CN113943982B - Volcanic rock thermal insulation fiber and thermal insulation sock - Google Patents
Volcanic rock thermal insulation fiber and thermal insulation sock Download PDFInfo
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- CN113943982B CN113943982B CN202111293045.9A CN202111293045A CN113943982B CN 113943982 B CN113943982 B CN 113943982B CN 202111293045 A CN202111293045 A CN 202111293045A CN 113943982 B CN113943982 B CN 113943982B
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- 239000000835 fiber Substances 0.000 title claims abstract description 56
- 239000011435 rock Substances 0.000 title claims abstract description 36
- 238000009413 insulation Methods 0.000 title abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 82
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 81
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- 239000000919 ceramic Substances 0.000 claims abstract description 65
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- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
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- 238000002156 mixing Methods 0.000 claims description 23
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- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000004472 Lysine Substances 0.000 claims description 16
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 14
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- 238000001035 drying Methods 0.000 claims description 12
- 230000003213 activating effect Effects 0.000 claims description 8
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- 239000003513 alkali Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- AEDZKIACDBYJLQ-UHFFFAOYSA-N ethane-1,2-diol;hydrate Chemical compound O.OCCO AEDZKIACDBYJLQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 244000309466 calf Species 0.000 claims description 4
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
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- 238000009987 spinning Methods 0.000 description 14
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- 238000010030 laminating Methods 0.000 description 2
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- 229920000742 Cotton Polymers 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
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- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- D01F6/92—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 polyesters
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
- A41B11/00—Hosiery; Panti-hose
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
- A41B11/00—Hosiery; Panti-hose
- A41B11/02—Reinforcements
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
- A41B17/00—Selection of special materials for underwear
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
- A41B2400/00—Functions or special features of shirts, underwear, baby linen or handkerchiefs not provided for in other groups of this subclass
- A41B2400/34—Functions or special features of shirts, underwear, baby linen or handkerchiefs not provided for in other groups of this subclass antimicrobial or antibacterial
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
- A41B2400/00—Functions or special features of shirts, underwear, baby linen or handkerchiefs not provided for in other groups of this subclass
- A41B2400/36—Deodorising or perfuming
Abstract
The application relates to volcanic rock thermal insulation fibers and thermal insulation socks, and belongs to the technical field of special functional fabrics. The application firstly discloses volcanic rock fiber, the raw materials of volcanic rock fiber include polyester master batch and far infrared master batch, far infrared master batch is prepared by the raw materials of at least the following mass portions: 100 parts of polyester particles; 50-60 parts of infrared ceramic powder; 5-10 parts of volcanic rock powder; 5-8 parts of graphene oxide; 3-5 parts of coupling agent. The application further discloses a thermal sock which is woven by blended yarns, wherein the blended yarns comprise the volcanic rock thermal fiber. The heat insulation and water washing resistance cloth has the effects of good heat insulation effect and water washing resistance.
Description
Technical Field
The application relates to the field of special functional fabrics, in particular to volcanic thermal insulation fibers and thermal insulation socks.
Background
The feet are weak places in the blood circulation process, are very easily affected by the ambient temperature, and are very easy to cool in winter. The most common foot warming mode at present is to wear thicker socks, and although the thicker socks have better warming effect, the thicker socks have poorer foot feeling, and because the size of the shoes of consumers is fixed, the feet can be pressed by passing through the thicker socks, and the blood circulation of the feet is influenced.
With the development of society and the improvement of economic level, the performance requirements of consumers on various textiles are increasingly improved, and the fabrics with the heat preservation performance improved by simply improving the thickness are difficult to meet the increasingly improved requirements of consumers. Therefore, if a light and thin fabric with good warm-keeping effect is prepared, the fabric is a great research direction of the current functional textile fabric.
At present, special functional fabrics with heat preservation and heating effects are generally prepared by after-finishing the fabrics, namely, special auxiliary agents with heat storage and heating capacities are finished on the fabrics through a finishing process, so that the light and thin fabrics have good heat preservation effects. However, although the fabric obtained by post-finishing the auxiliary agent has good warm keeping performance at first, the fabric is not resistant to washing, and the warm keeping performance of the fabric after washing for a plurality of times is greatly reduced.
Disclosure of Invention
In order to overcome the defect that the conventional after-finishing auxiliary agent for preparing the thermal fabric is not resistant to water washing, the application provides the volcanic thermal fiber and the thermal socks.
