CN116288794A - Acidic easy-dyeing spandex and preparation method thereof - Google Patents
Acidic easy-dyeing spandex and preparation method thereof Download PDFInfo
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- 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
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- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
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- 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
- D06P1/39—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 acid dyes
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- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/24—Polyamides; Polyurethanes
- D06P3/241—Polyamides; Polyurethanes using acid dyes
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Abstract
The invention provides an acidic easy-dyeing spandex and a preparation method thereof, wherein polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate react to obtain prepolymer, then N, N-dimethylacetamide is added for dilution, then ethylenediamine, propylenediamine, diethylamine and urea are selected to prepare mixed amine which is used as a chain extender and terminator solution, the chain extension reaction and the termination reaction are carried out under the condition of 30-50 ℃, then auxiliary materials such as titanium dioxide, zinc oxide, anti-yellowing agent and antioxidant are mixed and added into DMAC, after stirring is carried out uniformly, the mixed solution is added into a raw solution after chain extension, the mixed solution is stirred at the constant temperature of 40-50 ℃ for 1-2 hours and is cured for 10-40 hours, and the raw solution is spun after curing to obtain the acidic easy-dyeing spandex.
Description
Technical Field
The invention relates to a preparation method of spandex, which mainly utilizes urea as a terminator to improve the acid dyeability of spandex fiber, in particular to a preparation method of acid dyeable spandex.
Background
Spandex is an elastic fiber, which is the longest extension degree in synthetic fibers, and because of the excellent elasticity and recovery rate, good comfort can be obtained by adding a small amount of spandex into the textile fabric.
However, due to the self structural characteristics, only the disperse dye and the acid dye have certain affinity to the spandex fiber, and an active point which is chemically combined with the dye does not exist in the soft segment structure of the spandex, so that elasticity is only provided for the spandex; the hard segment part is mainly a carbamate bond generated by MDI and hydroxyl and a ureido formed by the MDI and amine, is positioned in a crystallization area in a microphase separation structure of spandex fiber, and dye micromolecules are difficult to enter the inside to dye.
Patent document CN107446099a discloses a high pressure resistant polyurethane material and a preparation method, in which in the prepolymer reaction in step 1, materials such as isocyanate and the like are added into a reaction kettle together to react, but the processes such as prepolymerization reaction, chain extension reaction, termination reaction and the like are mixed together to perform the reaction, so that the uniformity of the prepared spandex is poor.
Patent document CN103556459a discloses a composite thermal yellowing resistant finishing agent for chinlon, spandex and blended fabrics thereof, urea is added as a stabilizer into the prepared spandex fabrics. In the scheme disclosed in the patent document, urea is added into spandex in a physical addition mode, urea does not participate in reaction, and is gradually dissolved in water through water washing in the post-processing process of the elastic fabric, so that on one hand, the number of dyeing active points of acid dye is reduced, and on the other hand, undissolved urea is also dissolved in the soaping liquid to form a floating color after being combined with the acid dye through high-temperature soaping, so that the dyeing rate of the acid dye is not improved essentially. The advantages of urea are not fully exploited.
