CN107119447A - A kind of method for dyeing terylene of utilization nano lanthanum oxide - Google Patents

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

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CN107119447A
CN107119447A CN201710290813.2A CN201710290813A CN107119447A CN 107119447 A CN107119447 A CN 107119447A CN 201710290813 A CN201710290813 A CN 201710290813A CN 107119447 A CN107119447 A CN 107119447A
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terylene
lanthanum oxide
dyeing
nano lanthanum
lanthana
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CN107119447B (en
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李红
朱文庆
李莉
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Xian Polytechnic University
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Xian Polytechnic University
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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

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Abstract

The invention discloses a kind of method for dyeing terylene of utilization nano lanthanum oxide, surface modification is carried out to nano lanthanum oxide particle first, again to carrying out alkali process to terylene, terylene after nano lanthanum oxide and alkali process after surface modification is carried out by coupling reaction using silane coupler, finally, the terylene after coupling processing is dyed using support methods;Lanthana can improve the affinity between carrier and disperse dyes, carrier and polyester fiber after being esterified surface modification through stearic acid, so as to reduce the glass transition temperature of terylene, therefore, lanthana after stearic acid surface-modified is coupled to behind terylene surface, improve the diffusion rate of carrier and disperse dyes, carrier and disperse dyes is entered polyester fiber with either as singular molecular entities, improve the dye-uptake of dyeing rate and scattered dyestuff;And reaction temperature is relatively low, be conducive to carrying out terylene into the dyeing after blending.

Description

A kind of method for dyeing terylene of utilization nano lanthanum oxide
Technical field
The invention belongs to fabric dyeing method technical field, it is related to a kind of method for dyeing terylene of utilization nano lanthanum oxide.
Background technology
The basic structural unit of polyester fiber is PET, and terylene molecular weight is general 20000 or so, Impurity containing 1%-3%, its chemical structural formula is:
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 in 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 has no other polar groups in addition to it there are two terminal hydroxy groups, thus washs Synthetic fibre fiber belongs to 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 Electrostatic is also easy to produce, so as to influence being smoothed out for textile process, float, specking is caused.
The continuous personalized, abundantization of requirement and effect due to people to garment fabric, therefore, are emerged largely not With the fabric of fiber, such as silk, spandex, wool, vinegar fibre, but these fibers are easily denatured at high temperature.Terylene possesses parent Aqueous low, crystallinity is high, fiber alignment is close and is difficult the characteristics such as wetting, generally using water-soluble less non-ionic dispersant Dyestuff is dyed by dispersant NNO to it.Because the glass transition temperature of polyester fiber is higher, disperse dyes are made to exist Entered under Room-temperature low-pressure inside terylene with high dispersive degree reach thoroughly upper dye effect be difficult to complete, therefore how It is the focus studied now to carry out dyeing under atmospheric low-temperature to polyester fiber.Wherein, because terylene hydrophily is poor, it is unfavorable for dyeing Characteristic, current people by more sight invest terylene surface be modified.The surface of terylene, which is modified, to be referred to not change terylene fibre Premised on tieing up script material and its performance, PET fiber surface is obtained new characteristic, such as hydrophily, dyeability, resistance to ag(e)ing, Biocompatibility, antistatic behaviour 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 as dyeing assistant, depend primarily on Its skin effect.The skin effect of nano material depends primarily on the size of its particle diameter, as particle diameter reduces, and specific surface area is significantly Increase, skin effect greatly improves, therefore, how to obtain nano-particle compared with small particle to improve its assisting-dyeing performance have it is important Meaning.
The content of the invention
It is an object of the invention to provide a kind of method for dyeing terylene of utilization nano lanthanum oxide, terylene dye-uptake is improved.
