed: 0.4m/s, nozzle: cluster oiling) -pre-network device (0.08MPa), the first hot roll (90 ℃), the second hot roll (125 ℃), the main network device (0.35MPa) -winding molding (4800 m/min).
3) Dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
Wherein, the dyeing condition is that dyeing is started from 30 ℃, the temperature is raised to 90 ℃ at the heating rate of 2 ℃/min, and then the temperature is raised to 130 ℃ at the heating rate of 1 ℃/min, and the temperature is kept for 40min (high-temperature high-pressure dyeing is adopted, and the pressure is 0.4 MPa). The ECO dosage of the dye dispersed black is 5% o.w.f, the bath ratio is 1: 50, the dosage of the degreasing agent is 1g/L, and the pH value of the dye solution is 4-5. The reduction cleaning specifically comprises the following steps: adding 2g/L NaOH and 2g/L sodium hydrosulfite, and keeping the temperature at 80 ℃ for 30 min. The heat setting condition is 170 ℃ multiplied by 1 min.
Example 4
A preparation method of a sodium chloride high-temperature deep-dyed polyester fabric comprises the following steps:
1) polyester synthesis: adding 18.68kg of ethylene glycol into a reaction vessel, then adding a pretreated sodium chloride aqueous solution, then adding a catalyst containing 17.68g of Sb and 40kg of terephthalic acid, pulping, and reacting to obtain the sodium chloride deep-dyed polyester chip.
The reaction conditions are specifically as follows: firstly, carrying out esterification reaction, controlling the temperature to slowly rise (the temperature rise speed is 2 ℃/min), controlling the esterification temperature not to exceed 240 ℃, raising the temperature to 255 ℃ after the esterification is finished, and vacuumizing for 50min to 2000 pa; carrying out a polycondensation reaction: heating to above 270 deg.C, vacuumizing to 30pa, and controlling the melt viscosity at 0.75-0.78dl/g by controlling the discharge power, wherein the polycondensation temperature is not more than 282 deg.C.
2) Spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing, and heating by a hot roller to obtain fully drawn yarns.
Wherein the drying conditions of the slices are as follows: crystallization temperature 140 ℃ 20min, drying temperature 150 ℃ 9 h.
The spinning components used were: the size of the filter screen is 200 meshes.
The spinning process comprises the following steps: the screw temperature (screw first zone temperature: 290 ℃, second zone temperature: 293 ℃, third zone temperature: 296 ℃, fourth zone temperature: 299 ℃, fifth zone temperature: 302 ℃, sixth zone temperature: 305 ℃), the filter (mesh number: 40 mu), the box (spinning box temperature: 285 ℃), the side blowing (wind speed: 0.4m/s, nozzle: cluster oiling) -pre-network device (0.08MPa), the first hot roll (90 ℃), the second hot roll (125 ℃), the main network device (0.35MPa) -winding molding (4800 m/min).
3) Dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
Wherein, the dyeing condition is that dyeing is started from 30 ℃, the temperature is raised to 90 ℃ at the heating rate of 2 ℃/min, and then the temperature is raised to 130 ℃ at the heating rate of 1 ℃/min, and the temperature is kept for 40min (high-temperature high-pressure dyeing is adopted, and the pressure is 0.4 MPa). The ECO dosage of the dye dispersed black is 5% o.w.f, the bath ratio is 1: 50, the dosage of the degreasing agent is 1g/L, and the pH value of the dye solution is 4-5. The reduction cleaning specifically comprises the following steps: adding 2g/L NaOH and 2g/L sodium hydrosulfite, and keeping the temperature at 80 ℃ for 30 min. The heat setting condition is 170 ℃ multiplied by 1 min.
Comparative example 1
This comparative example differs from example 1 in that: to the ethylene glycol was added sodium chloride solid, not solution.
Comparative example 2
This comparative example differs from example 1 in that: sodium chloride is added after esterification.
Comparative example 3
This comparative example differs from example 1 in that: the addition amount of sodium chloride is slightly beyond the scope of claims, and the specific addition amount is 3%.
Comparative example 4
This comparative example differs from example 1 in that: the addition amount of sodium chloride is slightly lower than the scope of claims, and the specific addition amount is 0.5%.
Table 1: corresponding K/S values after dyeing of the spun-laid fabric of the sections prepared in the different examples and comparative examples
Note: the sliced rice of the above example was spun and woven by the same process and then dyed at 130 ℃ for 40min at a disperse black ECO dye concentration of 5% o.w.f.
