CN114541158B - Composite functional auxiliary agent for spinning and preparation method and application thereof - Google Patents
Composite functional auxiliary agent for spinning and preparation method and application thereof Download PDFInfo
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- CN114541158B CN114541158B CN202210118143.7A CN202210118143A CN114541158B CN 114541158 B CN114541158 B CN 114541158B CN 202210118143 A CN202210118143 A CN 202210118143A CN 114541158 B CN114541158 B CN 114541158B
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- Prior art keywords
- nylon
- composite functional
- auxiliary agent
- dyeing
- formaldehyde
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- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title description 5
- 238000009987 spinning Methods 0.000 title description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 128
- 238000004043 dyeing Methods 0.000 claims abstract description 43
- -1 aromatic sulfonic acid compound Chemical class 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 150000002989 phenols Chemical class 0.000 claims abstract description 13
- 239000002516 radical scavenger Substances 0.000 claims abstract description 13
- 229920001778 nylon Polymers 0.000 claims description 56
- 239000004677 Nylon Substances 0.000 claims description 47
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 238000004383 yellowing Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 18
- 239000004753 textile Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- XEVRDFDBXJMZFG-UHFFFAOYSA-N carbonyl dihydrazine Chemical compound NNC(=O)NN XEVRDFDBXJMZFG-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 8
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 claims description 7
- 229940044654 phenolsulfonic acid Drugs 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- JIRHAGAOHOYLNO-UHFFFAOYSA-N (3-cyclopentyloxy-4-methoxyphenyl)methanol Chemical compound COC1=CC=C(CO)C=C1OC1CCCC1 JIRHAGAOHOYLNO-UHFFFAOYSA-N 0.000 claims description 5
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 5
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 claims description 4
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 claims description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229960002887 deanol Drugs 0.000 claims description 4
- 239000012972 dimethylethanolamine Substances 0.000 claims description 4
- YAMHXTCMCPHKLN-UHFFFAOYSA-N imidazolidin-2-one Chemical compound O=C1NCCN1 YAMHXTCMCPHKLN-UHFFFAOYSA-N 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 claims description 3
- ODLIHNXQTJXBDT-UHFFFAOYSA-N 2-hydroxy-6-methylbenzenesulfonic acid Chemical compound CC1=CC=CC(O)=C1S(O)(=O)=O ODLIHNXQTJXBDT-UHFFFAOYSA-N 0.000 claims description 3
- DOBIZWYVJFIYOV-UHFFFAOYSA-N 7-hydroxynaphthalene-1,3-disulfonic acid Chemical compound C1=C(S(O)(=O)=O)C=C(S(O)(=O)=O)C2=CC(O)=CC=C21 DOBIZWYVJFIYOV-UHFFFAOYSA-N 0.000 claims description 3
- HUYJTJXLNBOVFO-UHFFFAOYSA-N 7-hydroxynaphthalene-1-sulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(O)=CC=C21 HUYJTJXLNBOVFO-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical compound CNN HDZGCSFEDULWCS-UHFFFAOYSA-N 0.000 claims description 3
- KVBGVZZKJNLNJU-UHFFFAOYSA-N naphthalene-2-sulfonic acid Chemical compound C1=CC=CC2=CC(S(=O)(=O)O)=CC=C21 KVBGVZZKJNLNJU-UHFFFAOYSA-N 0.000 claims description 3
- 229920006052 Chinlon® Polymers 0.000 abstract description 4
- 239000004744 fabric Substances 0.000 description 24
- 238000004321 preservation Methods 0.000 description 22
- 238000001816 cooling Methods 0.000 description 15
- 239000000498 cooling water Substances 0.000 description 12
- 238000010992 reflux Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229920002334 Spandex Polymers 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000008098 formaldehyde solution Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000004759 spandex Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007730 finishing process Methods 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/06—After-treatment with organic compounds containing nitrogen
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Coloring (AREA)
Abstract
The invention discloses a composite functional auxiliary agent for chinlon dyeing, which comprises the following components in percentage by mass: 15-30% of aromatic sulfonic acid compound, 0-15% of phenolic compound, 1-6% of catalyst, 5-15% of formaldehyde aqueous solution, 2-6% of formaldehyde scavenger, 10-30% of amine compound and the balance of deionized water.