The technical solution adopted in the present invention is, a kind of method for dyeing terylene of utilization nano lanthanum oxide, specifically according to Lower step is implemented:
Step 1:Surface modification is carried out to nano lanthanum oxide particle using absolute ethyl alcohol and stearic acid;
Step 2:Alkali process is carried out to terylene using sodium hydroxide solution;
Step 3:The terylene after the nano lanthanum oxide and alkali process after surface modification is carried out using silane coupler kh560 Coupling reaction;
Step 4:Configure dyestuff, acetic acid, dispersant NNO and gaultherolin mixed solution, using support methods to coupling at Terylene after reason is dyed, wherein, dyestuff, acetic acid, the consumption of dispersant NNO and gaultherolin are 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 is also resided in,
Step 1 is specifically implemented according to following steps:
Step 1.1:Nano lanthanum oxide powder is weighed, by it in 80 DEG C~90 DEG C dry 3h~4h;Measure absolute ethyl alcohol with Stearic acid is mixed, and dried nano lanthanum oxide powder 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 backflow, and oil bath temperature is 75 DEG C~85 DEG C, oil bath Time is 5.5h~6.5h;
Step 1.3:Suction filtration is carried out to the mixture A after step 1.2 oil bath, is rinsed using absolute ethyl alcohol, will Products therefrom is put into vacuum drying chamber and is dried, and drying temperature is 75 DEG C~85 DEG C, and drying time is 23h~25h, is obtained Surface finish nano lanthana.
Nano lanthanum oxide mass fraction is 0.9%~1.1% in step 1, and absolute ethyl alcohol consumption is 91.9%~94.1%, Stearic consumption is 5%~7%, and the content summation of above component is 100%.
Step 2 is specifically implemented according to following steps:
Step 2.1:Terylene is weighed, terylene is placed in sodium hydroxide solution, 93 DEG C~97 DEG C are heated up to, processing time is 3.5h~4.5h;
Step 2.2:Terylene after being handled through step 2.1 is pulled out, uses distilled water flushing, for neutrality, to be dried to acid-base 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 following steps:
Step 3.1:The surface finish nano lanthana dried obtained by step 1 is weighed, is placed in ethanol, ultrasonic vibration 10min~20min, obtains the ethanol solution of lanthana;
Step 3.2:Silane coupler is weighed, ethanol is added and is diluted, the silane coupler that gained dilutes is added and walked In the ethanol solution of rapid 3.1 gained lanthana, ultrasonic vibration is well mixed;
Step 3.3:The alkali process terylene dried obtained by step 2 is weighed, is placed in the mixed solution obtained by step 3.2, plus Heat is simultaneously stirred, until the volatilization of diluted silane coupling agent is finished, remaining solid material is put into vacuum drying chamber drying, drying temperature For 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 for dry alkali process terylene quality 0.8%~ 1.2%;The consumption of silane coupler is the 2%~3% of dry alkali process terylene quality.
Step 4 is specifically implemented according to following steps:
Step 4.1:Dyestuff is prepared, and dyestuff is dissolved in the water, and ultrasonic vibration is uniform, obtains concentration molten for 2g/L dyestuffs Liquid;
Step 4.2:Peracetic acid formulation, by acetic acid in water, ultrasonic vibration is uniform, obtains concentration molten for 2g/L acetic acid Liquid;
Step 4.3:Dispersant NNO is prepared, and dispersant NNO is dissolved in the water, and ultrasonic vibration is uniform, and obtaining concentration is 2g/L dispersant NNO solution;
Step 4.4:Gaultherolin emulsion is prepared, and is first dissolved emulsifying agent with hot water, is then added gaultherolin, plus Water dilutes, and adds absolute ethyl alcohol, stirs, obtains gaultherolin emulsion;
Step 4.5:Amount according to claim 1, takes dye solution, step 4.2 made from step 4.1 to make respectively Acetic acid solution, gaultherolin emulsion made from dispersant NNO solution made from step 4.3 and step 4.4, wherein, dye Material, acetic acid, the consumption of dispersant NNO and gaultherolin be respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%, it is well mixed and dilutes, obtains dyeing mixed liquor;
Step 4.6:Step 3 gained lanthana coupling terylene is placed in dyeing mixed liquor obtained by step 4.5, dye liquor is with washing The bath raio 45~55 of synthetic fibre:1,85 DEG C~95 DEG C are at the uniform velocity warming up to, 30min~50min is incubated, is then down to room temperature;
Step 4.7:Terylene after being dyed through step 4.6 is pulled out, with distillation water washing;
Step 4.8:Sodium dithionite and sodium hydroxide are weighed, plus distilled water is prepared into the aqueous solution, wherein per 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 is 85 DEG C~95 DEG C, clean 5min~15min;Then pull terylene out, be washed with distilled water to neutrality, be put into vacuum drying chamber drying, Temperature is 75 DEG C~85 DEG C.
Emulsifying agent is Tween-80 in step 4.
Gaultherolin and emulsifying agent mass ratio are 1 in step 4:10, gaultherolin emulsion emulsifiers concentration is 25%.
The beneficial effects of the invention are as follows, surface modification is carried out to nano lanthanum oxide particle first, then to carrying out alkali to terylene Processing, coupling reaction is carried out using silane coupler kh560 by the terylene after the nano lanthanum oxide and alkali process after surface modification, Finally, the terylene after coupling processing is dyed using support methods;Lanthana can be carried after being esterified surface modification through stearic acid Affinity between high carrier and disperse dyes, carrier and polyester fiber, so as to reduce the glass transition temperature of terylene, Therefore, the lanthana after stearic acid surface-modified is coupled to behind terylene surface, improves the diffusion rate of carrier and disperse dyes, Carrier and disperse dyes is entered polyester fiber with either as singular molecular entities, improve the dye-uptake of dyeing rate and scattered dyestuff;And reaction Temperature is relatively low, is conducive to carrying out terylene into the dyeing after blending.Utilize the method for dyeing terylene process letter of nano lanthanum oxide Single, reaction condition is gentle, and combined coefficient is high, and cost is low.
Embodiment
A kind of method for dyeing terylene using nano lanthanum oxide of the invention is carried out with reference to embodiment detailed Explanation.
Utilize the method for dyeing terylene of nano lanthanum oxide, it is characterised in that specifically implement according to following steps:
Step 1:Surface modification is carried out to nano lanthanum oxide particle using absolute ethyl alcohol and stearic acid,
Mass fraction is weighed for 0.9%~1.1% nano lanthanum oxide powder, by it in 80 DEG C~90 DEG C dry 3h~4h; Measure 91.9%~94.1% absolute ethyl alcohol to mix with 5%~7% stearic acid, the content summation of above component is 100%, will be dry 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 backflow 5.5h~6.5h, and oil bath temperature is 75 DEG C~85 DEG C, and suction filtration is carried out to the mixture A after oil bath, It is rinsed using absolute ethyl alcohol, products therefrom is put into vacuum drying chamber 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, terylene is placed in concentration in 45g/L~55g/L sodium hydroxide solutions, bath raio is 1:45~55, plus Temperature is to 93 DEG C~97 DEG C, and processing time is 3.5h~4.5h;Terylene is pulled out, uses distilled water flushing to acid-base value for neutrality, Drying, drying temperature is 75 DEG C~85 DEG C, obtains dry alkali process terylene;
Step 3:The terylene after the nano lanthanum oxide and alkali process after surface modification is carried out using silane coupler kh560 Coupling reaction,
The surface finish nano lanthana dried obtained by step 1 is weighed, is placed in ethanol, ultrasonic vibration 10min~ 20min, obtains the ethanol solution of lanthana;Silane coupler is weighed, ethanol is added and is diluted, the silane that gained is diluted is even Join agent to add in the ethanol solution of above-mentioned lanthana, ultrasonic vibration is well mixed, dry alkali process terylene is put into wherein, Heat and stir, until the volatilization of diluted silane coupling agent is finished, remaining solid material is put into vacuum drying chamber drying, drying temperature Spend for 75 DEG C~85 DEG C, drying time is 2.5h~3.5h, obtain the terylene of the lanthana coupling of surface modification, wherein, do Dry surface finish nano lanthana quality is the 0.8%~1.2% of dry alkali process terylene quality;The use of silane coupler Amount is the 2%~3% of dry alkali process terylene quality;
Step 4:Dyeing,
Configuration concentration is that 2g/L aqueous dye solutions, concentration are that 2g/L acetic acid aqueous solutions, concentration are that 2g/L dispersants NNO is water-soluble The gaultherolin emulsion mixed solution that liquid and emulsification concentration are 25%, wherein being used as gaultherolin by the use of Tween-80 The emulsifying agent of emulsion, gaultherolin emulsion gaultherolin is 1 with emulsifying agent mass ratio:10, four kinds of solution are well mixed And dilute, obtain dyeing mixed liquor, the consumption of wherein dyestuff, acetic acid, dispersant NNO and gaultherolin is respectively terylene quality 1.0%~3.0%, 1.0%~3.0%, 1.0%~3.0% and 1.0%~3.0%;By the coupling of step 3 gained lanthana Terylene is placed in above-mentioned dyeing mixed liquor, the bath raio 45~55 of dye liquor and terylene:1, at the uniform velocity it is warming up to 85 DEG C~95 DEG C, insulation 30min~50min, is down to room temperature, then pulls terylene out, with distillation water washing;Sodium dithionite and sodium hydroxide are weighed, Plus distilled water is prepared into the aqueous solution, wherein 0.25g containing sodium dithionite~0.35g and hydroxide in per the 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 is 85 DEG C~95 DEG C, clean 5min~15min;Then pull terylene out, be washed with distilled water to neutrality, be put into vacuum drying chamber drying, Temperature is 75 DEG C~85 DEG C, and dyeing is completed;
Wherein by the use of Tween-80 as the emulsifying agent of gaultherolin emulsion, gaultherolin emulsion salicylic acid first Ester is 1 with emulsifying agent mass ratio:10.
Embodiment 1
Step 1, surface modification is carried out to nano lanthanum oxide ball
94.1g absolute ethyl alcohols and 5g stearic acid are added in flask, 0.9g nano lanthanum oxides are weighed, added in flask, room Warm supersonic oscillations simultaneously stir 25min simultaneously;Flask is taken out, in the oil bath for being placed in 75 DEG C, after constant temperature backflow 5.5h, using Bu Shi Funnel carries out suction filtration, then is washed with absolute ethyl alcohol, finally puts it into vacuum drying chamber and 23h is dried at 75 DEG C, that is, obtain table The lanthana of face modification;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, concentration is placed in in 45g/L sodium hydroxide solutions, bath raio is 1:45, the isothermal reaction at 93 DEG C 3.5h, is washed at neutrality, 75 DEG C with distillation after the completion of reaction and dried;
Step 3, the lanthana after step 1 gained surface modification is coupled with the terylene after step 2 gained alkali process
The surface finish nano lanthana of 0.016g dryings is weighed, ethanol dissolving and ultrasonic vibration 10min with 95%;Claim 0.03g silane couplers are taken, are diluted using ethanol, are added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;2g is weighed to do Dry alkali process terylene, adds in above-mentioned mixed solution, heats and stir, until the volatilization of diluted silane coupling agent is finished, will be surplus Remaining solid matter is put into vacuum drying chamber 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
Weigh 2g dyestuffs to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acids are weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;Weigh 2g dispersants NNO to be dissolved in 1L water, obtain dispersant NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80s are dissolved with a small amount of hot water, 1000g gaultherolins are then added, used The mixer stirring 15min of 1000r/min rotating speeds, adds water to solution for 2850mL, continues stirring and is cooled to 50 DEG C or so, addition 50mL absolute ethyl alcohols, continue to stir, and it is 25% gaultherolin emulsion to obtain emulsification concentration;
The above-mentioned dye solutions of 10mL, the above-mentioned acetic acid solutions of 10mL, the above-mentioned dispersant NNO solution of 10mL, 0.08mL are taken respectively Above-mentioned gaultherolin emulsion, is well mixed and adds water to 100mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, 85 DEG C, insulation are at the uniform velocity warming up to 30min, is down to room temperature;Pull terylene distillation water washing out;
0.25g sodium dithionites and 0.5g sodium hydroxides are weighed, plus distilled water is prepared into the 100mL aqueous solution, to above-mentioned Distill the terylene after water washing and carry out reduction cleaning, bath raio 1:45, temperature is 85 DEG C, cleans 5min;Finally terylene is taken out and used Water washing is distilled to neutrality, 75 DEG C of drying of vacuum drying chamber are put into, and dyeing terylene is completed.
Embodiment 2
Step 1, surface modification is carried out to nano lanthanum oxide ball
91.9g absolute ethyl alcohols and 7g stearic acid are added in flask, 1.1g nano lanthanum oxides are weighed, added in flask, room Warm supersonic oscillations simultaneously stir 35min simultaneously;Flask is taken out, in the oil bath for being placed in 85 DEG C, after constant temperature backflow 6.5h, using Bu Shi Funnel carries out suction filtration, then is washed with absolute ethyl alcohol, finally puts it into vacuum drying chamber and 25h is dried at 85 DEG C, that is, obtain table The lanthana of face modification;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, concentration is placed in in 55g/L sodium hydroxide solutions, bath raio is 1:55, the isothermal reaction at 97 DEG C 4.5h, is washed at neutrality, 85 DEG C with distillation after the completion of reaction and dried;
Step 3, the lanthana after step 1 gained surface modification is coupled with the terylene after step 2 gained alkali process
The surface finish nano lanthana of 0.024g dryings is weighed, ethanol dissolving and ultrasonic vibration 20min with 95%;Claim 0.05g silane couplers are taken, are diluted using ethanol, are added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;2g is weighed to do Dry alkali process terylene, adds in above-mentioned mixed solution, heats and stir, until the volatilization of diluted silane coupling agent is finished, will be surplus Remaining solid matter is put into vacuum drying chamber 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
Weigh 2g dyestuffs to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acids are weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;Weigh 2g dispersants NNO to be dissolved in 1L water, obtain dispersant NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80s are dissolved with a small amount of hot water, 1000g gaultherolins are then added, used The mixer stirring 15min of 1000r/min rotating speeds, adds water to solution for 2850mL, continues stirring and is cooled to 50 DEG C or so, addition 50mL absolute ethyl alcohols, continue to stir, and it is 25% gaultherolin emulsion to obtain emulsification concentration;
The above-mentioned dye solutions of 30mL, the above-mentioned acetic acid solutions of 30mL, the above-mentioned dispersant NNO solution of 30mL, 0.24mL are taken respectively Above-mentioned gaultherolin emulsion, is well mixed and adds water to 300mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, 95 DEG C, insulation are at the uniform velocity warming up to 50min, is down to room temperature;Pull terylene distillation water washing out;
0.35g sodium dithionites and 1.5g sodium hydroxides are weighed, plus distilled water is prepared into the 100mL aqueous solution, to above-mentioned Distill the terylene after water washing and carry out reduction cleaning, bath raio 1:55, temperature is 95 DEG C, cleans 15min;Finally terylene is taken out and used Water washing is distilled to neutrality, 85 DEG C of drying of vacuum drying chamber are put into, and dyeing terylene is completed.
Embodiment 3
Step 1, surface modification is carried out to nano lanthanum oxide ball
93g absolute ethyl alcohols and 6g stearic acid are added in flask, 1g nano lanthanum oxides are weighed, added in flask, room temperature surpasses Sonication simultaneously stirs 30min simultaneously;Flask is taken out, in the oil bath for being placed in 80 DEG C, after constant temperature backflow 6h, is entered using Buchner funnel Row suction filtration, then washed with absolute ethyl alcohol, finally put it into vacuum drying chamber and 24h is dried at 80 DEG C, that is, obtain surface modification Lanthana;
Step 2, alkali process is carried out to terylene
2g terylene is weighed, concentration is placed in in 50g/L sodium hydroxide solutions, bath raio is 1:50, the isothermal reaction at 95 DEG C 4h, is washed at neutrality, 80 DEG C with distillation after the completion of reaction and dried;
Step 3, the lanthana after step 1 gained surface modification is coupled with the terylene after step 2 gained alkali process
The surface finish nano lanthana of 0.02g dryings is weighed, ethanol dissolving and ultrasonic vibration 15min with 95%;Claim 0.04g silane couplers are taken, are diluted using ethanol, are added in above-mentioned lanthana ethanol solution, ultrasonic vibration mixing;2g is weighed to do Dry alkali process terylene, adds in above-mentioned mixed solution, heats and stir, until the volatilization of diluted silane coupling agent is finished, will be surplus Remaining solid matter is put into vacuum drying chamber 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
Weigh 2g dyestuffs to be dissolved in 1L water, ultrasonic vibration is uniform, obtains dye solution;2g acetic acids are weighed in 1L water In, ultrasonic vibration is uniform, obtains acetic acid solution;Weigh 2g dispersants NNO to be dissolved in 1L water, obtain dispersant NNO solution, surpass Acoustic shock is swung uniformly;First 100g Tween-80s are dissolved with a small amount of hot water, 1000g gaultherolins are then added, used The mixer stirring 15min of 1000r/min rotating speeds, adds water to solution for 2850mL, continues stirring and is cooled to 50 DEG C or so, addition 50mL absolute ethyl alcohols, continue to stir, and it is 25% gaultherolin emulsion to obtain emulsification concentration;
The above-mentioned dye solutions of 30mL, the above-mentioned acetic acid solutions of 30mL, the above-mentioned dispersant NNO solution of 30mL, 0.24mL are taken respectively Above-mentioned gaultherolin emulsion, is well mixed and adds water to 100mL, obtains dyeing mixed liquor;
Step 3 gained lanthana coupling terylene is placed in above-mentioned dyeing mixed liquor, 95 DEG C, insulation are at the uniform velocity warming up to 50min, is down to room temperature;Pull terylene distillation water washing out;
0.3g sodium dithionites and 1g sodium hydroxides are weighed, plus distilled water is prepared into the 100mL aqueous solution, to above-mentioned distillation Terylene after water washing carries out reduction cleaning, bath raio 1:50, temperature is 90 DEG C, cleans 10min;Finally terylene taking-up is distilled Water washing is put into 80 DEG C of drying of vacuum drying chamber to neutrality, and dyeing terylene is completed.
Liquid after liquid before the dye of embodiment 1 and dye is detected respectively using ultraviolet specrophotometer, as a result such as the institute of table 1 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 the institute of table 2 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 that liquid enters Row detection, as a result as shown in table 3.
Table 3
The lanthana after stearic acid surface-modified is coupled at behind terylene surface it can be seen from table 1, table 2 and table 3, Matched using different dye liquors, its dye-uptake is followed successively by 39.83%, 43.39% and 79.37%.
As can be seen from Table 3, the dye-uptake of the terylene of surface modification rear oxidation lanthanum coupling is higher than the terylene without coupling, This lanthana of explanation after stearic acid surface-modified has rush dye effect to dyeing terylene, and this is probably because lanthana is through tristearin The affinity between carrier and disperse dyes, carrier and polyester fiber can be improved after Esterification 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, improves dyeing rate, so that dye-uptake is improved.
Present invention nano lanthanum oxide particle first carries out surface modification, then to carrying out alkali process to terylene, it is even using silane Join agent kh560 and the terylene after the nano lanthanum oxide and alkali process after surface modification is subjected to coupling reaction, finally, using support methods Terylene after coupling processing is dyed;Lanthana can improve carrier and scattered dye after being esterified surface modification through stearic acid Affinity between material, carrier and polyester fiber, so as to reduce the glass transition temperature of terylene, therefore, by stearic acid Lanthana after surface modification is coupled to behind terylene surface, improves the diffusion rate of carrier and disperse dyes, makes carrier and scattered 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 carrying out terylene into the dyeing after blending.Simple, the reaction condition temperature using the method for dyeing terylene process of nano lanthanum oxide High with, combined coefficient, cost is low.

Claims (9)

1. a kind of method for dyeing terylene of utilization nano lanthanum oxide, it is characterised in that specifically implement according to following steps:
Step 1:Surface modification is carried out to nano lanthanum oxide particle using absolute ethyl alcohol and stearic acid;
Step 2:Alkali process is carried out to terylene using sodium hydroxide solution;
Step 3:The terylene after the nano lanthanum oxide and alkali process after surface modification is coupled using silane coupler kh560 Reaction;
Step 4:Configure dyestuff, acetic acid, dispersant NNO and gaultherolin mixed solution, using support methods to coupling processing after Terylene dyed, wherein, dyestuff, acetic acid, the consumption of dispersant NNO and gaultherolin are 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. lanthana according to claim 1, is applied into dyeing terylene, it is characterised in that the step 1 it is specific according to Following steps are implemented:
Step 1.1:Nano lanthanum oxide powder is weighed, by it in 80 DEG C~90 DEG C dry 3h~4h;Measure absolute ethyl alcohol and tristearin Acid mixing, dried nano lanthanum oxide powder is added thereto, at room temperature supersonic oscillations, is stirred, mixing time is 25min ~35min, obtains mixture A;
Step 1.2:The mixture A that step 1.1 is obtained carries out oil bath backflow, and oil bath temperature is 75 DEG C~85 DEG C, oil bath time For 5.5h~6.5h;
Step 1.3:Suction filtration is carried out to the mixture A after step 1.2 oil bath, is rinsed using absolute ethyl alcohol, by gained Product is put into vacuum drying chamber 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 of utilization nano lanthanum oxide according to claim 2, it is characterised in that the step Nano lanthanum oxide mass fraction is 0.9%~1.1% in 1, and absolute ethyl alcohol consumption is 91.9%~94.1%, stearic consumption For 5%~7%, the content summation of above component is 100%.