In a first aspect, the present application provides a volcanic rock thermal fiber, which adopts the following technical scheme:
the volcanic rock thermal insulation fiber comprises the following raw materials in percentage by mass:
85-90% of polyester master batch;
10-15% of far infrared master batch;
the far infrared master batch is prepared from the following raw materials in parts by mass:
through adopting above-mentioned technical scheme, compare in common through finishing process, this application is specific, makes far infrared master batch with infrared ceramic powder, volcanic rock powder and the graphene oxide that have far infrared emission function to mix conventional polyester master batch and far infrared master batch when spinning, the thermal-insulated fibre of making has intrinsic far infrared emission function. No matter how many times the volcanic rock thermal insulation fiber is washed, the far infrared emission function of the volcanic rock thermal insulation fiber prepared by the method can still be kept at a higher level; correspondingly, the current common researches show that the heating performance of the heating fiber prepared by the conventional after-finishing process is almost lost after 50 times of water washing.
The far infrared emission performance of both the infrared ceramic powder and the volcanic rock is good, wherein minerals and trace elements of the volcanic rock easily absorb heat and convert the absorbed heat into infrared rays; in addition, volcanic rock can reflect infrared radiation generated by human body; and the infrared rays can be heated up through the action of water molecules in the human body, so that the active warm-keeping effect is achieved. The volcanic rock is in an irregular porous structure, so that a large amount of static air can be adsorbed, and the heat conductivity coefficient of the static air is only about 0.025W/(mdeg.C) and is far lower than that of the polyester fiber, so that the volcanic rock with the porous structure can generate good heat storage capacity.
The inventor finds that the heat accumulation and temperature rise effects of the graphene oxide are better than those of volcanic rock and common infrared ceramics, but the graphene oxide is used as a nano material, so that aggregation is easy to occur, a spinneret plate is easy to block, fiber defects are easy to cause, and the breaking strength of the fiber is reduced. The inventor finds that the breaking strength of the fiber can be remarkably improved by mixing graphene oxide, infrared ceramic powder and volcanic powder. This is probably because the infrared ceramic powder can be inserted between the flake-shaped graphene oxides, so that the steric hindrance of the graphene oxides is improved, and the porous volcanic powder can adsorb the graphene oxides and the infrared ceramic powder, so that the porous volcanic powder is more orderly arranged around the volcanic powder, thereby reducing fiber defects and improving the breaking strength of the fibers.
Optionally, the infrared ceramic powder is Al 2 O 3 、TiO 2 、SiO 2 、Cr 2 O 3 、ZrO 2 、B 4 C、SiC、ZrC、BN、AlN、Si 3 N 4 、TiN、TiSi 2 、WSi 2 、ZrB 2 、CrB 2 At least two of the above.
By adopting the technical scheme, different infrared ceramic powders have different far infrared emission frequency ranges, and at least more than two infrared ceramic powders can be selected for enabling the far infrared emission frequency ranges to be more complete. In addition, the person skilled in the art can select the required infrared ceramic powder according to the infrared emission frequency ranges of different infrared ceramic powders and the design of actual products.
Optionally, the infrared ceramic powder is subjected to activation treatment before use, and comprises the following steps:
a1, dispersing, namely firstly putting a dispersing agent into water to be uniformly dispersed, then adding infrared ceramic powder, and uniformly mixing to obtain a suspension;
a2, activating, namely grinding and activating the suspension obtained in the step A1 to obtain an activated liquid;
a3, drying, and spray drying the activation liquid obtained in the step A2 to obtain activated infrared ceramic powder.
By adopting the technical scheme, hydroxyl with stronger hydrophilicity is easy to form on the surface of the infrared ceramic powder, the specific surface area is overlarge, and the free energy of the surface is reduced, so that the ceramic powder is easy to agglomerate. These agglomerates tend to be several tens of times larger than the primary particles, and therefore, the infrared ceramic powder needs to be dispersed and activated before it is used, thereby reducing the impact of these agglomerates on the fiber properties.
The dispersion performance of the infrared ceramic powder can be greatly improved by adopting the modes of dispersing, grinding and activating and spray drying. The added dispersing agent can not only reduce the possibility of agglomeration of the infrared ceramic powder, but also improve the compatibility of the infrared ceramic powder and polyester particles, improve the mutual adhesion force of the infrared ceramic powder and the polyester, increase the fluidity of the melt and improve the spinnability.
Optionally, the dispersing agent comprises lysine and sodium tripolyphosphate according to a mass ratio of 1: (8-10) mixing.
