Preparation process of textile fabric capable of releasing far infrared rays and negative ions based on natural raw ores

Abstract

The invention discloses a preparation process of a textile fabric capable of releasing far infrared rays and negative ions based on natural raw ores, and belongs to the technical field of textile fabric processes, the preparation process comprises the following steps: 1, selecting ores with natural far infrared ray emission capability and negative ion release capability as raw material raw ores, and crushing the raw material raw ores by adopting crushing equipment to obtain crushed ores; the particle size of the crushed mineral powder is 40-60 nanometers; 2, mixing mineral powder with the particle size of 40-60 nanometers with a fiber raw material, carrying out blending treatment in a high-temperature molten state, and then carrying out extrusion pelletizing, so as to obtain mineral fiber composite master batches; according to the invention, nano-scale ore powder is subjected to in-situ compounding in a fiber melt spinning stage, so that functional factors are permanently wrapped and consolidated in the fiber instead of being attached to the surface. Natural raw ores are used, so that the finished cloth does not contain chemical residual substances such as formaldehyde and benzene, and allergic stimulation problems such as swelling and itching cannot be caused when the cloth is in contact with human skin for a long time.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of textile cloth process, in particular to a textile cloth preparation process based on natural ore for releasing far infrared rays and negative ions. BACKGROUND

[0002] With the popularization of health consumption concept, the textile cloth with far infrared ray emission and negative ion release function is widely used in close-fitting clothes, home textile products, health protection equipment and other fields due to its advantages in warmth retention and improvement of local microenvironment.

[0003] At present, the mainstream far infrared and negative ion textile cloth on the market generally relies on chemical synthesis finishing process to realize its function, that is, by means of coating, dipping, printing and other means, the artificially synthesized ceramic powder and other chemical synthesized far infrared ray emitters and negative ion generators are attached to the surface of the fabric to endow the fabric with corresponding functions.

[0004] In the traditional process, the chemical functional agent is only attached to the surface layer of the fabric through physical adhesion or shallow bonding, and does not form deep fusion with the fabric fibers. During daily use, the functional agent is easy to fall off and lose from the surface of the fabric after repeated washing, rubbing or long-term placement, resulting in rapid attenuation of far infrared emission efficiency and negative ion release amount. Usually, the function will decrease significantly or even completely fail after 5-10 times of washing, and the functional life is short.

[0005] In addition, although some technologies attempt to add functional powder to the spinning melt or solution before spinning for blending spinning, if the powder particle size is not properly controlled or the dispersion process is not good, it is easy to cause the spinning plate to be blocked, the fiber breakage rate to increase, and the functional components to be easily agglomerated in the fiber, affecting the function and spinning stability.

[0006] Therefore, we propose a textile cloth preparation process based on natural ore for releasing far infrared rays and negative ions to solve the above problems.

[0007] The above information disclosed in the background of the application is only used to increase the understanding of the background of the application, and therefore, it can include prior art known by those skilled in the art. SUMMARY

[0008] The present application aims to provide a textile cloth preparation process based on natural ore for releasing far infrared rays and negative ions to solve the problem that the current preparation technology relies on chemical synthesis finishing process, resulting in easy attenuation of function, and the blending spinning has the problems of spinning plate blockage, fiber breakage and functional component agglomeration due to improper control of powder particle size or poor dispersion.

[0009] To achieve the above object, the application provides a preparation process of a textile fabric based on natural ore releasing far infrared rays and negative ions, comprising the following steps:

[0010] Step one: select ore with natural far infrared emission and negative ion release capacity as raw material ore, use a crushing device to crush the raw material ore, and obtain ore powder with a particle size of 40-60 nm after crushing;

[0011] Step two: mix the ore powder with a particle size of 40-60 nm with fiber raw materials, and perform blending treatment under high-temperature melting state, then extrude and cut to obtain ore fiber composite master batch;

[0012] Step three: send the ore fiber composite master batch into a spinning device, and draw into continuous ore composite filaments through a spinning process;

[0013] Step four: wrap and blend the ore filaments with auxiliary fibers to form composite yarns, and then weave the composite yarns into cloth through a textile process to obtain ore textile fabric with far infrared and negative ion functions.

[0014] Preferably, in step one, the crushing device is a supermicro crushing device, and inert gas is used for protection during the crushing process.

[0015] Preferably, in step one, the ore with natural far infrared emission and negative ion release capacity is one or more of tourmaline, medical stone and tourmaline.

[0016] Preferably, in step two, the temperature of high-temperature melting ranges from 170 to 280 DEG C, and the melting and blending treatment is performed in a screw extruder, and the screw rotation speed of the screw extruder is 200-400 r / min.

[0017] The mass mixing ratio of the ore powder and the fiber raw materials is 1:3-1:10, and the fiber raw materials are one or more of polyester fiber, nylon fiber, polypropylene fiber and cotton fiber.

[0018] Preferably, in step three, the temperature of high-temperature melting is consistent, the spinning speed is 600-900 m / min, and the diameter of the obtained ore filaments is 0.08-0.12 mm.

[0019] Preferably, in step four, the wrapping and blending treatment is performed by using a doubling machine, the ore filaments are used as the core layer of the composite yarns, and the auxiliary fibers are used as the sheath layer of the composite yarns to form the composite yarns.

[0020] Preferably, the mass ratio of the core layer of ore filaments to the sheath layer of auxiliary fibers is 1:2-1:4, and the auxiliary fibers are one or more of cotton fiber, antibacterial polyester fiber and bamboo fiber.

[0021] Preferably, in step four, the textile process is a weaving process or a knitting process, wherein the weaving process adopts a plain weave, a twill weave or a satin weave, and the knitting process adopts a weft flat knitting, a rib or a double rib.

