CN111041593A - Process for preparing antistatic fiber for preparing chemical protective clothing - Google Patents
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- CN111041593A CN111041593A CN201911383640.4A CN201911383640A CN111041593A CN 111041593 A CN111041593 A CN 111041593A CN 201911383640 A CN201911383640 A CN 201911383640A CN 111041593 A CN111041593 A CN 111041593A
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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
- D01F6/90—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 polyamides
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to the technical field of chemical protection, in particular to a process for preparing antistatic fibers for preparing chemical protection clothes. Under the polar action of the self-made plant extract, the invention promotes the grinding powder to be effectively filled in the system, reduces the porosity of the system and ensures that the structure of the interlayer of the system is more compact, thereby improving the wear resistance of the anti-static fiber for preparing the chemical protective clothing, and because the chemical bond has stronger bonding force than the intermolecular acting force, the grinding powder is not easy to fall off due to the influence of factors such as friction and the like, wherein the grinding powder contains conductive metal ions, can take away the static on the surface of the system, achieves the effect of removing the static, is favorable for improving the anti-static property of the anti-static fiber for preparing the chemical protective clothing, and has wide application scenes.
Description
Technical Field
The invention relates to the technical field of chemical protection, in particular to a process for preparing antistatic fibers for preparing chemical protection clothes.
Background
The chemical protective clothing is designed for protecting self from chemical dangerous goods or corrosive substances, is used for resisting or reducing the damage caused by toxic steam, gas, particles, chemical splashing, immersion or contact with toxic materials, and the like, the chemical protective clothing widely used in the market at present can be mainly divided into three types according to different materials, one type is rubber chemical protective clothing which is made of natural rubber or modified rubber materials, has high mechanical strength, elasticity and repairability but has limited chemical protective capability and higher cost, the second type is composite chemical protective clothing which is compounded by a plurality of high polymer materials and can realize wide protection, the chemical protective clothing has low cost, strong chemical protective capability, high cost performance, good weather resistance but no elasticity and no repairability, has limited use times, the other type is plastic chemical protective clothing which is commonly provided with PVC chemical protective clothing and PE chemical protective clothing, the chemical protective clothing has lower cost and high mechanical strength, but the chemical protective clothing is hard in material and inconvenient for a detector to move.
The outer layer material used by the existing chemical protective clothing is heavy in weight and large in load during operation; the physical and mechanical properties are poor, and phenomena such as abrasion, tearing and the like are easy to occur when tactical technical actions are executed; in addition, the waterproof and oil-repellent functions and the antistatic functions are not provided, so that the requirements of the battle environment cannot be met. Inner layer material: the carbon layer has poor firmness, is not resistant to washing and has short wearing period; the material has poor air and moisture permeability, which affects the wearing time limit of the clothes; the protective dose is small, particularly the protective time for large-droplet toxicants is short, and the biological virus protective performance is not provided.
Therefore, there is a need for an antistatic fiber for chemical protective clothing that can solve the above performance problems.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects that the outer layer material used by the existing chemical protective clothing is heavy in weight, large in load during operation, poor in physical and mechanical properties, easy to wear and tear and the like during tactical technical action execution, and has no waterproof function and antistatic function, and the requirement of the battle environment cannot be met, the process for preparing the antistatic fiber for preparing the chemical protective clothing is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a process for preparing antistatic fibers for preparing chemical protective clothing is characterized by comprising the following specific preparation steps:
(1) mixing, grinding and crushing medical stone and hydrotalcite to obtain ground powder, then placing the ground powder in an oven for drying to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser pipe, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol, pouring the mixture into the four-neck flask for stirring, dripping 2-3 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat to obtain pretreated dry powder;
(2) mixing olive and deionized water, placing the mixture in an ultrasonic oscillator for ultrasonic extraction, filtering to remove filter residues, collecting filtrate, and performing reduced pressure distillation on the filtrate to obtain a self-made plant extracting solution;
(3) mixing the pre-treated dry powder and the self-made plant extract, stirring and reacting to obtain a reaction product, washing the reaction product with absolute ethyl alcohol to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven for drying, cooling and discharging to obtain modified dry powder;
(4) weighing 45-50 parts of polyamide chips, 12-16 parts of modified dry powder and 3-6 parts of absolute ethyl alcohol, mixing and placing in a stirrer for stirring to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder for extrusion and granulation, collecting particles, continuously placing the particles in a spinning machine for spinning to obtain a spinning blank, finally placing the spinning blank in a tractor, drawing at a drawing multiple of 3.5-4.0 times, cooling and discharging to obtain the antistatic fiber for preparing chemical protective clothing.
