CN107881811B - A kind of multi-functional polyamide fibre dye leveller and preparation method thereof - Google Patents
A kind of multi-functional polyamide fibre dye leveller and preparation method thereof Download PDFInfo
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- CN107881811B CN107881811B CN201711437121.2A CN201711437121A CN107881811B CN 107881811 B CN107881811 B CN 107881811B CN 201711437121 A CN201711437121 A CN 201711437121A CN 107881811 B CN107881811 B CN 107881811B
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- polyoxyethylene ether
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- octadecylamine
- trimethyl silane
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
- D06P1/607—Nitrogen-containing polyethers or their quaternary derivatives
- D06P1/6073—Nitrogen-containing polyethers or their quaternary derivatives containing CON=, OCON=, SO2N=, OSO2N= groups
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/46—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/56—Condensation products or precondensation products prepared with aldehydes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
- D06P1/607—Nitrogen-containing polyethers or their quaternary derivatives
- D06P1/6076—Nitrogen-containing polyethers or their quaternary derivatives addition products of amines and alkylene oxides or oxiranes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
- D06P1/613—Polyethers without nitrogen
- D06P1/6131—Addition products of hydroxyl groups-containing compounds with oxiranes
- D06P1/6135—Addition products of hydroxyl groups-containing compounds with oxiranes from aromatic alcohols or from phenols, naphthols
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/62—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
- D06P1/621—Compounds without nitrogen
- D06P1/622—Sulfonic acids or their salts
- D06P1/625—Aromatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to chemical assistant of textile dyeing and finishing industry and preparation method thereof, a kind of multi-functional polyamide fibre dye leveller and preparation method thereof, including a kind of multi-functional polyamide fibre dye leveller are disclosed, is made of each component of following mass percent：N polyoxyethylene ether sulfamate N polyoxyethylene ether trimethyl silanes octadecylamine 50~60%；Move dye component 5~10%；Dispersed component 5~10%；Oil removing component 10~15%；Solubilized component 15~20%.The present invention has the following advantages and effects：Pass through the various functions component of compounding, the slow metachromia of polyamide fibre levelling agent is improved, migration property, deflocculation ability, disperses to resist and returns viscous ability and emulsifying ability, polyamide fibre surface contamination oil or sundries can further be removed, improve the applicability to various complex working conditions, the stability of even dyeing effect is kept, coloring is improved.
Description
Technical field
The present invention relates to chemical assistant of textile dyeing and finishing industry and preparation method thereof, more particularly to a kind of multi-functional polyamide fibre is equal
Stain and preparation method thereof.
Background technology
Nylon fabric has the advantages that intensity is high, wearability is good, elasticity is good, fatigue durability is good, corrosion-resistant and dyeability is good,
So that people are higher and higher for the attention rate of nylon fibre, demand is also growing day by day.
Polyamide fibre dye leveller is to make nylon fibre yarn, line or the fabric even dyeing in dyeing course, does not generate vitta, color spot
Etc. faults dyeing and finishing auxiliaries.Nylon fibre yarn, line or the fabric preceding place in dyeing course can be frequently encountered in real dyeing course
It is undesirable to manage effect, to make silvalin, line or fabric surface contamination oil or sundries, oil or sundries that can influence dye leveller level dyeing effect
Fruit.But existing its single effect of polyamide fibre dye leveller, it is generally good in preceding processing, the effect of even dyeing can be reached
Fruit；Pre-treatment once go wrong or misoperation, such as dyeing course in heat up too fast, there is silvalin, line or fabric table
The case where face contamination oil or sundries, coloring is often impacted, unstable result.
Invention content
The object of the present invention is to provide a kind of multi-functional polyamide fibre dye levellers and preparation method thereof, can remove polyamide fibre surface
Contamination oil or sundries, improve the applicability to various complex working conditions, remain the stability of coloring.
The present invention above-mentioned technical purpose technical scheme is that：A kind of multi-functional polyamide fibre levelling
Agent is made of each component of following mass percent：
By using above-mentioned technical proposal, N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-ten
It has well slow metachromia energy for the synthesis of eight alkylamines, while can prevent the effect of zwitterion generation flocculation sediment；Move dye
Component its have improve polyamide fibre move dye rate；Dispersed component its have to the anti-wadding ability of dyestuff or the dispersion of oil droplet is returned be stained with energy
Power avoids the generation of polyamide fibre surface colour stain color dot；Oil removing component tool can promote emulsifying ability, ensure emulsion stability；Solubilized group
Part can improve N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine, shifting contaminates component,
The synergistic effect of dispersed component and oil removing component improves the overall performance of dye leveller.