Description
Technical Field
The invention relates to a composite functional auxiliary agent for spinning and a preparation method and application thereof, in particular to a composite functional auxiliary agent for nylon dyeing and a preparation method and application thereof, belonging to the technical field of textile dyeing and finishing.
Background
Nylon (also called nylon) fiber has the advantages of wear resistance, wearing ability, good wearing comfort and the like, and is widely used as various high-quality civil and military textile garments such as underwear, swimwear, sportswear, training wear and the like, and has been developed faster in recent years. The nylon fiber molecular structure contains unstable amide groups, amino groups and other characteristic groups, and the group structures have the problems of poor dyeing fastness, easy yellowing and the like while endowing the fiber with specific physical properties, so that higher requirements are provided for printing and dyeing processing aids and processes.
The dyeing principle of the nylon fiber is that under the acidic condition, the dyeing seat amino on the nylon fiber molecule is positively charged and has charge attraction to the anionic sulfonic group of the acid dye molecule, so that the dyeing is realized. However, the charge acting force is weak, dye molecules are easily desorbed from nylon fibers when the pH value is neutral or alkaline soaping, so that the color fastness of the nylon fibers is poor, and an acid color fixing agent is required to be used for color fixing treatment to improve the color fastness.
In addition, nylon fibers are easy to generate yellowing in the high-temperature heat treatment and storage process. When in high-temperature processing, amino and amido in a nylon molecular structure are easy to oxidize and yellow and even fragile by nitrogen oxides in air under the action of heat energy, so that nylon fabrics which need high-temperature hot-pressing processing and are used for making underwear mold cups need to be treated by a high-temperature yellowing resistant agent in advance so as to protect the nylon fiber structure from being damaged by high temperature. In the process of storage and transportation, when the nylon fiber is in direct contact with packaging materials such as polyethylene films containing antioxidant BHT, the BHT has small solubility in polyethylene, can be transferred to fabrics or clothing fabrics in the process of storage, and can undergo complex chemical reaction with oxides containing nitrogen to form yellow substances, so that the nylon textile undergoes storage yellowing. In order to effectively prevent the storage and transportation yellowing of textiles, a dye factory must use an anti-phenolic yellowing agent to perform anti-phenolic yellowing finishing on nylon textiles.
Compared with cotton and polyester fabrics, the dyeing and finishing process of nylon fabrics has the steps of fixation, phenol yellowing resistance, high-temperature yellowing resistance and the like, and has long processing procedures, large energy consumption, water consumption and pollution discharge besides the conventional pretreatment of degreasing, dyeing and washing. Therefore, the development of the composite functional auxiliary agent with color fixation, phenol yellowing resistance and high-temperature yellowing resistance simultaneously shortens the process flow and has important significance for energy conservation, consumption reduction and emission reduction in the nylon printing and dyeing processing link.
Disclosure of Invention
The invention aims to provide a composite functional auxiliary agent for nylon dyeing and a preparation method and application thereof, and the composite functional auxiliary agent has excellent color fixation, anti-phenolic yellowing and anti-high temperature yellowing performances, can integrate the conventional step-by-step dyeing and finishing processes of nylon fabric color fixation, anti-phenolic yellowing and anti-high temperature yellowing into one, improves the production efficiency, realizes energy conservation, consumption reduction and emission reduction of dyeing and finishing, and accords with the green development direction of double carbon.
The invention provides a composite functional auxiliary agent for chinlon dyeing, which comprises the following components in percentage by mass: 15-30% of aromatic sulfonic acid compound, 0-15% of phenolic compound, 1-6% of catalyst, 5-15% of formaldehyde aqueous solution, 2-6% of formaldehyde scavenger, 10-30% of amine compound and the balance of deionized water.