In order to solve the problems existing in the dyeing of spandex in the prior art, a new preparation method of the acidic easy-dyeing spandex is necessary to be provided.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and introduces more amino (/ -NH) into the molecular structure end group of the spandex fiber through the adjustment of a polymerization formula 2 The method for preparing the acid dyeable spandex comprises the following steps of:
step 1: mixing polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate together according to the mol ratio of 1:1.3-2.0 for a prepolymerization reaction to obtain a prepolymer, cooling to 30-50 ℃ after the prepolymerization reaction, adding an N, N-dimethylacetamide solvent for stirring, and fully dissolving the prepolymer;
step 2: adding a mixed amine solution of a chain extension terminator dissolved with urea into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
in this step, the reaction equation for urea as a terminator is:
2(NH 2 -CO-NH 2 )+O＝C＝N-R-N＝C＝O→
NH 2 -CO-NH-CO-NH-R-NH-CO-NH-CO-NH 2
in the step, urea is additionally used as a reactive chain extension terminating substance in the original polymerization process, so that more amino groups can be exposed in the polyurethane molecular end groups, active points are provided for dyeing of acid dyes, the dyeing performance of polyurethane fibers is further improved, urea is used as a reactive substance of a terminator in the chain extension process, and the self structure of polyurethane molecular chains is not influenced;
step 3: adding an auxiliary material additive into the product obtained in the step 2, uniformly stirring, adding the mixture into the chain-extended stock solution, stirring at the constant temperature of 40-50 ℃ for 1-2h, fully mixing, and curing for 10-40h;
step 4: and (3) curing the spandex spinning stock solution obtained in the step (3), spinning to obtain spandex, and testing the physical properties and dyeing properties of the spandex.
The prepolymerization reaction temperature in the step 1 is 70-90 ℃ and the reaction time is 60-120 min.
The chain terminator in the step 2 is a mixed amine solution prepared by mixing ethylenediamine, propylenediamine, diethylamine and urea and then adding the mixture into N, N-dimethylacetamide.
In the mixed amine solution, the mass part ratio of ethylenediamine, propylenediamine, diethylamine, urea and N, N-dimethylacetamide is 0-0.06: 0 to 0.07:0.001 to 0.013:0.003 to 0.012:1.
the temperature of the chain extension reaction in the step 2 is 30-50 DEG C
The mass fraction ratio of the prepolymer to the urea is 500-2000: 1.
the auxiliary material additive in the step 3 is obtained by mixing titanium dioxide, zinc oxide, an anti-yellowing agent and an antioxidant and then adding the mixture into N, N-dimethylacetamide.
In the invention, the auxiliary material additive is a functional auxiliary agent, and the addition amount of the auxiliary material additive has no special requirement, so long as the comprehensive performance and spinning performance of the spandex spinning solution are not degraded.
Preferably, the mass ratio of the titanium dioxide, the zinc oxide, the anti-yellowing agent, the antioxidant and the N, N-dimethylacetamide is 0.04:0.2:0.03:0.3:1.
the mass ratio of the auxiliary material additive to the product obtained in the step 2 is 0.03-0.05: 1.
the invention also provides an acidic easy-dyeing spandex, which comprises polyurethane fiber taking urea as a terminator, wherein the end group of the polyurethane fiber is-NH-CO-NH 2 The chemical formula is
R represents an inverse prepolymer structure having isocyanate groups.
The invention has the beneficial effects that:
1. in the invention, urea is additionally used as a reactive chain extension terminating substance in the original polymerization process, so that more amino groups can be exposed in the polyurethane molecular end groups, active points are provided for dyeing of acid dye, and the dyeing performance of polyurethane fiber is further improved.
2. Urea is used as a reaction substance of a terminator in the chain extension process, so that the self structure of a polyurethane molecular chain is not influenced.
3. The number of the amine with the end group is relatively large, and the ureido at the end of the molecule is easy to form hydrogen bond crosslinking, so that the heat resistance of the spandex yarn can be improved.
4. The product does not need to add an extra dyeing auxiliary agent in DOPE stock solution.
5. Due to the gradual introduction of amine with end groups of polyurethane molecular chain, -NH 3 The polyurethane fiber is tightly combined with acid dye, and the dyeing depth and various washing fastness of the dyed polyurethane fiber are improved.
Drawings
FIG. 1 is a schematic illustration of the reaction process of urea as a terminator in step 2 of the present application.