The present invention is further arranged to, the N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-
The molecular formula of octadecylamine is：
8≤n+m≤28。
By using above-mentioned technical proposal, obtained N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyls
Silane-octadecylamine has both polyoxyethylene ether functional group, silane functional and sulfonamide functionality, not only has good
Slow metachromia energy, and there is good rush dye effect；Ensure the one-time success rate of dyeing, and can ensure the reasonable profit of dyestuff
With playing the role of environmental protection and energy saving.
The present invention is further arranged to, and the shifting dye component is octadecylamine polyoxyethylene ether, polyoxyethylene ether polymerization
Degree 10~30.
By using above-mentioned technical proposal, octadecylamine polyoxyethylene ether can avoid because of fabric existing defects itself
Caused by dyeing defect phenomenon, further increase dyeing success rate.
The present invention is further arranged to, and the dispersed component is naphthalene sulfonic acid-formaldehyde condensation product and/or sodium lignin sulfonate.
By using above-mentioned technical proposal, naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate have the anti-wadding energy to dyestuff
Power returns the ability of being stained with to the dispersion of oil droplet, avoids the generation of polyamide fibre surface colour stain color dot.
The present invention is further arranged to, and the weight ratio of the naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate is：(3~
4):(6~7).
By using above-mentioned technical proposal, naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate all have the anti-wadding to dyestuff
Ability；Since sodium lignin sulfonate does not dissolve in organic solvent, the ability of being stained with is returned in the dispersion with oil droplet, avoids polyamide fibre surface colour stain color
The generation of point；Therefore the mixing of naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate not only has the anti-wadding ability to dyestuff, and
And with the ability of being stained with is returned to the dispersion of oil droplet, avoid the generation of polyamide fibre surface colour stain color dot.
The present invention is further arranged to, and the oil removing component is cardanol polyoxyethylene ether, polyoxyethylene degree of polymerization 7-15.
By using above-mentioned technical proposal, cardanol polyoxyethylene ether can improve emulsifying ability, ensure emulsion stability.
The present invention is further arranged to, and the solubilising component is cumene sodium sulfonate.
By using above-mentioned technical proposal, cumene sodium sulfonate is cosolvent, can improve N- polyoxyethylene ether amino
Sulphonic acid ester-N- polyoxyethylene ether trimethyl silane-octadecylamine, the collaboration effect for moving dye component, dispersed component and oil removing component
It answers, improves the overall performance of dye leveller.
A kind of preparation method of multi-functional polyamide fibre dye leveller, following steps：N- polyoxyethylene ether sulfamic acids are prepared first
Ester-N- polyoxyethylene ether trimethyl silane-octadecylamine is then preparing the N- polyoxyethylene ether sulfamate-completed
Solubilized component, shifting dye component, dispersed component and oil removing group are sequentially added in N- polyoxyethylene ether trimethyl silane-octadecylamine
Part simultaneously stirs evenly.
By using above-mentioned technical proposal, N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether front threes are prepared first
Base silane-octadecylamine is then preparing the N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silicanes completed
Solubilized component is added in alkane-octadecylamine, the addition of solubilized component is so that the shifting being subsequently added contaminates component, dispersed component and removes
Oily component can be sufficiently stirred with N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine
Uniformly.
The present invention is further arranged to, N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-ten eight
The preparation method of alkylamine includes the following steps：
(1) it using the aqueous isopropanol of triethanolamine as acid binding agent in octadecylamine polyoxyethylene ethereal solution, is added dropwise
Tri-methyl-chlorosilane, pH control ranges carry out 5~6h of reaction under the conditions of 30~40 DEG C, obtain N- between 8.5~9.5
Polyoxyethylene ether trimethyl silane octadecylamine；
(2) N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are acted in urea and mixed solvent
Under, under the conditions of 80~100 DEG C of temperature, refuxing esterification reacts 3~4h, obtains N- polyoxyethylene ether sulfamate-N- polyoxies
Vinethene trimethyl silane-octadecylamine；The mixed solvent is the mixture of tetrahydrofuran and 4-methyl-2 pentanone.
