CN114000214B - Improved flash evaporation polyethylene composite material - Google Patents
Improved flash evaporation polyethylene composite material Download PDFInfo
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- CN114000214B CN114000214B CN202111434010.2A CN202111434010A CN114000214B CN 114000214 B CN114000214 B CN 114000214B CN 202111434010 A CN202111434010 A CN 202111434010A CN 114000214 B CN114000214 B CN 114000214B
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- composite material
- barium sulfate
- antimony white
- spinning
- aging treatment
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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
- D01F6/44—Monocomponent 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
- D01F6/46—Monocomponent 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-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
- D04H1/54—Non-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
- D04H1/558—Non-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
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-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
- D04H1/72—Non-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
- D04H1/724—Non-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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
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 auxiliary agent; the loss value delta G of the bending rigidity of the composite material is 0.05-0.4; Δg=1-G2/G1; g1 is the flexural rigidity of the unaged composite material, in mN.cm; 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 aging, and the service life of the product can be prolonged.
Description
[ field of technology ]
The invention relates to the technical field of flash evaporation polyethylene, in particular to an improved flash evaporation polyethylene composite material.
[ background Art ]
Flash spinning, also known as flash spinning, flash spinning or flash spinning, transient solvent evaporation to net, is not melt spinning but dry spinning. 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 resolidified into fibers 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 technology, and is mainly characterized in that the flash evaporation technology adopts lower spinning solution viscosity and ejects the spinning solution from a spinning hole at extremely high pressure and speed. Because of the low viscosity and good fluidity of the solution, the liquid filaments solidify in high speed movement to form very fine fiber filaments, which are finally adsorbed onto a web-forming curtain to form a web directly.
Chinese patent publication No. CN111389288A discloses a method and apparatus for dissolving a polymer in a solvent, the method comprising two stages of series dissolution stages, the first stage using stirring equipment with high shear force and the second stage using equipment with strong convective mixing. The method can be used for efficiently dissolving the polymer in the spinning solvent, so that the discharged spinning solution is more uniform, and stable spinning is facilitated; the material contact time is reduced, and the equipment volume is reduced, so that the material holding quantity is reduced, and the risk value of the pressure container is reduced; the decomposition probability of materials at high temperature is reduced, and the product quality is improved; the amount of pollutants generated by pyrolysis of materials is reduced, and the harm to the environment and the corrosion to equipment are reduced.
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 box is controlled to be below 18 vol%. By the method for introducing the nonflammable gas into the spinning box body to reduce the oxygen content, explosion risks in the solution spinning process are avoided, and production safety is improved. And the solvent requirement can be reduced, the solvent selection range in the solution spinning process can be wider, the method is not limited to halogen-containing hydrocarbon solvents, and hydrocarbon solvents (such as cyclopentane and cyclohexane) with low flash points and only containing carbon atoms and hydrogen atoms can be adopted. In addition, this application through setting up rich VOC tail gas processing system 8, can reduce the organic compound content in the rich VOC tail gas effectively to obtain low VOC's nitrogen gas, so that the tail gas in the messenger spinning box can cyclic utilization, reduced manufacturing cost.
[ invention ]
The invention aims to overcome the defects of the prior art and provides an improved flash evaporation polyethylene composite material.
The aim of the invention is realized by the following technical scheme:
an improved flash evaporation polyethylene composite material is prepared from 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 D65 fluorescence brightness loss value delta F of the flash evaporation sheet is 0.05-0.20;
ΔG＝1-G2/G1；
g1 is the flexural rigidity of the unaged composite material, in mN.cm;
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 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: wavelength is 300-400 nmIrradiance within the range of 60+ -2 w/m 2 The black standard temperature is 65+/-2 ℃, the air temperature of the test bin is 38+/-3 ℃, the relative humidity is 50+/-10%, 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 bending rigidity of the composite material is 0.05-0.1.
The loss value delta G of the bending rigidity of the composite material is 0.1-0.2.
The loss value delta G of the bending rigidity of the composite material is 0.2-0.3.
The loss value delta G of the bending rigidity of the composite material is 0.3-0.4.
