CN113943982A - Volcanic rock thermal fiber and thermal socks - Google Patents
Volcanic rock thermal fiber and thermal socks Download PDFInfo
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- CN113943982A CN113943982A CN202111293045.9A CN202111293045A CN113943982A CN 113943982 A CN113943982 A CN 113943982A CN 202111293045 A CN202111293045 A CN 202111293045A CN 113943982 A CN113943982 A CN 113943982A
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- graphene oxide
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- ceramic powder
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- infrared ceramic
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Images
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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The application relates to volcanic rock thermal fibers and thermal socks, and belongs to the technical field of special functional fabrics. The application firstly discloses a volcanic fiber, and the raw materials of the volcanic fiber comprise polyester master batches and far infrared master batches, the far infrared master batches are prepared from at least 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 application further discloses warm-keeping socks which are woven by blended yarns, wherein the blended yarns comprise the volcanic warm-keeping fibers. This application has cold-proof effectual and effect of resistant washing.
Description
Technical Field
The application relates to the field of special functional fabrics, in particular to volcanic rock thermal fibers and thermal socks.
Background
The foot is a weak position in the blood circulation process and is very easily influenced by the ambient temperature, and the foot is very easily cooled in winter. At present, the most common foot warm-keeping mode is to wear thicker socks, although the thicker socks have better warm-keeping effect, the too thick socks have poorer foot feeling, and because the size of the shoes of consumers is fixed, the feet can be pressed by the thick socks to influence the blood circulation of the feet.
With the development of society and the improvement of economic level, the performance requirements of consumers on various textiles are increasingly improved, and the increasing requirements of consumers on fabrics with the warm-keeping performance improved by simply increasing the thickness are difficult to meet. Therefore, if the fabric which is light and thin and has good warm keeping effect is prepared, the preparation method is a great research direction of the current functional textile fabric.
At present, after finishing is generally adopted for preparing special functional fabrics with warm-keeping and heating effects, namely, special auxiliaries with heat storage and heating capacities are finished on the fabrics through a finishing process, so that the light and thin fabrics have good warm-keeping effects. However, although the fabric obtained by the auxiliary post-finishing has good heat retention performance at first, the fabric is not resistant to washing, and the heat retention performance of the fabric after multiple washing is often reduced greatly.
Disclosure of Invention
In order to overcome the defect that the existing common after-finishing auxiliary agent for preparing the thermal fabric is not washable, the application provides volcanic thermal fiber and thermal socks.
In a first aspect, the application provides a volcanic rock thermal fiber, which adopts the following technical scheme:
a volcanic rock thermal 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 at least the following raw materials in parts by mass:
by adopting the technical scheme, compared with the common post-finishing process, the infrared ceramic powder, the volcanic rock powder and the graphene oxide with the far infrared emission function are made into the far infrared master batches, the conventional polyester master batches and the far infrared master batches are mixed during spinning, and the prepared thermal fiber has the intrinsic far infrared emission function. The far infrared emission function of the volcanic thermal fiber prepared by the method can still keep a higher level no matter how many times the volcanic thermal fiber is washed; correspondingly, the common researches at present show that after 50 times of water washing, the heating fiber prepared by the conventional after-finishing process almost loses the heating performance.
The infrared ceramic powder or the volcanic rock has good far infrared emission performance, wherein minerals and trace elements of the volcanic rock easily absorb heat and convert the absorbed heat into infrared rays; in addition, the volcanic rock can reflect infrared radiation generated by a human body; the infrared rays can be heated up under the action of water molecules in a human body, so that the active warm-keeping effect is achieved. In addition, the volcanic rock has an irregular porous structure, so that a large amount of static air can be adsorbed, the heat conductivity coefficient of the static air is only about 0.025W/(m ℃) and is far lower than that of the polyester fiber, and therefore, the volcanic rock with the porous structure is added into the polyester fiber to generate good heat storage capacity.
The inventor finds that the heat storage and temperature rise effects of the graphene oxide are superior to those of volcanic rocks and common infrared ceramics, but the graphene oxide serving as a nano material is easy to agglomerate, so that a spinneret plate is easy to block, fiber defects are easy to cause, and the breaking strength of the fibers is reduced. The inventor finds that the fracture strength of the fiber can be remarkably improved by mixing the graphene oxide, the infrared ceramic powder and the volcanic rock powder. The reason for this is probably that the infrared ceramic powder can be inserted between the flaky graphene oxides to improve the steric hindrance of the graphene oxides, and the porous volcanic rock powder can adsorb the graphene oxides and the infrared ceramic powder and arrange the graphene oxides and the infrared ceramic powder around the volcanic rock powder more orderly, so that the fiber defects are reduced, and the breaking strength of the fibers is improved.