[0022] Compared with the prior art, the present application has the following advantages:

[0023] In the present application, the nanoscale ore powder is in-situ compounded in the fiber melt spinning stage, so that the functional factors are permanently wrapped and fixed in the fiber interior, rather than attached to the surface. As shown in Example 1, after 50 times of standard washing, the attenuation rates of far infrared emissivity and negative ion release amount are both less than 2.5%, which is far lower than the attenuation rate of more than 30% in the conventional finishing process.

[0024] In the present application, natural raw ore is used, so that there are no chemical residual substances such as formaldehyde and benzene in the finished fabric, and no allergic irritation problems such as redness and itching when in long-term contact with human skin.

[0025] In the present application, the mixing ratio of nanometer ore powder and fiber master batch is adjusted to control the far infrared emission intensity and the negative ion release amount of the fabric; according to the use scene of the target fabric, the corresponding fiber master batch and wrapped fiber can be selected, when producing close-fitting underwear, soft polyester / cotton fiber is selected; when producing medical fabric, disinfection-resistant polypropylene / antibacterial polyester fiber is selected; when producing home textile fabric, breathable nylon / bamboo fiber is selected. It can be adapted to many scenes such as close-fitting clothes, home textile products, medical protection, health protection equipment, etc., greatly expanding the application range of far infrared and negative ion textile fabric.

[0026] The above summary is intended to illustrate the present application and is not intended to be limiting in any way. Further aspects, implementations, and features of the present application will be apparent from the drawings and the following detailed description. BRIEF DESCRIPTION OF DRAWINGS

[0027] Figure 1 The flow chart of the textile fabric preparation process of the present application. DETAILED DESCRIPTION

[0028] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. It should be pointed out that the drawings are schematic and not drawn to scale. For the clarity and convenience in the drawings, the relative sizes and proportions of the parts shown in the drawings are exaggerated or reduced for illustration, and any size is only exemplary, but not limiting.

[0029] The preparation process of the textile fabric based on natural ore releasing far infrared rays and negative ions comprises the following steps:

[0030] Step one: select the ore with natural far infrared emission and negative ion release capacity as raw material, and use the crushing equipment to crush the raw material, and the particle size of the crushed ore powder is 40-60 nanometers;

[0031] Step two: mix the 40-60 nanometer particle size ore powder with fiber raw material, and blend under high temperature melting state, then extrude and cut into particles to obtain ore fiber composite master batch;

[0032] Step three: send the ore fiber composite master batch into the spinning equipment, and draw into continuous ore composite yarn through the spinning process;

[0033] Step four: wrap and blend the ore yarn with auxiliary fibers to form a composite yarn, and then weave the composite yarn into a fabric by using the textile process to obtain an ore textile fabric with far infrared and negative ion functions.

[0034] Example one, ore textile fabric for clothes

[0035] 1. Ore selection and pretreatment: select natural tourmaline ore as functional substrate, and after pretreatment detection, the far infrared emission rate is ≥85%, and the negative ion release amount is ≥1500 pieces / cm 3 , and does not contain heavy metal impurities. Cut the ore into blocks of 5cm x 5cm x 2cm, and put it into a blast drying oven at 80℃ for 2 hours to remove the water adsorbed in the ore, and avoid ore powder agglomeration during subsequent crushing.

[0036] The main chemical components and content range of the tourmaline ore are: SiO245%-48%, Al2O330%-32%, B2O38%-10%, Na2O 3%-5%, Fe2O32%-3%; the heavy metal impurity limit meets the requirements of GB18401-2010 "National Textile Product Basic Safety Technical Specification", in which Pb≤10ppm, Cd≤5ppm, Hg≤1ppm; the test standard conditions of far infrared emission rate and negative ion release amount are: environmental temperature 25℃±2℃, relative humidity 60%±5%, and the test equipment uses Fourier transform infrared spectrometer and air negative ion concentration tester.

[0037] 2. Ore crushing: use JZM-60 type ultrafine grinder to crush, and the specific steps are as follows:

[0038] 201. Put the dried tourmaline block ore into the grinder inlet, set the grinder speed to 3000r / min, and perform primary crushing to obtain coarse ore powder with particle size ≤1mm;

[0039] Specifically, the whole crushing process uses industrial nitrogen with a purity of ≥99.99% as a protective gas, which is introduced through the gas inlet of the crusher, with a gas flow of 5-10 L / min and a cavity pressure of 0.1-0.2 MPa, to avoid oxidation of the ore powder during crushing by contacting with air; the nitrogen pressure and flow rate are recorded every 30 minutes.

[0040] 202. Transfer the crude ore powder to the ultrafine grinding cavity of the crusher, add an appropriate amount of anhydrous ethanol as a dispersant, adjust the grinding speed to 6000 r / min, and grind for 4 hours;

[0041] 203. After grinding, use a Bettersize 2000 laser particle size analyzer to monitor the particle size of the ore powder in real time to ensure that the final ore powder particle size is stable at 50 nanometers, with a particle size deviation of ≤±2 nanometers;

[0042] Specifically, the ore powder dispersibility test: while monitoring the particle size with a laser particle size analyzer, take 1 g of ore powder sample and use a transmission electron microscope to observe the agglomeration of the ore powder. The agglomerate diameter is ≤5 μm, and the agglomerate proportion is ≤5%. If the agglomerate exceeds the standard, the grinding speed needs to be adjusted to 6500 r / min, and the grinding time needs to be extended by 30 minutes until the dispersibility meets the standard.

[0043] 204: Put the 50-nanometer ore powder into a DZF-6050 vacuum drying oven and dry it at 60°C for 1 hour to remove the anhydrous ethanol, obtaining dried tourmaline ore powder, which is sealed and stored for future use.

[0044] The mass of anhydrous ethanol added is 1-2 times the mass of the crude ore powder, and the purity of the anhydrous ethanol is ≥99.7%. After grinding, the residual ethanol content in the dried ore powder is ≤0.1%.