The composite auxiliary agent is a compound of antimony white-barium sulfate-magnesium oxide and 1,3, 5-trimethyl-2, 4, 6-tri (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-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 240-245 ℃, and the catalyst has good compatibility with organic solvents, especially with solvents of flash spinning, the melting point is lower than the temperature of flash spinning, the catalyst is suitable for being added as spinning auxiliary agents, and meanwhile, the catalyst is a hindered phenol antioxidant, and can effectively prevent thermal oxidative degradation of polyethylene, thereby preventing yellowing and deterioration of polyethylene composite materials and finally reducing the service cycle of products.
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 10-18%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (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 hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, unsaturated hydrocarbon, halogenated hydrocarbon, alcohol, ester, ether, ketone, nitrile, amide, fluorocarbon.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 the antimony white to the 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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:1-1:2.5.
The mass ratio of the isopropanol to the diphenyldiethoxysilane 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 the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1-1:1.3.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Antimony white and barium sulfate mainly play a role in physical whitening as a common whitening agent, but as an inorganic material, the dispersibility of the antimony white and the barium sulfate in a matrix is poor, so that the strength of the matrix is affected, and the whitening effect is deteriorated; the existing conventional method mainly adopts a coupling agent to modify the brightening agent to improve the compatibility with a matrix, but the brightening agent is inevitably degraded due to the introduction of organic components, particularly silicon-containing materials; and 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is used as an organic antioxidant, and has the main function of antioxidation, and the antioxidation effect is realized by using a group on a conjugated structure through a large conjugated structure in a molecule, but the binding force of the anti-oxidant and a matrix is weak, so that the strong loss on the matrix is large. According to the preparation method, diphenyl diethoxy silane is used as a coupling agent, and in order to have certain binding force with a matrix, the influence of a silicon-containing material on the molecules of the whitening agent is eliminated, magnesium ions with molecular chelation are introduced into the preparation process of the whitening agent, and the magnesium ions are introduced into 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 can be used as a large conjugated structure to have affinity with 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, so that the problem of weaker bonding force between 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and a matrix is avoided, the influence of the introduction of the whitening agent on the strength of the matrix is ensured, and meanwhile, the introduction of the coupling agent containing the benzene ring structure can play a synergistic whitening function with 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene, so that the damage to the matrix material caused by a single whitening agent or antioxidant is avoided.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 165-230 ℃, obtaining flash evaporation fiber, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 110-125 ℃.
Compared with the prior art, the invention has the following positive effects:
the flash evaporation sheet has the advantages that the brightness is kept, the bending length of the flash evaporation sheet is reduced, the service life of a product can be prolonged, and the application range is enlarged.
[ detailed description ] of the invention
Specific embodiments of an improved flash-distilled polyethylene composite of the present invention are provided below.
1. Flexural rigidity
The bending length of the fabric is one of characteristic indexes for representing the bending deformation resistance of the fabric, reflects the stiffness degree of the fabric, and a method for measuring the stiffness of the fabric at home and abroad is generally a slope method. Sampling tests were carried out by means of a bending length meter according to GB/T18318-2001 (determination of the bending length of textile fabrics) according to this national standard, the specific detailed test procedure being described internationally, a brief description of which is given here: the method comprises the steps of preparing 12 samples, wherein the long sides of 6 samples are parallel to the production and processing directions of the thin sheet, and the long sides of the other 6 samples are perpendicular to the production and processing directions of the thin sheet; the test was performed separately in two groups. The specific test process is as follows: a rectangular sample in a certain 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 is enabled to extend the platform and bend under the dead weight, the extending part is suspended, and the other end of the platform is pressed by a ruler. When the head end of the sample passes through the front edge of the platform and reaches the inclined plane with an inclination angle of 41.5 degrees with the horizontal line, the extension length is 2 times of the bending length of the sample, so that the bending length of one direction is calculated, the other end and the two ends of the other surface are replaced, the four bending lengths of the rectangular sample are respectively tested, then the steps are repeated, the rest 5 samples are tested, the measured bending lengths are averaged, the average bending length of the sample in one direction is obtained, and the average bending rigidity is calculated. Repeating the steps, continuously testing another group of samples, and measuring the average bending length in the other direction; further, the average bending rigidity was calculated. The average bending stiffness in both directions was again averaged to obtain the bending stiffness of the sample.