By using above-mentioned technical proposal, the N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether that is formulated
It not only has good slow metachromia energy to trimethyl silane-octadecylamine, but also has good rush dye effect；Ensure dyeing
One-time success rate can ensure the reasonable utilization of dyestuff again, play the role of environmental protection and energy saving.
The present invention is further arranged to, and the addition quality of the mixed solvent is more than N- polyoxyethylene ether trimethyl silanes
The 50% of octadecylamine and sulfamic acid total amount, the tetrahydrofuran and 4-methyl-2 pentanone mass ratio (1~3):1；It is described
The molar ratio of octadecylamine polyoxyethylene ethereal solution and tri-methyl-chlorosilane is (0.8~1.0):1, the N- polyoxyethylene
The molar ratio of ether trimethyl silane octadecylamine and sulfamic acid is 1:(1.0~1.5).
By using above-mentioned technical proposal, the addition quality of the mixed solvent is more than N- polyoxyethylene ether trimethyl silicanes
The 50% of alkane octadecylamine and sulfamic acid total amount ensures the normal flow of reaction solution；The tetrahydrofuran and 4- methyl-
2 pentanone mass ratio is in (1~3):In 1 range, the abundant dissolving of raw material can be effectively ensured, and the use of urea is greatly lowered
Amount；Urea be used for catalytic amino sulfonic acid esterification, in the presence of mixed solvent, amount ratio conventional amount used reduce 50% with
On so that the molar ratio of itself and sulfamic acid is less than 0.5.
In conclusion the invention has the advantages that：
1, its tool of the synthesis of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine
There is well slow metachromia energy, while the effect of zwitterion generation flocculation sediment can be prevented；Moving dye component, it has raising polyamide fibre
Move dye rate；It has the anti-wadding ability to dyestuff or returns the ability of being stained with to the dispersion of oil droplet dispersed component, avoids polyamide fibre surface colour stain
The generation of color dot；Oil removing component tool can improve emulsifying ability, ensure emulsion stability；Solubilized component can improve N- polyoxyethylene
Ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine moves dye component, dispersed component and oil removing component
Synergistic effect improves the overall performance of dye leveller；
2, N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine, has both polyoxy second
Xi Mi functional groups, silane functional and sulfonamide functionality not only have good slow metachromia energy, but also with good rush dye
Effect；Ensure that the one-time success rate of dyeing can ensure the reasonable utilization of dyestuff again, plays the role of environmental protection and energy saving；
3, octadecylamine polyoxyethylene ether can avoid because fabric existing defects itself caused by dyeing defect phenomenon, into
One step improves dyeing success rate；
4, naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate all have the anti-wadding ability to dyestuff；Due to lignin sulfonic acid
Sodium does not dissolve in organic solvent, and the ability of being stained with is returned in the dispersion with oil droplet, avoids the generation of polyamide fibre surface colour stain color dot；Therefore naphthalene sulfonic acids
The mixing of formaldehyde condensation products and sodium lignin sulfonate not only has the anti-wadding ability to dyestuff, but also has and returned to the dispersion of oil droplet
It is stained with ability, avoids the generation of polyamide fibre surface colour stain color dot.
Specific implementation mode
Embodiment 1
A kind of multi-functional polyamide fibre dye leveller, is made of each component of following mass percent：
The molecular formula of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine is：
8≤n+m≤28。
It is octadecylamine polyoxyethylene ether, the polyoxyethylene ether degree of polymerization 10~30 to move dye component.
Dispersed component is naphthalene sulfonic acid-formaldehyde condensation product.
Oil removing component is cardanol polyoxyethylene ether, polyoxyethylene degree of polymerization 7-15.
Solubilized component is cumene sodium sulfonate.
A kind of preparation method of multi-functional polyamide fibre dye leveller, includes the following steps：N- polyoxyethylene ether amino is prepared first
Sulphonic acid ester-N- polyoxyethylene ether trimethyl silane-octadecylamine is then preparing the N- polyoxyethylene ether sulfamic acids completed
Solubilized component, shifting dye component, dispersed component are sequentially added in ester-N- polyoxyethylene ether trimethyl silane-octadecylamine and are removed
Oily component simultaneously stirs evenly.
