CN111118654B - Preparation method of spandex easy to dye - Google Patents
Preparation method of spandex easy to dye Download PDFInfo
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- CN111118654B CN111118654B CN201911377224.3A CN201911377224A CN111118654B CN 111118654 B CN111118654 B CN 111118654B CN 201911377224 A CN201911377224 A CN 201911377224A CN 111118654 B CN111118654 B CN 111118654B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of spandex easy to dye, belonging to the field of spandex materials and comprising the following steps of: (1) mixing and reacting raw materials of polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate to obtain a prepolymer; (2) fully dissolving the prepolymer by adopting N, N-dimethylacetamide as a solvent to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing a diamine chain extender and a monoamine terminator to perform chain extension and chain termination to obtain a polymer solution; (3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and simultaneously quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution; (4) and (4) preparing the spandex spinning solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method. The preparation method of the easy-dyeing spandex improves the dye uptake and the color fixing rate, and has good dyeing performance.
Description
Technical Field
The invention relates to the field of spandex, in particular to a preparation method of spandex easy to dye.
Background
Spandex is a short for polyurethane fiber and is an elastic fiber. Spandex is a polyurethane elastic fiber called as 'fabric monosodium glutamate', and has a 'non-ammonia non-cloth forming' statement in the industry, so that the spandex is one of key factors for improving the fabric quality. However, in the dyeing process of the spandex fiber, the spandex fiber is difficult to color, which is mainly caused by a high polymer structure of the spandex fiber, wherein the high polymer structure of the spandex fiber consists of a hard segment and a soft segment, the hard segment has strong polarity, but the dye is difficult to enter, and the soft segment has weak polarity, but the action on dye molecules is poor, so that the spandex fiber is difficult to color and has low color fastness. With the continuous improvement of the national living standard, the aesthetic concept of consumers is continuously improved, the color requirement on clothes is higher and higher, and the development of the spandex fiber easy to dye is increasingly important.
Disclosure of Invention
The invention aims to provide a preparation method of easy-dyeing spandex, which improves the dye uptake and the fixation rate and has good dyeing performance.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of spandex easy to dye comprises the following steps:
(1) mixing polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate serving as raw materials, reacting at 82-88 ℃ for 110-115 min, and cooling to obtain a prepolymer;
(2) putting the prepolymer into a high-speed dissolving machine, adopting N, N-dimethylacetamide as a solvent, fully dissolving the prepolymer to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing diamine chain extenders and monoamine terminators at low temperature to perform chain extension and chain termination to obtain a polymer solution;
(3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution;
(4) and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method.
Preferably, in the step (1), the molar ratio of 4, 4-diphenylmethane diisocyanate to polytetramethylene ether glycol is (1.60-1.92): 1.
preferably, in the step (2), the mass percentage concentration of the polymer solution is 34-40%.
Preferably, in the step (2), the diamine chain extender comprises, by weight, 1 to 4 parts of ethylenediamine, 0.5 to 3.4 parts of butanediamine, and 89 to 93 parts of N, N-dimethylacetamide.
Preferably, in step (2), the mono-amine terminator is diethylamine.
Preferably, in the step (3), the adjuvant mixed solution comprises the following raw materials in parts by weight: 0.3-1 part of anti-ultraviolet agent, 1-3 parts of antioxidant, 0.1-0.8 part of lubricant, 0.4-1.4 parts of delustering agent, 3-5 parts of dyeing assistant and 18-20 parts of N, N-dimethylacetamide.
Preferably, the dyeing assistant comprises, by weight, 18-20 parts of cetylpyridinium chloride, 0.03-0.1 part of tartaric acid and 3-7 parts of sodium dibutylnaphthalenesulfonate.
Preferably, the preparation method of the auxiliary material mixed solution comprises the following steps of grinding the anti-ultraviolet agent, the antioxidant, the lubricant, the delustering agent and the dyeing assistant for 16-20 hours by a grinding machine, adding N, N-dimethylacetamide, and uniformly mixing and stirring to obtain the auxiliary material mixed solution.
