CN107119447B - A kind of method for dyeing terylene using nano lanthanum oxide - Google Patents

A kind of method for dyeing terylene using nano lanthanum oxide Download PDF

Info

Publication number
CN107119447B
CN107119447B CN201710290813.2A CN201710290813A CN107119447B CN 107119447 B CN107119447 B CN 107119447B CN 201710290813 A CN201710290813 A CN 201710290813A CN 107119447 B CN107119447 B CN 107119447B
Authority
CN
China
Prior art keywords
terylene
lanthanum oxide
dyeing
nano lanthanum
solution
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.)
Expired - Fee Related
Application number
CN201710290813.2A
Other languages
Chinese (zh)
Other versions
CN107119447A (en
Inventor
李红
朱文庆
李莉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Polytechnic University
Original Assignee
Xian Polytechnic University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Xian Polytechnic University filed Critical Xian Polytechnic University
Priority to CN201710290813.2A priority Critical patent/CN107119447B/en
Publication of CN107119447A publication Critical patent/CN107119447A/en
Application granted granted Critical
Publication of CN107119447B publication Critical patent/CN107119447B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/45Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/16General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/62General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
    • D06P1/621Compounds without nitrogen
    • D06P1/622Sulfonic acids or their salts
    • D06P1/625Aromatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65125Compounds containing ester groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/653Nitrogen-free carboxylic acids or their salts
    • D06P1/6533Aliphatic, araliphatic or cycloaliphatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34Material containing ester groups
    • D06P3/52Polyesters
    • D06P3/54Polyesters using dispersed dyestuffs

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Coloring (AREA)

Abstract

The invention discloses a kind of method for dyeing terylene using nano lanthanum oxide, nano lanthanum oxide particle is surface modified first, alkali process is carried out to terylene again, using silane coupling agent by after surface modification nano lanthanum oxide and alkali process after terylene carry out coupling reaction, finally, to coupling, treated that terylene dyes using support methods;The affinity between carrier and disperse dyes, carrier and polyester fiber can be improved through stearic acid esterification in lanthana after surface modification, so as to reduce the glass transition temperature of terylene, therefore, after lanthana after stearic acid surface-modified is coupled to terylene surface, improve the diffusion rate of carrier and disperse dyes, so that carrier and disperse dyes is entered polyester fiber with either as singular molecular entities, improves the dye-uptake of dyeing rate and scattered dyestuff;And reaction temperature is relatively low, be conducive to carry out terylene it is blended after dyeing.