The preparation method packet of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine
Include following steps：
(1) it using the aqueous isopropanol of triethanolamine as acid binding agent in octadecylamine polyoxyethylene ethereal solution, is added dropwise
Tri-methyl-chlorosilane, pH control ranges carry out reaction 5h 8.5 under the conditions of 40 DEG C, obtain N- polyoxyethylene ether trimethyls
Silane octadecylamine；
(2) N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are acted in urea and mixed solvent
Under, under the conditions of 80 DEG C of temperature, refuxing esterification reacts 4h, obtains N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether front threes
Base silane-octadecylamine；The mixed solvent is the mixture of tetrahydrofuran and 4-methyl-2 pentanone；Urea and amino sulphur
The molar ratio of acid amount is 0.25.
The addition quality of the mixed solvent is that N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are total
The 60% of amount, the tetrahydrofuran and 4-methyl-2 pentanone mass ratio 1:1；The octadecylamine polyoxyethylene ethereal solution with
The molar ratio of tri-methyl-chlorosilane is 0.9:1, the N- polyoxyethylene ether trimethyl silane octadecylamine and sulfamic acid
Molar ratio be 1:1.5.
Embodiment 2
A kind of multi-functional polyamide fibre dye leveller, is made of each component of following mass percent：
The molecular formula of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine is：
8≤n+m≤28。
It is octadecylamine polyoxyethylene ether, the polyoxyethylene ether degree of polymerization 10~30 to move dye component.
Dispersed component is sodium lignin sulfonate.
Oil removing component is cardanol polyoxyethylene ether, polyoxyethylene degree of polymerization 7-15.
Solubilized component is cumene sodium sulfonate.
A kind of preparation method of multi-functional polyamide fibre dye leveller, includes the following steps：N- polyoxyethylene ether amino is prepared first
Sulphonic acid ester-N- polyoxyethylene ether trimethyl silane-octadecylamine is then preparing the N- polyoxyethylene ether sulfamic acids completed
Solubilized component, shifting dye component, dispersed component are sequentially added in ester-N- polyoxyethylene ether trimethyl silane-octadecylamine and are removed
Oily component simultaneously stirs evenly.
The preparation method packet of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine
Include following steps：
(1) it using the aqueous isopropanol of triethanolamine as acid binding agent in octadecylamine polyoxyethylene ethereal solution, is added dropwise
Tri-methyl-chlorosilane, pH control ranges carry out reaction 6h 9.5 under the conditions of 30 DEG C, obtain N- polyoxyethylene ether trimethyls
Silane octadecylamine；
(2) N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are acted in urea and mixed solvent
Under, under the conditions of 100 DEG C of temperature, refuxing esterification reacts 3h, obtains N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether front threes
Base silane-octadecylamine；The mixed solvent is the mixture of tetrahydrofuran and 4-methyl-2 pentanone；Urea and amino sulphur
The molar ratio of acid amount is 0.05.
The addition quality of the mixed solvent is that N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are total
The 100% of amount, the tetrahydrofuran and 4-methyl-2 pentanone mass ratio 3:1；The octadecylamine polyoxyethylene ethereal solution with
The molar ratio of tri-methyl-chlorosilane is 1:1, the N- polyoxyethylene ether trimethyl silane octadecylamine and sulfamic acid
Molar ratio is 1：1.
Embodiment 3
A kind of multi-functional polyamide fibre dye leveller, is made of each component of following mass percent：
The molecular formula of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine is：
8≤n+m≤28。
It is octadecylamine polyoxyethylene ether, the polyoxyethylene ether degree of polymerization 10~30 to move dye component.
Dispersed component is naphthalene sulfonic acid-formaldehyde condensation product and sodium lignin sulfonate, naphthalene sulfonic acid-formaldehyde condensation product and lignin sulfonic acid
The weight ratio of sodium is：(3~4):(6~7).
Oil removing component is cardanol polyoxyethylene ether, polyoxyethylene degree of polymerization 7-15.
Solubilized component is cumene sodium sulfonate.
A kind of preparation method of multi-functional polyamide fibre dye leveller, includes the following steps：N- polyoxyethylene ether amino is prepared first
Sulphonic acid ester-N- polyoxyethylene ether trimethyl silane-octadecylamine is then preparing the N- polyoxyethylene ether sulfamic acids completed
Solubilized component, shifting dye component, dispersed component are sequentially added in ester-N- polyoxyethylene ether trimethyl silane-octadecylamine and are removed
Oily component simultaneously stirs evenly.
The preparation method packet of N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine
Include following steps：
(1) it using the aqueous isopropanol of triethanolamine as acid binding agent in octadecylamine polyoxyethylene ethereal solution, is added dropwise
Tri-methyl-chlorosilane, pH control ranges carry out reaction 5.5h 9 under the conditions of 35 DEG C, obtain N- polyoxyethylene ether trimethyls
Silane octadecylamine；
(2) N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are acted in urea and mixed solvent
Under, under the conditions of 90 DEG C of temperature, refuxing esterification reacts 3.5h, obtains N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether three
Methyl-monosilane-octadecylamine；The mixed solvent is the mixture of tetrahydrofuran and 4-methyl-2 pentanone.
The addition quality of the mixed solvent is that N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid are total
The 80% of amount, the tetrahydrofuran and 4-methyl-2 pentanone mass ratio 2:1；The octadecylamine polyoxyethylene ethereal solution with
The molar ratio of tri-methyl-chlorosilane is 0.8:1, the N- polyoxyethylene ether trimethyl silane octadecylamine and sulfamic acid
Molar ratio be 1:1.2；The molar ratio of urea and sulfamic acid is 0.10.
Following tests uses the universally recognized PA-1C60 types polyamide fibre levelling agent of Vehicles Collected from Market sample as a comparison.
(1) delay metachromia test (with reference to HG/T 4731.1-2014 standards：《Dyeing and finishing auxiliaries for textile polyamide fibre levelling agent application
The measurement of energy》)
Cloth specimen processed is contaminated according to above-mentioned technique, cloth specimen is taken out when 40 DEG C, 60 DEG C, 80 DEG C, 98 DEG C, 98 DEG C of * 40min,
By washing, drying.The depth (K/S values) of the corresponding dyeing cloth specimen of each temperature is tested respectively, and the results are shown in Table 1.
The depth table of comparisons of cloth specimen is dyed under 1 different temperatures of table
| Temperature | 40℃ | 60℃ | 80℃ | 98℃ | 98℃*40min |
| Example 1 | 0.96 | 2.65 | 9.87 | 11.31 | 11.43 |
| Example 2 | 0.98 | 2.66 | 9.58 | 11.14 | 11.35 |
| Example 3 | 0.95 | 2.72 | 9.67 | 11.20 | 11.48 |
| Comparative sample | 1.15 | 3.07 | 10.06 | 11.08 | 11.23 |
| Blank sample | 1.42 | 2.85 | 10.49 | 10.82 | 11.19 |
The case where cloth specimen K/S values being compared from table 1, it can be seen that polyamide fibre levelling agent of the present invention is in 40 DEG C, 60 DEG C, 80 DEG C of items
Under part, the depth value of dyeing cloth specimen is below comparative sample and blank sample；When temperature reaches 98 DEG C and in 98 DEG C of * 40min,
The depth value of dyeing cloth specimen is above comparative sample and blank sample, it is seen that the polyamide fibre levelling agent that each example obtains in the present invention is 40
DEG C, 60 DEG C, have under the conditions of 80 DEG C and preferably delay metachromia energy than comparative sample polyamide fibre levelling agent, and when temperature reaches 98 DEG C and 98
Have again when DEG C * 40min and promotees dye effect well.Not only it can ensure the one-time success rate of dyeing but also can ensure the reasonable of dyestuff
It utilizes, plays the role of environmental protection and energy saving.
(2) migration property is tested
Cloth specimen processed is contaminated according to above-mentioned technique, cloth specimen is taken out when 98 DEG C of * 40min, by washing, drying.Test pair respectively
The depth (K/S values) for the dyeing cloth specimen answered, and calculate shifting dye rate and (move the K/S values of white cloth and black cloth after shifting dye after contaminating
The ratio of K/S values), specific data are as shown in table 2.
The influence table of comparisons of the different levelling agents of table 2 to migration property
Each data from above-mentioned table are it is found that the migration property for the polyamide fibre levelling agent that each embodiment obtains in the present invention compares comparative sample
Polyamide fibre levelling agent is good.Migration property outstanding can preferably avoid because dyeing defect is existing caused by fabric existing defects itself
As further increasing dyeing success rate.