Optionally, the infrared ceramic powder is Al2O3、TiO2、SiO2、Cr2O3、ZrO2、B4C、SiC、ZrC、BN、AlN、Si3N4、TiN、TiSi2、WSi2、ZrB2、CrB2A mixture of at least two of (a).
By adopting the technical scheme, different infrared ceramic powders have different far infrared emission frequency bands, and at least more than two kinds of infrared ceramic powders can be selected in order to ensure that the far infrared emission frequency bands are more complete. In addition, the skilled person can select the required infrared ceramic powder according to the infrared emission frequency bands of different infrared ceramic powders and the design of the actual product.
Optionally, the infrared ceramic powder is activated before use, and includes the following steps:
a1, dispersing, namely firstly, putting a dispersing agent into water for uniform dispersion, then adding the 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 solution;
and A3, drying, namely spray drying the activating solution obtained in the step A2 to obtain the activated infrared ceramic powder.
By adopting the technical scheme, hydroxyl with stronger hydrophilicity is often easily formed on the surface of the infrared ceramic powder, and the surface free energy is reduced due to overlarge specific surface area, so that the ceramic powder is easily agglomerated. These agglomerates are often several tens of times larger than the primary particles, and therefore, prior to using the infrared ceramic powder, it is necessary to activate the infrared ceramic powder for dispersion, thereby reducing the influence of these agglomerates on the fiber properties.
The dispersion performance of the infrared ceramic powder can be greatly improved by adopting a mode of dispersing, grinding, activating and spray drying. The added dispersing agent can reduce the possibility of agglomeration of the infrared ceramic powder, improve the compatibility of the infrared ceramic powder and polyester particles, improve the mutual bonding force of the infrared ceramic powder and the polyester, increase the fluidity of a melt and improve the spinnability.
Optionally, the dispersing agent is prepared from 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 generally, the sodium tripolyphosphate has better dispersibility under an alkaline condition. At present, a common mode is to add strong base such as sodium hydroxide in a 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, step a3 is a spray drying method, which can omit the subsequent grinding steps, but can leave sodium tripolyphosphate and alkaline substances on the far infrared ceramic powder. However, the polyester contained in the system is easily decomposed to form internal damage under the action of strong alkali such as sodium hydroxide, so that the system cannot use strong alkali such as sodium hydroxide.
According to the application, lysine is specifically added into the dispersing agent and is basic amino acid, so that the dispersing effect of sodium tripolyphosphate can be improved, and in addition, the lysine is also positively charged after self ionization and can be adsorbed to the surface of the infrared ceramic powder so as to further improve the charge amount on the surface of the infrared ceramic powder and further improve the dispersing effect of the infrared ceramic powder.
Optionally, in the step a1, the concentration of the dispersant is 20 to 25mg/L, and the concentration of the infrared ceramic powder is 0.8 to 1.2 g/L.
Through the technical scheme, the inventor finds that sodium tripolyphosphate has a good dispersing effect on the infrared ceramic powder, but after part of the sodium tripolyphosphate is replaced by lysine, the effect of the dispersing agent is remarkably improved, and on the basis of ensuring the whole dispersing effect, the using amount of the dispersing agent can be reduced from about 40-50mg/L to about 20-25 mg/L.
In addition, the concentration of the infrared ceramic powder needs to be strictly controlled, because different suspension concentrations affect the final crushing effect, so that the finally obtained activated infrared ceramic powder has different particle sizes. If the concentration of the suspension is too high, problems such as too poor fluidity and a low circulation rate tend to occur during the polishing.
Optionally, the graphene oxide is modified before being added, and specifically includes the following steps:
b1, dissolving graphene oxide, namely putting the graphene oxide into a solvent to be uniformly dispersed to obtain a graphene oxide solution;
b2, mixing materials, namely adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture;
and B3, modifying, heating the mixture to 95 +/-2 under the protection of inert gas atmosphere, carrying out reflux reaction, and filtering and washing to obtain the modified graphene oxide.