Detailed Description
Example 1
The preparation method of the acid easy-to-dye spandex comprises the following specific steps:
step 1: 100kg of polytetramethylene ether glycol (molecular weight 1800) and 18kg of 4, 4-diphenylmethane diisocyanate were reacted in a molar ratio of 1:1.3, mixing the materials together in proportion, carrying out a prepolymerization reaction to obtain a prepolymer, cooling to 30 ℃ after the prepolymerization reaction, adding 180kg of N, N-dimethylacetamide solvent, stirring, and fully dissolving the prepolymer;
step 2: mixing 0.8kg of ethylenediamine, 0.34kg of propylenediamine, 0.11kg of diethylamine and 0.06kg of urea, adding the mixture into 17kg of mixed amine solution prepared in N, N-dimethylacetamide, and adding the mixed amine solution into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: and (2) adding an auxiliary material additive formed by mixing 0.6kg of titanium dioxide, 3kg of zinc oxide, 0.4kg of anti-yellowing agent and 1kg of antioxidant into 10kg of N, N-dimethylacetamide, uniformly stirring, adding the auxiliary material additive into the chain-extended stock solution, stirring at a constant temperature of 40 ℃ for 1h, fully mixing, and curing for 20h.
Step 4: and (3) curing the spandex spinning solution obtained in the step (3) and then spinning to obtain the acidic easy-dyeing spandex.
The spandex bare yarn prepared by the steps is dyed by acid dye, and the dyeing rate is detected to be 32%, the fixation rate is detected to be 30%, the K/S is detected to be 0.5, and the soaping fastness is detected to be 4 grades.
Details are shown in Table 1.
Example two
The preparation method of the acid easy-to-dye spandex comprises the following specific steps:
step 1: 100kg of polytetramethylene ether glycol (molecular weight 1800) and 20kg of 4, 4-diphenylmethane diisocyanate were reacted in a molar ratio of 1:1.5, mixing the materials together in proportion, carrying out a prepolymerization reaction to obtain a prepolymer, cooling to 30 ℃ after the prepolymerization reaction, adding 180kg of N, N-dimethylacetamide solvent, stirring, and fully dissolving the prepolymer;
step 2: mixing 0.49kg of ethylenediamine, 1.22kg of propylenediamine, 0.2kg of diethylamine and 0.13kg of urea, adding the mixture into 24kg of mixed amine solution prepared from N, N-dimethylacetamide, and adding the mixed amine solution into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: and (2) adding an auxiliary material additive formed by mixing 0.6kg of titanium dioxide, 3kg of zinc oxide, 0.4kg of anti-yellowing agent and 1kg of antioxidant into 10kg of N, N-dimethylacetamide, uniformly stirring, adding the auxiliary material additive into the chain-extended stock solution, stirring at a constant temperature of 40 ℃ for 1h, fully mixing, and curing for 20h.
Step 4: and (3) curing the spandex spinning solution obtained in the step (3) and then spinning to obtain the acidic easy-dyeing spandex.
The spandex bare yarn prepared by the steps is dyed by acid dye, and the dyeing rate is detected to be 47%, the fixation rate is detected to be 43%, the K/S is detected to be 1.1, and the soaping fastness is detected to be grade 4.
Details are shown in Table 1.
Example III
The preparation method of the acid easy-to-dye spandex comprises the following specific steps:
step 1: 100kg of polytetramethylene ether glycol (molecular weight 1800) and 26kg of 4, 4-diphenylmethane diisocyanate were reacted in a molar ratio of 1:1.9, mixing the materials together in proportion, carrying out a prepolymerization reaction to obtain a prepolymer, cooling to 30 ℃ after the prepolymerization reaction, adding 180kg of N, N-dimethylacetamide solvent, stirring, and fully dissolving the prepolymer;
step 2: mixing 2.1kg of ethylenediamine, 0.78kg of propylenediamine, 0.31kg of diethylamine and 0.44kg of urea, adding the mixture into 46kg of mixed amine solution prepared from N, N-dimethylacetamide, and adding the mixed amine solution into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: and (2) adding an auxiliary material additive formed by mixing 0.6kg of titanium dioxide, 3kg of zinc oxide, 0.4kg of anti-yellowing agent and 1kg of antioxidant into 10kg of N, N-dimethylacetamide, uniformly stirring, adding the auxiliary material additive into the chain-extended stock solution, stirring at a constant temperature of 40 ℃ for 1h, fully mixing, and curing for 20h.
