CN110699778B - Preparation method of phase-change thermoregulation alginate fiber - Google Patents
Preparation method of phase-change thermoregulation alginate fiber Download PDFInfo
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- CN110699778B CN110699778B CN201910969819.1A CN201910969819A CN110699778B CN 110699778 B CN110699778 B CN 110699778B CN 201910969819 A CN201910969819 A CN 201910969819A CN 110699778 B CN110699778 B CN 110699778B
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/04—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of alginates
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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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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Abstract
The invention discloses a preparation method of phase-change thermoregulation seaweed fiber, which comprises the following steps: 1) and mixing the phase change material, the emulsifier and water according to the ratio of 20-50: 0.5-6: stirring and mixing the materials in a mass ratio of 44-79.5 to obtain phase-change microemulsion; 2) preparing a sodium alginate aqueous solution with the mass concentration of 3-10%; 3) mixing the phase-change microemulsion with a sodium alginate aqueous solution according to the ratio of 1: mixing the materials in a mass ratio of 30-80 to obtain a sodium alginate spinning solution; 4) and preparing the sodium alginate spinning solution into the phase-change thermoregulation alginate fiber by adopting a wet spinning process. The method of the invention can improve the temperature adjusting performance and the mechanical property of the temperature adjusting alginate fiber.
Description
Technical Field
The invention belongs to the technical field of fiber materials. In particular to a synthesis method and a spinning method of microemulsion.
Background
The phase-change thermoregulation fiber is produced by coating phase-change microcapsules in a fiber body. The size of the phase-change microcapsule needs to be controlled to be about 3 microns in the spinning process, and in addition, the dispersion uniformity of the phase-change microcapsule in a solution is not ideal. The content of the phase-change microcapsules in the fiber is low, and the temperature adjusting effect is limited.
Patent 200480019016.1 reports a method for preparing phase-change microcapsules; patent 200610069976.X reports a method for wet spinning by blending phase-change microcapsule and sodium alginate; patent 201210412977.5 reports that a phase-change thermoregulation seaweed fiber with hygroscopicity is prepared by adding a phase-change microcapsule into a sodium alginate solution; patent 201510031063.8 reports a method for preparing alginate fibers by wet spinning; patent 201810105447.3 reports a melt process for making a temperature regulating fiber in a sheath-core structure.
In patent 200610069976.X and patent 201210412977.5, phase change microcapsule is added into sodium alginate solution, and temperature-regulating alginate fiber is prepared by wet spinning; the phase-change microcapsule has the technical defects of easy agglomeration, uneven dispersion, larger size, limited addition amount and the like, so that the temperature regulating capacity of the temperature-regulating fiber is limited, and the mechanical property of the fiber is low.
Disclosure of Invention
The invention aims to provide a preparation method of phase-change thermoregulation alginate fiber, which is beneficial to improving the thermoregulation performance of the phase-change thermoregulation alginate fiber.
In order to solve the technical problems, the invention provides a preparation method of phase-change thermoregulation seaweed fiber, which comprises the following steps:
1) and mixing the phase change material, the emulsifier and water according to the weight ratio of 20-50: 0.5-6: stirring and mixing the materials in a mass ratio of 44-79.5 to obtain phase-change microemulsion;
2) preparing a sodium alginate aqueous solution with the mass concentration of 3-10%;
3) mixing the phase-change microemulsion with a sodium alginate aqueous solution according to the ratio of 1: mixing the materials in a mass ratio of 30-80 to obtain a sodium alginate spinning solution (serving as a spinning stock solution);
4) and preparing the sodium alginate spinning solution into the phase-change thermoregulation alginate fiber by adopting a wet spinning process.
The improvement of the preparation method of the phase-change thermoregulation seaweed fiber of the invention is as follows:
the phase-change material is paraffin (liquid paraffin) and alkane; the alkanes are n-tetradecane, n-hexadecane, n-octadecane and n-eicosane;
the emulsifier is a mixture obtained by mixing alkylphenol polyoxyethylene and sodium dodecyl sulfate according to the mass ratio of 4: 1-1: 3.