By adopting the technical scheme, acrylonitrile is easy to perform addition reaction with a compound containing active hydrogen atoms, and under the alkaline condition, the acrylonitrile can react with oxygen-containing groups on the surface of graphene oxide so as to be grafted onto the graphene oxide to form composite powder similar to a core-shell structure, so that the compatibility of the graphene oxide and polyester particles is greatly improved. It should be noted that since the modified graphene oxide needs to be washed, in step B2, it is finally eluted even if a strong base such as sodium hydroxide is added, and thus, there is no need to consider its effect on the properties of the polyester.
In addition, the inventors surprisingly found that compared with the addition of unmodified graphene oxide, the addition of modified graphene oxide can enable the finally prepared thermal fibers to have a significantly better warming effect. The reason for this is probably that acrylonitrile is mixed into polyester after being grafted to graphene oxide, and in the subsequent finishing process, such as the alkali weight reduction process, the nitrile group is converted into carboxylate with moisture absorption and heat generation properties, so that the thermal fiber has a better heating effect.
In addition, the inventors found that mixing the modified graphene oxide with the activated infrared ceramic powder has significantly better compatibility than mixing the modified graphene oxide with the unactivated infrared ceramic powder. The reason is probably that the activated infrared ceramic powder has lysine, and the lysine has active hydrogen and can react with acrylonitrile on the modified graphene oxide, so that the activated infrared ceramic powder, the modified graphene oxide, the polyester particles and the like have good compatibility.
Optionally, the solvent used in step B1 is a mixture of water and diethylene glycol, and the ratio by volume of water: 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 turns black from faint yellow along with the modification, which means that the graphene oxide is gradually reduced. The reduced graphene oxide exhibits a certain hydrophobicity, and thus, the reduced graphene oxide is easily agglomerated. And the mixed solvent obtained by adding a certain amount of diethylene glycol into water can improve the stability of the graphene oxide and the reduced graphene oxide and reduce the possibility of agglomeration of the graphene oxide and the reduced graphene oxide.
It should be noted that, although the maximum temperature of extrusion granulation temperature of polyester is generally about 270 ℃, the addition of infrared ceramic powder, volcanic rock powder and graphene oxide at a high content increases the apparent viscosity of the melt, decreases the fluidity, and makes the melt difficult to flow during melt extrusion. In order to increase the fluidity of the melt, it is necessary to increase the spinning temperature to about 280 ℃, but the increase in the spinning temperature easily causes degradation of the polyester.
However, the inventors have surprisingly found that the addition of diethylene glycol to water not only improves the stability of the overall system, but also improves the rheology of the melt, thereby lowering the final spinning temperature and improving spinnability. This is probably because acrylonitrile and diethylene glycol can form polyether nitrile under alkaline conditions, polyether nitrile introduces ether bond in polyester, and introduction of ether bond improves flexibility of polyester, entropy change is increased in melting process, so that melting point of polyester is reduced, and low temperature spinnability is improved on the basis of ensuring intrinsic viscosity of polyester. And the ether bond also improves the moisture absorption of the thermal fiber, which leads the carboxylate group introduced by the nitrile group to have better moisture absorption and heat generation.
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 15-20 min.
By adopting the technical scheme, the graphene oxide can be better dissolved in the solvent by ultrasonic dispersion after being put into the solvent, and is not easy to agglomerate into aggregates.
In a second aspect, the application provides a pair of warm-keeping socks, which adopts the following technical scheme:
a warm-keeping sock is woven by blended yarns, and the blended yarns comprise the volcanic warm-keeping fibers.
By adopting the technical scheme, the yarns obtained by blending the volcanic thermal fibers can be thinner and thinner on the premise of ensuring the thermal effect. In addition, the volcanic rock powder added into the warm-keeping yarns has good odor absorption performance and good sterilization effect, and the added graphene oxide has better sterilization and deodorization performance, so that the yarn is very suitable for being used as yarns of socks.
Optionally, including the socks body and stack shell, the socks body and stack shell link to each other, the arch of foot department of the socks body is equipped with the shrink ring, the heel department of the 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 rid cuff.