By adopting the technical scheme, cations in the sodium tripolyphosphate can be adsorbed by the infrared ceramic powder to form an electric double layer, so that the dispersibility of the infrared ceramic powder is improved, and in general, the sodium tripolyphosphate has better dispersibility under alkaline conditions. At present, a common mode is to add strong alkali such as sodium hydroxide into the system, and adjust the pH value of the system to be alkaline so as to improve the dispersion effect of sodium tripolyphosphate. However, in the present application, the spray drying method is selected in step A3, and the spray drying can omit the subsequent steps of grinding, but can also cause sodium tripolyphosphate and alkaline substances to remain on the far infrared ceramic powder. The system contains a large amount of polyester, and the polyester is easy to decompose under the action of strong alkali such as sodium hydroxide to form internal damage, so that the system cannot use strong alkali such as sodium hydroxide.
Lysine is specifically added in the dispersing agent, and lysine is an alkaline amino acid, so that the dispersing effect of sodium tripolyphosphate can be improved, lysine is positively charged after self ionization, and the lysine can be adsorbed on the surface of the infrared ceramic powder, so that the electric charge quantity on the surface of the infrared ceramic powder is further improved, and the dispersing effect of the infrared ceramic powder is further improved.
Optionally, in the step A1, the concentration of the dispersing agent is 20-25mg/L, and the concentration of the infrared ceramic powder is 0.8-1.2g/L.
By adopting the technical scheme, the inventor finds that although the sodium tripolyphosphate has better dispersing effect on the infrared ceramic powder, after part of sodium tripolyphosphate is replaced by lysine, the effect of the dispersing agent is obviously improved, and the consumption of the dispersing agent can be reduced from about 40-50mg/L to about 20-25mg/L on the basis of ensuring the overall dispersing effect.
In addition, the concentration of the infrared ceramic powder needs to be strictly controlled, because different suspension concentrations affect the final pulverizing effect, so that the particle sizes of the finally obtained activated infrared ceramic powder are different. If the concentration of the suspension is too high, problems such as poor fluidity and slow circulation speed tend to occur during polishing.
Optionally, the graphene oxide is modified before being added, and specifically comprises the following steps:
b1, dissolving graphene oxide, namely putting the graphene oxide into a solvent for uniform dispersion to obtain a graphene oxide solution;
b2, mixing, namely adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture;
and B3, modifying, namely heating the mixture to 95+/-2 under the protection of inert gas atmosphere, carrying out reflux reaction, and then filtering and washing to obtain the modified graphene oxide.
By adopting the technical scheme, the acrylonitrile is easy to perform addition reaction with the compound containing active hydrogen atoms, and under alkaline conditions, the acrylonitrile can react with oxygen-containing groups on the surface of the graphene oxide, so that the acrylonitrile is grafted onto the graphene oxide, and composite powder similar to a core-shell structure is formed, so that the compatibility of the graphene oxide and polyester particles is greatly improved. It is to be noted that since the modified graphene oxide needs to be washed, in step B2, even if a strong base such as sodium hydroxide is added, it is finally eluted, and thus, its influence on the polyester properties is not considered.
In addition, the inventor unexpectedly found that, compared with the addition of unmodified graphene oxide, the addition of modified graphene oxide can enable the finally prepared thermal insulation fiber to have a significantly better heating effect. This is probably due to the fact that the acrylonitrile is mixed into the polyester after being grafted on the graphene oxide, and nitrile groups are converted into carboxylate with moisture absorption and heating properties in the subsequent finishing process, such as the alkali reduction process, so that the thermal insulation fiber has a better heating effect.
In addition, the inventors found that mixing the modified graphene oxide and the activated infrared ceramic powder clearly has better compatibility than mixing the modified graphene oxide and the unactivated infrared ceramic powder. This is probably due to the fact that the activated infrared ceramic powder has lysine, and the lysine has active hydrogen, which can react with acrylonitrile on the modified graphene oxide, so that the activated infrared ceramic powder, the modified graphene oxide, polyester particles and the like have good compatibility.
Optionally, the solvent used in the step B1 is a mixture of water and diethylene glycol, and the water is in a volume ratio: diethylene glycol= (8-10): 1.
by adopting the technical scheme, the inventor finds that if only water is used as a solvent in the process of modifying the graphene oxide, the system gradually blackens from light yellow as the modification is carried out, which means that the graphene oxide is gradually reduced. And reduced graphene oxide exhibits a certain hydrophobicity, so that the reduced graphene oxide is easily agglomerated. And the mixed solvent obtained by adding a certain amount of diglycol into water can improve the stability of graphene oxide and reduced graphene oxide, and reduce the possibility of agglomeration of the graphene oxide and the reduced graphene oxide.