In the composite functional auxiliary agent for chinlon dyeing, the aromatic sulfonic acid compound can be one or more of phenol sulfonic acid, m-cresol sulfonic acid, beta-naphthalene sulfonic acid, 2-naphthol-8-sulfonic acid and 2-naphthol-6, 8-disulfonic acid;
the phenolic compound can be one or more of phenol, naphthol and bisphenol S;
the catalyst can be one or more of concentrated sulfuric acid, p-toluenesulfonic acid and xylenesulfonic acid with mass fraction more than 98%;
the formaldehyde scavenger can be one or more of urea, carbohydrazide and 2-imidazolidone;
the formaldehyde aqueous solution is 36-42% industrial formaldehyde;
the amine compound can be one or more of ammonia water, ethanolamine, diethanolamine, triethanolamine, diethylamine, triethylamine, dimethylethanolamine, diethylethanolamine, hydrazine hydrate, methyl hydrazine and unsymmetrical dimethylhydrazine.
The composite functional auxiliary agent for dyeing nylon provided by the invention is prepared by a method comprising the following steps:
1) Deionized water, aromatic sulfonic acid compounds, phenolic compounds and catalysts are sequentially added into a reaction device;
2) Stirring and heating;
3) After the temperature of the materials is increased to 80-98 ℃, the rotating speed is adjusted to 150-250 rpm;
4) Dropwise adding formaldehyde aqueous solution into the material;
5) After formaldehyde is added dropwise, reacting for 1-3 hours at constant temperature;
6) Heating to 98-120 deg.c and constant temperature reaction for 4-10 hr;
7) The temperature of the materials is reduced to 70-90 ℃;
8) Adding formaldehyde scavenger, and reacting at constant temperature for 1-3 hours;
9) The temperature of the materials is reduced to 30-50 ℃;
10 Adding amine compound, and reacting for 0.5-2 hours at constant temperature;
11 Stopping stirring, filtering and discharging to obtain the composite functional assistant for nylon dyeing.
In the step 2), the stirring rotating speed is controlled to be 40-80 rpm;
in the step 4), the dripping time is controlled to be 0.5-2 hours;
in step 10), the reaction temperature is controlled to be not more than 70 ℃.
The application of the composite functional auxiliary agent for nylon dyeing in the composite functional treatment of the textile containing the nylon component also belongs to the protection scope of the invention.
Specifically, the application is the application of the composite functional auxiliary agent for nylon dyeing in improving the color fastness, high-temperature yellowing resistance and storage yellowing resistance of the textile containing the nylon component.
Wherein, the textile containing nylon component can be nylon fabric, nylon spandex elastic fabric, etc.
The invention also provides a use method of the composite functional auxiliary agent for dyeing nylon, and the composite functional auxiliary agent for dyeing nylon can be applied to nylon and blended textiles thereof through an impregnation process.
The application method of the composite functional auxiliary agent for nylon dyeing comprises the steps of using 1-5% of the composite functional auxiliary agent (for fabric weight), 0.2-1g/L of acetic acid, and treating at 60-85 ℃ for 10-40min at a bath ratio of 1:10-20.
The composite functional auxiliary agent for dyeing nylon has the following beneficial effects:
1) The composite functional auxiliary agent for dyeing nylon has multiple composite functions of excellent fixation, high-temperature yellowing resistance, phenol yellowing resistance and the like, can effectively improve the color fastness of nylon fabrics such as washing, water immersion, perspiration and the like, simultaneously endows the fabrics with excellent yellowing resistance, and is beneficial to improving the quality and added value of the fabrics;
2) The composite functional auxiliary agent for chinlon dyeing can integrate the conventional 3 procedures of color fixation, phenol yellowing resistance and high temperature yellowing resistance into one, saves energy, water and emission while improving the production efficiency, and is beneficial to clean production of printing and dyeing technology;
the composite functional auxiliary agent for nylon dyeing is an environment-friendly product, and the treated textile meets the highest A-level standard requirement of national ecological textiles.
Detailed Description
The following detailed description of the invention is provided in connection with the accompanying drawings that are presented to illustrate the invention and not to limit the scope thereof. The examples provided below are intended as guidelines for further modifications by one of ordinary skill in the art and are not to be construed as limiting the invention in any way.