Through adopting above-mentioned technical scheme, the tight circle of tightening that arch of foot department has can make the socks body higher with the laminating degree of foot, can also further provide the anti-skidding support of arch of foot portion. The thickening design of the heel department of the socks body not only can provide better buffering shock attenuation effect, can also improve the wear resistance of socks body heel. The segmentation pressure setting of stack shell department can reduce the possibility that the stack shell excessively deforms and damages under the prerequisite of guaranteeing the laminating degree of stack shell with the calf. 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. the volcanic rock powder, the infrared ceramic powder and the graphene oxide are compounded and added into the polyester particles to prepare the far infrared master batch, and the far infrared master batch and the polyester master batch are mixed and spun to obtain the volcanic rock thermal fiber, so that the volcanic rock thermal fiber has good antibacterial, thermal and deodorizing functions, and the volcanic rock powder, the infrared ceramic powder and the graphene oxide are compounded to improve respective dispersing effects, so that the defects of the fiber are reduced, and the breaking strength of the fiber is improved;
2. by activating the infrared ceramic powder, the particle size of the infrared ceramic powder can be reduced, and the dispersion performance of the infrared ceramic powder and the compatibility with polyester particles are improved;
3. by limiting the composition and the proportion of the dispersing agent, the dispersing agent and the dispersing agent are cooperated to obtain a remarkably better dispersing effect, so that the concentration of the dispersing agent can be greatly reduced, the cost is reduced, and the benefit is increased;
4. the modified graphene oxide is subjected to modification treatment, 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 temperature rise effect;
5. by limiting the solvent during the modification of the graphene oxide, the stability of the system can be improved, ether bonds of soft chain segments can be introduced into the polyester system, and the introduced ether bonds can reduce the temperature during final spinning and improve the spinnability of the system, so that the possibility of degradation of the polyester during high-temperature spinning is reduced;
6. yarns formed by blending volcanic thermal fibers are used as raw materials of the socks, so that the socks are lighter and thinner on the premise of ensuring the thermal effect;
7. the anti-skid and damping effects of the warm-keeping socks are improved by specially designing the structure of the warm-keeping socks, and the service life of the warm-keeping socks is prolonged.
Drawings
Fig. 1 is a schematic view showing the structure of warm socks according to examples 1 to 18 and comparative examples 1 to 3 of the present application.
Description of reference numerals: 1. a sock body; 11. a contraction ring; 12. thickening part; 2. a barrel body; 21. a low-pressure section; 22. a high pressure section; 23. and (4) a rib top.
Detailed Description
The present application will be described in further detail with reference to the drawings, preparation examples and examples.
The raw material sources in the preparation examples and examples of the application are shown as the following table:
except for the raw materials in the table above, the other raw materials are all conventionally sold on the market except for special description.
Preparation example of far Infrared mother particle
Preparation example 1
In the preparation example, every 1 part of the far infrared master batch is prepared from the following raw materials in parts by mass:
because the volcanic thermal fibers prepared in the application are finally applied to thermal socks, the inventor selects Cr with equal mass ratio to the infrared ceramic powder according to actual needs2O3、ZrO2、Si3N4、TiSi2A mixture of (a). It should be noted that the inventor can select the infrared ceramic powder combinations with different radiation frequency bands according to the requirements of different application scenarios.
KH-570 is selected as the coupling agent.
The preparation process of the far infrared master batch specifically comprises the following process steps:
step one, 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 a mixture.
And step two, drying, namely heating the mixture obtained 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 12h, so as to obtain a dried material.
And step three, extruding and granulating, namely mixing the dried material obtained in the step two with a coupling agent, performing melt extrusion by using a screw extruder, and performing water cooling and granulation to obtain the far infrared master batch. Wherein the screw temperature of the screw extruder is sequentially set from one zone to ten zones as follows: 160-250-280-270 ℃.
Preparation examples 2 to 3
The difference between the preparation examples 2-3 and the preparation example 1 is that the mixture ratio of the required raw materials is different for each 1 part of far infrared master batch, and the mixture ratio is shown as the following table:
preparation example 4
The difference between the preparation example 4 and the preparation example 2 is that the infrared ceramic powder is subjected to activation treatment before the first step of mixing, and the method specifically comprises the following steps:
and A1, dispersing, namely firstly, 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.
And A2, activating, namely grinding and activating the suspension obtained in the step A1, wherein the rotation speed of a grinding machine is 2500r/min, and the grinding time is 70min, so that an activation solution is obtained.
And A3, drying, namely spray drying the activating solution obtained in the step A2 to obtain the activated infrared ceramic powder.
The inventors found that under these conditions, the suspension obtained in step A1 could be maintained without delamination for about 30 days, and had excellent dispersing effect.