It should be noted that, in general, the highest extrusion granulation temperature of polyester is about 270 ℃, but the addition of high-content infrared ceramic powder, volcanic powder and graphene oxide leads to an increase in apparent viscosity of the melt, a decrease in fluidity, and difficulty in flow during melt extrusion. In order to increase the melt flowability, it is necessary to increase the spinning temperature to about 280 ℃, but the increase in the spinning temperature tends to cause degradation of the polyester.
However, the inventors have unexpectedly found that the addition of diethylene glycol to water not only increases the stability of the overall system, but also increases the rheology of the melt, thereby reducing the final spinning temperature and improving spinnability. This is probably due to the fact that acrylonitrile and diethylene glycol can form polyether nitrile under alkaline conditions, polyether nitrile introduces ether linkage into polyester, and the introduction of ether linkage improves the flexibility of polyester, and entropy change increases in the melting process, so that the melting point of polyester is lowered, and the low-temperature spinnability is improved on the basis of guaranteeing the intrinsic viscosity of polyester. And the ether bond also improves the hygroscopicity of the thermal insulation fiber, which also leads the carboxylate group introduced through the nitrile group to have better hygroscopicity and heat generation property.
Optionally, in the step B1, the graphene oxide is placed in a solvent and then subjected to ultrasonic dispersion, wherein the dispersion temperature is 35-40 ℃, and the ultrasonic time is 15-20min.
By adopting the technical scheme, the graphene oxide can be better dissolved in the solvent by ultrasonic dispersion after being placed in the solvent, so that the graphene oxide is not easy to agglomerate into an agglomerate.
In a second aspect, the present application provides a thermal sock, which adopts the following technical scheme:
a thermal sock is woven by blended yarns, wherein the blended yarns comprise the volcanic thermal fiber.
By adopting the technical scheme, the yarn obtained by blending the volcanic thermal insulation fibers can be lighter and thinner on the premise of ensuring the thermal insulation effect. In addition, volcanic rock powder added in the thermal-insulation yarn has good odor absorbing performance and good sterilization effect, and the added graphene oxide has better sterilization and deodorization performance, so that the thermal-insulation yarn is very suitable for being used as yarn of socks.
Optionally, including socks body and stack shell, socks body and stack shell link to each other, the arch of socks body department is equipped with the shrink circle, the heel department of socks body is equipped with thickening portion, the stack shell includes low pressure section and high pressure section, the low pressure section is located the calf department of stack shell, the high pressure section has two and is located low pressure section both sides, the opening part of stack shell is equipped with the roating.
Through adopting above-mentioned technical scheme, the tight circle of receipts that arch department had can make the socks body higher with the laminating degree of foot, can also further provide the antiskid support of arch portion. The thickening design of the heel department of the sock body not only can provide better buffering shock attenuation effect, can also improve the wear resistance of the heel portion of the sock body. The sectional pressure setting of stack shell department can reduce the stack shell and excessively warp and damage under the prerequisite of guaranteeing stack shell and calf's laminating degree. In addition, the segmented pressure setting can also reduce the impact on leg blood circulation.
In summary, the present application includes at least one of the following beneficial technical effects:
1. far infrared master batches are prepared by adding volcanic rock powder, infrared ceramic powder and graphene oxide into polyester particles in a compounding way, and the far infrared master batches and the polyester master batches are mixed and spun to obtain volcanic rock thermal insulation fibers, so that the volcanic rock thermal insulation fibers have good antibacterial, thermal insulation and deodorizing functions, and the respective dispersing effect can be improved by the volcanic rock powder, the infrared ceramic powder and the graphene oxide in the compounding way, so that defects of the fibers are reduced by people, and the breaking strength of the fibers is improved;
2. the particle size of the infrared ceramic powder can be reduced by activating the infrared ceramic powder, and the dispersion performance of the infrared ceramic powder and the compatibility with polyester particles are improved;
3. through the limitation of the composition and the proportion of the dispersing agent, the composition and the proportion can cooperate to obtain a significantly better dispersing effect, thereby greatly reducing the concentration of the dispersing agent, reducing the cost and increasing the benefit;
4. the graphene oxide is modified, and an acrylonitrile monomer is grafted to the graphene oxide, so that composite powder similar to a core-shell structure is formed, the possibility of graphene oxide agglomeration is reduced, the compatibility of the graphene oxide and polyester particles is improved, and in addition, the modified graphene oxide can enable the finally obtained limit to have a better heating effect;
5. the solvent used for modifying the graphene oxide is limited, so that the stability of the system can be improved, the ether bond of the soft chain segment can be introduced into the polyester system, the temperature during final spinning can be reduced by the introduced ether bond, and the spinnability of the system is improved, thereby reducing the possibility of degradation of the polyester during high-temperature spinning;
6. the yarns formed by blending the volcanic thermal insulation fibers are used as the raw materials of the socks, so that the sock is lighter and thinner on the premise of ensuring the thermal insulation effect;
7. by means of specific design of the structure of the thermal sock, the anti-skidding and shock-absorbing effects of the thermal sock are improved, and the service life of the thermal sock is prolonged.