2. Aging treatment
The aging treatment process conditions are as follows: irradiance of 300-400 nm is 60+ -2 w/m2, black standard temperature is 65+ -2 ℃, air temperature of test chamber is 38+ -3 ℃, relative humidity is 50+ -10%, and drying time is 168 hours.
3. D65 fluorescent brightness
Whiteness is the degree of whiteness from ideal, and also the degree of whiteness of the surface of a substance, expressed as a percentage of the white content. Brightness test is specifically described in GBT 7974-2013 for determination of blue diffuse reflectance factor D65 of paper, paperboard and pulp, and the test is performed according to the paper and paperboard method to determine D on the front side of the sample 65 Fluorescent brightness of F Positive direction The D65 fluorescence brightness of the back of the sample is measured to be F Back of body Again, this definition: d65 fluorescence brightness f= (F) of sample Positive direction +F Back of body )/2. D65 refers to fluorescence excited with a D65 light source, about ISO2470-1.
Example 1
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 10%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (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%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:1.
The mass ratio of the isopropanol to the diphenyldiethoxysilane is 1:0.04.
The mass ratio of diphenyldiethoxysilane to vinyltrimethoxysilane is 1:1.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 195 ℃, obtaining flash evaporation fiber, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 110 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 2
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 11%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the modified flash evaporation polyethylene composite material is 0.05%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:1-1:2.5.
The mass ratio of the isopropanol to the diphenyldiethoxysilane is 1:0.08.
The mass ratio of diphenyldiethoxysilane to vinyltrimethoxysilane was 1:1.1.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1.1.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 200 ℃, obtaining flash evaporation fiber, 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 GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 3
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 13%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the modified flash evaporation polyethylene composite material is 0.25%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:1.8.
The mass ratio of the isopropanol to the diphenyldiethoxysilane is 1:0.15.
The mass ratio of diphenyldiethoxysilane to vinyltrimethoxysilane was 1:1.2.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1.2.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, obtaining flash evaporation fiber, 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 GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 4
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 14%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene.
The mass fraction of the composite additive in the modified flash evaporation polyethylene composite material is 0.35%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:2.
The mass ratio of the isopropanol to the diphenyldiethoxysilane is 1:0.18.
The mass ratio of diphenyldiethoxysilane to vinyltrimethoxysilane was 1:1.2.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1.2.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 210 ℃, obtaining flash evaporation fiber, 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 GBT 7974-2013, GBT 7974-2013 and aging treatment.
Example 5
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 15%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
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-tri (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%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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-tri (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 aqueous solution of isopropanol 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 initial product to the diphenyl diethoxysilane is 1:2.5.
The mass ratio of the isopropanol to the diphenyldiethoxysilane is 1:0.25.
The mass ratio of diphenyldiethoxysilane to vinyltrimethoxysilane was 1:1.3.
The mass ratio of the modified antimony white-barium sulfate-magnesium oxide composite material to the 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene is 1:1-1:1.3.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 215 ℃, obtaining flash evaporation fiber, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 125 ℃. The performance parameters of the test samples are shown in Table 1 according to national standards GBT 7974-2013, GBT 7974-2013 and aging treatment.
Comparative example 1
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 13%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the mass fraction of the composite additive in the modified flash evaporation polyethylene composite material is 0.25%.
The raw materials of the composite auxiliary agent 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: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, obtaining flash evaporation fiber, 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 GBT 7974-2013, GBT 7974-2013 and aging treatment.
Comparative example 2
The production process of improved flash evaporation polyethylene composite material includes the following steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the mass fraction of the spinning raw material in the spinning solution is 13%;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the composite auxiliary agent is a modified antimony white-barium sulfate-magnesium oxide composite material.
The mass fraction of the composite additive in the modified flash evaporation polyethylene composite material is 0.25%.
The production process of composite assistant includes the following steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain antimony white-barium sulfate-magnesium oxide, namely 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 aqueous solution of isopropanol is 8%.