Preparation example 5
Preparation example 5 differs from preparation example 4 in that in step a1, an equal mass of lysine was used instead of sodium tripolyphosphate as the dispersing agent.
The inventors have found that under these conditions, the suspension obtained in step a1 does not delaminate in about 10 days, and has a good dispersing 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 the ratio by mass of lysine: sodium tripolyphosphate is 1: 9 and the concentration of the final dispersant was 23 mg/L.
The inventors found that under these conditions, the suspension obtained in step A1 could be maintained without delamination for about 30 days, and had excellent dispersing effect.
Preparation examples 7 to 8
Preparations 7 to 8 differ from preparation 6 in the process parameters of step A1 and are shown in the following table:
the inventors found that the suspension obtained in step a1 could be maintained without delamination for about 27 days under the conditions in preparation example 7, and had an excellent dispersing effect.
The inventors found that the suspension obtained in step a1 could be maintained without delamination for about 31 days under the conditions in preparation example 8, and had an excellent dispersing effect.
In addition, it should be noted that when the concentration of the infrared ceramic powder exceeds 1.2g/L, the viscosity of the suspension obtained in step A1 is high, and the grinding machine may not grind smoothly, so that the production cannot be continued.
Preparation example 9
The difference between the preparation example 9 and the preparation example 2 is that the graphene oxide is subjected to modification treatment before the material mixing in the first step, and the method specifically comprises the following process steps:
and B1, dissolving graphene oxide, namely putting the graphene oxide into solvent water, then performing ultrasonic dispersion at the temperature of 35 ℃ for 20min, wherein the ultrasonic power is 100W, and in the ultrasonic process, stopping performing ultrasonic dispersion for 30s every 3min to obtain a graphene oxide solution with the concentration of 1 g/L.
And B2, mixing materials, and adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture. Wherein the addition concentration of acrylonitrile is 1g/L, and the alkali is sodium hydroxide and the addition concentration is 0.5 g/L.
And B3, modifying, heating the mixture to 95 +/-2 ℃ under the protection of inert gas nitrogen atmosphere, carrying out reflux reaction for 24 hours, then carrying out suction filtration, washing with DMF (dimethyl formamide) for three times, and drying to obtain the modified graphene oxide.
Preparation example 10
The difference between preparation example 10 and preparation example 4 is that the graphene oxide is subjected to modification treatment before the material mixing in step one, and the modification process is the same as that in preparation example 9, and is not described again.
Preparation example 11
The difference between preparation example 11 and preparation example 5 is that the graphene oxide is subjected to modification treatment before the first step of mixing, and the modification process is the same as that of preparation example 9 and is not described again.
Preparation example 12
The difference between preparation example 12 and preparation example 6 is that the graphene oxide is subjected to modification treatment before the first step of mixing, and the modification process is the same as that of preparation example 9 and is not described again.
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 the ratio by volume of water: diethylene glycol ═ 9: 1.
preparation examples 14 to 16
Preparation examples 14 to 16 are different from preparation example 13 in that the process parameters in the modification process of graphene oxide are different, and are shown as follows:
examples
Example 1
The embodiment of the application firstly discloses volcanic thermal insulation fiber, and the following raw materials in parts by mass are required for preparing one part of fiber:
850g of polyester master batch;
150g of far infrared master batch;
the far infrared mother particle prepared in preparation example 1 is selected as the far infrared mother particle.
The spinning process of the volcanic thermal fiber specifically comprises the following process steps:
s1, preparing materials, namely taking the polyester master batch 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; and (3) taking the far infrared master batch according to the proportion, drying the far infrared master batch at the temperature of 160 ℃ for 12 hours, and mixing the dried polyester master batch and the far infrared master batch to obtain the spinning material.
And S2, melt extrusion, wherein the spinning material obtained in the step S1 is melt extruded by a double-screw extruder to obtain a spinning solution. The double-screw extruder has five zones, and the screw temperatures of the first zone to the fifth zone are sequentially set as follows: 265-275-280-283-285 ℃.
And S3, filtering and spinning, namely filtering the spinning solution in the step S2 by using a 35-micrometer filter element and spinning to obtain semi-finished yarn.
And S4, post-processing, namely, sequentially carrying out air blowing cooling, oiling, winding and elasticizing on the semi-finished product yarn obtained in the step S3 to obtain the volcanic thermal fiber.