Drawings
Fig. 1 is a schematic view of the construction of the thermal socks of examples 1 to 18 and comparative examples 1 to 3 of the present application.
Reference numerals illustrate: 1. a sock body; 11. a shrink ring; 12. a thickened portion; 2. a barrel body; 21. a low pressure section; 22. a high pressure section; 23. a rib top.
Detailed Description
The present application is described in further detail below with reference to the drawings, preparations and examples.
The sources of the raw materials in the preparation examples and the examples are shown in the following table:
except for the raw materials in the above table, the other raw materials are all conventionally commercially available except for the specific descriptions.
Preparation example of far infrared master batch
Preparation example 1
In the preparation example, each 1 part of far infrared master batch is prepared, the following raw materials in parts by mass are needed:
as the volcanic rock thermal insulation fiber prepared in the application is finally applied to thermal socks, the inventor selects Cr with equal mass ratio according to actual needs 2 O 3 、ZrO 2 、Si 3 N 4 、TiSi 2 Is a mixture of (a) and (b). It should be noted that the inventor can select the combination of the infrared ceramic powder with different radiation frequency bands according to the requirements of different application scenes.
KH-570 is used as the coupling agent.
The preparation process of the far infrared master batch specifically comprises the following process steps:
firstly, mixing materials, namely weighing polyester particles, infrared ceramic powder, volcanic rock powder and graphene oxide according to the proportion, mixing and stirring at the stirring speed of 500r/min for 15min to obtain the mixture.
And step two, drying, namely heating the mixture in the step one to 140 ℃ for drying, and keeping stirring in the drying process, wherein the stirring speed is 100r/min, and the drying time is 12 hours, so as to obtain the dried material.
And thirdly, extruding and granulating, mixing the drying material and the coupling agent in the second step, and carrying out melt extrusion and water-cooling granulating by using a screw extruder to obtain the far infrared master batch. Wherein, screw temperature of screw extruder sets gradually from one district to ten districts: 160-250-280-280-270 deg.c.
PREPARATION EXAMPLES 2-3
Preparation examples 2 to 3 are different from preparation example 1 in that the proportions of the required raw materials are different for each 1 part of far infrared master batch prepared, and are recorded as the following table:
preparation example 4
Preparation example 4 differs from preparation example 2 in that the infrared ceramic powder is subjected to an activation treatment before the mixing in step one, and specifically includes the steps of:
a1, dispersing, namely putting a dispersing agent into water to be uniformly dispersed, wherein the dispersing agent is sodium tripolyphosphate to obtain a sodium tripolyphosphate solution with the concentration of 45mg/L, then adding infrared ceramic powder with the concentration of 1g/L, and uniformly mixing to obtain a suspension.
A2, activating, namely grinding and activating the suspension obtained in the step A1, wherein the rotating speed of a grinder is 2500r/min, and the grinding time is 70min, so as to obtain an activated liquid.
A3, drying, and spray drying the activation liquid obtained in the step A2 to obtain activated infrared ceramic powder.
The inventors found that under this condition, the suspension obtained in step A1 was able to be kept free from delamination for about 30 days, with excellent dispersion effect.
Preparation example 5
Preparation example 5 differs from preparation example 4 in that in step A1, lysine of equal mass is used instead of sodium tripolyphosphate as a dispersant.
The inventors found that under this condition, the suspension obtained in step A1 was able to be free from delamination for about 10 days, with a good dispersion effect.
Preparation example 6
Preparation example 6 differs from preparation example 4 in that in step A1, the dispersant is a mixture of lysine and sodium tripolyphosphate, and lysine: sodium tripolyphosphate is 1:9, and the final dispersant concentration was 23mg/L.