[0045] 3. Preparation of ore fiber composite master batch

[0046] 301. Raw material ratio: select a polyester fiber chip with a melt index of 25 g / 10 min as the fiber matrix, and the mass ratio of tourmaline ore powder to polyester fiber chip is 1:5.

[0047] The melt index (MI) of the polyester fiber chip is tested under the following conditions: test temperature 230°C, load 2.16 kg; the intrinsic viscosity of the chip is 0.62-0.65 dL / g, and the carboxyl end group content is ≤28 mol / t.

[0048] 302. High temperature melt blending and pelletizing: melt blending was performed using a SHJ-35 twin-screw extruder, with the following parameters: screw section temperature: zone 1 180℃, zone 2 260℃, zone 3 270℃, zone 4 280℃, die temperature 275℃, matching the melt temperature of the polyester fiber so that the fiber is completely melted and the mineral powder is uniformly dispersed; screw speed: 300 r / min; feeding speed: 20 kg / h.

[0049] Blending process: the tourmaline mineral powder and polyester fiber chips were simultaneously fed into the double feeding port of the twin-screw extruder, with the mineral powder being fed from the side feeding port. The melt after melt blending was extruded through the die head to form a strip-shaped material with a diameter of 3 mm;

[0050] Pelletizing: after the strip-shaped material was cooled in a cooling water tank with water temperature of 25℃, it was fed into a QG-600 pelletizer with a pelletizing speed of 500 r / min to obtain tourmaline-polyester composite masterbatch with a length of 3 mm and a diameter of 3 mm, which was sealed and stored to prevent moisture absorption.

[0051] Specifically, the premixing process: first, the tourmaline mineral powder and polyester fiber chips were fed into a high-speed mixer, with the mixing speed set to 1200-1500 r / min and the mixing time set to 8-10 minutes. The material temperature was controlled to be ≤50℃ during the mixing process. After premixing, the sample was observed to ensure that the mineral powder and the chips were not obviously layered and the mixing uniformity was ≥95%.

[0052] Screw extruder parameters: the SHJ-35 twin-screw extruder used had a screw length-diameter ratio (L / D) of 32:1 and a compression ratio of 3.5:1. The screw configuration was conveying, compression, melting, mixing, and homogenization. When feeding, the mineral powder was fed from the side feeding port at a position that was 2 / 3 of the total length of the screw.

[0053] Masterbatch quality detection: the tourmaline-polyester composite masterbatch after pelletizing needed to meet the following requirements: ① moisture content ≤0.05%; ② mineral powder dispersion uniformity: under a microscope with 400 times magnification, the diameter of the mineral powder agglomerates was ≤5 μm, and the number of agglomerates in each 100 μm 2 field of view was ≤3; ③ bulk density 1.2-1.3 g / cm 3 .

[0054] 4. Mineral filament preparation: spinning was performed using a FA506 spinning machine, with the following specific steps:

[0055] Pre-treatment of masterbatch before spinning: the composite masterbatch was placed in a hot air drying oven and dried at 110℃ for 3 hours, with the moisture content of the masterbatch being controlled to be ≤0.05%;

[0056] The spinning temperature was matched with the melting temperature of the composite masterbatch, and the temperature of each zone of the spinning machine was set as follows: zone 1 265℃, zone 2 270℃, zone 3 275℃, spinneret temperature 270℃;

[0057] The spinneret is selected as a 36-hole circular spinneret, and the spinning hole diameter is 0.12 mm; the spinning speed is 800 m / min.

[0058] Cooling and solidification: the primary filaments extruded from the spinneret immediately enter a side-blowing cooling device, the cooling air temperature is 22℃, the air speed is 0.8 m / s, and the cooling distance is 18 cm;

[0059] Winding and collecting filaments: the cooled mineral filaments are guided by a guide roller and enter a WZ-1200 type winding machine, the winding speed is 800 m / min, the tension control is 5 cN, the mineral filaments are wound on a paper yarn tube to form a mineral filament bobbin with a diameter of 25 cm, and finally the tourmaline polyester mineral filaments with a diameter of 0.1 mm are obtained.

[0060] Specifically, the material of the 36-hole circular spinneret is zirconia ceramic, the length-diameter ratio (L / D) of the spinning hole is 4:1 (hole length 0.48 mm, hole diameter 0.12 mm), the hole spacing is 2 mm, and the spinneret thickness is 10 mm; before spinning, the spinning hole needs to be cleaned with an ultrasonic cleaning machine, the cleaning time is 30 minutes, and the spinning hole diameter tolerance is ≤±0.005 mm.

[0061] The air type of the side-blowing cooling device is laminar flow, the cooling air temperature fluctuation range is ≤±1℃, and the relative humidity is 40%-60%; the contact angle between the cooling air and the filaments is 90°, the outlet height of the cooling air ring is 5 cm, and it is ensured that the filaments are uniformly cooled within 5 cm after being extruded from the spinneret.

[0062] The winding machine adopts a constant tension control mode, the initial tension is 5 cN, and when the bobbin diameter increases from 10 cm to 25 cm, the tension is adjusted according to the compensation coefficient of 0.2 cN per 1 cm increase in diameter as the bobbin diameter increases; during the winding process, the lateral swing amplitude of the filaments is ≤2 mm, which avoids the overlapping of the filaments on the bobbin.

[0063] 5. Mineral filament wrapping and composite yarn preparation: select combed cotton fibers with a count of 40S and a foreign matter content of ≤0.5% as the outer wrapping fiber, and use an A272F type doubling machine for wrapping and blending, with tourmaline polyester mineral filaments as the core layer and combed cotton fibers as the sheath layer;

[0064] Doubling parameters: the core layer mineral filament feeding speed is 80 m / min, the sheath layer combed cotton fiber feeding speed is 240 m / min, and the core-sheath mass ratio is 1:3; the twist is set to 80 twists / 10 cm; a 16 English composite yarn is obtained, the yarn fineness is uniform, and the breaking strength is ≥25 cN.