The mass ratio of the medical stone to the hydrotalcite in the step (1) is 1: 3, the grinding and crushing time is 21-25 min, the drying temperature is 60-65 ℃, the drying time is 15-18 min, the mass ratio of the dry powder to the deionized water to the absolute ethyl alcohol is 6: 3: 1, the stirring temperature is 75-80 ℃, the stirring time is 27-32 min, and the heat preservation time is 10-12 min.
The mass ratio of the olive to the deionized water in the step (2) is 1: 3, the ultrasonic extraction temperature is 75-81 ℃, the ultrasonic extraction frequency is 23-27 kHz, the ultrasonic extraction time is 27-32 min, and the reduced pressure distillation time is 15-18 min.
The mass ratio of the pretreated dry powder to the self-made plant extract in the step (3) is 3: 1, the stirring reaction time is 2-3 hours, the washing times are 3-5 times, the drying temperature is 65-70 ℃, and the drying time is 2-4 hours.
The stirring speed of the step (4) is 150-160 r/min, the stirring time is 1-2 h, the granulation temperature is 480-520 ℃, the granulation pressure is 3-5 MPa, the spinning temperature is 270-300 ℃, the spinning speed is 760-800 m/min, the spinning time is 3-4 h, the drafting speed is 560-600 m/min, and the drafting time is 1-2 h.
Compared with other methods, the method has the beneficial technical effects that:
the invention takes the chinlon slices as raw materials, medical stone and hydrotalcite as modifiers and absolute ethyl alcohol as auxiliary materials to prepare the antistatic fiber for preparing the chemical protective clothing, firstly, the medical stone and the hydrotalcite are ground and crushed to obtain grinding powder, then, the self-made plant extract is utilized to carry out surface chemical modification on the grinding powder, and strong polar side groups are introduced on the main chain of the grinding powder, so that the compatibility of the grinding powder and the raw materials is enhanced, simultaneously, the affinity of the grinding powder and the raw materials is improved, under the polar action of the self-made plant extract, the grinding powder is effectively filled in a system, the porosity of the system is reduced, the structure of a system interlayer is more compact, thereby improving the wear resistance of the antistatic fiber for preparing the chemical protective clothing, and because the chemical bond has stronger binding force compared with intermolecular force, the grinding powder is not easy to fall off due to the influence of factors such as friction and the like, the grinding powder contains conductive metal ions, can take away static on the surface of a system, achieves the effect of removing the static, is beneficial to improving the antistatic property of antistatic fibers for preparing chemical protective clothing, and has wide application scenes.
Detailed Description
Mixing medical stone and hydrotalcite according to the mass ratio of 1: 3, grinding and crushing for 21-25 min to obtain ground powder, then placing the ground powder in an oven, drying at the temperature of 60-65 ℃ for 15-18 min to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol according to the mass ratio of 6: 3: 1, pouring the mixture into the four-neck flask, stirring at the temperature of 75-80 ℃ for 27-32 min, dropwise adding 2-3 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat for 10-12 min to obtain pretreated dry powder; according to the mass ratio of 1: 3, mixing the olive and deionized water, placing the mixture in an ultrasonic oscillator, carrying out ultrasonic extraction for 27-32 min at the temperature of 75-81 ℃ and the frequency of 23-27 kHz, filtering to remove filter residues, collecting filtrate, and carrying out reduced pressure distillation on the filtrate for 15-18 min to obtain a self-made plant extracting solution; mixing the pre-treated dry powder and the self-made plant extract according to the mass ratio of 3: 1, stirring and reacting for 2-3 h to obtain a reaction product, washing the reaction product with absolute ethyl alcohol for 3-5 times to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven, drying for 2-4 h at the temperature of 65-70 ℃, cooling and discharging to obtain modified dry powder; weighing 45-50 parts of nylon chips, 12-16 parts of modified dry powder and 3-6 parts of absolute ethyl alcohol, mixing and placing in a mixer, stirring at a rotation speed of 150-160 r/min for 1-2 hours to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder, extruding and granulating at a temperature of 480-520 ℃ and a pressure of 3-5 MPa, collecting particles, continuously placing the particles into a spinning machine, spinning at a temperature of 270-300 ℃ and a spinning speed of 760-800 m/min for 3-4 hours to obtain a spinning blank, finally placing the spinning blank into a traction machine, traction for 1-2 hours under the conditions of a traction multiple of 3.5-4.0 times and a traction speed of 560-600 m/min, and cooling and discharging to obtain the antistatic fiber for preparing the chemical protective clothing.