Referring to fig. 1, the volcanic 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 thermal fiber and 290dtex combed cotton yarn. The warm-keeping sock comprises a sock body 1 and a leg body 2, wherein the sock body 1 and the leg body 2 are sewn or woven into a whole and are communicated. The arch of foot department of the socks body 1 is equipped with shrink ring 11, and the heel department of the socks body 1 is equipped with thickening portion 12, and stack shell 2 includes low pressure section 21 and high pressure section 22, and the calf department of stack shell 2 is located to low pressure section 21, and high pressure section 22 has two and is located the both sides of low pressure section 21 respectively, and the opening part of stack shell 2 is equipped with rid of the mouth 23.
Examples 2 to 3
Examples 2-3 differ from example 1 in the composition of the starting material of the volcanic thermal fibers and are shown in the following table:
examples 4 to 18
Examples 4 to 18 differ from example 3 in the source of the far infrared mother particle and are shown in the following table:
it is to be noted that the twin-screw extruder of step S2 in examples 15 to 18 had five zones, and the screw temperatures in the first zone to the five zones were set in this order: 250-258-263-265-268 ℃.
Comparative example
Comparative example 1
The difference between the comparative example 1 and the example 1 is that volcanic rock powder is replaced by graphene oxide with equal mass when preparing the far infrared master batch.
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the graphene oxide powder is replaced by equal-quality volcanic rock powder 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 mother particle is replaced with the polyester mother particle of the same mass when the far-infrared mother particle is prepared.
Performance test experiments and data
1. Warming effect and washing resistance
1.1 warming effect
1.1.1 moisture absorption exothermicity
The warm-keeping socks prepared in each embodiment and each comparative example are taken and tested according to the method recorded in GB/T29866-2013 method for testing the moisture absorption and heat generation performance of textiles. The test temperature is 20 ℃, the relative humidity is 90%, and the average maximum temperature rise data and the average temperature rise data within 30min are recorded.
1.1.2 Infrared heating Effect
The warm-keeping socks prepared in each embodiment and comparative example are taken, and the infrared performance of the sample is tested and analyzed according to the method recorded in GB/T30127-.
1.2 Water Wash resistance
The warm socks prepared in each example and comparative example were taken, and the samples were washed for 50 times by referring to the method (4N washing procedure, suspended drying) described in GB/T8629-2017 Home washing and drying procedure for textile testing. And (3) carrying out performance detection on the washed sample by using two detection methods of 1.1.2 infrared heating effect.
2. Breaking strength of fiber
The volcanic thermal fibers obtained in each preparation example and each proportion are taken as samples and tested according to the method recorded in GB/T14337-.
The results of the various tests are reported in the following table:
conclusion
1. By comparing the dispersing performance of the suspensions obtained in the step a1 in the preparation examples 4 and 5, it can be found that, at the same concentration, the dispersing effect of sodium tripolyphosphate on the infrared ceramic powder is obviously better than that of lysine on the infrared ceramic powder. Further comparing the dispersing performance of the suspensions obtained in the step a1 in preparation example 4 and preparation examples 6 to 8, it can be seen that when the dispersing agent is a mixture of sodium tripolyphosphate and lysine, there is a significant synergistic effect on the dispersing effect of the infrared ceramic powder. The compound dispersing agent only needs 23mg/L concentration to obtain the dispersing effect which can be achieved by 45mg/L of single sodium tripolyphosphate.
2. By comparing the breaking strength of the fibers of the samples of preparation example 4 and preparation example 5, it can be shown that the sodium tripolyphosphate in preparation example 4 has better dispersion effect on the infrared ceramic powder than the lysine in preparation example 5 under the same concentration. Further comparing the breaking strength of the sample fibers of preparation example 10 and preparation example 11, the breaking strength of the two samples is substantially the same, whereas preparation example 10 modifies graphene oxide on the basis of preparation example 4, preparation example 11 modifies graphene oxide on the basis of preparation example 5, and the breaking strength of the sample fibers of preparation example 4 is substantially the same as that of preparation example 11 on the premise that the breaking strength of the sample fibers of preparation example 5 is higher than that of the sample fibers of preparation example 10. This is probably because the acrylonitrile added in the modified graphene oxide in preparation example 11 and the lysine added in the infrared ceramic powder activation in preparation example 5 produce a synergistic effect, and the dispersibility and compatibility of the graphene oxide and the infrared ceramic powder are improved.