Step 4: and (3) curing the spandex spinning solution obtained in the step (3) and then spinning to obtain the acidic easy-dyeing spandex.
The spandex bare yarn prepared by the steps is dyed by acid dye, and the dyeing rate is 86%, the fixation rate is 82%, the K/S is 2.6 and the soaping fastness is 4 levels.
Details are shown in Table 1.
Comparative example one
The preparation method of the acid easy-to-dye spandex comprises the following specific steps:
step 1: 100kg of polytetramethylene ether glycol (molecular weight 1800) and 20kg of 4, 4-diphenylmethane diisocyanate were reacted in a molar ratio of 1:1.5, mixing the materials together in proportion to perform a prepolymerization reaction to obtain a prepolymer, cooling the prepolymer to 30 ℃ after the prepolymerization reaction, adding 180kg of N, N-dimethylacetamide solvent to stir, and fully dissolving the prepolymer;
step 2: mixing 0.58kg of ethylenediamine, 1.22kg of propylenediamine and 0.2kg of diethylamine, adding the mixture into 24kg of mixed amine solution prepared in N, N-dimethylacetamide, and adding the mixture into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: and (2) adding an auxiliary material additive formed by mixing 0.6kg of titanium dioxide, 3kg of zinc oxide, 0.4kg of anti-yellowing agent and 1kg of antioxidant into 10kg of N, N-dimethylacetamide, uniformly stirring, adding the auxiliary material additive into the chain-extended stock solution, stirring at a constant temperature of 40 ℃ for 1h, fully mixing, and curing for 20h.
Step 4: and (3) curing the spandex spinning solution obtained in the step (3) and then spinning to obtain the acidic easy-dyeing spandex.
This comparative example differs from example 2 in that no urea was added.
The spandex bare yarn prepared by the steps is dyed by acid dye, and the dyeing rate is detected to be 10%, the fixation rate is 9%, the K/S is 0.1 and the soaping fastness is 4 levels, and the details are shown in table 1.
Comparative example two
The preparation method of the acid easy-to-dye spandex comprises the following specific steps:
step 1: 100kg of polytetramethylene ether glycol (molecular weight 1800) and 20kg of 4, 4-diphenylmethane diisocyanate were reacted in a molar ratio of 1:1.5, mixing the materials together in proportion, carrying out a prepolymerization reaction to obtain a prepolymer, cooling to 30 ℃ after the prepolymerization reaction, adding 180kg of N, N-dimethylacetamide solvent, stirring, and fully dissolving the prepolymer;
step 2: mixing 1.5kg of ethylenediamine, 0.43kg of propylenediamine and 0.16kg of diethylamine, adding the mixture into 0.12kg of mixed amine solution prepared from N, N-dimethylacetamide, and adding the mixed amine solution into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: and 2, adding an auxiliary material additive formed by mixing 0.6kg of titanium dioxide, 3kg of zinc oxide, 0.4kg of anti-yellowing agent, 1kg of antioxidant and 0.29kg of urea into 10kg of N, N-dimethylacetamide, uniformly stirring, adding the auxiliary material additive into the chain-extended stock solution, stirring at a constant temperature of 40 ℃ for 1h, fully mixing, and curing for 20h.
Step 4: and (3) curing the spandex spinning solution obtained in the step (3) and then spinning to obtain the acidic easy-dyeing spandex.
The difference between this comparative example and example 2 is that urea was not added during the chain extension reaction, and the timing of the addition of urea was one component of the adjuvant additive in step 3.