[0065] Among them, the linear density of the combed cotton fiber is 14.6 tex, the twist is 80 twists / 10 cm, the breaking strength is ≥2.8 cN / dtex, and the breaking elongation is 7%-9%; the moisture regain of the fiber is 8.5%-9.5%, and it does not contain fluorescent whitening agent.

[0066] 501. Package blending details: the twist direction of the composite yarn is S twist, and the twist deviation is ≤±2 twists / 10 cm; and the twist tension control of the twisting machine is: the core mineral filament tension is 3 cN, and the sheath layer combed cotton fiber tension is 8 cN, to ensure that the core and sheath layer are tightly combined, and there is no core exposure phenomenon.

[0067] The warp and weft density of the air jet loom is 120 / 100, and the warp and weft density deviation is ≤±2 / 1; the selvage width of the plain cloth is 1.5 cm, and a 3 / 1 diagonal strengthening weaving method is adopted; during the weaving process, the on-machine tension fluctuation range of the warp yarn is ≤±5 N, and the flight time of the weft yarn is controlled to be 8-10 ms.

[0068] Pre-shrinking treatment: after weaving is completed, pre-shrinking treatment is carried out by using a pre-shrinking machine, the pre-shrinking temperature is 80℃, the pre-shrinking rate is 3%-5%, and the width deviation of the cloth after pre-shrinking is ≤±1 cm, and the length shrinkage rate is ≤2%.

[0069] 6. Weaving forming: ZAX-e type air jet loom is used for weaving, and a knitted plain structure suitable for close-fitting underwear is adopted, and composite yarns are used for warp and weft, wherein the loom speed is 600 r / min, the shedding time is 310°, the warp yarn tension is 200 N, and the weft yarn tension is 15 cN; the woven cloth is a plain cloth with a width of 150 cm and a weight of 180 g / m 2 , the cloth surface is flat, and there is no broken yarn or pilling phenomenon;

[0070] Only conventional water washing is carried out to remove oil stains in the weaving process, and no additional functional finishing is required, and finally a mineral textile cloth for close-fitting clothes is obtained.

[0071] 7. Performance verification, function durability experiment after washing

[0072] According to the standards: GB / T8629-2017 (washing procedure), GB / T30127-2013 (far infrared), QB / T4069-2010 (negative ions)

[0073] Experimental equipment: standard washing machine (SW-12), Fourier transform infrared spectrometer (Nicolet iS50), air negative ion concentration tester (COM-3200PRO)

[0074] 701. Test sample preparation:

[0075] ① Sampling method: According to the sampling rules in Appendix A of GB / T 17592-2011 "Determination of Prohibited Azo Dyes in Textiles", 10 cm x 10 cm samples were cut from the 150 cm x 200 cm plain cloth, with a total of 5 positions, i.e. the warp direction (10 cm from the cloth edge), the weft direction (10 cm from the cloth edge), and the diagonal line (left upper-right lower, right upper-left lower), with 3 parallel samples taken from each position, a total of 15 samples;

[0076] ② Sample pretreatment: All samples were placed in a hot air drying oven at 80℃±2℃ for 30 min, then taken out and balanced in a standard environment at a temperature of 25℃±2℃ and a relative humidity of 60%±5% for 24 h. The initial weight of each sample was measured using an electronic balance, and the initial dimensions of the sample were measured using a ruler, with 3 measurements of length and width taken and averaged.

[0077] Test process:

[0078] ① Water washing procedure control: The washing capacity of the standard washing machine was set to 5 kg, the neutral detergent dosage was 5 g / L, the water temperature was 30℃±1℃, the washing time was 20 min, the dehydration rotation speed was 800 r / min, and the dehydration was naturally dried. After each washing, the sample pretreatment step was repeated before the next washing, for a total of 50 times.

[0079] ② Far infrared emissivity test: The wavelength scanning range of the Fourier transform infrared spectrometer was 8-14 μm, the scanning interval was 0.1 μm, the resolution was 4 cm -1 , and the number of scans was 32. During testing, the samples were laid flat on the sample stage, with a vertical distance of 5 cm between the sample and the detector. The instrument was calibrated before each test using a standard black body. Each sample was tested at 3 different regions, and the average value was taken.

[0080] ③ Negative ion release amount test: The test mode of the air negative ion concentration tester was static testing, with an air flow rate of ≤0.1 m / s in the test environment. The sample was hung in the center of the test chamber, with a vertical distance of 3 cm between the tester probe and the sample surface. Each sample was tested 5 times, and the average value was taken. The test results are shown in Table 1.

[0081] Test index Test value before water washing Test value after 50 times of water washing Attenuation rate Far infrared emissivity (8-14 μm) 83.5％ 81.8％ 2.0％ Amount of negative ions released (pieces / cm 3 )]]> 1290 1260 2.3％

[0082] Table 1

[0083] This experiment verifies that the far infrared emissivity attenuation rate is only 2.0% and the negative ion release amount attenuation rate is 2.3% after 50 washes, which is much lower than the traditional chemical finishing process, proving that the ore powder is deeply combined with the fiber through high-temperature melting, and the function is not dependent on surface attachment, achieving permanent release.

[0084] Example Two, Medical Protective Ore Textile Cloth

[0085] 1. Raw ore screening and pretreatment: Select natural medical stone raw ore, which has a far-infrared emission rate of ≥80%, a negative ion release amount of ≥1200 / cm, and an Escherichia coli inhibition rate of ≥90%, meeting the medical antibacterial requirements; crush the raw ore into small pieces of 3cm x 3cm x 1cm, and place them in a microwave drying device with a model of MW-1000, dry at 70°C for 1.5 hours to remove free water and crystal water in the raw ore. 3

[0086] The main chemical components and content ranges of the medical stone raw ore are: SiO265%-70%, Al2O312%-15%, K2O 2%-4%, Na2O 1%-2%, and CaO 3%-5%; the biological safety indicators meet the requirements of YY / T0506.1-2016 "Textiles for Patients, Medical Staff and Equipment Part 1: General", with a total bacterial count of ≤10 CFU / g and an endotoxin of ≤0.5 EU / g; the heavy metal limits are the same as in Example One, with lead (Pb) ≤10 ppm, cadmium (Cd) ≤5 ppm, and mercury (Hg) ≤1 ppm.

[0087] 2. Raw ore crushing: use a QM-3SP4 planetary ball mill for crushing, with the following specific steps:

[0088] 201. Put the dried medical stone pieces and agate grinding balls into the ball mill tank together, with a ball-to-material ratio of 5:1, add deionized water, and set the rotation speed of the ball mill to 200 r / min for primary ball milling for 2 hours to obtain coarse ore powder with a particle size of ≤500μm;

[0089] Specifically, inert gas protection and replenishment: during the crushing process of the planetary ball mill, pure argon gas with a purity of ≥99.99% is introduced into the ball mill tank, the argon gas filling amount is 1 / 3 of the volume of the ball mill tank, the sealed ball mill tank is vacuumized to a vacuum degree of 10 Pa, then argon gas is introduced to normal pressure, and the process is repeated twice to replace the air in the tank; maintain the pressure in the tank at 0.1 MPa during the ball milling process to prevent oxidation of the ore powder.

[0090] 202. Transfer the coarse ore powder to the ultra-fine ball milling chamber, adjust the rotation speed to 400 r / min, and ball mill for 6 hours, with a 10-minute shutdown every 1 hour to prevent overheating of the equipment and deterioration of the ore powder;

[0091] 203. Real-time monitoring by a laser particle size analyzer to ensure that the particle size of the ore powder is stable at 50 nanometers with a deviation of ≤±3 nanometers;

[0092] ​Specifically, by dispersion verification, 2 g of ore powder is taken and added to deionized water to prepare a 0.5% ore powder suspension. The particle size distribution span is tested using a Malvern laser particle size analyzer. The Span is required to be (D90-D10) / D50≤1.5 (D10, D50, D90 are 10%, 50%, and 90% volume particle size, respectively). If the Span exceeds the standard, 0.5% polyethylene glycol (PEG-400) is added as a dispersant, and the ball milling is performed for 1 hour again.

[0093] 204. The ore powder is placed in a freeze dryer of LGJ-10 type, dried at -50°C and a vacuum degree of 10 Pa for 2 hours to completely remove the water, and a dried ore powder is obtained and stored in a sterile bag.

[0094] 3. Preparation of ore-fiber composite master batch

[0095] 301. Raw material ratio: The medical protective cloth needs to be resistant to high temperature sterilization. Polypropylene fiber chips with a melt index of 18 g / 10 min are selected as the fiber matrix. The mass ratio of ore powder to polypropylene fiber chips is 1:4.

[0096] The melt index (MI) of the polypropylene fiber chips is tested under the following conditions: test temperature 230°C, load 2.16 kg; isotacticity ≥ 95%, ash content ≤ 0.03%, heat resistance temperature ≥ 121°C, and atactic polypropylene content ≤ 2% to avoid the generation of low molecular volatile substances during melt blending.

[0097] 302. High temperature melt blending and pelletization: TE-35 single screw extruder is used with the following parameters:

[0098] Screw zone temperature: Zone 1 160°C, Zone 2 170°C, Zone 3 180°C, Zone 4 190°C, and die temperature 185°C; screw speed 250 r / min;

[0099] Feeding method: After mixing the ore powder with the polypropylene chips, they are uniformly fed through a single feeding port at a speed of 15 kg / h to avoid stratification of the ore powder;

[0100] Melt filtration: A 300-mesh stainless steel filter screen is installed at the die to filter impurities and undispersed ore powder agglomerates from the molten material;

[0101] Pelletization: After extrusion, the molten material is air-cooled and fed into an XQ-500 pelletizer at a speed of 400 r / min to obtain a composite master batch with a length of 2.5 mm and a diameter of 2.5 mm, which is stored in a sterile manner.

[0102] Specifically, the pre-mixing control: the pre-mixing of the medical stone powder and the polypropylene chips uses a horizontal mixer, the mixing speed is 800-1000 r / min, the mixing time is 12-15 minutes, a small amount of nitrogen is introduced during the mixing process to prevent the polypropylene chips from absorbing moisture; after pre-mixing, a screening method is used for detection, and the sieve residue is ≤1%.

[0103] Single screw parameters: the length-diameter ratio (L / D) of the TE-35 type single screw extruder is 28:1, the compression ratio is 3:1, the screw head is provided with a flow divider (200 mesh) and a 300 mesh stainless steel filter screen; the temperature control deviation of each section of the extruder is ≤±2℃.

[0104] Mother granule aseptic detection: the composite mother granule is subjected to aseptic detection, 10 g of the mother granule is taken, and a plate count method is used for detection according to YY / T0506.2-2016 “Textiles for patients, medical staff and equipment Part 2: Performance requirements”, the total number of bacteria is ≤10 CFU / g, the total number of molds is ≤5 CFU / g, and there is no pathogenic bacteria.

[0105] 4. Preparation of mineral filaments: a JSFA288 type spinning machine is used, and the steps are as follows:

[0106] Mother granule pretreatment: the composite mother granule is placed in a vacuum drying oven and dried at 90℃ for 4 hours, and the water content is controlled to be ≤0.03%;

[0107] Spinning temperature: zone 1 175℃, zone 2 180℃, zone 3 185℃, spinneret temperature 180℃;

[0108] Spinneret selection: 24-hole circular spinneret, spinneret hole diameter 0.15mm; spinning speed 600m / min;

[0109] Cooling and solidification: ring blowing cooling is used, the cooling air temperature is 20℃, the air speed is 1.0m / s, and the cooling distance is 20cm;

[0110] Winding and collecting filaments: the winding machine rotates at 600m / min, the tension is controlled to be 8cN, the mineral filaments are wound on a sterile plastic yarn tube, and the mineral filaments with a diameter of 0.12mm are obtained.

[0111] 5. Mineral filament wrapping and composite yarn preparation: select the antibacterial polyester staple with a staphylococcus aureus inhibition rate ≥95% as the outer wrapping fiber, use a FA726 type doubling machine, the medical stone-polypropylene mineral filament is the core layer, and the antibacterial polyester staple is the sheath layer; the core layer feeding speed is 60m / min, the sheath layer feeding speed is 120m / min, the core-sheath mass ratio is 1:2; 100 twists / 10cm;

[0112] Finished yarn: 20 English composite yarn, breaking strength ≥30cN, and the finished yarn is subjected to ultraviolet disinfection for 30 minutes for antibacterial pretreatment and standby.

[0113] The type of the antibacterial agent of the antibacterial polyester staple fiber is an internal silver ion antibacterial agent, and the antibacterial durability meets the requirements of GB / T20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method", and the antibacterial rate on Staphylococcus aureus is still greater than or equal to 90% after 50 times of washing; the linear density of the staple fiber is 1.56 dtex, the length is 38 mm, the breaking strength is greater than or equal to 4.0 cN / dtex, and the elongation at break is 25%-30%.

[0114] The twist direction of the composite yarn is Z twist, and the twist variation coefficient is less than or equal to 3%; the spindle speed of the twisting machine is 8000 r / min, and the guide yarn speed is 20 m / min, so that the covering degree of the core layer of mineral filaments and the sheath layer of antibacterial polyester fibers is greater than or equal to 95%.

[0115] The twill weave of the rapier loom is 2 / 1 right twill, the warp and weft density is 130 / 110, the warp tension is 250 N±5 N, the weft tension is 20 N±1 N; the opening time during weaving is 300°±2°, the beating-up force is 1800 N, so as to avoid wrinkles on the fabric surface caused by excessive beating-up force; the warp breaking strength of the fabric is greater than or equal to 350 N, and the weft breaking strength is greater than or equal to 300 N.

[0116] During high-temperature setting at 120°C, the setting temperature is 120°C±2°C, the setting time is 30 min, the drying speed of the setting machine is 10 m / min, and the heat shrinkage rate of the fabric after setting is less than or equal to 1.5%, so as to ensure that there is no obvious shrinkage during subsequent 121°C high-pressure steam sterilization.

[0117] 6. Weaving: GA747 rapier loom is used to weave twill fabric, and the warp and weft are both the above-mentioned composite yarn; the speed of the loom is 500 r / min, the opening time is 300°, the warp tension is 250 N, and the weft tension is 20 cN;

[0118] Fabric specifications: width 120 cm, weight 220 g / m 2 The selvedge is woven by reinforcing method.

[0119] Post-processing: only high-temperature setting at 120°C for 30 min is performed, and no other chemical finishing is performed, to obtain mineral textile fabric.

[0120] 7. Performance verification, high-pressure steam sterilization stability experiment

[0121] According to the standards: GB19258-2012 (medical textile sterilization), GB / T30127-2013 (far infrared), GB / T20944.3-2008 (antibacterial)

[0122] Experimental equipment: high-pressure steam sterilizer with model LS-B50L, Fourier transform infrared spectrometer, and antibacterial circle tester with model HJY-300.

[0123] Test sample preparation:

[0124] ① Sampling method: According to the sampling method of YY / T0506.2-2016 Textiles for patients, medical staff and equipment Part 2: Performance requirements, 10 cm x 10 cm functional test samples and 5 cm x 5 cm antibacterial test samples were cut from the middle of the warp and weft of the 120 cm x 200 cm twill fabric, and 3 parallel samples were taken from each test sample;

[0125] ② Sample sterilization pretreatment: the antibacterial test sample needs to be sterilized by 121 ℃ high pressure steam for 20 min, and cooled to room temperature in a sterile operation table after sterilization to avoid secondary pollution; the functional test sample does not need to be sterilized, only to be balanced in the standard environment for 24 h.

[0126] Test process:

[0127] ① High pressure steam sterilization control: the sterilization program of the high pressure steam sterilizer is set to medical fabric sterilization mode, temperature 121 ℃ ± 1 ℃, pressure 0.1 MPa ± 0.005 MPa, holding time 30 min, after sterilization, natural cooling to balance the pressure in the cabin with the atmospheric pressure, taking out the sample and testing after balancing in the standard environment for 24 h;

[0128] ② Antibacterial test: according to the oscillation method of GB / T20944.3-2008, the concentration of E. coli bacterial solution is adjusted to 1 x 10 6 -5 x 10 6 CFU / mL, 5 cm x 5 cm antibacterial sample is put into a 250 mL flask, 100 mL of 0.85% sterile physiological saline and 5 mL of bacterial solution are added, and it is placed in a shaking bed for 24 h; after shaking, 1 mL of bacterial solution is taken, diluted with sterile physiological saline, and 0.1 mL of diluted solution is spread on a nutrient agar plate, which is cultured at 37 ℃ for 24 h, and then the number of bacteria is counted, the antibacterial rate = (the number of bacteria in the blank control group - the number of bacteria in the sample group) / the number of bacteria in the blank control group x 100% (the blank control group is the bacterial solution system without adding sample);

[0129] ③ Far infrared and negative ion test: the same as the test details of example one, the far infrared emissivity test sample needs to be flat without wrinkles, and the negative ion test needs to be carried out in a sterile environment. The test results are shown in Table 2.