As can be seen from the data in table 1, the depth of staining is significantly higher than conventional in example 1, with an increase in the depth of staining of 15.7%, and a further increase in the depth of staining of 24.6% after pretreatment with sodium chloride in example 2. Examples 3 and 4 show that the increase in the depth of staining achieved 24% after scale-up of the yield. Comparative example 1 with solid sodium chloride addition, the depth of dyeing was only 10.4%, which is clearly below the saturation value of the dyeing for the best process. In comparative example 2, the addition after esterification had no effect on dye enhancement, indicating that sodium chloride did not form crystals inside the fiber. In comparative example 3 and comparative example 4, the increase in the dyeing depth was not significant when the amount of sodium chloride added was changed.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of a sodium chloride high-temperature deep-dyed polyester fabric is characterized by comprising the following steps:
1) polyester synthesis: adding part of ethylene glycol into a reaction container, adding a dissolved sodium chloride aqueous solution, adding the rest ethylene glycol containing a catalyst and terephthalic acid, pulping, and reacting to obtain sodium chloride deep-dyed polyester chips; the mass of the sodium chloride is 0.5-2% of that of the sodium chloride deep-dyed polyester slice; the sodium chloride is pretreated: dispersing isobutyl triethoxy silane in distilled water to make its concentration be 2.3-2.5wt%, heating in 65-75 deg.C water for 15-25 min; then adding the obtained solution into a prepared sodium chloride solution, and simultaneously adding chitosan with the mass of 8-12% of the sodium chloride to control the crystallization of the sodium chloride;
2) spinning: drying sodium chloride deep-dyed polyester chips, carrying out melt spinning, cooling by side blowing to obtain pre-drawn yarns with uniform yarn levelness, and drawing and texturing to obtain drawn textured yarns;
3) dyeing: weaving the stretch yarn, then dyeing at high temperature and high pressure, reducing and cleaning, and finally removing internal stress after heat setting to obtain a finished product.
2. The process according to claim 1, wherein, in step 1),
the molar ratio of the ethylene glycol to the terephthalic acid is 1.15-1.35: 1; and/or
The catalyst is an Sb catalyst; the addition amount of the catalyst is 0.02-0.06% of the mass of the terephthalic acid.
3. The process according to claim 1, wherein in step 1), the reaction conditions are in particular: firstly, carrying out esterification reaction, controlling the temperature to slowly rise at the temperature rise speed of 1.5-2.5 ℃, ensuring the esterification temperature not to exceed 240 ℃, raising the temperature to 255 ℃ after the esterification is finished, and vacuumizing for 50-60min until the vacuum degree is 1800-; carrying out a polycondensation reaction: heating to above 270 deg.C, vacuumizing to 60-80pa, polycondensation temperature not exceeding 282 deg.C, and melt viscosity controlled at 0.75-0.78 dl/g.
4. The method according to claim 1, wherein in the step 2), the drying conditions are: the crystallization temperature is 135-.
5. The method according to claim 1 or 4, wherein, in the step 2),
the spinning components used were: the size of the filter screen is 150-250 meshes;
the spinning process comprises the following steps: the parameters of the screw extruder used for melting were as follows: screw temperature: the temperature of the first zone of the screw is 285-295 ℃, the temperature of the second zone is 290-295 ℃, the temperature of the third zone is 295-298 ℃, the temperature of the fourth zone is 298-300 ℃, the temperature of the fifth zone is 300-303 ℃, and the temperature of the sixth zone is 303-306 ℃; the mesh number of the filter screen of the filter is 35-45 μm; the temperature of a spinning box is 280-290 ℃; the cross air blowing speed is 0.35-0.45 m/s; the pressure of the pre-networking device is 0.07-0.09 MPa; the temperature of the first hot roller is 85-95 ℃; the second hot roller is 120-130 ℃; the pressure of the main network device is 0.3-0.4 Mpa; the winding forming speed is 4600-5000 m/min.
6. The method as claimed in claim 1, wherein in the step 3), the dyeing condition is that dyeing is started from 25-35 ℃, the temperature is raised to 85-95 ℃ at a heating rate of 1.5-2.5 ℃/min, and then the temperature is raised to 125-135 ℃ at a heating rate of 0.5-1.5 ℃/min and the temperature is maintained for 35-45 min; the dyeing pressure is 0.3-0.5 MPa.
7. The process according to claim 1 or 6, wherein in the step 3), the amount of the dye is 3 to 7% o.w.f, the bath ratio is 1:45 to 55, the amount of the oil removing agent is 0.8 to 1.2g/L, and the pH of the dye solution is 4 to 5.