Description

A kind of method for dyeing terylene using nano lanthanum oxide
Technical field
The invention belongs to fabric dyeing method technical fields, are related to a kind of method for dyeing terylene using nano lanthanum oxide.
Background technique
The basic structural unit of polyester fiber is polyethylene terephthalate, terylene molecular weight generally 20000 or so, Impurity containing 1%-3%, chemical structural formula are as follows:
It is the basic chain link of terylene macromolecular in square brackets in formula, n is average degree of polymerization, about 130.Polyester fiber it is big There are two kinds of conformational forms of folded chain and extended chain for strand, from the point of view of polyester fiber molecular composition, it be by short fat hydrocarbon chain, Ester group, phenyl ring and terminal hydroxy group are constituted.Therefore, polyester fiber is except having no other polar groups there are in addition to two terminal hydroxy groups, thus washs Synthetic fibre fiber category hydrophobic fibre.The skin-friction coefficient of polyester fiber is very big, about 0.26-0.58, and electrical insulating property is high, and rub pole It is easy to produce static electricity, to influence going on smoothly for textile process, cause float, specking.
The continuous personalized, abundantization of requirement and effect due to people to garment fabric, it emerges largely not With the fabric of fiber, such as silk, spandex, wool, vinegar fibre, but these fibers are easy denaturation at high temperature.Terylene possesses parent The aqueous low, characteristics such as crystallinity is high, fiber alignment is close and is not easy to soak, generally use water-soluble lesser non-ionic dispersant Dyestuff dyes it by dispersing agent NNO.Since the glass transition temperature of polyester fiber is higher, disperse dyes is made to exist Entered inside terylene under Room-temperature low-pressure with high dispersive degree and achieve the effect that thoroughly upper dye is difficult to complete, thus how Carrying out dyeing to polyester fiber under atmospheric low-temperature is the hot spot studied now.Wherein, since terylene hydrophily is poor, it is unfavorable for dyeing Characteristic, the surface that more sight are invested terylene by current people is modified.The surface modification of terylene, which refers to, does not change terylene fibre Premised on tieing up script material and its performance, PET fiber surface is made to obtain new characteristic, as hydrophily, dyeability, resistance to ag(e)ing, Biocompatibility, antistatic property etc. make the characteristic of terylene maximize favourable factors and minimize unfavourable ones, are more widely used.
With the development of textile printing and dyeing science and technology, it should be noted that nano material is depended primarily on as dyeing assistant Its skin effect.The skin effect of nano material depends primarily on the size of its partial size, and as partial size reduces, specific surface area is significantly Increase, skin effect greatly improves, and therefore, how to obtain compared with the nanoparticle of small particle to its assisting-dyeing performance of raising with important Meaning.
Summary of the invention
The object of the present invention is to provide a kind of method for dyeing terylene using nano lanthanum oxide, improve terylene dye-uptake.
The technical scheme adopted by the invention is that a kind of method for dyeing terylene using nano lanthanum oxide, specifically according to Lower step is implemented:
Step 1: nano lanthanum oxide particle being surface modified using dehydrated alcohol and stearic acid;
Step 2: alkali process is carried out to terylene using sodium hydroxide solution;
Step 3: using silane coupling agent kh560 by after surface modification nano lanthanum oxide and alkali process after terylene carry out Coupling reaction;
Step 4: configuration dyestuff, acetic acid, dispersing agent NNO and gaultherolin mixed solution, using support methods to coupling at Terylene after reason is dyed, wherein dyestuff, acetic acid, dispersing agent NNO and gaultherolin dosage be respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%, reaction temperature is 85 DEG C~95 DEG C, instead It is 30min~50min between seasonable.
The features of the present invention also characterized in that
Step 1 is specifically implemented according to the following steps:
Step 1.1: nano lanthanum oxide powder is weighed, by it in 80 DEG C~90 DEG C dry 3h~4h;Measure dehydrated alcohol with Stearic acid mixing, the nano lanthanum oxide powder after drying is added thereto, at room temperature supersonic oscillations, is stirred, and mixing time is 25min~35min obtains mixture A;
Step 1.2: the mixture A that step 1.1 is obtained carries out oil bath reflux, and oil bath temperature is 75 DEG C~85 DEG C, oil bath Time is 5.5h~6.5h;
Step 1.3: the mixture A after step 1.2 oil bath is filtered, is rinsed using dehydrated alcohol, it will Products therefrom is put into vacuum oven and is dried, and drying temperature is 75 DEG C~85 DEG C, and drying time is 23h~25h, obtains Surface finish nano lanthana.
Nano lanthanum oxide mass fraction is 0.9%~1.1% in step 1, and dehydrated alcohol dosage is 91.9%~94.1%, Stearic dosage is 5%~7%, and the content summation of the above component is 100%.
Step 2 is specifically implemented according to the following steps:
Step 2.1: weighing terylene, terylene is placed in sodium hydroxide solution, be heated up to 93 DEG C~97 DEG C, the processing time is 3.5h~4.5h;
Step 2.2: will through step 2.1, treated that terylene is pulled out, use distilled water flushing, for neutrality, to dry to pH value Dry, drying temperature is 75 DEG C~85 DEG C, obtains dry alkali process terylene.
Concentration of sodium hydroxide solution is 45g/L~55g/L in step 2, and bath raio of the terylene in sodium hydroxide solution is 1: 45~55.
Step 3 is specifically implemented according to the following steps:
Step 3.1: weighing surface finish nano lanthana dry obtained by step 1, be placed in ethyl alcohol, ultrasonic vibration 10min~20min obtains the ethanol solution of lanthana;
Step 3.2: weighing silane coupling agent, ethyl alcohol is added and is diluted, step is added in the diluted silane coupling agent of gained In the ethanol solution of rapid 3.1 gained lanthana, ultrasonic vibration is uniformly mixed;
Step 3.3: weighing alkali process terylene dry obtained by step 2, be placed in the resulting mixed solution of step 3.2, add Heat simultaneously stirs, until the volatilization of diluted silane coupling agent finishes, remaining solid substance is put into vacuum oven drying, drying temperature It is 75 DEG C~85 DEG C, drying time is 2.5h~3.5h, obtains the terylene of the lanthana coupling of surface modification;
Wherein, dry surface finish nano lanthana quality be dry alkali process terylene quality 0.8%~ 1.2%;The dosage of silane coupling agent is the 2%~3% of dry alkali process terylene quality.
Step 4 is specifically implemented according to the following steps:
Step 4.1: dyestuff is prepared, and dyestuff is dissolved in the water, and ultrasonic vibration is uniform, and obtaining concentration is that 2g/L dyestuff is molten Liquid;
Step 4.2: peracetic acid formulation, by acetic acid Yu Shuizhong, ultrasonic vibration is uniform, and obtaining concentration is that 2g/L acetic acid is molten Liquid;
Step 4.3: dispersing agent NNO is prepared, and dispersing agent NNO is dissolved in the water, ultrasonic vibration is uniform, obtains concentration and is 2g/L dispersing agent NNO solution;
Step 4.4: gaultherolin lotion is prepared, and first dissolves emulsifier with hot water, gaultherolin is then added, add Water dilution, adds dehydrated alcohol, stirs evenly, obtain gaultherolin lotion;
Step 4.5: amount according to claim 1 takes dye solution made from step 4.1, step 4.2 system respectively Acetic acid solution, gaultherolin lotion made from dispersing agent NNO solution made from step 4.3 and step 4.4, wherein dye Material, acetic acid, dispersing agent NNO and gaultherolin dosage be respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%, it is uniformly mixed and dilutes, obtain dyeing mixed liquor;
Step 4.6: step 3 gained lanthana coupling terylene is placed in obtained by step 4.5 in dyeing mixed liquor, dye liquor with wash 45~55:1 of bath raio of synthetic fibre is at the uniform velocity warming up to 85 DEG C~95 DEG C, keeps the temperature 30min~50min, is then down to room temperature;
Step 4.7: the terylene after step 4.6 dyeing being pulled out, is washed with distilled water;
Step 4.8: weighing sodium dithionite and sodium hydroxide, distilled water is added to be prepared into aqueous solution, wherein every 100mL water 0.25g containing sodium dithionite~0.35g and sodium hydroxide 0.5g~1.5g in solution;
Step 4.9: step 4.7 gained terylene is placed in step 4.8 obtained aqueous solution and carries out reduction cleaning, temperature 85 DEG C~95 DEG C, clean 5min~15min;Then it pulls terylene out, is washed with distilled water to neutrality, be put into vacuum oven drying, Temperature is 75 DEG C~85 DEG C.
Emulsifier is Tween-80 in step 4.
Gaultherolin and emulsifier mass ratio are 1:10 in step 4, and gaultherolin emulsion emulsifiers concentration is 25%.
The invention has the advantages that being surface modified first to nano lanthanum oxide particle, then alkali is carried out to terylene Processing, using silane coupling agent kh560 by after surface modification nano lanthanum oxide and alkali process after terylene carry out coupling reaction, Finally, to coupling, treated that terylene dyes using support methods;Lanthana can mention after surface modification through stearic acid esterification Affinity between high carrier and disperse dyes, carrier and polyester fiber, so as to reduce the glass transition temperature of terylene, Therefore, after the lanthana after stearic acid surface-modified being coupled to terylene surface, the diffusion rate of carrier and disperse dyes is improved, So that carrier and disperse dyes is entered polyester fiber with either as singular molecular entities, improves the dye-uptake of dyeing rate and scattered dyestuff;And it reacts Temperature is relatively low, be conducive to carry out terylene it is blended after dyeing.Utilize the method for dyeing terylene process letter of nano lanthanum oxide Single, reaction condition is mild, and combined coefficient is high, at low cost.
Specific embodiment
The method for dyeing terylene using nano lanthanum oxide a kind of to the present invention carries out detailed With reference to embodiment Explanation.
Utilize the method for dyeing terylene of nano lanthanum oxide, which is characterized in that be specifically implemented according to the following steps:
Step 1: nano lanthanum oxide particle is surface modified using dehydrated alcohol and stearic acid,
Weighing mass fraction is 0.9%~1.1% nano lanthanum oxide powder, by it in 80 DEG C~90 DEG C dry 3h~4h; It measures 91.9%~94.1% dehydrated alcohol to mix with 5%~7% stearic acid, the content summation of the above component is 100%, will be done Nano lanthanum oxide powder after dry is added thereto, at room temperature supersonic oscillations, is stirred 25min~35min, is obtained mixture A, will Mixture A carries out oil bath reflux 5.5h~6.5h, and oil bath temperature is 75 DEG C~85 DEG C, filters to the mixture A after oil bath, It being rinsed using dehydrated alcohol, products therefrom is put into vacuum oven and is dried, drying temperature is 75 DEG C~85 DEG C, Drying time is 23h~25h, obtains surface finish nano lanthana;
Step 2: alkali process is carried out to terylene using sodium hydroxide solution,
Terylene is weighed, it is in 45g/L~55g/L sodium hydroxide solution that terylene, which is placed in concentration, and bath raio is 1:45~55, is added For temperature to 93 DEG C~97 DEG C, the processing time is 3.5h~4.5h;Terylene is pulled out, uses distilled water flushing to pH value for neutrality, Drying, drying temperature are 75 DEG C~85 DEG C, obtain dry alkali process terylene;
Step 3: using silane coupling agent kh560 by after surface modification nano lanthanum oxide and alkali process after terylene carry out Coupling reaction,
Surface finish nano lanthana dry obtained by step 1 is weighed, is placed in ethyl alcohol, ultrasonic vibration 10min~ 20min obtains the ethanol solution of lanthana;Silane coupling agent is weighed, ethyl alcohol is added and is diluted, the diluted silane of gained is even Connection agent is added in the ethanol solution of above-mentioned lanthana, and ultrasonic vibration is uniformly mixed, dry alkali process terylene is put into wherein, It heats and stirs, until the volatilization of diluted silane coupling agent finishes, remaining solid substance is put into vacuum oven drying, drying temperature Degree is 75 DEG C~85 DEG C, and drying time is 2.5h~3.5h, obtains the terylene of the lanthana coupling of surface modification, wherein dry Dry surface finish nano lanthana quality is the 0.8%~1.2% of dry alkali process terylene quality;The use of silane coupling agent Amount is the 2%~3% of dry alkali process terylene quality;
Step 4: dyeing,
Configuration concentration is 2g/L aqueous dye solutions, concentration is 2g/L acetic acid aqueous solution, concentration is that 2g/L dispersing agent NNO is water-soluble The gaultherolin lotion mixed solution that liquid and emulsification concentration are 25%, wherein using Tween-80 as gaultherolin The emulsifier of lotion, gaultherolin lotion gaultherolin and emulsifier mass ratio are 1:10, and four kinds of solution are uniformly mixed And dilute, dyeing mixed liquor is obtained, wherein the dosage of dyestuff, acetic acid, dispersing agent NNO and gaultherolin is respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%;Step 3 gained lanthana is coupled Terylene is placed in above-mentioned dyeing mixed liquor, 45~55:1 of bath raio of dye liquor and terylene, is at the uniform velocity warming up to 85 DEG C~95 DEG C, heat preservation 30min~50min is down to room temperature, then pulls terylene out, is washed with distilled water;Sodium dithionite and sodium hydroxide are weighed, Distilled water is added to be prepared into aqueous solution, wherein 0.25g containing sodium dithionite~0.35g and hydroxide in every 100mL aqueous solution Sodium 0.5g~1.5g;Above-mentioned terylene is placed in sodium dithionite-sodium hydrate aqueous solution and carries out reduction cleaning, temperature 85 DEG C~95 DEG C, clean 5min~15min;Then it pulls terylene out, is washed with distilled water to neutrality, be put into vacuum oven drying, Temperature is 75 DEG C~85 DEG C, and dyeing is completed;
Wherein using Tween-80 as the emulsifier of gaultherolin lotion, gaultherolin lotion salicylic acid first Ester and emulsifier mass ratio are 1:10.
Embodiment 1
Step 1, nano lanthanum oxide ball is surface modified
94.1g dehydrated alcohol and 5g stearic acid are added in flask, 0.9g nano lanthanum oxide is weighed, is added in flask, room Warm supersonic oscillations simultaneously stir 25min simultaneously;Flask is taken out, is placed in 75 DEG C of oil bath, constant temperature flows back after 5.5h, using Bu Shi Funnel is filtered, then is washed with dehydrated alcohol, is finally put it into vacuum oven and is dried 23h at 75 DEG C to get table is arrived The lanthana of face modification;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, being placed in concentration is bath raio 1:45 in 45g/L sodium hydroxide solution, the isothermal reaction at 93 DEG C 3.5h is washed to neutrality with distillation after the reaction was completed, dries at 75 DEG C;
Step 3, the lanthana obtained by step 1 after surface modification is coupled with the terylene after step 2 gained alkali process
The dry surface finish nano lanthana of 0.016g is weighed, with 95% ethyl alcohol dissolution and ultrasonic vibration 10min;Claim 0.03g silane coupling agent is taken, is diluted using ethyl alcohol, is added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;It is dry to weigh 2g Dry alkali process terylene, is added in above-mentioned mixed solution, heats and stirs, until the volatilization of diluted silane coupling agent finishes, will remain Remaining solid matter is put into vacuum oven drying, and 85 DEG C of baking 2.5h obtain lanthana coupling terylene;
Step 4, coupling terylene obtained by step 3 is dyed using support methods
It weighs 2g dyestuff to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acid is weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;It weighs 2g dispersing agent NNO to be dissolved in 1L water, obtains dispersing agent NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80 is dissolved with a small amount of hot water, 1000g gaultherolin is then added, is used The blender of 1000r/min revolving speed stirs 15min, and adding water to solution is 2850mL, continues stirring and is cooled to 50 DEG C or so, is added 50mL dehydrated alcohol continues to stir, and obtaining emulsification concentration is 25% gaultherolin lotion;
The above-mentioned dye solution of 10mL, the above-mentioned acetic acid solution of 10mL, the above-mentioned dispersing agent NNO solution of 10mL, 0.08mL are taken respectively Above-mentioned gaultherolin lotion is uniformly mixed and adds water to 100mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, is at the uniform velocity warming up to 85 DEG C, heat preservation 30min is down to room temperature;Terylene is pulled out to be washed with distilled water;
0.25g sodium dithionite and 0.5g sodium hydroxide are weighed, adds distilled water to be prepared into 100mL aqueous solution, to above-mentioned Terylene after distilling water washing carries out reduction cleaning, bath raio 1:45, and temperature is 85 DEG C, cleans 5min;Finally terylene is taken out and is used Water washing is distilled to neutrality, is put into 75 DEG C of vacuum oven drying, dyeing terylene is completed.
Embodiment 2
Step 1, nano lanthanum oxide ball is surface modified
91.9g dehydrated alcohol and 7g stearic acid are added in flask, 1.1g nano lanthanum oxide is weighed, is added in flask, room Warm supersonic oscillations simultaneously stir 35min simultaneously;Flask is taken out, is placed in 85 DEG C of oil bath, constant temperature flows back after 6.5h, using Bu Shi Funnel is filtered, then is washed with dehydrated alcohol, is finally put it into vacuum oven and is dried 25h at 85 DEG C to get table is arrived The lanthana of face modification;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, being placed in concentration is bath raio 1:55 in 55g/L sodium hydroxide solution, the isothermal reaction at 97 DEG C 4.5h is washed to neutrality with distillation after the reaction was completed, dries at 85 DEG C;
Step 3, the lanthana obtained by step 1 after surface modification is coupled with the terylene after step 2 gained alkali process
The dry surface finish nano lanthana of 0.024g is weighed, with 95% ethyl alcohol dissolution and ultrasonic vibration 20min;Claim 0.05g silane coupling agent is taken, is diluted using ethyl alcohol, is added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;It is dry to weigh 2g Dry alkali process terylene, is added in above-mentioned mixed solution, heats and stirs, until the volatilization of diluted silane coupling agent finishes, will remain Remaining solid matter is put into vacuum oven drying, and 75 DEG C of baking 3.5h obtain lanthana coupling terylene;
Step 4, coupling terylene obtained by step 3 is dyed using support methods
It weighs 2g dyestuff to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acid is weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;It weighs 2g dispersing agent NNO to be dissolved in 1L water, obtains dispersing agent NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80 is dissolved with a small amount of hot water, 1000g gaultherolin is then added, is used The blender of 1000r/min revolving speed stirs 15min, and adding water to solution is 2850mL, continues stirring and is cooled to 50 DEG C or so, is added 50mL dehydrated alcohol continues to stir, and obtaining emulsification concentration is 25% gaultherolin lotion;
The above-mentioned dye solution of 30mL, the above-mentioned acetic acid solution of 30mL, the above-mentioned dispersing agent NNO solution of 30mL, 0.24mL are taken respectively Above-mentioned gaultherolin lotion is uniformly mixed and adds water to 300mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, is at the uniform velocity warming up to 95 DEG C, heat preservation 50min is down to room temperature;Terylene is pulled out to be washed with distilled water;
0.35g sodium dithionite and 1.5g sodium hydroxide are weighed, adds distilled water to be prepared into 100mL aqueous solution, to above-mentioned Terylene after distilling water washing carries out reduction cleaning, bath raio 1:55, and temperature is 95 DEG C, cleans 15min;Finally terylene is taken out and is used Water washing is distilled to neutrality, is put into 85 DEG C of vacuum oven drying, dyeing terylene is completed.
Embodiment 3
Step 1, nano lanthanum oxide ball is surface modified
93g dehydrated alcohol and 6g stearic acid are added in flask, 1g nano lanthanum oxide is weighed, is added in flask, room temperature is super Sonication simultaneously stirs 30min simultaneously;Take out flask, be placed in 80 DEG C of oil bath, constant temperature flow back 6h after, using Buchner funnel into Row filters, then is washed with dehydrated alcohol, and it is dry for 24 hours to get to surface modification at 80 DEG C finally to put it into vacuum oven Lanthana;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, being placed in concentration is bath raio 1:50 in 50g/L sodium hydroxide solution, the isothermal reaction at 95 DEG C 4h is washed to neutrality with distillation after the reaction was completed, dries at 80 DEG C;
Step 3, the lanthana obtained by step 1 after surface modification is coupled with the terylene after step 2 gained alkali process
The dry surface finish nano lanthana of 0.02g is weighed, with 95% ethyl alcohol dissolution and ultrasonic vibration 15min;Claim 0.04g silane coupling agent is taken, is diluted using ethyl alcohol, is added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;It is dry to weigh 2g Dry alkali process terylene, is added in above-mentioned mixed solution, heats and stirs, until the volatilization of diluted silane coupling agent finishes, will remain Remaining solid matter is put into vacuum oven drying, and 80 DEG C of baking 3h obtain lanthana coupling terylene;
Step 4, coupling terylene obtained by step 3 is dyed using support methods
It weighs 2g dyestuff to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acid is weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;It weighs 2g dispersing agent NNO to be dissolved in 1L water, obtains dispersing agent NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80 is dissolved with a small amount of hot water, 1000g gaultherolin is then added, is used The blender of 1000r/min revolving speed stirs 15min, and adding water to solution is 2850mL, continues stirring and is cooled to 50 DEG C or so, is added 50mL dehydrated alcohol continues to stir, and obtaining emulsification concentration is 25% gaultherolin lotion;
The above-mentioned dye solution of 30mL, the above-mentioned acetic acid solution of 30mL, the above-mentioned dispersing agent NNO solution of 30mL, 0.24mL are taken respectively Above-mentioned gaultherolin lotion is uniformly mixed and adds water to 100mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, is at the uniform velocity warming up to 95 DEG C, heat preservation 50min is down to room temperature;Terylene is pulled out to be washed with distilled water;
0.3g sodium dithionite and 1g sodium hydroxide are weighed, distilled water is added to be prepared into 100mL aqueous solution, to above-mentioned distillation Terylene after water washing carries out reduction cleaning, bath raio 1:50, and temperature is 90 DEG C, cleans 10min;Finally terylene is taken out with distillation Water washing is put into 80 DEG C of vacuum oven drying, dyeing terylene is completed to neutrality.
Liquid after liquid before the dye of embodiment 1 and dye is detected respectively using ultraviolet specrophotometer, as a result such as 1 institute of table Show.
Table 1
Liquid after liquid before the dye of embodiment 2 and dye is detected respectively using ultraviolet specrophotometer, as a result such as 2 institute of table Show.
Table 2
Using ultraviolet specrophotometer respectively to liquid after the dye of embodiment 3, be not coupled after dye after liquid and coupling after stain liquid into Row detection, the results are shown in Table 3.
Table 3
After the lanthana after stearic acid surface-modified is coupled at terylene surface it can be seen from table 1, table 2 and table 3, It is matched using different dye liquors, dye-uptake is followed successively by 39.83%, 43.39% and 79.37%.
As can be seen from Table 3, the dye-uptake for the terylene that lanthana is coupled after surface modification is higher than the terylene without coupling, This lanthana of explanation after stearic acid surface-modified, which has dyeing terylene, promotees dye effect, this may be since lanthana is through tristearin The Esterification affinity that can be improved between carrier and disperse dyes, carrier and polyester fiber after surface modification, so as to drop The glass transition temperature of low terylene improves the diffusion rate of carrier and disperse dyes, makes carrier and disperse dyes with unimolecule Form enters polyester fiber, dyeing rate is improved, so that dye-uptake be made to improve.
Present invention nano lanthanum oxide particle first is surface modified, then carries out alkali process to terylene, using silane idol Join agent kh560 by after surface modification nano lanthanum oxide and alkali process after terylene carry out coupling reaction, finally, using support methods To coupling, treated that terylene dyes;Carrier can be improved after surface modification through stearic acid esterification for lanthana and dispersion contaminates Affinity between material, carrier and polyester fiber, so as to reduce the glass transition temperature of terylene, therefore, by stearic acid After lanthana after surface modification is coupled to terylene surface, the diffusion rate of carrier and disperse dyes is improved, carrier and dispersion are made Dyestuff enters polyester fiber with either as singular molecular entities, improves the dye-uptake of dyeing rate and scattered dyestuff;And reaction temperature is relatively low, Be conducive to carry out terylene it is blended after dyeing.Simple, the reaction condition temperature using the method for dyeing terylene process of nano lanthanum oxide It is high with, combined coefficient, it is at low cost.

Claims (9)

1. a kind of method for dyeing terylene using nano lanthanum oxide, which is characterized in that be specifically implemented according to the following steps:
Step 1: nano lanthanum oxide particle being surface modified using dehydrated alcohol and stearic acid;
Step 2: alkali process is carried out to terylene using sodium hydroxide solution;
Step 3: using silane coupling agent kh560 by after surface modification nano lanthanum oxide and alkali process after terylene be coupled Reaction;
Step 4: configuration dyestuff, acetic acid, dispersing agent NNO and gaultherolin mixed solution, using support methods to coupling processing after Terylene dyed, wherein dyestuff, acetic acid, dispersing agent NNO and gaultherolin dosage be respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%, reaction temperature is 85 DEG C~95 DEG C, instead It is 30min~50min between seasonable.
2. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 1, which is characterized in that the step 1 is specifically implemented according to the following steps:
Step 1.1: nano lanthanum oxide powder is weighed, by it in 80 DEG C~90 DEG C dry 3h~4h;Measure dehydrated alcohol and tristearin Acid-mixed is closed, and the nano lanthanum oxide powder after drying is added thereto, at room temperature supersonic oscillations, is stirred, mixing time 25min ~35min obtains mixture A;
Step 1.2: the mixture A that step 1.1 is obtained carries out oil bath reflux, and oil bath temperature is 75 DEG C~85 DEG C, the oil bath time For 5.5h~6.5h;
Step 1.3: the mixture A after step 1.2 oil bath being filtered, is rinsed using dehydrated alcohol, by gained Product is put into vacuum oven and is dried, and drying temperature is 75 DEG C~85 DEG C, and drying time is 23h~25h, obtains surface Modify nano lanthanum oxide.
3. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 2, which is characterized in that the step Nano lanthanum oxide mass fraction is 0.9%~1.1% in 1, and dehydrated alcohol dosage is 91.9%~94.1%, stearic dosage It is 5%~7%, the content summation of the above component is 100%.
4. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 1 or 3, which is characterized in that described Step 2 is specifically implemented according to the following steps:
Step 2.1: weighing terylene, terylene is placed in sodium hydroxide solution, be heated up to 93 DEG C~97 DEG C, the processing time is 3.5h ~4.5h;
Step 2.2: will through step 2.1, treated that terylene is pulled out, use distilled water flushing, for neutrality, to dry, dry to pH value Dry temperature is 75 DEG C~85 DEG C, obtains dry alkali process terylene.
5. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 4, which is characterized in that the step Concentration of sodium hydroxide solution is 45g/L~55g/L in 2, and bath raio of the terylene in sodium hydroxide solution is 1:45~55.
6. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 1, which is characterized in that the step 3 are specifically implemented according to the following steps:
Step 3.1: surface finish nano lanthana dry obtained by step 1 is weighed, is placed in ethyl alcohol, ultrasonic vibration 10min~ 20min obtains the ethanol solution of lanthana;
Step 3.2: weighing silane coupling agent, ethyl alcohol is added and is diluted, step 3.1 is added in the diluted silane coupling agent of gained In the ethanol solution of gained lanthana, ultrasonic vibration is uniformly mixed;
Step 3.3: weighing alkali process terylene dry obtained by step 2, be placed in the resulting mixed solution of step 3.2, heating is simultaneously Remaining solid substance is put into vacuum oven drying, drying temperature 75 until the volatilization of diluted silane coupling agent finishes by stirring DEG C~85 DEG C, drying time is 2.5h~3.5h, obtains the terylene of the lanthana coupling of surface modification;
Wherein, dry surface finish nano lanthana quality is the 0.8%~1.2% of dry alkali process terylene quality;Silicon The dosage of alkane coupling agent is the 2%~3% of dry alkali process terylene quality.
7. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 6, which is characterized in that the step 4 are specifically implemented according to the following steps:
Step 4.1: dyestuff is prepared, and dyestuff is dissolved in the water, and ultrasonic vibration is uniform, and obtaining concentration is 2g/L dye solution;
Step 4.2: peracetic acid formulation, by acetic acid Yu Shuizhong, ultrasonic vibration is uniform, and obtaining concentration is 2g/L acetic acid solution;
Step 4.3: dispersing agent NNO is prepared, and dispersing agent NNO is dissolved in the water, and ultrasonic vibration is uniform, obtains concentration as 2g/L points Powder NNO solution;
Step 4.4: gaultherolin lotion is prepared, and first dissolves emulsifier with hot water, gaultherolin is then added, add water dilute It releases, adds dehydrated alcohol, stir evenly, obtain gaultherolin lotion;
Step 4.5: amount according to claim 1 takes dye solution made from step 4.1, made from step 4.2 respectively Gaultherolin lotion made from dispersing agent NNO solution made from acetic acid solution, step 4.3 and step 4.4, wherein dyestuff, second The dosage of acid, dispersing agent NNO and gaultherolin is respectively 1.0%~3.0%, 1.0%~3.0%, the 1.0% of terylene quality ~3.0% and 1.0%~3.0%, it is uniformly mixed and dilutes, obtain dyeing mixed liquor;
Step 4.6: step 3 gained lanthana coupling terylene is placed in obtained by step 4.5 in dyeing mixed liquor, dye liquor and terylene 45~55:1 of bath raio is at the uniform velocity warming up to 85 DEG C~95 DEG C, keeps the temperature 30min~50min, is then down to room temperature;
Step 4.7: the terylene after step 4.6 dyeing being pulled out, is washed with distilled water;
Step 4.8: weighing sodium dithionite and sodium hydroxide, distilled water is added to be prepared into aqueous solution, wherein every 100mL aqueous solution In 0.25g containing sodium dithionite~0.35g and sodium hydroxide 0.5g~1.5g;
Step 4.9: step 4.7 gained terylene is placed in step 4.8 obtained aqueous solution and carries out reduction cleaning, temperature be 85 DEG C~ 95 DEG C, clean 5min~15min;Then it pulls terylene out, is washed with distilled water to neutrality, be put into vacuum oven drying, temperature It is 75 DEG C~85 DEG C.
8. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 7, which is characterized in that the step Emulsifier is Tween-80 in 4.
9. a kind of method for dyeing terylene using nano lanthanum oxide according to claim 8, which is characterized in that the step Gaultherolin and emulsifier mass ratio are 1:10 in 4, and gaultherolin emulsion emulsifiers concentration is 25%.
CN201710290813.2A 2017-04-28 2017-04-28 A kind of method for dyeing terylene using nano lanthanum oxide Expired - Fee Related CN107119447B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710290813.2A CN107119447B (en) 2017-04-28 2017-04-28 A kind of method for dyeing terylene using nano lanthanum oxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710290813.2A CN107119447B (en) 2017-04-28 2017-04-28 A kind of method for dyeing terylene using nano lanthanum oxide

Publications (2)

Publication Number Publication Date
CN107119447A CN107119447A (en) 2017-09-01
CN107119447B true CN107119447B (en) 2019-05-17

Family

ID=59726054

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710290813.2A Expired - Fee Related CN107119447B (en) 2017-04-28 2017-04-28 A kind of method for dyeing terylene using nano lanthanum oxide

Country Status (1)

Country Link
CN (1) CN107119447B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108486932A (en) * 2018-03-28 2018-09-04 方建波 A kind of preparation method of high stable type environmental protection color fixing agent

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1834336A (en) * 2005-03-15 2006-09-20 朱樑 Low temp fast dyeing method of polyester fibre
CN102561063A (en) * 2012-02-08 2012-07-11 上海工程技术大学 Rare earth mordant dyeing method for kapok fiber and textile thereof
CN102561065A (en) * 2012-01-13 2012-07-11 上海工程技术大学 Method for improving dye uptake and fixation rate of reactive dye on kapok fiber by using rare earth
CN104911908A (en) * 2015-05-19 2015-09-16 武汉纺织大学 Polyelectrolyte nano-membrane-mediated terylene textile normal temperature normal pressure dyeing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1834336A (en) * 2005-03-15 2006-09-20 朱樑 Low temp fast dyeing method of polyester fibre
CN102561065A (en) * 2012-01-13 2012-07-11 上海工程技术大学 Method for improving dye uptake and fixation rate of reactive dye on kapok fiber by using rare earth
CN102561063A (en) * 2012-02-08 2012-07-11 上海工程技术大学 Rare earth mordant dyeing method for kapok fiber and textile thereof
CN104911908A (en) * 2015-05-19 2015-09-16 武汉纺织大学 Polyelectrolyte nano-membrane-mediated terylene textile normal temperature normal pressure dyeing method

Also Published As

Publication number Publication date
CN107119447A (en) 2017-09-01

Similar Documents

Publication Publication Date Title
CN100537889C (en) The method of a kind of cation hybrid collosol and raising printing clearness and fastness
CN105131174B (en) It is common to lasting uvioresistant finishing agent of cotton and terylene and preparation method thereof
CN101446047B (en) Polyester fiber disperse dye low-temperature coloring accelerant BENTE and technique
CN110230216A (en) A kind of Lyocell fibers fabric of natural dye dying and preparation method thereof
CN107419462B (en) A kind of supercritical CO 2 dyeing system and dyeing
CN104894841A (en) Color-deepening finishing agent for dyed polyester textiles
CN107119447B (en) A kind of method for dyeing terylene using nano lanthanum oxide
CN107700216A (en) A kind of preparation method of nano modification fluorine-containing textile finishing agent
CN105862476A (en) Formaldehyde-free activated dye color fixing agent and preparation method thereof
CN108179642A (en) A kind of preparation method of color fixing agent for reactive dyeing
CN110004746A (en) A kind of efficient fabric dyeing accelerant
CN109403069A (en) A kind of dyeing of TR looped fabric
CN106333569B (en) A kind of polyimides Rachael blanket and its non-aqueous solvent dyeing method
WO2019006940A1 (en) Artificial compound staining agent for textiles and preparation method therefor
CN110359299A (en) A kind of terylene low temperature dyeing dyeing carrier and its preparation method and application
CN104480562B (en) A kind of high dye-uptake polyester fiber POY silk and preparation method thereof
CN113832744B (en) Environment-friendly clothing dye and application thereof in clothing printing and dyeing
CN105671995B (en) A kind of environmental protection dyeing antishifting agent and preparation method thereof
CN110922575A (en) Colored conductive polyester fiber and preparation method thereof
CN113832710B (en) Crease-resistant fabric and preparation method thereof
CN105113219B (en) Black rice anthocyanin-based cotton fabric anti-ultraviolet finishing agent
CN104499084B (en) A kind of high dye-uptake polyester fiber FDY silk and preparation method thereof
CN107513872A (en) It is a kind of be exclusively used in washing, the mixed base dyeing technique of silk blend looped fabric
US2833613A (en) Process for dyeing polyester fiber
CN107778402B (en) A kind of preparation method of high color fastness everbright fast red

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
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20190517

Termination date: 20200428