The experimental methods in the following examples, unless otherwise specified, are conventional methods, and are carried out according to techniques or conditions described in the literature in the field or according to the product specifications. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
22.3 parts of phenolsulfonic acid, 8.7 parts of bisphenol S, 1.5 parts of sulfuric acid (mass fraction 98%), 4.5 parts of p-toluenesulfonic acid and 20 parts of deionized water are added into a reaction device with a stirrer, a thermometer, an equilibrium feeder and a condenser, stirring is started, the rotating speed is controlled at 60 revolutions per minute, and heating is carried out to 80 ℃; regulating the stirring rotation speed to 200 revolutions per minute, dropwise adding 12.5 parts of formaldehyde aqueous solution (37% industrial formaldehyde), heating to 98 ℃ after dropwise adding is completed within 1.5 hours, and carrying out heat preservation reflux reaction for 10 hours; starting cooling water, cooling to 90 ℃, adding 6 parts of carbohydrazide, and continuing to perform heat preservation reaction for 2 hours; adding 12.2 parts of deionized water, and introducing cooling water again to cool the reaction materials; and cooling to 40 ℃, adding 6.5 parts of ethanolamine and 5.8 parts of diethyl ethanolamine, continuously carrying out heat preservation reaction for 1 hour, filtering, and discharging to obtain the composite functional auxiliary agent for dyeing nylon.
The composite functional auxiliary agent in the embodiment 1 comprises the following components in percentage by weight: 22.3% of aromatic sulfonic acid compound, 8.7% of phenolic compound, 6% of catalyst, 12.5% of formaldehyde aqueous solution, 6% of formaldehyde scavenger and 12.3% of amine compound.
Example 2
Adding 20 parts of phenolsulfonic acid, 6 parts of m-cresol sulfonic acid, 4.5 parts of phenol, 1.8 parts of sulfuric acid (98% by mass), 4 parts of xylenesulfonic acid and 24.4 parts of deionized water into a reaction device with a stirrer, a thermometer, a balance feeder and a condenser, starting stirring, controlling the rotating speed to be 80 revolutions per minute, and heating to 98 ℃; regulating the stirring rotation speed to 200 revolutions per minute, dropwise adding 5.5 parts of formaldehyde aqueous solution (37% industrial formaldehyde), and carrying out heat preservation reaction for 1.5 hours after dropwise adding is completed within 0.5 hour; heating to 110 ℃, and carrying out heat preservation and reflux reaction for 6 hours; starting cooling water, cooling to 80 ℃, adding 4 parts of carbohydrazide, and continuing to perform heat preservation reaction for 1 hour; and cooling the reaction materials by introducing cooling water again, adding 29.8 parts of triethanolamine after cooling to 55 ℃, continuously preserving heat and reacting for 0.5 hour, filtering, and discharging to obtain the composite functional auxiliary agent for dyeing nylon.
The composite functional auxiliary agent in the embodiment 2 comprises the following components in percentage by weight: 26% of aromatic sulfonic acid compound, 4.5% of phenolic compound, 5.8% of catalyst, 5.5% of formaldehyde aqueous solution, 4% of formaldehyde scavenger and 29.8% of amine compound.
Example 3
26.2 parts of beta-naphthalene sulfonic acid, 11 parts of bisphenol S, 2 parts of sulfuric acid (98% by mass fraction) and 26 parts of deionized water are added into a reaction device with a stirrer, a thermometer, an equilibrium feeder and a condenser, stirring is started, the rotating speed is controlled at 40 revolutions per minute, and heating is carried out to 90 ℃; regulating the stirring rotation speed to 150 rpm, dropwise adding 9.8 parts of formaldehyde aqueous solution (37% industrial formaldehyde), and after dropwise adding is completed within 1.5 hours, carrying out heat preservation reaction for 2 hours; heating to 120 ℃, and carrying out heat preservation and reflux reaction for 4 hours; starting cooling water, cooling to 70 ℃, adding 2 parts of urea, 2 parts of carbohydrazide and 2 parts of 2-imidazolidone, and continuing to perform heat preservation reaction for 2 hours; and cooling the reaction materials by introducing cooling water again, sequentially adding 5 parts of diethylamine, 7 parts of diethanolamine and 7 parts of dimethylethanolamine after cooling to 40 ℃, continuing to perform heat preservation reaction for 2 hours, filtering, and discharging to obtain the composite functional assistant for dyeing the nylon.
The composite functional auxiliary agent of the embodiment 3 comprises the following components in percentage by weight: 26.2% of aromatic sulfonic acid compound, 11% of phenolic compound, 2% of catalyst, 9.8% of formaldehyde solution, 6% of formaldehyde scavenger and 19% of amine compound.
Example 4
19.3 parts of phenolsulfonic acid, 10.7 parts of 2-naphthol-6, 8-disulfonic acid, 1 part of sulfuric acid (mass fraction 98%), 3 parts of p-toluenesulfonic acid and 23.8 parts of deionized water are added into a reaction device with a stirrer, a thermometer, an equilibrium feeder and a condenser, stirring is started, the rotating speed is controlled to be 80 revolutions per minute, and heating is carried out to 85 ℃; regulating the stirring rotation speed to 180 revolutions per minute, dropwise adding 12.2 parts of formaldehyde aqueous solution (37% industrial formaldehyde), and after dropwise adding is completed within 1.5 hours, carrying out heat preservation reaction for 1.5 hours; heating to 115 ℃, and carrying out heat preservation and reflux reaction for 5 hours; starting cooling water, cooling to 85 ℃, adding 2 parts of carbohydrazide and 2 parts of 2-imidazolidone, and continuing to perform heat preservation reaction for 2 hours; and cooling the reaction materials by introducing cooling water again, sequentially adding 3.5 parts of ammonia water, 5.5 parts of unsymmetrical dimethylhydrazine and 17 parts of dimethylethanolamine after cooling to 30 ℃, continuously carrying out heat preservation reaction for 2 hours, filtering, and discharging to obtain the composite functional auxiliary agent for dyeing the nylon.
The composite functional auxiliary agent in the embodiment 4 comprises the following components in percentage by weight: 30% of aromatic sulfonic acid compound, 0% of phenolic compound, 4% of catalyst, 12.2% of formaldehyde solution, 4% of formaldehyde scavenger and 26% of amine compound.
Example 5
Adding 15 parts of phenolsulfonic acid, 15 parts of naphthol, 1 part of sulfuric acid (98% by mass), 4 parts of xylenesulfonic acid and 18.3 parts of deionized water into a reaction device with a stirrer, a thermometer, an equilibrium feeder and a condenser, starting stirring, controlling the rotating speed to be 60 revolutions per minute, and heating to 92 ℃; regulating the stirring rotation speed to 210 revolutions per minute, dropwise adding 8.7 parts of formaldehyde aqueous solution (37% industrial formaldehyde), and after dropwise adding is completed within 1 hour, carrying out heat preservation reaction for 2 hours; heating to 105 ℃, and carrying out heat preservation and reflux reaction for 6 hours; starting cooling water, cooling to 75 ℃, adding 3 parts of carbohydrazide, and continuing to perform heat preservation reaction for 2 hours; adding 12 parts of deionized water, introducing cooling water again to cool the reaction materials, sequentially adding 3.5 parts of triethanolamine, 4.5 parts of methyl hydrazine and 15 parts of diethyl ethanolamine after cooling to 45 ℃, continuing to perform heat preservation reaction for 2 hours, filtering, and discharging to obtain the composite functional auxiliary agent for dyeing the nylon.
The composite functional auxiliary agent in the embodiment 5 comprises the following components in percentage by weight: 15% of aromatic sulfonic acid compound, 15% of phenolic compound, 5% of catalyst, 8.7% of formaldehyde solution, 3% of formaldehyde scavenger and 23% of amine compound.
Example 6
Adding 8 parts of phenolsulfonic acid, 12 parts of 2-naphthol-8-sulfonic acid, 5 parts of naphthol, 7 parts of bisphenol S, 2 parts of sulfuric acid, 4 parts of xylene sulfonic acid and 23.5 parts of deionized water into a reaction device with a stirrer, a thermometer, a balance feeder and a condenser, starting stirring, controlling the rotating speed to be 60 revolutions per minute, and heating to 95 ℃; regulating the stirring rotation speed to 230 rpm, dropwise adding 13.5 parts of formaldehyde aqueous solution (37% industrial formaldehyde), and after dropwise adding is completed within 2 hours, carrying out heat preservation reaction for 3 hours; heating to 102 ℃, and carrying out heat preservation and reflux reaction for 7 hours; starting cooling water, cooling to 85 ℃, adding 2 parts of urea and 2 parts of carbohydrazide, and continuing to perform heat preservation reaction for 3 hours; adding 6 parts of deionized water, introducing cooling water again to cool the reaction materials, sequentially adding 3.5 parts of hydrazine hydrate, 8 parts of triethylamine and 3.5 parts of ethanolamine after cooling to 50 ℃, continuing to perform heat preservation reaction for 2 hours, filtering, and discharging to obtain the composite functional auxiliary agent for dyeing the nylon.
The composite functional auxiliary agent of the embodiment 6 comprises the following components in percentage by weight: 20% of aromatic sulfonic acid compound, 12% of phenolic compound, 6% of catalyst, 13.5% of formaldehyde solution, 4% of formaldehyde scavenger and 15% of amine compound.
The composite functional auxiliary agent of the embodiment is applied to dyeing and finishing treatment of the nylon spandex fabric, and the untreated fabric is taken as a reference sample to be compared and tested for color fastness, phenol yellowing and high-temperature yellowing of the treated fabric, and the specific experimental method and test result are as follows:
1. treatment process
1) A fabric: a rose-red nylon spandex fabric;
2) Treatment conditions: the dosage of the composite functional auxiliary agent is 3%, the dosage of acetic acid is 0.5g/L, the bath ratio is 1:20, the treatment temperature is 70 ℃, the treatment time is 30min, and the dehydration and drying are carried out.
2. Test method
1. The fastness of the fabrics was tested with reference to the international standard ISO 105-E04:2003 textile colour fastness test part E04 perspiration fastness.
2. The phenolic yellowing of the fabrics was tested with reference to the international standard ISO 105-X18:2007 test for the fastness to phenolic yellowing of textiles.
3. The fabric was tested for high temperature yellowing using the following method: and (3) performing heat setting treatment (setting process: 190 ℃ C. X200 sec) on the fabric to be tested on a setting machine, and then performing color change grading by using GB/T250-2008 grey sample card for evaluating color change of textile color fastness test.
4. Formaldehyde content was tested with reference to GB/T2912.1-2009 "determination of textile formaldehyde part 1 free and hydrolyzed formaldehyde (water extraction method)".
3. Test results
The performance test results of the embodiment of the invention are as follows:
| project | Color fastness/grade | Phenol yellowing/grade | High temperature yellowing/grade | Formaldehyde content/ppm |
| Example 1 | 4 | 4 | 4 | Not detected |
| Example 2 | 3-4 | 4-5 | 4 | Not detected |
| Example 3 | 3-4 | 4-5 | 3-4 | Not detected |
| Example 4 | 4 | 4-5 | 3-4 | Not detected |
| Example 5 | 3-4 | 4 | 4 | Not detected |
| Example 6 | 4 | 4 | 4 | Not detected |
| Blank sample | 1-2 | 2 | 2-3 | Not detected |
As shown in the table, compared with untreated fabric, the nylon spandex fabric treated by the composite functional auxiliary agent is remarkably improved in color fastness, phenol yellowing resistance and high-temperature yellowing resistance, and the composite functional auxiliary agent has the composite functions of improving the color fastness of the nylon fabric, improving phenol yellowing, high-temperature yellowing and the like, and is beneficial to shortening printing and dyeing procedures, improving production efficiency, saving energy and reducing emission.
The present invention is described in detail above. It will be apparent to those skilled in the art that the present invention can be practiced in a wide range of equivalent parameters, concentrations, and conditions without departing from the spirit and scope of the invention and without undue experimentation. While the invention has been described with respect to specific embodiments, it will be appreciated that the invention may be further modified. In general, this application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains.
Claims (4)
1. The composite functional auxiliary agent for dyeing nylon comprises the following components in percentage by mass: 15-30% of aromatic sulfonic acid compound, 4.5-15% of phenolic compound, 1-6% of catalyst, 5-15% of formaldehyde aqueous solution, 2-6% of formaldehyde scavenger, 10-30% of amine compound and the balance of deionized water;
the catalyst is one or more of concentrated sulfuric acid, p-toluenesulfonic acid and xylenesulfonic acid with mass fraction more than 98%;
the method for preparing the composite functional auxiliary agent for nylon dyeing comprises the following steps:
1) Deionized water, aromatic sulfonic acid compounds, phenolic compounds and catalysts are sequentially added into a reaction device;
2) Stirring and heating;
3) After the temperature of the materials is increased to 80-98 ℃, the rotating speed is adjusted to 150-250 rpm;
4) Dropwise adding formaldehyde aqueous solution into the material;
5) After formaldehyde is added dropwise, reacting for 1-3 hours at constant temperature;
6) Heating to 98-120 deg.c and constant temperature reaction for 4-10 hr;
7) The temperature of the materials is reduced to 70-90 ℃;
8) Adding formaldehyde scavenger, and reacting at constant temperature for 1-3 hours;
9) The temperature of the materials is reduced to 30-50 ℃;
10 Adding amine compound, and reacting for 0.5-2 hours at constant temperature;
11 Stopping stirring, filtering and discharging to obtain the composite functional auxiliary agent for dyeing nylon;
the aromatic sulfonic acid compound is one or more of phenol sulfonic acid, m-cresol sulfonic acid, beta-naphthalene sulfonic acid, 2-naphthol-8-sulfonic acid and 2-naphthol-6, 8-disulfonic acid;
the phenolic compound is one or more of phenol, naphthol and bisphenol S;
the formaldehyde scavenger is one or more of urea, carbohydrazide and 2-imidazolidone;
the formaldehyde aqueous solution is 37% industrial formaldehyde;
the amine compound is one or more of ammonia water, ethanolamine, diethanolamine, triethanolamine, diethylamine, triethylamine, dimethylethanolamine, diethylethanolamine, hydrazine hydrate, methyl hydrazine and unsymmetrical dimethylhydrazine.
2. The complex functional auxiliary according to claim 1, wherein: in the step 2), the rotation speed of stirring is controlled to be 40-80 revolutions per minute;
in the step 4), the dripping time is controlled to be 0.5-2 hours;
in step 10), the reaction temperature is controlled to be not more than 70 ℃.
3. Use of the composite functional auxiliary agent for nylon dyeing according to claim 1 or 2 in the composite functional treatment of a textile containing a nylon component;
the application is the application of the composite functional auxiliary agent for nylon dyeing in improving the color fastness, high-temperature yellowing resistance and storage yellowing resistance of the textile containing the nylon component.
4. The method for using the composite functional assistant for nylon dyeing according to claim 1 or 2, which is to apply the composite functional assistant for nylon dyeing to nylon and blended textiles thereof through an impregnation process, wherein the impregnation process comprises the steps of using 1-5% of the composite functional assistant, 0.2-1g/L of acetic acid, and a bath ratio of 1:10-20, a treatment temperature of 60-85 ℃ and a treatment time of 10-40min.
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| CN108442150A (en) * | 2018-04-23 | 2018-08-24 | 东莞市中纺化工有限公司 | A kind of environment-friendly type syntannin color fixing agent and the preparation method and application thereof |
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| US5310855A (en) * | 1990-09-07 | 1994-05-10 | Bayer Aktiengesellschaft | Aromatic condensation products |
| CN102850500A (en) * | 2012-08-24 | 2013-01-02 | 浙江传化股份有限公司 | Acid reaction resistant chinlon fixer and application thereof |
| CN105220544A (en) * | 2015-10-20 | 2016-01-06 | 湖州博仁纺织品有限公司 | A kind of Novel acidic dye color-fixing agent and its preparation method and application method |
| CN108004768A (en) * | 2017-11-14 | 2018-05-08 | 广州先盈生物科技有限公司 | One kind is used for anti-storage xanthochromia agent of nylon and preparation method thereof |
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