8. The method according to claim 1 or 6, wherein in step 3), the reduction washing is specifically: adding 1.5-2.5g/L NaOH and 1.5-2.5g/L sodium hydrosulfite, at 75-85 deg.C for 20-40 min; the heat setting condition is 165-175 ℃ multiplied by 0.5-1.5 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910937413.5A CN110670166B (en) | 2019-09-29 | 2019-09-29 | Preparation method of sodium chloride high-temperature deep-dyed polyester fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910937413.5A CN110670166B (en) | 2019-09-29 | 2019-09-29 | Preparation method of sodium chloride high-temperature deep-dyed polyester fabric |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110670166A CN110670166A (en) | 2020-01-10 |
| CN110670166B true CN110670166B (en) | 2022-04-22 |
Family
ID=69080330
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910937413.5A Active CN110670166B (en) | 2019-09-29 | 2019-09-29 | Preparation method of sodium chloride high-temperature deep-dyed polyester fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110670166B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112111791B (en) * | 2020-09-01 | 2021-07-23 | 杭州新天元织造有限公司 | Environment-friendly high-elasticity color-difference-free garment fabric zero-dyeing spinning process |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200702505A (en) * | 2005-07-11 | 2007-01-16 | Ind Tech Res Inst | Nanofiber and fabrication methods thereof |
| CN103320889B (en) * | 2013-06-27 | 2015-10-21 | 上海贵达科技有限公司 | Hydrophilic hygroscopic and preparation method thereof |
| CN105133067B (en) * | 2015-09-07 | 2017-07-28 | 佛山轻子精密测控技术有限公司 | A kind of manufacture method of the porous nano-fibre of controllable bore diameter |
-
2019
- 2019-09-29 CN CN201910937413.5A patent/CN110670166B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110670166A (en) | 2020-01-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018040690A1 (en) | Different-shrinkage composite yarn and preparation method therefor | |
| EP3257975B1 (en) | Method of making a fiber of polyacrylonitrile - cellulose acetate | |
| CN106400166B (en) | A kind of three leaf special-shaped polyester fiber of porous superbright light and preparation method thereof | |
| CN104480564A (en) | Super-bright light trefoil irregular FDY fiber and preparation method thereof | |
| CN104480568A (en) | Linen-like type differential shrinkage composite filament and preparation method thereof | |
| CN111910288B (en) | High-strength composite elastic fiber and preparation method thereof | |
| CN110670166B (en) | Preparation method of sodium chloride high-temperature deep-dyed polyester fabric | |
| CN106400168A (en) | Porous super-soft cotton-like polyester fiber, and preparation method thereof | |
| CN105671675A (en) | Low-color-difference polyester cotton-imitating different-shrinking composite filament and preparation method thereof | |
| CN104532392A (en) | Porous super-bright polyester fiber and preparation method thereof | |
| CN102080285A (en) | Production method of spunbonded polyester embroidery thread and product of same | |
| CN106319678A (en) | Super-soft wool-like porous polyester and preparation method thereof | |
| CN106400170B (en) | Porous super soft imitative numb polyester fiber of one kind and preparation method thereof | |
| CN115651177B (en) | Hydrophilic polyester granules and preparation method thereof | |
| CN108251909B (en) | Blending-copolymerization modified superfine denier polyester fiber and preparation method thereof | |
| CN104031251B (en) | A kind of cation dye chromophil, the continuous polymerization preparation method of anlistatig PTT copolymer | |
| CN105648594A (en) | Low-aberration polyester flax-like differential-shrinkage composite filament and preparation method thereof | |
| CN102321980A (en) | Method for dyeing terylene fabric with low temperature | |
| CN105646857B (en) | A kind of leaf shaped filaments of low aberration polyester superbright light three and preparation method thereof | |
| CN114753047A (en) | Fish scale protein modified polyamide-ammonia skin-friendly fabric and processing technology thereof | |
| AU2022273103A1 (en) | Alginate fiber and preparation method therefor | |
| CN114164516A (en) | Production method of colored polyester high-shrinkage fully drawn yarn with high light fastness | |
| CN106835406B (en) | Fabric containing aromatic polyester-aliphatic polyester block copolyester fiber and regenerated cellulose fiber and preparation method thereof | |
| CN113400684A (en) | Preparation method of gum dipping cord fabric for passenger radial tire | |
| CN111850735A (en) | Preparation method of anti-fracture sea-island composite fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |