CN114000214A - Improved flash evaporation polyethylene composite material - Google Patents

Improved flash evaporation polyethylene composite material Download PDF

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Publication number
CN114000214A
CN114000214A CN202111434010.2A CN202111434010A CN114000214A CN 114000214 A CN114000214 A CN 114000214A CN 202111434010 A CN202111434010 A CN 202111434010A CN 114000214 A CN114000214 A CN 114000214A
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composite material
flash evaporation
aging treatment
polyethylene
barium sulfate
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CN202111434010.2A
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CN114000214B (en
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叶孔萌
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Jiangsu Qingyun New Material Technology Co ltd
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Jiangsu Qingyun New Material Technology Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/558Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in combination with mechanical or physical treatments other than embossing
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/724Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged forming webs during fibre formation, e.g. flash-spinning

Abstract

The invention relates to an improved flash evaporation polyethylene composite material which is characterized in that the raw materials of the composite material are polyethylene and a composite additive; the loss value delta G of the bending rigidity of the composite material is 0.05-0.4; Δ G ═ 1-G2/G1; g1 is the flexural rigidity in mN cm of the composite material without aging treatment; g2 is the bending rigidity of the composite material after aging treatment, and the unit is mN cm; the bending rigidity G2 of the composite material after aging treatment is 20-100 mN & cm. The product of the application still has certain bending rigidity after ageing, can postpone the life of product.

Description

Improved flash evaporation polyethylene composite material
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of flash polyethylene, in particular to an improved flash polyethylene composite material.
[ background of the invention ]
Flash spinning, also called flash evaporation method, flash spinning method or flash spinning, instantaneous solvent evaporation web forming method, not melt spinning, but dry spinning technology is adopted. The high polymer is dissolved in a certain solvent to prepare spinning solution, and then the spinning solution is sprayed out from a spinneret orifice, and the high polymer is solidified into fibers again due to the rapid volatilization of the solvent. The dry spinning technology adopted by the flash evaporation method is different from the common dry spinning, and is mainly characterized in that the flash evaporation process adopts lower viscosity of spinning solution and sprays the spinning solution from a spinneret orifice at extremely high pressure and speed. Because the solution has low viscosity and good fluidity, the liquid filaments are solidified to form extremely fine fiber filaments in high-speed motion and finally adsorbed on a net forming curtain to directly form a fiber net.
Chinese patent publication No. CN111389288A discloses a method and apparatus for dissolving a polymer in a solvent, the method comprising two stages of dissolution in series, the first stage using a stirring apparatus with high shear, and the second stage using an apparatus with strong convective mixing. The method can efficiently dissolve the polymer in the spinning solvent, so that the discharged spinning solution is more uniform, and stable spinning is facilitated; the contact time of the materials is reduced, and the volume of the equipment is reduced, so that the holding quantity of the materials is reduced, and the risk value of the pressure container is reduced; the decomposition probability of the materials at high temperature is reduced, and the product quality is improved; reduce the amount of pollutants generated by the pyrolysis of materials, and reduce the harm to the environment and the corrosion to equipment.
Chinese patent publication No. CN111286790A discloses a safe solution spinning method, which is characterized in that in the solution spinning process, the oxygen content of the mixed gas in the spinning beam is controlled below 18 vol%. By the method for introducing the non-combustible gas into the spinning manifold to reduce the oxygen content, the explosion risk in the solution spinning process is avoided, and the production safety is improved. And the requirement on the solvent can be reduced, the selection range of the solvent in the solution spinning process can be wider, the solvent is not limited to halogen-containing hydrocarbon solvents, and low-flash-point hydrocarbon solvents (such as cyclopentane and cyclohexane) containing only carbon atoms and hydrogen atoms can also be adopted. In addition, this application can reduce the organic compound content in the rich VOC tail gas effectively through setting up rich VOC tail gas processing system 8 to obtain low VOC's nitrogen gas, so that make the tail gas in the spinning manifold can cyclic utilization, reduced manufacturing cost.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides an improved flash evaporation polyethylene composite material.
The purpose of the invention is realized by the following technical scheme:
an improved flash evaporation polyethylene composite material, wherein the raw materials of the composite material are polyethylene and a composite auxiliary agent; the loss value delta G of the bending rigidity of the composite material is 0.05-0.4; the loss value delta F of the D65 fluorescence brightness of the flash evaporation sheet is 0.05-0.20;
ΔG=1-G2/G1;
g1 is the flexural rigidity in mN cm of the composite material without aging treatment;
g2 is the bending rigidity of the composite material after aging treatment, and the unit is mN cm;
the bending rigidity G2 of the composite material after aging treatment is 20-100 mN & cm;
ΔF=1-F2/F1
f1 is the D65 fluorescence brightness of the flash sheet without aging treatment;
f2 is the D65 fluorescence brightness of the flash evaporation sheet after aging treatment;
the aging treatment process conditions are as follows: the irradiance of the wave length in the range of 300-400 nm is 60 +/-2 w/m2The black standard temperature is 65 +/-2 ℃, the air temperature of the test chamber is 38 +/-3 ℃, the relative humidity is 50 +/-10 percent, and the drying time is 168 hours.
The bending rigidity G2 of the composite material after aging treatment is 20-30 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 30-40 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 40-50 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 50-60 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 60-70 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 70-80 mN · cm.
The bending rigidity G2 of the composite material after aging treatment is 80-90 mN & cm.
The bending rigidity G2 of the composite material after aging treatment is 90-100 mN & cm.
The loss value Delta G of the flexural rigidity of the composite material is 0.05-0.1.
The loss value Delta G of the flexural rigidity of the composite material is 0.1-0.2.
The loss value Delta G of the flexural rigidity of the composite material is 0.2-0.3.
The loss value Delta G of the flexural rigidity of the composite material is 0.3-0.4.
The composite additive is a compound of antimony white-barium sulfate-magnesium oxide and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene with a three-layer composite structure.
The melting point of the 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 240-245 ℃, the benzene has good compatibility with an organic solvent, particularly good compatibility with a solvent for flash spinning, the melting point of the benzene is lower than the temperature for flash spinning, the benzene is suitable for being added as a spinning auxiliary agent, and the benzene is a hindered phenol antioxidant which can effectively prevent the thermal oxidative degradation of polyethylene, so that the yellowing and deterioration of the polyethylene composite material are prevented, and the service cycle of a product is finally reduced.
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 10-18%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.01-0.5%.
The solvent is selected from aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, unsaturated hydrocarbons, halogenated hydrocarbons, alcohols, esters, ethers, ketones, nitriles, amides, and fluorocarbon compounds.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.01-1: 0.05.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol aqueous solution is 3-13%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.2-1: 0.3.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1: 1-1: 2.5.
The mass ratio of the isopropanol to the diphenyl diethoxysilane is 1: 0.04-1: 0.25.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1: 1-1: 1.3.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1: 1-1: 1.3.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Antimony white and barium sulfate, which are commonly used whitening agents, mainly play a role in physical whitening, but as inorganic materials, the antimony white and the barium sulfate have poor dispersibility in a matrix, so that the strength of the matrix is influenced, and the whitening effect is poor; the existing conventional method mainly adopts a coupling agent to modify the whitening agent, so as to improve the compatibility with a matrix, but inevitably leads to the introduction of organic components, particularly silicon-containing materials, to cause the deterioration of the whitening agent; 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is used as an organic antioxidant, the main function of the organic antioxidant is antioxidation, the antioxidation effect is realized by utilizing radicals on a conjugated structure through a large conjugated structure in a molecule, but the bonding force between the organic antioxidant and a matrix is weak, so that the strong loss to the matrix is large. In the method, diphenyldiethoxysilane is used as a coupling agent, and in order to have a certain binding force with a substrate and eliminate the influence of a silicon-containing material on the molecules of the whitening agent, magnesium ions with a molecular chelation effect are introduced in the preparation process of the whitening agent and introduced on the surface of the whitening agent, so that the influence of the coupling agent on the whitening agent is eliminated; meanwhile, the benzene ring structure introduced into the whitening agent molecule as a large conjugated structure can have affinity with 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, thereby avoiding the problem that the bonding force of the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and the matrix is weaker, ensuring the influence of the introduction of the whitening agent on the matrix strength, meanwhile, the introduction of the coupling agent containing a benzene ring structure can play a role in synergistic whitening with 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, so that the damage to a matrix material caused by a single whitening agent or antioxidant is avoided.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method at the spinning temperature of 165-230 ℃ to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabrics at the hot press temperature of 110-125 ℃.
Compared with the prior art, the invention has the following positive effects:
the flash evaporation sheet material keeps brightness, meanwhile, the reduction of the bending length is low, the service life of a product can be prolonged, and the application range is expanded.
[ detailed description ] embodiments
The following provides specific embodiments of an improved flash-evaporated polyethylene composite material according to the present invention.
First, bending rigidity
The bending length of the fabric is one of characteristic indexes for representing the bending deformation resistance of the fabric, the stiffness degree of the fabric is reflected, and a method for measuring the stiffness of the fabric at home and abroad is generally a slope method. The sampling test was carried out by means of a bending length meter according to GB/T18318-2001 (determination of the bending length of textile fabrics), according to the national standard, the detailed test procedure being described in International, which is briefly mentioned here: making the samples into 12 samples, wherein the long sides of 6 samples are parallel to the production and processing direction of the sheet, and the long sides of the other 6 samples are perpendicular to the production and processing direction of the sheet; the test was carried out in two groups. The specific test process is as follows: a rectangular sample in a group of samples is prevented from being on a horizontal platform, the long axis of the sample is parallel to the long axis of the platform, the sample is pushed along the long axis direction of the platform, the sample extends out of the platform and bends under the self-weight, the extending part is suspended, and the sample is pressed by a ruler and still positioned at the other end of the platform. When the head end of the sample passes through the front edge of the platform and reaches an inclined plane with an inclination angle of 41.5 degrees with the horizontal line, the extending length is equal to 2 times of the bending length of the sample, so that the bending length in one direction is calculated, the other end is replaced, the two ends of the other surface are replaced, the four bending lengths of the rectangular sample are obtained through respective tests, then the steps are repeated, the remaining 5 samples are tested, the measured bending lengths are averaged, the average bending length in one direction of the sample is obtained, and the average bending rigidity is further calculated. Repeating the steps, continuously testing another group of samples, and measuring the average bending length in another direction; and then the average bending rigidity is calculated. The average bending stiffness in both directions was again averaged to obtain the bending stiffness of the sample.
Second, aging treatment
The aging treatment process conditions are as follows: the irradiance with the wavelength within the range of 300-400 nanometers is 60 +/-2 w/m2, the black mark temperature is 65 +/-2 ℃, the air temperature of the test chamber is 38 +/-3 ℃, the relative humidity is 50 +/-10%, and the drying time is 168 hours.
III, D65 fluorescence intensity
Whiteness is the degree of whiteness from the ideal whiteness, and also the degree of whiteness on the surface of a material, expressed as a percentage of the white content. The brightness test is specifically referred to the measurement of the brightness of the blue light diffuse reflection factor D65 of GBT 7974-2013 paper, paperboard and pulp, and the test is carried out according to the method of the paper and the paperboard, and the D of the front surface of the sample is measured65Fluorescence intensity of FIs justD65 fluorescence intensity on the back of the sample was measured as FBack of bodyThen, this definition: d65 fluorescence intensity of sample F ═ F (F)Is just+FBack of body)/2. D65 refers to fluorescence excited with a D65 light source, about ISO 2470-1.
Example 1
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 10 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.03%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.01.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 3%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.2.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1:1.
The mass ratio of isopropanol to diphenyldiethoxysilane was 1: 0.04.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1:1.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method at the spinning temperature of 195 ℃ to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabrics at the hot press temperature of 110 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 2
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 11 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.05%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.02.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 8%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.25.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1: 1-1: 2.5.
The mass ratio of isopropanol to diphenyldiethoxysilane was 1: 0.08.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1: 1.1.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1: 1.1.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 200 ℃, so as to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 15 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 3
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 13 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.25%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.03.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 8%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.25.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1: 1.8.
The mass ratio of isopropanol to diphenyldiethoxysilane was 1: 0.15.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1: 1.2.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1: 1.2.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, so as to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 118 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 4
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 14 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.35%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.04.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 10%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.25.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1:2.
The mass ratio of isopropanol to diphenyldiethoxysilane was 1: 0.18.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1: 1.2.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1: 1.2.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 210 ℃, so as to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 120 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 5
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 15 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a compound of a modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.5%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the primary antimony white-barium sulfate-magnesium oxide product in isopropanol water solution of diphenyldiethoxysilane, adding vinyltrimethoxysilane, treating at 45-62 ℃ for 10-25 minutes, filtering, and vacuum drying filter residues to obtain a modified antimony white-barium sulfate-magnesium oxide composite material; grinding and mixing the modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene to obtain the composite additive.
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1:1: 0.05.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 13%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.3.
The mass ratio of the antimony white-barium sulfate-magnesium oxide primary product to the diphenyl diethoxysilane is 1: 2.5.
The mass ratio of isopropanol to diphenyldiethoxysilane was 1: 0.25.
The mass ratio of the diphenyl diethoxy silane to the vinyl trimethoxy silane is 1: 1.3.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1: 1-1: 1.3.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method at the spinning temperature of 215 ℃ to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabrics at the hot press temperature of 125 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Comparative example 1
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 13 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.25%.
The raw materials of the composite additive are antimony white, barium sulfate, magnesium oxide and polyvinyl alcohol; the mass ratio of antimony white to barium sulfate is 1: 1; the mass ratio of antimony white to polyvinyl alcohol is 1: 0.03; the mass ratio of antimony white to magnesium oxide is 1: 0.25.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, so as to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 118 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
Comparative example 2
A production method of an improved flash evaporation polyethylene composite material comprises the following specific steps:
the method comprises the following steps: preparing a spinning solution, adding a solvent into a reaction kettle, adding a spinning raw material into the solvent, and dissolving to obtain a spinning solution;
the mass fraction of the spinning raw materials in the spinning solution is 13 percent;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite additive is a modified antimony white-barium sulfate-magnesium oxide composite material.
The mass fraction of the composite additive in the improved flash evaporation polyethylene composite material is 0.25%.
A production method of a composite additive comprises the following specific steps:
carrying out dry grinding on antimony white, barium sulfate and polyvinyl alcohol to obtain an antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an isopropanol aqueous solution, adding a magnesium chloride solution, adsorbing the magnesium hydroxide precipitate on the surface of the antimony white-barium sulfate double-layer material, filtering, drying, and calcining to obtain antimony white-barium sulfate-magnesium oxide, namely the composite auxiliary agent; .
The mass ratio of antimony white to barium sulfate is 1:1.
The mass ratio of antimony white to polyvinyl alcohol is 1: 0.03.
The volume ratio of isopropanol to water in the aqueous solution of isopropanol was 1:1.
The mass fraction of the antimony white-barium sulfate composite material in the isopropanol water solution is 8%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1: 0.25.
The calcination process comprises the steps of rapidly heating at the temperature of below 300 ℃ at the heating rate of 20 ℃/min, slowly heating at the temperature of 300-550 ℃ at the heating rate of 10 ℃/min.
Step two: and (3) spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, so as to obtain flash evaporation fibers, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 118 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards of GBT 7974-2013, GBT 7974-2013 and aging treatment.
TABLE 1 test data Table for examples and comparative examples
G2 G1 ΔG F2 F1 ΔF
Example 1 21.89 33.81 0.356 0.718 0.853 0.158
Example 2 33.21 46.15 0.280 0.74 0.861 0.141
Example 3 47.81 62.61 0.236 0.77 0.873 0.118
Example 4 63.82 71.91 0.113 0.803 0.880 0.087
Example 5 84.63 90.87 0.069 0.841 0.900 0.066
Comparative example 1 24.6 25.42 0.032 0.569 0.754 0.245
Comparative example 2 31.32 60.54 0.483 0.825 0.862 0.043
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.

Claims (15)

1. An improved flash evaporation polyethylene composite material is characterized in that raw materials of the composite material are polyethylene and a composite additive; the loss value delta G of the bending rigidity of the composite material is 0.05-0.4; the loss value delta F of the D65 fluorescence brightness of the flash evaporation sheet is 0.05-0.20;
ΔG=1-G2/G1;
g1 is the flexural rigidity in mN cm of the composite material without aging treatment;
g2 is the bending rigidity of the composite material after aging treatment, and the unit is mN cm;
the bending rigidity G2 of the composite material after aging treatment is 20-100 mN & cm;
ΔF=1-F2/F1
f1 is the D65 fluorescence brightness of the flash sheet without aging treatment;
f2 is the D65 fluorescence brightness of the flash evaporation sheet after aging treatment;
the aging treatment process conditions are as follows: the irradiance of the wave length in the range of 300-400 nm is 60 +/-2 w/m2The black standard temperature is 65 +/-2 ℃, the air temperature of the test chamber is 38 +/-3 ℃, the relative humidity is 50 +/-10 percent, and the drying time is 168 hours.
2. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 20-30 mN-cm.
3. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 30-40 mN-cm.
4. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 40-50 mN-cm.
5. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 50-60 mN-cm.
6. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 60-70 mN-cm.
7. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 70-80 mN-cm.
8. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 80-90 mN-cm.
9. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the bending stiffness G2 of the composite material after aging treatment is 90-100 mN-cm.
10. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the loss Δ G of flexural rigidity of the composite material is 0.05-0.1.
11. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the loss Δ G of flexural rigidity of the composite material is 0.1-0.2.
12. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the loss Δ G of flexural rigidity of the composite material is 0.2-0.3.
13. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the loss Δ G of flexural rigidity of the composite material is 0.3-0.4.
14. The improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the mass fraction of the composite auxiliary agent in the improved flash evaporation polyethylene composite material is 0.01-0.5%.
15. An improved flash evaporation polyethylene composite material as claimed in claim 1, wherein the composite auxiliary agent is a compound of modified antimony white-barium sulfate-magnesium oxide composite material and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
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