The inventors found that under this condition, the suspension obtained in step A1 was able to be kept free from delamination for about 30 days, with excellent dispersion effect.
Preparation examples 7 to 8
Preparation examples 7-8 differ from preparation example 6 in that the process parameters in step A1 are different and are noted in the following table:
the inventors found that the suspension obtained in step A1 was able to be kept from delamination for about 27 days under the conditions in preparation example 7, with excellent dispersion effect.
The inventors found that the suspension obtained in step A1 was able to be kept from delamination for about 31 days under the conditions in preparation example 8, with excellent dispersion effect.
In addition, it should be noted that when the concentration of the infrared ceramic powder exceeds 1.2g/L, the suspension obtained in the step A1 has high viscosity, and the grinding machine has poor grinding, so that the production cannot be continued.
Preparation example 9
Preparation example 9 differs from preparation example 2 in that graphene oxide is subjected to modification treatment before mixing in the first step, and specifically includes the following process steps:
b1, dissolving graphene oxide, namely putting the graphene oxide into solvent water, then performing ultrasonic dispersion at 35 ℃ for 20min, wherein the ultrasonic power is 100W, and stopping ultrasonic for 30s every 3min of ultrasonic dispersion in the ultrasonic process to obtain a graphene oxide solution with the concentration of 1 g/L.
And B2, mixing, namely adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture. Wherein, the adding concentration of the acrylonitrile is 1g/L, the alkali is sodium hydroxide, and the adding concentration is 0.5g/L.
And B3, modifying, namely heating the mixture to 95+/-2 ℃ under the protection of inert gas nitrogen atmosphere, carrying out reflux reaction for 24 hours, carrying out suction filtration, washing with DMF (dimethyl formamide), and drying for three times to obtain the modified graphene oxide.
Preparation example 10
The difference between preparation example 10 and preparation example 4 is that graphene oxide is modified before mixing in the first step, and the modification process is the same as preparation example 9, and is not repeated.
PREPARATION EXAMPLE 11
Preparation example 11 is different from preparation example 5 in that graphene oxide is modified before mixing in step one, and the modification process is the same as preparation example 9, and is not repeated.
Preparation example 12
Preparation example 12 is different from preparation example 6 in that graphene oxide is modified before mixing in the first step, and the modification process is the same as preparation example 9, and is not repeated.
Preparation example 13
Preparation example 13 differs from example 12 in that the solvent used in step B1 is a mixture of water and diethylene glycol, and in terms of volume ratio, water: diethylene glycol=9: 1.
preparation examples 14 to 16
Preparation examples 14 to 16 are different from preparation example 13 in that each process parameter in the modification process of graphene oxide is different and is described as the following table:
examples
Example 1
The embodiment of the application firstly discloses volcanic rock thermal insulation fiber, which comprises the following raw materials in parts by mass:
850g of polyester master batch;
150g of far infrared master batch;
the far infrared master batch prepared in preparation example 1 is selected as the far infrared master batch.
The spinning process of the volcanic rock thermal fiber specifically comprises the following process steps:
s1, preparing materials, namely taking polyester master batches according to the proportion, pre-crystallizing for 15min at the temperature of 170 ℃, and drying for 12h at the temperature of 160 ℃ after the pre-crystallization is finished; taking far infrared master batches according to the proportion, drying for 12 hours at 160 ℃, and mixing the dried polyester master batches with the far infrared master batches to obtain the spinning material.
S2, melt extrusion, namely melt extrusion is carried out on the spinning material obtained in the step S1 by using a double-screw extruder, so as to obtain spinning solution. Five zones are altogether adopted in the double-screw extruder, and the screw temperatures from one zone to five zones are sequentially set as follows: 265-275-280-283-285 deg.c.
And S3, filtering and spinning, namely filtering and spinning the spinning solution in the step S2 by using a 35 mu m filter element to obtain semi-finished yarn.
S4, post-treatment, namely sequentially carrying out air blast cooling, oiling, winding and texturing on the semi-finished yarn obtained in the step S3 to obtain the volcanic rock thermal insulation fiber.
Referring to fig. 1, the volcanic rock thermal fiber is applied to manufacturing of thermal socks, the thermal socks are woven by blended yarns, and the blended yarns are obtained by blending 111dtex volcanic rock thermal fibers and 290dtex combed cotton yarns. The thermal sock comprises a sock body 1 and a sock body 2, wherein the sock body 1 and the sock body 2 are sewn or woven into a whole and communicated. The arch of socks body 1 department is equipped with shrink circle 11, and socks body 1's heel department is equipped with thickening portion 12, and barrel 2 includes low pressure section 21 and high pressure section 22, and low pressure section 21 locates barrel 2's calf department, and high pressure section 22 has two and is located the both sides of low pressure section 21 respectively, and barrel 2's opening part is equipped with the roating 23.