Example 1
Mixing medical stone and hydrotalcite according to the mass ratio of 1: 3, grinding and crushing for 21min to obtain ground powder, then placing the ground powder in an oven, drying for 15min at the temperature of 60 ℃ to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser pipe, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol according to the mass ratio of 6: 3: 1, pouring the mixture into the four-neck flask, stirring for 27min at the temperature of 75 ℃, dropwise adding 2 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat for 10min to obtain pretreated dry powder; mixing olive and deionized water according to a mass ratio of 1: 3, placing in an ultrasonic oscillator, performing ultrasonic extraction at 75 deg.C and 23kHz for 27min, filtering to remove residue, collecting filtrate, and distilling the filtrate under reduced pressure for 15min to obtain self-made plant extract; mixing the pre-treated dry powder and the self-made plant extract according to the mass ratio of 3: 1, stirring and reacting for 2 hours to obtain a reaction product, washing the reaction product with absolute ethyl alcohol for 3 times to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven, drying for 2 hours at the temperature of 65 ℃, cooling and discharging to obtain modified dry powder; weighing 45 parts of nylon chips, 12 parts of modified dry powder and 3 parts of absolute ethyl alcohol, mixing and placing the mixture in a stirrer, stirring for 1h at the rotation speed of 150r/min to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder, extruding and granulating at the temperature of 480 ℃ and the pressure of 3MPa, collecting particles, continuously placing the particles into a spinning machine, spinning for 3h at the temperature of 270 ℃ and the spinning speed of 760m/min to obtain a spinning blank, finally placing the spinning blank into a traction machine, drawing for 1h at the traction multiple of 3.5 times and the traction speed of 560m/min, and cooling and discharging to obtain the antistatic fiber for preparing the chemical protective clothing.
Example 2
Mixing medical stone and hydrotalcite according to the mass ratio of 1: 3, grinding and crushing for 23min to obtain ground powder, then placing the ground powder in an oven, drying for 17min at the temperature of 62 ℃ to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser pipe, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol according to the mass ratio of 6: 3: 1, pouring the mixture into the four-neck flask, stirring for 28min at the temperature of 77 ℃, dropwise adding 2 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat for 11min to obtain pretreated dry powder; mixing fructus Canarii albi and deionized water at a mass ratio of 1: 3, placing in an ultrasonic oscillator, ultrasonically extracting at 77 deg.C and 25kHz for 30min, filtering to remove residue, collecting filtrate, and distilling the filtrate under reduced pressure for 16min to obtain self-made plant extractive solution; mixing the pre-treated dry powder and the self-made plant extract according to the mass ratio of 3: 1, stirring and reacting for 2.5 hours to obtain a reaction product, washing the reaction product with absolute ethyl alcohol for 4 times to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven, drying for 3 hours at the temperature of 68 ℃, cooling and discharging to obtain modified dry powder; weighing 48 parts of nylon chips, 14 parts of modified dry powder and 5 parts of absolute ethyl alcohol, mixing and placing the mixture in a stirrer, stirring the mixture for 1.5 hours at the rotating speed of 155r/min to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder, extruding and granulating the mixture at the temperature of 500 ℃ and the pressure of 4MPa, collecting particles, continuously placing the particles into a spinning machine, spinning the particles for 3.5 hours at the temperature of 280 ℃ and the spinning speed of 770m/min to obtain a spinning blank, finally placing the spinning blank into a traction machine, drawing the spinning blank for 1.5 hours at the drawing multiple of 3.8 times and the drawing speed of 580m/min, and cooling and discharging the mixture to obtain the antistatic fiber for preparing chemical protective clothing.