Compared with the prior art, the invention has the beneficial effects that:
compared with the conventional fiber, the spandex fiber prepared by the invention has more excellent dyeing property. Secondly, the dyeing auxiliary is added, the dyeing auxiliary has good compatibility with a spandex spinning solution, the dye uptake and the color fixation rate of spandex are greatly improved, tartar is added into cetylpyridinium chloride and sodium dibutylnaphthalenesulfonate, the dyeing auxiliary is effectively dispersed in the fiber and on the surface of the fiber, and the easy dyeing characteristic of the spandex fiber is greatly improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of spandex easy to dye comprises the following steps:
(1) 5000g of polytetramethylene ether glycol (with the molecular weight of 1800) and 1160g of 4, 4-diphenylmethane diisocyanate are mixed, reacted for 112min at 82 ℃, and then cooled to obtain a prepolymer;
(2) putting the prepolymer into a high-speed dissolving machine, adopting 16000g N, N-dimethylacetamide as a solvent, fully dissolving the prepolymer to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing a diamine chain extender and a monoamine terminator at low temperature for chain extension and chain termination, wherein the diamine chain extender comprises 96g of ethylenediamine, 21g of butanediamine, 1855g of N, N-dimethylacetamide and 12.9g of monoamine terminator diethylamine in parts by weight, and reacting to obtain a polymer solution;
(3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and simultaneously quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution, wherein the auxiliary material mixed solution comprises the following raw materials in parts by weight: 0.108g of anti-ultraviolet agent, 0.36g of antioxidant, 0.036g of lubricant, 0.144g of matting agent, 1.08g of dyeing assistant and 141g of N, N-dimethylacetamide, wherein the dyeing assistant comprises the following components in parts by weight, namely, 6.48g of cetylpyridinium chloride, 0.01g of trueturgital, and 1.08g of sodium dibutylnaphthalenesulfonate, and the preparation method of the auxiliary material mixed solution comprises the following steps of grinding the anti-ultraviolet agent, the antioxidant, the lubricant, the matting agent and the dyeing assistant by a grinder for 16 hours, adding the N, N-dimethylacetamide, mixing and stirring uniformly to obtain an auxiliary material mixed solution;
(4) and (4) preparing the spandex spinning solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method.
Example 2
A preparation method of spandex easy to dye comprises the following steps:
(1) 4950g of polytetramethylene ether glycol (molecular weight is 1800) and 1143g of 4, 4-diphenylmethane diisocyanate are mixed, reacted for 110min at 82 ℃, and then cooled to obtain a prepolymer;
(2) putting the prepolymer into a high-speed dissolving machine, adopting 15900g N, N-dimethylacetamide as a solvent, fully dissolving the prepolymer to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing a diamine chain extender and a monoamine terminator at low temperature for chain extension and chain termination, wherein the diamine chain extender comprises the following components in parts by weight, 94g of ethylenediamine, 20g of butanediamine, 1850g of N, N-dimethylacetamide and 13.0g of monoamine terminator diethylamine, and reacting to obtain a polymer solution;
(3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and simultaneously quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution, wherein the auxiliary material mixed solution comprises the following raw materials in parts by weight: the auxiliary material mixed solution is prepared by the following steps of grinding the anti-ultraviolet agent, the antioxidant, the lubricant, the matting agent and the dyeing assistant for 18 hours by a grinder, adding N, N-dimethylacetamide, mixing and stirring uniformly to obtain an auxiliary material mixed solution;
(4) and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method.
Example 3
A preparation method of easy-dyeing spandex comprises the following steps:
(1) mixing 5100g of polytetramethylene ether glycol (molecular weight is 1800) and 1175g of 4, 4-diphenylmethane diisocyanate, reacting at 88 ℃ for 115min, and cooling to obtain a prepolymer;
(2) putting the prepolymer into a high-speed dissolving machine, adopting 16610g of N, N-dimethylacetamide as a solvent, fully dissolving the prepolymer to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing a diamine chain extender and a monoamine terminator at low temperature for chain extension and chain termination, wherein the diamine chain extender comprises the following components in parts by weight, namely 98g of ethylenediamine, 22.5g of butanediamine, 1930g of N, N-dimethylacetamide and 13.1g of monoamine terminator diethylamine, and reacting to obtain a polymer solution;
(3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and simultaneously quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution, wherein the auxiliary material mixed solution comprises the following raw materials in parts by weight: 0.158g of anti-ultraviolet agent, 0.41g of antioxidant, 0.088g of lubricant, 0.185g of matting agent, 2.15g of dyeing assistant and 176g of N, N-dimethylacetamide, wherein the dyeing assistant comprises 7.2g of cetylpyridinium chloride, 0.036g of truettarite and 2.52g of sodium dibutylnaphthalene sulfonate in parts by weight, and the auxiliary material mixed solution is prepared by grinding the anti-ultraviolet agent, the antioxidant, the lubricant, the matting agent and the dyeing assistant by a grinder for 20 hours, adding the N, N-dimethylacetamide, mixing and stirring uniformly to obtain an auxiliary material mixed solution;
(4) and (4) preparing the spandex spinning stock solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method.
Comparative examples 1 to 2
Comparative example 1 differs from example 2 in that: the dyeing assistant in comparative example 1 was composed of, by weight, 6.86g of cetylpyridinium chloride, 1.8g of sodium dibutylnaphthalenesulfonate, and no tartrate.
Comparative example 2 differs from example 2 in that: the dyeing assistant in comparative example 1 was composed of the following components in parts by weight, cetylpyridinium chloride 8.64g, and tartaric acid 0.025g, and did not contain sodium dibutylnaphthalenesulfonate.
Comparative example 3 is a conventional spandex filament.
The fixation rate represents the ratio of the amount of dye combined on the fiber to the total amount of dye used, the dye uptake represents the ratio of the amount of dye dyed on the fiber to the total amount of dye in the initial dye bath, and the fixation rate and the dye uptake are important parameters of the reactive dyeability; the bare spandex yarns prepared in the embodiments 1 to 3 and the comparative example of the invention are subjected to boiling dyeing by using an acid dye, and the conventional fixation rate detection method and dye-uptake rate detection method are respectively used for detection, so that the following results can be found: the spandex produced by the embodiment of the invention has the dye uptake and the color fixing rate with the conventional spandex silk. Specific test data comparisons are shown in table 1:
TABLE 1 test data Table for examples 1 to 3 of the present invention and comparative examples
| Dye uptake (%) | Fixation ratio (%) | |
| Example 1 | 98.78 | 74.35 |
| Example 2 | 99.51 | 76.78 |
| Example 3 | 99.23 | 73.26 |
| Comparative example 1 | 93.24 | 53.09 |
| Comparative example 2 | 92.73 | 58.23 |
| Comparative example 3 | 84.31 | 25.74 |
As can be seen from Table 1, the spandex material prepared by the method has high dye uptake and color fixing rate and good dyeing performance. Secondly, the tartaric acid is added into the dyeing assistant, so that the dye uptake and the fixation rate are greatly improved.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (6)
1. The preparation method of the spandex easy to dye is characterized by comprising the following steps of:
(1) mixing polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate which are used as raw materials, reacting for 110-115 min at 82-88 ℃, and then cooling to obtain a prepolymer;
(2) putting the prepolymer into a high-speed dissolving machine, fully dissolving the prepolymer by using N, N-dimethylacetamide as a solvent to obtain a prepolymer solution, transferring the prepolymer solution into a polymerization reactor, uniformly stirring, and controlling and adding a mixed amine DMAC solution containing a diamine chain extender and a monoamine terminator at low temperature to perform chain extension and chain termination to obtain a polymer solution;
(3) continuously transferring a polymer solution continuously generated in a polymerization reactor into a stirring tank, and quantitatively adding a prepared auxiliary material mixed solution into the stirring tank to obtain a spandex spinning stock solution; the auxiliary material mixed solution comprises the following raw materials in parts by weight: 0.3-1 part of an anti-ultraviolet agent, 1-3 parts of an antioxidant, 0.1-0.8 part of a lubricant, 0.4-1.4 parts of a delustering agent, 3-5 parts of a dyeing assistant and 18-20 parts of N, N-dimethylacetamide; the dyeing assistant comprises, by weight, 18-20 parts of cetylpyridinium chloride, 0.03-0.1 part of tartaric acid and 3-7 parts of sodium dibutylnaphthalenesulfonate;
(4) and (4) preparing the spandex spinning solution prepared in the step (3) into spandex fibers easy to dye by adopting a solution spinning method.
2. The process of claim 1 for preparing an dyeable spandex, comprising: in the step (1), the molar ratio of 4, 4-diphenylmethane diisocyanate to polytetramethylene ether glycol is (1.60-1.92): 1.
3. the process of claim 1 for preparing an dyeable spandex, comprising: in the step (2), the mass percentage concentration of the polymer solution is 34-40%.
4. The process of claim 1 for preparing an dyeable spandex, comprising: in the step (2), in the mixed amine DMAC solution of the diamine chain extender and the monoamine terminator, 1-4 parts of ethylenediamine, 0.5-3.4 parts of butanediamine and 89-93 parts of N, N-dimethylacetamide are used as the diamine chain extender.
5. The process of claim 1 for preparing an dyeable spandex, comprising: in the step (2), the monoamine terminator is diethylamine.
6. The process of claim 1 for preparing an dyeable spandex, comprising: the preparation method of the auxiliary material mixed solution comprises the following steps of grinding the anti-ultraviolet agent, the antioxidant, the lubricant, the delustering agent and the dyeing assistant for 16-20 hours by a grinding machine, adding N, N-dimethylacetamide, and mixing and stirring uniformly to obtain the auxiliary material mixed solution.
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| CN112127006A (en) * | 2020-08-25 | 2020-12-25 | 烟台泰和新材料股份有限公司 | Easy-to-dye spandex fiber and preparation method thereof |
| CN114164519B (en) * | 2021-12-21 | 2024-09-20 | 泰和新材集团股份有限公司 | Hollow spandex and preparation method thereof |
| CN116732637A (en) * | 2023-08-14 | 2023-09-12 | 烟台舜康生物科技有限公司 | Preparation method of high-elasticity spandex |
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