The preparation method of the phase-change thermoregulation seaweed fiber is further improved as follows:
in the step 1), the stirring speed is 5000-20000 rpm; the stirring time is 5-25 minutes.
The preparation method of the phase-change thermoregulation seaweed fiber is further improved as follows:
in the wet spinning process of the step 4), the coagulating bath is 4% CaCl2The temperature of the solution is 30-45 ℃.
The preparation method of the phase-change thermoregulation seaweed fiber is further improved as follows:
the step 1) is as follows: stirring and mixing 4 g of alkylphenol polyoxyethylene, 1 g of sodium dodecyl sulfate, 40 g of liquid paraffin and 45 g of water to obtain phase-change microemulsion;
the step 2) is as follows: preparing a sodium alginate aqueous solution with the mass concentration of 5%;
the step 3) is as follows: and adding 10 g of phase-change microemulsion into 600 g of sodium alginate aqueous solution, and uniformly mixing to obtain the sodium alginate spinning solution.
The phase-change microemulsion prepared in the step 1) is spherical; the average diameter is 3 μm, and the majority of the diameters are distributed between 0.5 and 10 μm. As shown in fig. 1.
The method comprises the synthesis of phase-change microemulsion and the preparation of the temperature-regulating alginate fiber by using the phase-change microemulsion in wet spinning. The invention adopts the blending spinning of the phase-change microemulsion and the sodium alginate, compared with the traditional phase-change fiber preparation process, the phase-change material is directly prepared into the phase-change microemulsion, and the shell material in the phase-change microcapsule is saved, so the content proportion of the phase-change material in the fiber is improved when the phase-change material is mixed with the sodium alginate solution; in addition, the phase-change microemulsion is suspended in the sodium alginate solution, so that the phase-change microemulsion has better compatibility and dispersibility (figure 1), can further improve the content proportion of the phase-change material in the fiber, and is also beneficial to preparing the fiber with more uniform structure; thereby improving the temperature regulating performance and the mechanical property of the temperature regulating alginate fiber.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an optical microscope picture of a phase-change microemulsion in a sodium alginate solution;
FIG. 2 is the electron microscope image of the side (left) and cross section (right) of the phase-change alginate fiber.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1, a method for preparing phase-change thermoregulation seaweed fiber, which comprises the following steps:
1) adding 4 g of alkylphenol polyoxyethylene, 1 g of sodium dodecyl sulfate and 40 g of liquid paraffin into 45 g of water, and stirring for 15 minutes at the speed of 20000 revolutions per minute to form phase-change microemulsion;
2) pouring 5 g of sodium alginate into 95 g of water to prepare a sodium alginate aqueous solution with the mass concentration of 5%;
3) and adding 10 g of phase-change microemulsion into 600 g of sodium alginate aqueous solution, and uniformly mixing to prepare the sodium alginate spinning solution.
4) Preparing the sodium alginate spinning solution into the phase-change thermoregulation alginate fiber by adopting a conventional wet spinning process, which comprises the following specific steps:
5.0 percent of CaCl by mass percentage2The calcium chloride is a metal coagulation bath, the conventional wet spinning is carried out at the coagulation bath temperature of 40 ℃, the coagulation time of the alginate fibers in the coagulation bath is 3 minutes, the draw ratio is 2, and the alginate fibers are stretched, wound and naturally dried; obtaining the phase-change thermoregulation seaweed fiber.
Taking the phase-change microemulsion obtained in the step 1), and carrying out performance test according to the standards GB T27596-.
Taking the phase change temperature-regulating alginate fiber obtained in the step 4), and carrying out performance test according to GB T36422-.
TABLE 1 Properties of phase-Change microemulsions and phase-Change thermoregulation seaweed fibers
The phase change enthalpy of the obtained phase change thermoregulation seaweed fiber is 22J/g, and is obviously greater than 12J/g of the phase change enthalpy of the current commercial thermoregulation fiber outlast.
Comparative example 1, step 1) in example 1 was changed as follows:
1) adding 40 g of liquid paraffin into 45 g of water, and stirring for 15 minutes at the speed of 20000 revolutions per minute to form phase change liquid;
performing subsequent steps by using the phase change liquid; the rest is equivalent to embodiment 1.
Comparative example 2, step 1) in example 1 was modified as follows: changing 4 g of alkylphenol polyoxyethylene ether and 1 g of lauryl sodium sulfate into 5 g of alkylphenol polyoxyethylene ether; the rest is equivalent to embodiment 1.
Comparative example 3, step 1) in example 1 was modified as follows: changing 4 g of alkylphenol polyoxyethylene ether and 1 g of sodium dodecyl sulfate into 5 g of sodium dodecyl sulfate; the rest is equivalent to embodiment 1.
The results of comparative examples 1 to 3 were obtained, and the corresponding performance tests were carried out as in example 1, and the results are shown in table 2 below.
TABLE 2 Properties of comparative examples
Comparative example 4, step 1) in example 1 was changed as follows:
1) changing 4 g of alkylphenol polyoxyethylene ether and 1 g of sodium dodecyl sulfate into 5 g of alkylphenol polyoxyethylene ether and 5 g of sodium dodecyl sulfate;
performing subsequent steps by using the phase change liquid; the rest is equivalent to embodiment 1.
Comparative example 5, step 2) in example 1 was changed as follows:
2) pouring 5 g of sodium alginate into 95 g of water to prepare a sodium alginate aqueous solution with the mass concentration of 5 percent, and changing into pouring 15 g of sodium alginate into 85 g of water to prepare a sodium alginate aqueous solution with the mass concentration of 15 percent;
carrying out subsequent steps by using the sodium alginate aqueous solution; the rest is equivalent to embodiment 1.
Comparative example 6, step 3) in example 1 was changed as follows:
3) adding 10 g of phase-change microemulsion into 600 g of sodium alginate aqueous solution to change the phase-change microemulsion into 10 g of phase-change microemulsion and adding the phase-change microemulsion into 1000 g of sodium alginate aqueous solution;
carrying out subsequent steps by using the sodium alginate spinning solution; the rest is equivalent to embodiment 1.
The results of comparative examples 4 to 6 were obtained, and the corresponding performance tests were carried out as in example 1, and the results are shown in Table 3 below.
TABLE 3 Properties of comparative examples
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (2)
1. The preparation method of the phase-change thermoregulation seaweed fiber is characterized by sequentially carrying out the following steps:
1) adding 4 g of alkylphenol ethoxylates, 1 g of sodium dodecyl sulfate and 40 g of liquid paraffin into 45 g of water, and stirring for 15 minutes at the speed of 20000 revolutions per minute to form phase-change microemulsion;
2) pouring 5 g of sodium alginate into 95 g of water to prepare a sodium alginate aqueous solution with the mass concentration of 5%;
3) adding 10 g of phase-change microemulsion into 600 g of sodium alginate aqueous solution, and uniformly mixing to prepare sodium alginate spinning solution;
4) and preparing the sodium alginate spinning solution into the phase-change thermoregulation alginate fiber by adopting a wet spinning process.
2. The method for preparing the phase-change thermoregulation seaweed fiber according to claim 1, characterized in that the step 4) is:
5.0 percent of CaCl by mass percentage2The method is characterized in that the method is a metal coagulation bath, the conventional wet spinning is carried out at the coagulation bath temperature of 40 ℃, the coagulation time of alginate fibers in the coagulation bath is 3 minutes, the draw ratio is 2, and the alginate fibers are stretched, wound and naturally dried; obtaining the phase-change thermoregulation seaweed fiber.
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