4. the method for dyeing terylene of a kind of utilization nano lanthanum oxide according to claim 1 or 3, it is characterised in that described Step 2 is specifically implemented according to following steps:
Step 2.1:Terylene is weighed, terylene is placed in sodium hydroxide solution, 93 DEG C~97 DEG C are heated up to, processing time is 3.5h ~4.5h;
Step 2.2:Terylene after being handled through step 2.1 is pulled out, uses distilled water flushing, for neutrality, to dry, dry to acid-base value Dry temperature is 75 DEG C~85 DEG C, obtains dry alkali process terylene.
5. a kind of method for dyeing terylene of utilization nano lanthanum oxide according to claim 4, it is characterised 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 of utilization nano lanthanum oxide according to claim 1, it is characterised in that the step 3 specifically implement according to following steps:
Step 3.1:The surface finish nano lanthana dried obtained by step 1 is weighed, is placed in ethanol, ultrasonic vibration 10min~ 20min, obtains the ethanol solution of lanthana;
Step 3.2:Silane coupler is weighed, ethanol is added and is diluted, the silane coupler that gained dilutes is added into step 3.1 In the ethanol solution of gained lanthana, ultrasonic vibration is well mixed;
Step 3.3:The alkali process terylene dried obtained by step 2 is weighed, is placed in the mixed solution obtained by step 3.2, heating is simultaneously Stirring, until the volatilization of diluted silane coupling agent is finished, is put into vacuum drying chamber drying, drying temperature is 75 by remaining solid material 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 consumption of alkane coupling agent is the 2%~3% of dry alkali process terylene quality.
7. a kind of method for dyeing terylene of utilization nano lanthanum oxide according to claim 6, it is characterised in that the step 4 specifically implement according to following steps:
Step 4.1:Dyestuff is prepared, and dyestuff is dissolved in the water, and ultrasonic vibration is uniform, obtains concentration for 2g/L dye solutions;
Step 4.2:Peracetic acid formulation, by acetic acid in water, ultrasonic vibration is uniform, obtains concentration for 2g/L acetic acid solutions;
Step 4.3:Dispersant NNO is prepared, and dispersant NNO is dissolved in the water, and ultrasonic vibration is uniform, and it is 2g/L points to obtain concentration Powder NNO solution;
Step 4.4:Gaultherolin emulsion is prepared, and is first dissolved emulsifying agent with hot water, is then added gaultherolin, adds water dilute Release, add absolute ethyl alcohol, stir, obtain gaultherolin emulsion;
Step 4.5:Amount according to claim 1, takes dye solution made from step 4.1, made from step 4.2 respectively Gaultherolin emulsion made from dispersant NNO solution made from acetic acid solution, step 4.3 and step 4.4, wherein, dyestuff, second The consumption of acid, dispersant 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 well mixed and dilutes, obtains dyeing mixed liquor;
Step 4.6:Step 3 gained lanthana coupling terylene is placed in dyeing mixed liquor obtained by step 4.5, dye liquor and terylene Bath raio 45~55:1,85 DEG C~95 DEG C are at the uniform velocity warming up to, 30min~50min is incubated, is then down to room temperature;
Step 4.7:Terylene after being dyed through step 4.6 is pulled out, with distillation water washing;
Step 4.8:Sodium dithionite and sodium hydroxide are weighed, plus distilled water is prepared into the aqueous solution, wherein per the 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 pull terylene out, be washed with distilled water to neutrality, be put into vacuum drying chamber drying, temperature For 75 DEG C~85 DEG C.
8. a kind of method for dyeing terylene of utilization nano lanthanum oxide according to claim 7, it is characterised in that the step Emulsifying agent is Tween-80 in 4.
9. a kind of method for dyeing terylene of utilization nano lanthanum oxide according to claim 8, it is characterised in that the step Gaultherolin and emulsifying agent mass ratio are 1 in 4:10, gaultherolin emulsion emulsifiers concentration is 25%.
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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
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