CN114736538B - Modified hydrotalcite for spandex and preparation method thereof - Google Patents
Modified hydrotalcite for spandex and preparation method thereof Download PDFInfo
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- CN114736538B CN114736538B CN202210283214.9A CN202210283214A CN114736538B CN 114736538 B CN114736538 B CN 114736538B CN 202210283214 A CN202210283214 A CN 202210283214A CN 114736538 B CN114736538 B CN 114736538B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
- 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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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention discloses a preparation method of modified hydrotalcite for spandex, which comprises the following specific steps: dissolving the modifier in water, heating to boil, adding hydrotalcite, stirring, reacting completely, and drying to obtain the modified hydrotalcite for spandex. The preparation method of the modified hydrotalcite for the spandex is simple, the raw materials are easy to obtain, and the prepared modified hydrotalcite can be applied to the spandex and can greatly improve the chlorine resistance and yellowing resistance.
Description
Technical Field
The invention belongs to the field of inorganic material coating modification, and particularly relates to modified hydrotalcite for spandex and a preparation method thereof.
Background
Hydrotalcite was found in the schist ore layer in sweden in 1842, and its single crystal structure was determined in 1969, confirming the carbonate intercalation structure of hydrotalcite. Later, the ionic intercalated layered metal hydroxides with similar structure to hydrotalcite were called hydrotalcite-like compounds, also called Layered Double Hydroxides (LDHs). The most widely used hydrotalcite is magnesium-aluminum-based hydrotalcite at present, and the common chemical structure is Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O。
Based on the supermolecular structure of LDHs metal hydroxide laminates and interlayer anions, the LDHs have the following structural characteristics: the controllability of the species and proportion of cations in the laminate, the controllability of the species of anions between layers, memory effect and the like. The controllability of cations of the laminate can endow LDHs with different metal element properties, and the properties of ultraviolet absorption, magnetism, electricity, catalysis and the like can be obtained by introducing transition metal into the laminate, and the corresponding properties can be adjusted and controlled by changing the content of introduced elements. The controllability of anions can not only enable the LDHs to have the properties of corresponding anion optics, catalysis, ultraviolet absorption and the like, but also enable the LDHs to be used as an organic carrier to realize the functions of drug delivery, slow release and the like. The structure memory effect means that the LDHs can recover the characteristics of the self-assembled supermolecular structure of the metal hydroxide laminate and the interlayer anions when the temperature is reduced and the LDHs are in an intercalation anion solution environment after being heated to a certain temperature and decomposed to lose moisture and interlayer anions. In view of the excellent designability and controllability of the LDHs in structure and property, the targeted design and preparation of LDHs with different properties can become an important way for high-value utilization of magnesium chloride resources.
In recent years, the application of magnesium-aluminum based hydrotalcite in the field of polymer modification has been greatly developed, such as adding the hydrotalcite into polyvinyl chloride plastics to prevent yellowing of polyvinyl chloride in the processing process, and the like. Among them, the application of hydrotalcite in spandex is also a very important application scene. Spandex fibers have high elasticity and excellent stretching force, and are widely used in swimwear, sportswear, and the like. Spandex can weaken in its tensile strength when exposed to chlorine (e.g., when the garment is exposed to a swimming pool with 84 disinfectant); in addition, the spandex can yellow and carbonize itself during processing (about 250 ℃). The hydrotalcite is added into spandex, so that the two problems can be effectively improved. The dispersion uniformity and the adhesion firmness of hydrotalcite particles in spandex become key factors influencing the performance of the hydrotalcite. According to the research of our literature, stearic acid is a commonly used coating agent at present for improving the dispersibility, and although the modification has certain effect, the modification still has defects in the aspects of chlorine resistance, yellowing resistance and carbonization.
Based on this, we propose a new polyfunctional group coating modifier, acetamido diacetic acid amine, this kind of coating agent contains two carboxyls, can combine firmly with hydrotalcite, compare in the stearic acid coating agent of traditional only a carboxyls, the bonding strength of coating agent and hydrotalcite can promote greatly, in addition, the acylamino that has can participate in the polymerization of spandex fiber, firmly fix in spandex fiber, make hydrotalcite adhere to the fastness in spandex and promote by a wide margin like this, chlorine-resistant and yellowing-resistant performance have all had obvious promotion.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the primary object of the present invention is to provide a method for preparing a modified hydrotalcite for spandex.
The second purpose of the invention is to provide the modified hydrotalcite for spandex prepared by the preparation method.
The primary purpose of the invention is realized by the following technical scheme:
a preparation method of modified hydrotalcite for spandex comprises the following specific steps: dissolving the modifier in water, heating to boil, adding hydrotalcite, stirring, reacting completely, and drying to obtain the modified hydrotalcite for spandex.
Preferably, the modifier is acetamido diacetic acid amine, and the specific structure is as follows:
preferably, the modifier accounts for 0.5-5% of the hydrotalcite by mass.
Preferably, the modifier accounts for 1% of the hydrotalcite by mass.
Preferably, the reaction time is 20 to 180min.
Preferably, the reaction time is 180min.
Preferably, the hydrotalcite has a specific structure of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O、Mg 8 Al 4 (OH) 16 O 4 (CO 3 ) 2 、Mg 8 Al 4 (OH) 16 O 4 (CO 3 ) 2 ·6H 2 O、Mg 9.6 Al 2.4 (OH) 14.4 O 4.8 (CO 3 ) 2 ·6H 2 And O is one of the compounds.
Preferably, the hydrotalcite has a specific structure of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O。
Preferably, in the present invention, the hydrotalcite has a nanosheet structure, and a size of less than 1 micron is most effective.
The second purpose of the invention is realized by the following technical scheme:
a modified hydrotalcite for spandex prepared by the above preparation method.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) The modifier is acetamido diacetic acid amine, two carboxyl groups of the acetamido diacetic acid amine are used for carrying out adsorption coordination with the surface of the hydrotalcite to realize coating, an amide group can participate in the polymerization of spandex fibers and is firmly fixed in the spandex fibers, so that the adhesion firmness of the hydrotalcite in the spandex is greatly improved, and the acetamido diacetic acid amine also contains a benzene ring, so that the thermal stability of the modified hydrotalcite can be obviously improved.
(2) The preparation method of the modified hydrotalcite for spandex is simple, the raw materials are easy to obtain, and the prepared modified hydrotalcite can be applied to spandex and can greatly improve the chlorine resistance and yellowing resistance.
Drawings
FIG. 1 is a schematic view; thermogravimetry of hydrotalcite before and after modification;
FIG. 2 is a graph showing yellowing performance of spandex employing unmodified hydrotalcite after 5 minutes;
FIG. 3 is a graph of yellowing performance of spandex using unmodified hydrotalcite after 10 minutes;
FIG. 4 is a graph showing yellowing performance of spandex after 15 minutes using unmodified hydrotalcite;
FIG. 5 is a graph showing yellowing performance of spandex with unmodified hydrotalcite after 20 minutes;
FIG. 6 is a graph showing yellowing performance of hydrotalcite modified with stearic acid after 5 minutes in spandex;
FIG. 7 is a graph showing yellowing performance of spandex modified hydrotalcite with stearic acid after 10 minutes;
FIG. 8 is a graph showing yellowing performance of hydrotalcite modified with stearic acid after 15 minutes in spandex;
FIG. 9 is a graph showing yellowing performance of spandex modified hydrotalcite with stearic acid after 20 minutes;
FIG. 10 is a graph showing yellowing performance of hydrotalcite imported from abroad after spandex for 5 minutes using hydrotalcite of a certain known brand;
FIG. 11 is a graph showing the yellowing performance of polyurethane fiber 10 minutes after hydrotalcite of a certain brand is imported abroad:
FIG. 12 is a graph showing yellowing performance of hydrotalcite imported from abroad after 15 minutes using spandex of a certain known brand of hydrotalcite;
FIG. 13 is a graph showing yellowing performance of a hydrotalcite obtained by importing hydrotalcite from abroad after 20 minutes in the presence of spandex of a known brand;
FIG. 14 is a graph showing yellowing performance of a hydrotalcite imported from abroad after spandex for 25 minutes, wherein the hydrotalcite is of a known brand;
FIG. 15 is a graph of yellowing performance of spandex modified by the patented method after 5 minutes;
FIG. 16 is a graph of yellowing performance of spandex modified by the patented method after 10 minutes;
FIG. 17 is a graph of yellowing performance of spandex modified by the patented method after 15 minutes;
FIG. 18 is a graph showing the yellowing properties of spandex modified by the patented process after 20 minutes;
FIG. 19 is a graph of yellowing performance of spandex modified by the patented method after 25 minutes;
FIG. 20 is a graph showing yellowing performance of spandex modified by the patented method after 30 minutes.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Dissolving 1g of the surface modifier acetamido-diacetic acid amine (purchased directly) in water, heating to boiling, and then slowly adding 10g of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O (produced by the company), stirring vigorously, reacting for 180min, and drying to obtain the modified hydrotalcite for spandex, wherein thermogravimetric analysis shows that the thermal stability of the modified hydrotalcite is obviously improved, and the decomposition temperature is increased from 100 ℃ to 200 ℃, which is beneficial to improving the yellowing resistance of the hydrotalcite in the subsequent spandex processing process (fig. 15-20). Fully mixing the obtained modified hydrotalcite with spandex material, heating and melting, testing the yellowing resistance of the modified hydrotalcite, and testing the formulaThe method is to sample at equal time intervals and observe the color change, as shown in fig. 15 to 20.
Example 2
Dissolving 0.5g of acetamido diacetic acid amine as a surface modifier in water, heating to boiling, and slowly adding 10g of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 And O, violently stirring, reacting for 180min, and drying to prepare the modified hydrotalcite for spandex. And (3) fully mixing the obtained modified hydrotalcite with a spandex material, heating and melting, and testing the yellowing resistance of the modified hydrotalcite, wherein the testing method comprises the steps of sampling at equal time intervals and observing color change.
Example 3
Dissolving 5g of acetamido-diacetic acid amine as a surface modifier in water, heating to boiling, and slowly adding 10g of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 And O, violently stirring, reacting for 180min, and drying to prepare the modified hydrotalcite for spandex. And (3) fully mixing the obtained modified hydrotalcite with a spandex material, heating and melting, and testing the yellowing resistance of the modified hydrotalcite by sampling at equal time intervals and observing the color change.
Example 4 Strength test experiment
After the product obtained in example 1 was sufficiently mixed with spandex, heat melt-spun to obtain spandex yarn, which was tested for chlorine resistance by immersing spandex yarn in 84 disinfectant containing 3.5ppm of available chlorine at PH =7.5 for 24 hours and measuring its strength by hanging 1Kg of steel ball on a 5cm long sample, as specifically tested in patent (CN 101528993A) with strength retention = strength after immersion/strength before immersion x 100%.
In terms of strength retention rate, the modifier disclosed by the invention can greatly improve the adhesion firmness of the hydrotalcite, and therefore, particularly excellent strength retention rate is shown.
Example 5 yellowing resistance test
In order to illustrate the effect of the modified hydrotalcite on the modification of spandex by comparison, compared with example 1, three groups of control spandex are simultaneously made, the difference is that the used hydrotalcites are different, and the control experiment is respectively 1) unmodified hydrotalcite;
2) Stearic acid-modified hydrotalcite; 3) Some known brand of hydrotalcite is imported abroad.
The results show that the spandex prepared by the scheme of the invention has the most excellent yellowing resistance, for example, fig. 2 to 5 are graphs of yellowing performance of spandex adopting unmodified hydrotalcite after different times, the obvious yellowing time is 14min40s, fig. 6 to 9 are graphs of yellowing performance of spandex adopting stearic acid modified hydrotalcite after different times, the obvious yellowing time is 18min, fig. 10 to 14 are graphs of yellowing performance of spandex adopting hydrotalcite of a certain known brand imported from abroad after different times, and the obvious yellowing time is 19min40s. FIGS. 15 to 20 are graphs of yellowing performance of spandex modified by the patented method of example 1 at different times, and the obvious yellowing time is 25min20s.