[0130] Test index Test value before sterilization Test value after sterilization Attenuation rate Far infrared emissivity (8-14 μm) 79.8％ 79.0％ 1.0％ Escherichia coli inhibition rate (%) 92.5％ 91.8％ 0.7％ Amount of negative ions released (pieces / cm 3 ) 1090 1070 1.8％

[0131] Table 2

[0132] The experiment verifies the tolerance of the process to extreme conditions. The attenuation rate of far-infrared, antibacterial, and negative ion performance after sterilization at 121℃ is ≤1.8%, which proves the stability of the combination of mineral filaments and polypropylene fibers, and the natural antibacterial property of the original ore is not affected by sterilization, meeting the requirements of long-term repeated use of medical protective cloth.

[0133] Example Three, Mineral Textile Cloth for Bed Sheet

[0134] 1. Original ore screening and pretreatment: Select natural tombarthite ore. The far-infrared emission rate is ≥88%, and the negative ion release amount is ≥1800 / cm 3 ; Cut the original ore into blocks of 4cm x 4cm x 2cm, and put it into a hot air circulating drying oven at 85℃ for 2.5 hours to completely remove the moisture.

[0135] The main chemical components and content range of the tombarthite ore are: SiO242%-45%, Al2O333%-35%, B2O39%-11%, FeO 4%-6%, MgO 2%-3%; the heavy metal impurity limit meets the requirements of GB18401-2010, Pb ≤10ppm, Cd ≤5ppm, Hg ≤1ppm; the far-infrared emission rate test wavelength range is 8-14μm, and the test method refers to GB / T30127-2013 "Textiles - Determination and Evaluation of Far-Infrared Properties".

[0136] 2. The specific steps for pulverizing the original ore with LM-100 air jet pulverizer are as follows:

[0137] 201. Put the dried tombarthite blocks into the air jet pulverizer feed hopper, the compressed air pressure is 0.8MPa, and the primary pulverization is carried out to obtain coarse ore powder with a particle size of ≤200μm;

[0138] 202. Adjust the compressed air pressure to 1.0MPa, and carry out superfine pulverization, the pulverization time is 3 hours, and the particle size is controlled by the classification wheel during this period, wherein the rotation speed is 12000r / min;

[0139] 203. Laser particle size analyzer monitoring to ensure that the ore powder particle size is 50 nanometers, and the deviation is ≤±2 nanometers;

[0140] 204. After the ore powder is collected by the cyclone separator, it is put into a vacuum drying oven at 65℃ for 1.5 hours to remove residual air and moisture, and the tombarthite ore powder is obtained and sealed for storage.

[0141] 3. Preparation of mineral-fiber composite master batch

[0142] 301. Raw material ratio: Select polyamide fiber chips as the fiber matrix, and the mass ratio of tombarthite ore powder to polyamide fiber chips is 1:6.

[0143] Wherein, the nylon fiber chip is polycaprolactam chip, the relative viscosity is 2.7-2.9; the melt index (MI) is 15 g / 10 min (test temperature 230℃, load 2.16 kg), the water content is ≤0.08%, and the end amino group content is 40-50 mmol / kg.

[0144] 302. High temperature melt blending and granulation: SHJ-45 type double screw extruder is used, and the parameters are as follows:

[0145] The temperature of each zone of the screw is 200℃ for the first zone, 220℃ for the second zone, 230℃ for the third zone, 240℃ for the fourth zone, and the die temperature is 235℃; the screw speed is 350 r / min; the feeding speed is 25 kg / h, and the mineral powder is fed from the side feeding port;

[0146] Melt homogenization: a static mixer is arranged at the end of the screw to ensure that the mineral powder and the nylon melt are fully mixed;

[0147] Granulation: after the molten material is water-cooled, it is fed into a QG-800 type granulator, the granulation speed is 600 r / min, the composite master batch with a length of 3 mm and a diameter of 3 mm is obtained, and it is stored in a moisture-proof manner.

[0148] 4. Mineral filament preparation: FK6-1000 type spinning machine is used, and the steps are as follows:

[0149] Master batch pretreatment: the composite master batch is dried in a 100℃ hot air drying oven for 3.5 hours, and the water content is ≤0.04%;

[0150] Spinning temperature: 225℃ for the first zone, 230℃ for the second zone, 235℃ for the third zone, and 230℃ for the spinneret temperature;

[0151] The spinneret is selected as a 48-hole circular spinneret with a spinneret hole diameter of 0.1 mm; the spinning speed is 700 m / min;

[0152] Cooling and solidification: side blowing cooling, air temperature 23℃, air speed 0.6 m / s, cooling distance 15 cm;

[0153] Winding and collecting yarn: winding speed 700 m / min, tension 5 cN, winding on paper yarn pipe, and obtaining mineral filament with a diameter of 0.08 mm.

[0154] 5. Mineral filament wrapping and composite yarn preparation: bamboo fiber short fiber is selected as the outer wrapping fiber, A272G type doubling machine is used, and tourmaline-nylon mineral filament is used as the core layer and bamboo fiber short fiber is used as the sheath layer; the core feeding speed is 70 m / min, the sheath feeding speed is 280 m / min, and the core-sheath mass ratio is 1:4;

[0155] The twist is 70 twists / 10 cm; the finished yarn is 12 English composite yarn, and the breaking strength is ≥22 cN.

[0156] The bamboo fiber short fiber is regenerated bamboo pulp fiber, the linear density is 1.67 dtex, the length is 38 mm, the breaking strength is greater than or equal to 3.0 cN / dtex, the breaking elongation is 16%-18%, the moisture absorption rate is greater than or equal to 12%, the air permeability is greater than or equal to 800 mm / s, and the formaldehyde is not contained.