3. By comparing the breaking strengths of the fibers of the samples of preparation examples 12 and 13, it can be seen that the dispersibility of graphene oxide can be improved by using a mixed solvent of water and diethylene glycol, compared to directly using water as a solvent for modifying graphene oxide.
4. By comparing the process parameters of example 14 and examples 15 to 18, it can be seen that the final spinning temperature can be reduced by about 10 ℃ or more when modifying graphene oxide, compared to when using a single solvent, water, or a mixed solvent of water and diethylene glycol. This is probably because the diethylene glycol introduced during the modification of graphene oxide can react with the acrylonitrile introduced during the activation of the infrared ceramic powder to generate soft chain segment ether bonds, thereby improving the rheological properties of the polyester system.
5. By comparing the experimental data of example 1, comparative example 1 and comparative examples 1 to 3, it can be shown that, compared with the infrared ceramic powder, graphene oxide has a significantly better infrared heating performance, and correspondingly, graphene oxide has a greater influence on the breaking strength of the fiber. Although the infrared heating effect of the infrared ceramic powder is weaker than that of graphene oxide, the influence of the infrared ceramic powder on the breaking strength of the fiber is obviously smaller. Under the premise of existence of volcanic rock powder, infrared ceramic powder and graphene oxide are compounded, so that the influence of the graphene oxide on the fiber fracture strength can be obviously reduced (the fiber fracture strength difference of the samples of the preparation example 1 and the comparative example 2 is very small, and the graphene oxide is added in the preparation example 1 compared with the comparative example 2), which shows that the volcanic rock powder, the graphene oxide and the infrared ceramic powder have the synergistic dispersion effect.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A volcanic rock thermal fiber is characterized in that: the material 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 at least the following raw materials in parts by mass:
2. the volcanic thermal fiber as claimed in claim 1, wherein: the infrared ceramic powder is Al2O3、TiO2、SiO2、Cr2O3、ZrO2、B4C、SiC、ZrC、BN、AlN、Si3N4、TiN、TiSi2、WSi2、ZrB2、CrB2A mixture of at least two of (a).
3. The volcanic thermal fiber as claimed in claim 2, wherein: the infrared ceramic powder is activated before use and comprises the following steps:
a1, dispersing, namely firstly, putting a dispersing agent into water for uniform dispersion, then adding the 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 solution;
and A3, drying, namely spray drying the activating solution obtained in the step A2 to obtain the activated infrared ceramic powder.
4. A volcanic rock thermal fiber as claimed in claim 3, wherein: the dispersing agent is prepared from lysine and sodium tripolyphosphate according to a mass ratio of 1: (8-10) mixing.
5. A volcanic rock thermal fiber as claimed in claim 3 or 4, wherein: in the step A1, the concentration of the dispersing agent is 20-25mg/L, and the concentration of the infrared ceramic powder is 0.8-1.2 g/L.
6. The volcanic thermal fiber as claimed in claim 1, wherein: the graphene oxide is modified before being added, and the method specifically comprises the following steps:
b1, dissolving graphene oxide, namely putting the graphene oxide into a solvent to be uniformly dispersed to obtain a graphene oxide solution;
b2, mixing materials, namely adding acrylonitrile and alkali into the graphene oxide solution obtained in the step B1 to obtain a mixture;
and B3, modifying, 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.
7. The volcanic thermal fiber as claimed in claim 6, wherein: the solvent used in the step B1 is a mixture of water and diethylene glycol, and the volume ratio of water: diethylene glycol ═ (8-10): 1.
8. a volcanic rock thermal fiber as claimed in claim 6 or 7, wherein: and B1, placing the graphene oxide into a solvent, and then performing ultrasonic dispersion at 35-40 ℃ for 15-20 min.
9. A kind of warm socks, its characteristic is: is woven from a blended yarn comprising volcanic thermal fibers as recited in any of claims 1-8.
10. A thermal sock according to claim 9, wherein: including the socks body (1) and stack shell (2), the socks body (1) and stack shell (2) link to each other, the arch of foot department of the socks body (1) is equipped with shrink ring (11), the heel department of the socks body (1) is equipped with thickening portion (12), stack shell (2) are including low pressure section (21) and high pressure section (22), low pressure section (21) are located the calf department of stack shell (2), 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 rid cuff (23).
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