The molar ratio of the antimony white-barium sulfate composite material to the magnesium chloride is 1:0.25.
The calcination process is to rapidly raise the temperature below 300 ℃ at 20 ℃/min and slowly raise the temperature at 300-550 ℃ at 10 ℃/min.
Step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 205 ℃, obtaining flash evaporation fiber, 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 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 merely a preferred embodiment of the present invention, and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the concept of the present invention, and are intended to be within the scope of the present invention.
Claims (15)
1. An improved flash evaporation polyethylene composite material is characterized in that 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 D65 fluorescence brightness loss value delta F of the flash evaporation sheet is 0.05-0.20;
△G=1-G2/G1；
g1 is the flexural rigidity of the unaged composite material, in mNCm;
g2 is the bending rigidity of the composite material after aging treatment, and the unit is mNCm;
the bending rigidity G2 of the composite material after aging treatment is 20-100 mNCm;
△F=1-F2/F1
f1 is D65 fluorescence brightness of the flash sheet without aging treatment;
f2 is the D65 fluorescence brightness of the flash evaporation sheet after aging treatment;
ageing treatment process stripThe piece is: irradiance of 60+ -2 w/m in the wavelength range of 300-400 nm 2 The black standard temperature is 65+/-2 ℃, the air temperature of the test bin is 38+/-3 ℃, the relative humidity is 50+/-10%, and the drying time is 168 hours;
the production method of the improved flash evaporation polyethylene composite material comprises the following specific steps:
step one: preparing spinning solution, adding a solvent into a reaction kettle, adding spinning raw materials into the solvent, and dissolving to obtain spinning solution;
the spinning raw material comprises polyethylene and a composite auxiliary agent;
the production method of the composite additive comprises the following specific steps:
grinding antimony white, barium sulfate and polyvinyl alcohol by a dry method to obtain a antimony white-barium sulfate double-layer composite material; adding the antimony white-barium sulfate composite material into an aqueous solution of isopropanol, adding a magnesium chloride solution, adsorbing on the surface of the antimony white-barium sulfate double-layer material to generate magnesium hydroxide precipitate, filtering, drying and calcining to obtain an antimony white-barium sulfate-magnesium oxide primary product; dispersing the antimony white-barium sulfate-magnesium oxide initial product in the isopropanol water solution of diphenyl diethoxy silane, adding vinyl trimethoxy silane, treating for 10-25 minutes at 45-62 ℃, 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 a composite auxiliary agent;
step two: spinning, namely spinning the spinning solution obtained in the step one by a flash evaporation method, wherein the spinning temperature is 165-230 ℃, obtaining flash evaporation fiber, and performing hot press molding to obtain flash evaporation non-woven fabric, wherein the hot press temperature is 110-125 ℃.
2. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 20-30 mNcm.
3. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 30-40 mNcm.
4. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 40-50 mNcm.
5. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 50-60 mNcm.
6. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 60-70 mNcm.
7. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 70-80 mNcm.
8. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 80-90 mNcm.
9. An improved flash-distilled polyethylene composite material according to claim 1, wherein the flexural rigidity G2 of the composite material after aging treatment is 90-100 mNcm.
10. An improved flash-distilled polyethylene composite material according to claim 1, wherein the composite material has a flexural rigidity loss value Δg of 0.05 to 0.1.
11. An improved flash-distilled polyethylene composite material according to claim 1, wherein the composite material has a flexural rigidity loss value Δg of 0.1 to 0.2.
12. An improved flash-distilled polyethylene composite material according to claim 1, wherein the composite material has a flexural rigidity loss value Δg of 0.2 to 0.3.
13. An improved flash-distilled polyethylene composite material according to claim 1, wherein the composite material has a flexural rigidity loss value Δg of 0.3 to 0.4.
14. An improved flash-evaporated polyethylene composite material according to claim 1, wherein the mass fraction of the composite auxiliary agent in the improved flash-evaporated polyethylene composite material is 0.01-0.5%.
15. The improved flash evaporation polyethylene composite material according to claim 1, wherein the composite auxiliary agent 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.
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