The spandex bare yarn prepared by the steps is dyed by acid dye, and the dyeing rate is detected to be 70%, the fixation rate is 25%, the K/S is 0.4, and the soaping fastness is 2 levels, and the details are shown in Table 1.
Table 1 spandex dyeing effect test table of each example
| Examples | The dye uptake is% | The fixation rate is% | K/S | Soaping firmness level |
| Example 1 | 32 | 30 | 0.5 | 4 |
| Example two | 47 | 43 | 1.1 | 4 |
| Example III | 86 | 82 | 2.6 | 4 |
| Comparative example one | 10 | 9 | 0.1 | 4 |
| Comparative example two | 70 | 25 | 0.4 | 2 |
Compared with example 2, in comparative example 1, the amino content on the common spandex fiber is low, the dye-uptake of the acid dye is low, and the color of the fiber is light because urea is not added.
In comparison with example 2, in comparative example 2, urea was not added during the termination reaction, and the timing of adding urea was one component of the auxiliary additive in step 3, resulting in less fixation of the acid dye after adsorption, deep flooding, and low soaping fastness.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced with equivalents; such modifications and substitutions do not depart from the spirit of the technical solutions according to the embodiments of the present invention.
Claims (9)
1. The preparation method of the acid easy-to-dye spandex is characterized by comprising the following specific steps:
step 1: mixing polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate together according to the mol ratio of 1:1.3-2.0 for a prepolymerization reaction to obtain a prepolymer, cooling to 30-50 ℃ after the prepolymerization reaction, adding an N, N-dimethylacetamide solvent for stirring, and fully dissolving the prepolymer;
step 2: adding a mixed amine solution of a chain extension terminator dissolved with urea into the prepolymer solution obtained in the step 1 to perform chain extension reaction and termination reaction;
step 3: adding an auxiliary material additive into the product obtained in the step 2, uniformly stirring, adding the mixture into the chain-extended stock solution, stirring at the constant temperature of 40-50 ℃ for 1-2 hours, fully mixing, and curing for 10-40 hours;
step 4: and (3) curing the spandex spinning stock solution obtained in the step (3) and then spinning to obtain spandex.
2. The method for preparing the acid dyeable spandex according to claim 1, wherein the prepolymerization reaction temperature in the step 1 is 70-90 ℃ and the reaction time is 60-120 min.
3. The method for preparing the acid dyeable spandex according to claim 1, wherein the chain extender in the step 2 is a mixed amine solution prepared by mixing ethylenediamine, propylenediamine, diethylamine and urea and adding the mixed amine solution to N, N-dimethylacetamide.
4. The method for preparing the acid dyeable spandex according to claim 3, wherein the mixed amine solution comprises 0 to 0.06 parts by mass of ethylenediamine, propylenediamine, diethylamine, urea and N, N-dimethylacetamide: 0 to 0.07:0.001 to 0.013:0.003 to 0.012:1.
5. the method for preparing acid dyeable spandex according to claim 1, wherein the chain extension reaction temperature in the step 2 is 30-50 ℃.
6. The method for preparing the acidic dyeable spandex according to claim 1, wherein the mass fraction ratio of the prepolymer to the urea is 500-2000: 1.
7. the method for preparing the acid dyeable spandex according to claim 1, wherein the auxiliary additive in the step 3 is an auxiliary additive obtained by mixing titanium dioxide, zinc oxide, a yellowing inhibitor and an antioxidant and then adding the mixture into N, N-dimethylacetamide.
8. The method for preparing the acid dyeable spandex according to claim 1, wherein the mass ratio of the auxiliary material additive to the product obtained in the step 2 is 0.03-0.05: 1.
9. an acidic easy-dyeing polyurethane fiber is characterized in that the acidic easy-dyeing polyurethane fiber comprises polyurethane fiber taking urea as a terminator and takes-NH-CO-NH as a terminal group 2 The chemical formula is
R represents an inverse prepolymer structure having isocyanate groups.
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