(3) high temperature dispersibility is tested
Preparation dye liquor is carried out according to above-mentioned formula, and dye liquor is put in steel bowl, 98 DEG C are warming up to the speed of 2 DEG C/min
Keep the temperature 40min, then cool to after 80 DEG C by dye liquor pour into preprepared with filter paper Buchner funnel in filter,
It is graded after drying by observing dyestuff flocculating degree, it is micro- to have with the flocculation of no dyestuff for 5 grades to judge the quality of dispersion performance
Dyestuff flocculation is 4 grades, and it is 3 grades to have dye granule, and more apparent dyestuff flocculation is 2 grades, and dyestuff flocculation is seriously 1 grade, and test obtains
Rating result it is as shown in table 3.
The high temperature dispersibility table of comparisons of the different levelling agents of table 3
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative sample | Blank |
| Dispersion grading | 5 | 5 | 5 | 4~4.5 | 3 |
From the point of view of 3 rating result of table, the polyamide fibre levelling agent of various embodiments of the present invention flocculates without dyestuff substantially on filter paper, and
Comparative sample polyamide fibre levelling agent dye granule on filter paper is opposite or obvious, illustrates the polyamide fibre level dyeing of various embodiments of the present invention
Agent has that return the ability of being stained with to the dispersion of oil droplet in other words for the deflocculation ability of dyestuff particularly pertinent, can effectively prevent color stain
The generation of color dot.
(4) oiliness is removed to test
The mixture of 1.0 grams of levelling agents and 10 milliliters of white oils, mineral oil, low viscosity dimethyl silicone oils etc. is uniformly mixed
Afterwards, moisturizing is to 100 milliliters, after then stirring 1 minute under high velocity agitation, goes out 5 milliliters of finish institutes with stopwatch record stratification
Criterion of the time needed as emulsifying ability performance is measured 5 times and is averaged, and the results are shown in Table 4：
The emulsifying ability table of comparisons of the different levelling agents of table 4
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative sample |
| Emulsifying ability | 6 points 43 seconds | 7 points 26 seconds | 6 points 15 seconds | Less than 2 minutes |
Each data from above-mentioned table 4 it is found that the polyamide fibre levelling agent that each embodiment obtains in the present invention its isolate 5 milliliters of oil
The agent required time is all higher than comparative sample and isolates 5 milliliters of finish required times, illustrates the brocade of various embodiments of the present invention
Synthetic fibre levelling agent ensures emulsion stability with that can improve emulsifying ability.
(5) correction data in the case of the present invention adds different components and do not add
(1) embodiment 1 is whether there is or not N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecanes
Slow metachromia comparison under base amine component, the results are shown in Table 5：
Table 5 retarding agents components influence dye level (K/S values) table of comparisons
| Temperature | 40℃ | 60℃ | 80℃ | 98℃ | 98℃*40min |
| It is dyed point containing slow | 0.96 | 2.65 | 9.87 | 11.31 | 11.43 |
| It is dyed point without slow | 1.1 | 2.81 | 9.89 | 11.02 | 11.09 |
| Blank sample | 1.42 | 2.85 | 10.49 | 10.82 | 11.19 |
As can be seen from Table 5, in the case where there is slow dye point, hence it is evident that there are the effects that the slow dye of low temperature, high temperature promote to contaminate.
(2) embodiment 1 is whether there is or not the migration properties moved under dying point to compare, and the results are shown in Table 6：
Table 6 moves stain components influence evaluation table
| Levelling agent | It is dyed point containing shifting | It is dyed point without shifting | Blank |
| Move dye rate | 96.29% | 94.1% | 87.54% |
As can be seen from Table 6, in the case of thering is shifting to dye point, hence it is evident that improve migration property energy.
(3) embodiment 1 is whether there is or not the dispersibility comparison under dispersion component, and the results are shown in Table 7：
7 dispersant component of table influences evaluation table
| Levelling agent | Containing dispersion component | Without dispersion component | Blank |
| Dispersion grading | 5 | 4~4.5 | 3 |
As can be seen from Table 7, in the case where there is dispersion component, hence it is evident that improve dispersion performance.
(4) embodiment 1 is whether there is or not except the emulsifying ability comparison under oil component, and the results are shown in Table 8：
The evaluation table that 8 degreaser component of table influences emulsifying ability
| Levelling agent | Containing except oil component | Without except oil component | Blank |
| Emulsifying ability | 6 points 43 seconds | Less than 2 minutes | Less than 2 minutes |
As can be seen from Table 8, in the case where having except oil component, stratification goes out the time of 5ml oil, hence it is evident that being longer than does not have
Except the time of oil ingredient, the emulsifying ability containing degreaser ingredient significantly improves.