[0157] 6. A plain weave home textile fabric is woven by using a TP500 air jet loom: the warp and weft are both the composite yarns; the loom speed is 650 r / min, the shedding time is 320°, the warp tension is 180 N, and the weft tension is 12 cN; the fabric width is 200 cm, and the fabric weight is 150 g / m 2 The plain weave fabric has a warp and weft density of 120 / 2.54 cm x 100 / 2.54 cm;

[0158] The fabric is subjected to soft finishing, and the drying temperature is 80℃, so as to obtain the mineral textile fabric.

[0159] 7. Performance verification, fabric air permeability test

[0160] According to the standard: GB / T5453-1997 "Determination of air permeability of textile fabrics"

[0161] Experimental equipment: fabric air permeability tester (YG461E)

[0162] Test sample preparation:

[0163] ① Sampling method: according to the sampling requirements of GB / T5453-1997, 5 test points are selected on the center (coordinate (100 cm, 110 cm)) and four edge positions (coordinates (20 cm, 20 cm), (180 cm, 20 cm), (20 cm, 200 cm), and (180 cm, 200 cm)) of the 200 cm x 220 cm plain weave fabric, and 2 parallel samples are cut from each test point.

[0164] ② Sample pretreatment: the sample is placed in a hot air drying oven at 70℃±2℃ and dried for 40 min to remove the water adsorbed by the sample, and then balanced in a standard environment for 16 h, the thickness of each sample is measured by using a fabric thickness tester to ensure that the sample thickness deviation is less than or equal to 0.05 mm.

[0165] Test process:

[0166] ① Test environment control: the fabric air permeability tester needs to be placed in a standard environment, and the machine is preheated for 30 min before testing, and the standard air permeable film is used to calibrate the instrument, and the calibration error is less than or equal to ±2%;

[0167] ②Air permeability test operation: The circular sample was fixed flat on the test table, ensuring that the sample was not stretched or wrinkled, the test pressure was set to 100 Pa ± 2 Pa, and the air permeability (unit: mm / s) was automatically recorded by the instrument; each sample was tested 3 times, and the sample position was changed after each test to avoid repeated testing of the same area, and the average value was taken;

[0168] ③Air permeability resistance calculation: According to GB / T5453-1997, air permeability resistance (Pa·s / m) = test pressure (Pa) / air permeability (m / s), wherein the air permeability unit needs to be converted from "mm / s" to "m / s" (1 mm / s = 0.001 m / s), and the calculation result is rounded to the integer;

[0169] ④Data validity judgment: The test results of two parallel samples at the same measuring point deviated by ≤5%, and the average value of the two samples was taken as the data of the measuring point; when the deviation > 5%, the sample needed to be retested. The test results are shown in Table 3.

[0170]

[0171] Table 3

[0172] The experiment verified that the process ensured the far-infrared function while being compatible with the basic performance of the fabric. The average value of 860 mm / s far exceeded the industry standard (≥600 mm / s), and the air permeability resistance was low (118 Pa·s / m), which realized the permanent emission of tourmaline mineral filaments and ensured the comfort of home textile fabrics.

[0173] Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent substitutions for part of the technical features, and any modification, equivalent substitution, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A process for preparing a textile fabric based on natural ore for releasing far infrared rays and negative ions, characterized in that, The method comprises the following steps: Step one: select a mineral with natural far infrared emission and negative ion release ability as raw material, and use a crushing device to crush the raw material, and the particle size of the crushed mineral powder is 40-60 nm; Step two: mix the 40-60 nm particle size mineral powder with fiber raw materials, and blend under high temperature melting state, then extrude and cut to obtain a mineral fiber composite master batch; Step three: send the mineral fiber composite master batch into a spinning device, and draw into continuous mineral composite yarn through a spinning process; Step four: wrap and blend the mineral yarn with auxiliary fibers to form a composite yarn, and then weave the composite yarn into a cloth through a weaving process to obtain a mineral textile cloth with far infrared and negative ion functions.

2. The process for preparing natural ore-based textile fabric releasing far infrared rays and negative ions according to claim 1, characterized in that: In step one, the crushing device is a super micro crushing device, and inert gas is used for protection during the crushing process.

3. The process as claimed in claim 1, wherein the natural ore based textile fabric is prepared by releasing far infrared rays and negative ions. In step one, the mineral with natural far infrared emission and negative ion release ability is one or more of tourmaline, medical stone and tourmaline.

4. The natural ore-based textile fabric preparation process for releasing far infrared rays and negative ions according to claim 1, characterized in that: In step two, the temperature of high temperature melting is 170-280℃, and the melting and blending process is carried out in a screw extruder, and the screw rotation speed of the screw extruder is 200-400 r / min; The mass mixing ratio of mineral powder and fiber raw materials is 1:3-1:10, and the fiber raw materials are one or more of polyester fiber, nylon fiber, polypropylene fiber and cotton fiber.

5. The natural ore-based textile fabric preparation process for releasing far infrared rays and negative ions according to claim 1, characterized in that: In step three, the temperature of high temperature melting is the same, the spinning speed is 600-900 m / min, and the diameter of the prepared mineral yarn is 0.08-0.12 mm.

6. The natural ore-based textile fabric preparation process for releasing far infrared rays and negative ions according to claim 1, characterized in that: In step four, the wrapping and blending process is carried out by a doubling machine, and the mineral yarn is used as the core layer of the composite yarn, and the auxiliary fiber is used as the sheath layer of the composite yarn to form the composite yarn.

7. The process as claimed in claim 6, wherein the natural ore based textile fabric is prepared by releasing far infrared rays and negative ions. The mass ratio of core mineral yarn to sheath auxiliary fiber is 1:2-1:4, and the auxiliary fiber is one or more of cotton fiber, antibacterial polyester fiber and bamboo fiber.

8. The natural ore-based textile fabric preparation process for releasing far infrared rays and negative ions according to claim 1, characterized in that: In step four, the weaving process is a weaving process or a knitting process, wherein the weaving process adopts plain weave, twill weave or satin weave, and the knitting process adopts weft plain stitch, rib stitch or double rib stitch.

Images