Examples 2 to 3
Examples 2-3 differ from example 1 in the raw material composition of the volcanic thermal fiber and are noted in the following table:
examples 4 to 18
Examples 4-18 differ from example 3 in the source of the far infrared masterbatch and are noted in the following table:
it should be noted that the twin-screw extruder of step S2 in examples 15 to 18 has five zones in total, and the screw temperatures from one zone to five zones are set in order as follows: 250-258-263-265-268 deg.c.
Comparative example
Comparative example 1
Comparative example 1 is different from example 1 in that volcanic rock powder is replaced with graphene oxide of equal mass when preparing far infrared master batch.
Comparative example 2
Comparative example 2 is different from example 1 in that the graphene oxide powder was replaced with a volcanic powder of equal mass when preparing the far infrared master batch.
Comparative example 3
Comparative example 3 is a blank control, and is different from example 1 in that the far infrared master batch is replaced with a polyester master batch of equal mass when the far infrared master batch is prepared.
Performance test experiments and data
1. Warming effect and washability
1.1 thermal insulation Effect
1.1.1 moisture absorption and Heat release properties
The thermal socks prepared in each example and comparative example were tested by referring to the method described in GB/T29866-2013 test method for moisture absorption and heating Property of textiles. The test temperature was 20deg.C and the relative humidity was 90%, and average highest temperature elevation data and average temperature elevation data were recorded over 30 min.
1.1.2 Infrared heating Effect
The thermal socks prepared in each example and comparative example were taken, and infrared properties of samples were tested and analyzed with reference to the method described in GB/T30127-2013 detection and evaluation of far infrared properties of textiles.
1.2 resistance to washing with Water
The thermal socks prepared in each example and comparative example were taken, and the samples were washed 50 times by referring to the method (4N washing procedure, hanging and airing) described in GB/T8629-2017 household washing and drying procedure for textile test. And performing performance detection on the washed sample by using two detection methods of 1.1.2 infrared heating effect.
2. Fiber breaking strength
The volcanic rock thermal insulation fibers obtained in each preparation example and each comparative example are taken as samples, and tested according to the method described in the standard GB/T14337-2008 "chemical fiber short fiber tensile property test method".
The test results are shown in the following table:
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conclusion(s)
1. By comparing the dispersion properties of the suspensions obtained in the step A1 in preparation example 4 and preparation example 5, it can be obtained that the dispersion effect of sodium tripolyphosphate on the infrared ceramic powder is significantly better than the dispersion effect of lysine on the infrared ceramic powder at the same concentration. Further comparing the dispersion properties of the suspensions obtained in the step A1 in preparation examples 4 and 6 to 8, it can be obtained that when the dispersant is a mixture of sodium tripolyphosphate and lysine, there is a remarkable synergy in the dispersion effect of the infrared ceramic powder. The compounded dispersing agent can obtain the dispersing effect of 45mg/L of sodium tripolyphosphate alone only by the concentration of 23mg/L.
2. By comparing the breaking strength of the sample fibers of preparation example 4 and preparation example 5, it can be seen that the sodium tripolyphosphate of preparation example 4 has a better dispersion effect on the infrared ceramic powder at the same concentration than the lysine of preparation example 5. Further comparing the breaking strength of the sample fibers of preparation 10 and preparation 11, it was found that the breaking strength of the two samples was substantially the same, whereas preparation 10 was a modification of graphene oxide based on preparation 4, preparation 11 was a modification of graphene oxide based on preparation 5, and preparation 10 and preparation 11 were substantially the same on the premise that the breaking strength of the sample fiber of preparation 4 was higher than that of preparation 5. This is probably because acrylonitrile added in the modification of graphene oxide in preparation example 11 and lysine added in the activation of the infrared ceramic powder in preparation example 5 produce a synergistic effect, and the dispersibility and compatibility of graphene oxide and the infrared ceramic powder are improved.
3. By comparing the breaking strength of the sample fibers of preparation examples 12 and 13, it can be obtained that the dispersibility of graphene oxide can be improved by using a mixed solvent of water and diethylene glycol, as compared with the case where water is directly used as the solvent for modifying graphene oxide.