(5) embodiment 1 is whether there is or not the comparison of the properties under solubilizing component, and the results are shown in Table 9：
9 solubilizer component of table influences evaluation table
As can be seen from Table 9, it in the case where there is solubilizing component, finds in slow dye, move dye, dispersion, emulsifying ability etc.
Good synergistic effect is all played, the performance of integral formula is substantially increased.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, people in the art
Member can as needed make the present embodiment the modification of not creative contribution after reading this specification, but as long as at this
It is all protected by Patent Law in the right of invention.
Claims (10)
1. a kind of multi-functional polyamide fibre dye leveller, it is characterized in that being made of each component of following mass percent：
2. a kind of multi-functional polyamide fibre dye leveller according to claim 1, it is characterized in that：The N- polyoxyethylene ether amino sulphur
The molecular formula of acid esters-N- polyoxyethylene ether trimethyl silane-octadecylamine is：
8≤n+m≤28。
3. a kind of multi-functional polyamide fibre dye leveller according to claim 1, it is characterized in that：The shifting dye component is octadecyl
Amine polyoxyethylene ether, the polyoxyethylene ether degree of polymerization are 10~30.
4. a kind of multi-functional polyamide fibre dye leveller according to claim 1, it is characterized in that：The dispersed component is naphthalene sulfonic acids first
Aldehyde condensate and/or sodium lignin sulfonate.
5. a kind of multi-functional polyamide fibre dye leveller according to claim 4, it is characterized in that：The naphthalene sulfonic acid-formaldehyde condensation product with
The weight ratio of sodium lignin sulfonate is：(3~4):(6~7).
6. a kind of multi-functional polyamide fibre dye leveller according to claim 1, it is characterized in that：The oil removing component is poly- for anacardol
Ethylene oxide ether, the polyoxyethylene degree of polymerization are 7-15.
7. a kind of multi-functional polyamide fibre dye leveller according to claim 1, it is characterized in that：The solubilising component is isopropylbenzene sulphur
Sour sodium.
8. a kind of preparation method of multi-functional polyamide fibre dye leveller according to claim 1, feature include the following steps：It is first
N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine is first prepared, is then preparing completion
N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine in sequentially add solubilized component,
It moves dye component, dispersed component and oil removing component and stirs evenly.
9. a kind of preparation method of multi-functional polyamide fibre dye leveller according to claim 8, it is characterized in that：The N- polyoxies second
The preparation method of alkene ether sulfamate-N- polyoxyethylene ether trimethyl silane-octadecylamine includes the following steps：
(1) using the aqueous isopropanol of triethanolamine as acid binding agent in octadecylamine polyoxyethylene ethereal solution, front three is added dropwise
One chlorosilane of base, pH control ranges carry out 5~6h of reaction between 8.5~9.5 under the conditions of 30~40 DEG C, obtain N- polyoxies
Vinethene trimethyl silane octadecylamine；
(2) by N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid under urea and mixed solvent effect,
Under the conditions of 80~100 DEG C of temperature, refuxing esterification reacts 3~4h, obtains N- polyoxyethylene ether sulfamate-N- polyoxyethylene ether
Trimethyl silane-octadecylamine；The mixed solvent is the mixture of tetrahydrofuran and 4-methyl-2 pentanone.
10. a kind of preparation method of multi-functional polyamide fibre dye leveller according to claim 9, it is characterized in that：The mixing is molten
The addition quality of agent is more than the 50% of N- polyoxyethylene ether trimethyl silane octadecylamines and sulfamic acid total amount, described four
Hydrogen furans and 4-methyl-2 pentanone mass ratio (1~3):1；The octadecylamine polyoxyethylene ethereal solution and one chlorine of trimethyl
The molar ratio of silane is (0.8~1.0):1, the N- polyoxyethylene ether trimethyl silane octadecylamine and sulfamic acid rub
You are than being 1:(1.0~1.5).
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| CN109267393B (en) * | 2018-07-26 | 2019-07-26 | 浙江丝科院轻纺材料有限公司 | A kind of preparation method of the oil removing level dyeing compound emulsifying agent for dacron |
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