Example 3
Mixing medical stone and hydrotalcite according to the mass ratio of 1: 3, grinding and crushing for 25min to obtain ground powder, then placing the ground powder in an oven, drying for 18min at the temperature of 65 ℃ to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser pipe, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol according to the mass ratio of 6: 3: 1, pouring the mixture into the four-neck flask, stirring for 32min at the temperature of 80 ℃, dropwise adding 3 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat for 12min to obtain pretreated dry powder; mixing olive and deionized water according to a mass ratio of 1: 3, placing in an ultrasonic oscillator, performing ultrasonic extraction at 81 deg.C and 27kHz for 32min, filtering to remove residue, collecting filtrate, and distilling the filtrate under reduced pressure for 18min to obtain self-made plant extract; mixing the pre-treated dry powder and the self-made plant extract according to the mass ratio of 3: 1, stirring and reacting for 3 hours to obtain a reaction product, washing the reaction product with absolute ethyl alcohol for 5 times to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven, drying for 4 hours at the temperature of 70 ℃, cooling and discharging to obtain modified dry powder; weighing 50 parts of nylon chips, 16 parts of modified dry powder and 6 parts of absolute ethyl alcohol, mixing and placing the mixture in a mixer, stirring for 2 hours at the rotating speed of 160r/min to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder, extruding and granulating at the temperature of 520 ℃ and the pressure of 5MPa, collecting particles, continuously placing the particles into a spinning machine, spinning for 4 hours at the temperature of 300 ℃ and the spinning speed of 800m/min to obtain a spinning blank, finally placing the spinning blank into a traction machine, drawing for 2 hours at the traction multiple of 4.0 times and the traction speed of 600m/min, and cooling and discharging to obtain the antistatic fiber for preparing the chemical protective clothing.
Comparative example
Antistatic fiber for chemical protective clothing manufactured by Kunshan corporation was used as a comparative example
The antistatic fiber for preparing chemical protective clothing prepared by the invention and the antistatic fiber for preparing chemical protective clothing in the comparative example are detected, and the detection results are shown in table 1:
testing by adopting a surface resistivity tester;
the friction voltage test is detected according to GB/T12703.5-2010;
TABLE 1 coating Property measurement results
According to the data in the table 1, the anti-static fiber for preparing the chemical protective clothing has stable and high grinding efficiency, the grinding crack is reduced by 98 percent compared with the anti-static fiber for preparing the chemical protective clothing in the using process, in addition, static electricity can not be generated, the harm to human health can not be generated, the sample is obviously superior to a comparative sample, and the important market value and social value are realized.
Claims (5)
1. A process for preparing antistatic fibers for preparing chemical protective clothing is characterized by comprising the following specific preparation steps:
(1) mixing, grinding and crushing medical stone and hydrotalcite to obtain ground powder, then placing the ground powder in an oven for drying to obtain dry powder, continuously introducing nitrogen into a four-neck flask with a condenser pipe, a thermometer, a stirrer and a micro-sampling device in advance, mixing the dry powder, deionized water and absolute ethyl alcohol, pouring the mixture into the four-neck flask for stirring, dripping 2-3 drops of ammonia water with the mass fraction of 15% in the stirring process, and preserving heat to obtain pretreated dry powder;
(2) mixing olive and deionized water, placing the mixture in an ultrasonic oscillator for ultrasonic extraction, filtering to remove filter residues, collecting filtrate, and performing reduced pressure distillation on the filtrate to obtain a self-made plant extracting solution;
(3) mixing the pre-treated dry powder and the self-made plant extract, stirring and reacting to obtain a reaction product, washing the reaction product with absolute ethyl alcohol to make the supernatant liquid neutral, collecting the lower-layer solid precipitate, finally placing the lower-layer solid precipitate in a drying oven for drying, cooling and discharging to obtain modified dry powder;
(4) weighing 45-50 parts of polyamide chips, 12-16 parts of modified dry powder and 3-6 parts of absolute ethyl alcohol, mixing and placing in a stirrer for stirring to obtain mixed slurry, pouring the mixed slurry into a double-screw extruder for extrusion and granulation, collecting particles, continuously placing the particles in a spinning machine for spinning to obtain a spinning blank, finally placing the spinning blank in a tractor, drawing at a drawing multiple of 3.5-4.0 times, cooling and discharging to obtain the antistatic fiber for preparing chemical protective clothing.
2. The process for preparing antistatic fibers for chemical protective clothing according to claim 1, wherein: the mass ratio of the medical stone and the hydrotalcite in the step (1) is 1: 3, grinding and crushing for 21-25 min, drying at 60-65 ℃, drying for 15-18 min, wherein the mass ratio of the dry powder to the deionized water to the absolute ethyl alcohol is 6: 3: 1, stirring at 75-80 ℃, stirring for 27-32 min, and keeping the temperature for 10-12 min.
3. The process for preparing antistatic fibers for chemical protective clothing according to claim 1, wherein: the mass ratio of the olives to the deionized water in the step (2) is 1: 3, the ultrasonic extraction temperature is 75-81 ℃, the ultrasonic extraction frequency is 23-27 kHz, the ultrasonic extraction time is 27-32 min, and the reduced pressure distillation time is 15-18 min.
4. The process for preparing antistatic fibers for chemical protective clothing according to claim 1, wherein: the mass ratio of the pretreated dry powder to the self-made plant extract in the step (3) is 3: 1, stirring and reacting for 2-3 h, washing for 3-5 times, drying at 65-70 ℃ for 2-4 h.
5. The process for preparing antistatic fibers for chemical protective clothing according to claim 1, wherein: the stirring speed of the step (4) is 150-160 r/min, the stirring time is 1-2 h, the granulation temperature is 480-520 ℃, the granulation pressure is 3-5 MPa, the spinning temperature is 270-300 ℃, the spinning speed is 760-800 m/min, the spinning time is 3-4 h, the drafting speed is 560-600 m/min, and the drafting time is 1-2 h.
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Citations (5)
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| CN104233501A (en) * | 2014-08-29 | 2014-12-24 | 广东新会美达锦纶股份有限公司 | Preparation method of far infrared PA6 fiber containing multiple inorganic powder |
| CN107761186A (en) * | 2016-08-22 | 2018-03-06 | 湖南景竹新材料开发有限公司 | A kind of preparation method being knitted with digital yarn |
| CN108517578A (en) * | 2018-04-20 | 2018-09-11 | 刘凡领 | A kind of preparation method of modified medical stone base nylon fibre |
| CN109295528A (en) * | 2018-08-29 | 2019-02-01 | 海安县中山合成纤维有限公司 | A kind of production method of functionality 6 alloy germanium far IR fibre of polyamide fibre |
| CN109913172A (en) * | 2018-05-25 | 2019-06-21 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of wear-resisting Antistatic type grinding-material |
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2019
- 2019-12-28 CN CN201911383640.4A patent/CN111041593A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233501A (en) * | 2014-08-29 | 2014-12-24 | 广东新会美达锦纶股份有限公司 | Preparation method of far infrared PA6 fiber containing multiple inorganic powder |
| CN107761186A (en) * | 2016-08-22 | 2018-03-06 | 湖南景竹新材料开发有限公司 | A kind of preparation method being knitted with digital yarn |
| CN108517578A (en) * | 2018-04-20 | 2018-09-11 | 刘凡领 | A kind of preparation method of modified medical stone base nylon fibre |
| CN109913172A (en) * | 2018-05-25 | 2019-06-21 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of wear-resisting Antistatic type grinding-material |
| CN109295528A (en) * | 2018-08-29 | 2019-02-01 | 海安县中山合成纤维有限公司 | A kind of production method of functionality 6 alloy germanium far IR fibre of polyamide fibre |
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