4. By comparing the process parameters of example 14 and examples 15-18, it can be seen that the use of a mixed solvent of water and diethylene glycol results in a reduction in the final spinning temperature of about 10 ℃ or more when graphene oxide is modified, as compared to the use of pure solvent water. This is probably due to the fact that diethylene glycol introduced during the modification of graphene oxide can react with acrylonitrile introduced during the activation of the infrared ceramic powder to generate soft segment ether bonds, thereby improving the rheological properties of the polyester system.
5. From the experimental data of comparative example 1, comparative example 1 and comparative examples 1 to 3, it can be obtained that graphene oxide has significantly better infrared heating performance than infrared ceramic powder, and correspondingly, graphene oxide has a larger influence on the breaking strength of fibers. While infrared ceramic powder has weaker infrared heating effect than graphene oxide, the influence on the breaking strength of the fiber is obviously smaller. On the premise that the volcanic rock powder exists, the infrared ceramic powder and the graphene oxide are compounded, so that the influence of the graphene oxide on the fiber breaking strength can be obviously reduced (the difference of the fiber breaking strength of samples in preparation example 1 and comparative example 2 is small, and the preparation example 1 is compared with the comparative example 2 in which the graphene oxide is added), and the effect of synergetic dispersion among the volcanic rock powder, the graphene oxide and the infrared ceramic powder is demonstrated.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (7)
1. The utility model provides a volcanic rock thermal fiber which characterized in that: comprises the following raw materials in percentage by mass:
85-90% of polyester master batch;
10-15% of far infrared master batch;
the far infrared master batch is prepared from the following raw materials in parts by mass:
100 parts of polyester particles;
50-60 parts of infrared ceramic powder;
5-10 parts of volcanic rock powder;
5-8 parts of graphene oxide;
3-5 parts of a coupling agent;
the infrared ceramic powder is Al 2 O 3 、TiO 2 、SiO 2 、Cr 2 O 3 、ZrO 2 、B 4 C、SiC、ZrC、BN、AlN、Si 3 N 4 、TiN、TiSi 2 、WSi 2 、ZrB 2 、CrB 2 A mixture of at least two of (a) and (b);
the infrared ceramic powder is subjected to activation treatment before use, and comprises the following steps:
a1, dispersing, namely firstly putting a dispersing agent into water to be uniformly dispersed, then adding infrared ceramic powder, and uniformly mixing to obtain a suspension;
a2, activating, namely grinding and activating the suspension obtained in the step A1 to obtain an activated liquid;
a3, drying, namely spray drying the activation liquid obtained in the step A2 to obtain activated infrared ceramic powder;
the dispersing agent is prepared from lysine and sodium tripolyphosphate according to the mass ratio of 1: (8-10) mixing.
2. A volcanic thermal fiber as claimed in claim 1, wherein: in the step A1, the concentration of the dispersing agent is 20-25mg/L, and the concentration of the infrared ceramic powder is 0.8-1.2g/L.
3. A volcanic thermal fiber as claimed in claim 1, wherein: the graphene oxide is modified before being added, and specifically comprises the following steps:
b1, dissolving graphene oxide, namely putting the graphene oxide into a solvent for uniform dispersion to obtain a graphene oxide solution;
b2, mixing, namely adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture;
and B3, modifying, namely heating the mixture to 95+/-2 ℃ under the protection of inert gas atmosphere, carrying out reflux reaction, and then filtering and washing to obtain the modified graphene oxide.
4. A volcanic thermal fiber according to claim 3 wherein: the solvent used in the step B1 is a mixture of water and diethylene glycol, and the volume ratio of water is as follows: diethylene glycol= (8-10): 1.
5. a volcanic thermal fiber according to claim 3 wherein: and B1, placing graphene oxide into a solvent, and performing ultrasonic dispersion, wherein the dispersion temperature is 35-40 ℃ and the ultrasonic time is 15-20min.
6. A thermal sock, characterized in that: woven from a blend yarn comprising the volcanic thermal fiber of any one of claims 1-5.
7. A thermal sock according to claim 6, wherein: including socks body (1) and stack shell (2), socks body (1) and stack shell (2) link to each other, the arch of socks body (1) department is equipped with shrink circle (11), the heel department of socks body (1) is equipped with thickening portion (12), stack shell (2) include low pressure section (21) and high pressure section (22), low pressure section (21) are located claim 3 stack shell (2) calf department, high pressure section (22) have two and are located low pressure section (21) both sides, the opening part of stack shell (2) is equipped with roar (23).
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