Meanwhile, the heat stability of the hydrotalcite is obviously improved before and after modification, the weight loss of the unmodified hydrotalcite is started at 150 ℃, the weight loss of the modified hydrotalcite is started all the time after 200 ℃, the possibility that the interaction between the coating agent and the hydrotalcite brings the stability of the hydrotalcite is high, and the specific mechanism is still researched. Needless to say, the thermal stability of the hydrotalcite coated and modified is increased, which is beneficial to improving the yellowing resistance of spandex.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A preparation method of modified hydrotalcite for spandex is characterized by comprising the following specific steps: dissolving a modifier in water, heating to boil, adding hydrotalcite, stirring, reacting completely, and drying to obtain modified hydrotalcite for spandex;
the modifier is acetamido diacetic acid amine, and has the following specific structure:
2. the method for preparing modified hydrotalcite for spandex according to claim 1, characterized in that the modifier is 0.5 to 5% by mass of the hydrotalcite.
3. The method for producing a modified hydrotalcite for spandex according to claim 2, characterized in that the modifier accounts for 1% by mass of the hydrotalcite.
4. The method for preparing modified hydrotalcite for spandex according to claim 1, wherein the reaction time is 20 to 180min.
5. The method for preparing modified hydrotalcite for spandex according to claim 4, characterized in that the reaction time is 180min.
6. The method for preparing modified hydrotalcite for spandex according to claim 1, wherein the hydrotalcite has a specific structure of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O、Mg 8 Al 4 (OH) 16 O 4 (CO 3 ) 2 、Mg 8 Al 4 (OH) 16 O 4 (CO 3 ) 2 ·6H 2 O、Mg 9.6 Al 2.4 (OH) 14.4 O 4.8 (CO 3 ) 2 ·6H 2 And O.
7. The process for producing a modified hydrotalcite for spandex according to claim 6, characterized in that,the hydrotalcite has a specific structure of Mg 4 Al 2 (OH) 2 CO 3 ·3H 2 O。
8. A modified hydrotalcite for spandex, prepared according to the preparation method of any one of claims 1 to 7.
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| CN202210283214.9A CN114736538B (en) | 2022-03-22 | 2022-03-22 | Modified hydrotalcite for spandex and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000313852A (en) * | 1999-04-30 | 2000-11-14 | Kansai Paint Co Ltd | Cationic electrodeposition coating material |
| CN1720353A (en) * | 2002-12-02 | 2006-01-11 | 阿科玛股份有限公司 | Composition and method for copper chemical mechanical planarization |
| CN103865296A (en) * | 2014-02-26 | 2014-06-18 | 北京化工大学 | Sulfamic acid group intercalation modified hydrotalcite and preparation method thereof |
| CN104830408A (en) * | 2015-06-07 | 2015-08-12 | 烟台顺隆化工科技有限公司 | Emulsified metal cutting fluid |
| CN105218861A (en) * | 2015-11-16 | 2016-01-06 | 济南泰星精细化工有限公司 | A kind of flame-retardant smoke inhibition organically-modified hydrotalcite and preparation method thereof |
| CN107096870A (en) * | 2017-07-03 | 2017-08-29 | 李吕军 | Reduce precoated sand of cast member surface detail and preparation method thereof |
-
2022
- 2022-03-22 CN CN202210283214.9A patent/CN114736538B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000313852A (en) * | 1999-04-30 | 2000-11-14 | Kansai Paint Co Ltd | Cationic electrodeposition coating material |
| CN1720353A (en) * | 2002-12-02 | 2006-01-11 | 阿科玛股份有限公司 | Composition and method for copper chemical mechanical planarization |
| CN103865296A (en) * | 2014-02-26 | 2014-06-18 | 北京化工大学 | Sulfamic acid group intercalation modified hydrotalcite and preparation method thereof |
| CN104830408A (en) * | 2015-06-07 | 2015-08-12 | 烟台顺隆化工科技有限公司 | Emulsified metal cutting fluid |
| CN105218861A (en) * | 2015-11-16 | 2016-01-06 | 济南泰星精细化工有限公司 | A kind of flame-retardant smoke inhibition organically-modified hydrotalcite and preparation method thereof |
| CN107096870A (en) * | 2017-07-03 | 2017-08-29 | 李吕军 | Reduce precoated sand of cast member surface detail and preparation method thereof |
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