CN114575041A - Hydrophilic spun-bonded nonwoven fabric, preparation method thereof and hydrophilic silk thread - Google Patents
Hydrophilic spun-bonded nonwoven fabric, preparation method thereof and hydrophilic silk thread Download PDFInfo
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- CN114575041A CN114575041A CN202210191580.1A CN202210191580A CN114575041A CN 114575041 A CN114575041 A CN 114575041A CN 202210191580 A CN202210191580 A CN 202210191580A CN 114575041 A CN114575041 A CN 114575041A
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- hydrophilic
- polypropylene
- spun
- oleic acid
- propylene
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- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title abstract description 58
- 239000004743 Polypropylene Substances 0.000 claims abstract description 61
- -1 polypropylene Polymers 0.000 claims abstract description 61
- 229920001155 polypropylene Polymers 0.000 claims abstract description 61
- 239000005642 Oleic acid Substances 0.000 claims abstract description 59
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 57
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 54
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 54
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 54
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 53
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 21
- WPDDXKNWUVLZMQ-UHFFFAOYSA-M potassium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound [K+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F WPDDXKNWUVLZMQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000012968 metallocene catalyst Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000002074 melt spinning Methods 0.000 claims abstract description 4
- 238000009987 spinning Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 61
- VWOTWOPAYZNLIU-UHFFFAOYSA-L C[SiH]C.Cl[Zr](Cl)(C1C=CC=C1)C1C=CC=C1 Chemical compound C[SiH]C.Cl[Zr](Cl)(C1C=CC=C1)C1C=CC=C1 VWOTWOPAYZNLIU-UHFFFAOYSA-L 0.000 claims description 26
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- CPOFMOWDMVWCLF-UHFFFAOYSA-N methyl(oxo)alumane Chemical compound C[Al]=O CPOFMOWDMVWCLF-UHFFFAOYSA-N 0.000 claims description 21
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004744 fabric Substances 0.000 claims description 6
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000012442 inert solvent Substances 0.000 claims description 4
- WPDDXKNWUVLZMQ-UHFFFAOYSA-N potassium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoic acid Chemical compound [K+].OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F WPDDXKNWUVLZMQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 125000003944 tolyl group Chemical group 0.000 claims 1
- 230000035515 penetration Effects 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 238000001223 reverse osmosis Methods 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 44
- 229910052757 nitrogen Inorganic materials 0.000 description 22
- 238000011049 filling Methods 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 238000010926 purge Methods 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- QRUYYSPCOGSZGQ-UHFFFAOYSA-L cyclopentane;dichlorozirconium Chemical compound Cl[Zr]Cl.[CH]1[CH][CH][CH][CH]1.[CH]1[CH][CH][CH][CH]1 QRUYYSPCOGSZGQ-UHFFFAOYSA-L 0.000 description 3
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000005098 hot rolling Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 239000002759 woven fabric Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- AQZWEFBJYQSQEH-UHFFFAOYSA-N 2-methyloxaluminane Chemical compound C[Al]1CCCCO1 AQZWEFBJYQSQEH-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004750 melt-blown nonwoven Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
-
- 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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
-
- 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
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/30—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising olefins as the major constituent
-
- 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
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/36—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated carboxylic acids or unsaturated organic esters as the major constituent
-
- 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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/007—Addition polymers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The application relates to the field of spun-bonded non-woven fabrics, and particularly discloses a hydrophilic spun-bonded non-woven fabric, a preparation method thereof and hydrophilic silk threads. The hydrophilic spun-bonded non-woven fabric is made of hydrophilic silk threads, and the material of the hydrophilic silk threads comprises hydrophilic polypropylene; the hydrophilic polypropylene is obtained by copolymerizing propylene and oleic acid under the action of a metallocene catalyst. The preparation method of the hydrophilic spun-bonded non-woven fabric comprises the steps of taking hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate, and spinning to prepare hydrophilic threads; and laying hydrophilic threads into a net and bonding to obtain the hydrophilic spun-bonded non-woven fabric. The hydrophilic silk thread is prepared by melt spinning hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate. The spun-bonded non-woven fabric obtained by the application has the water drop penetration time of less than 1s and the reverse osmosis amount of less than 0.2g, and shows good hydrophilicity. The application endows the spun-bonded non-woven fabric prepared by the copolymerization product of the oleic acid and the propylene with good and durable hydrophilicity through the synergistic cooperation of the oleic acid and the propylene.
Description
Technical Field
The application relates to the field of spun-bonded nonwovens, in particular to a hydrophilic spun-bonded nonwoven, a preparation method thereof and hydrophilic threads.
Background
A nonwoven fabric refers to a sheet material made by forming fibers into a network structure by orientation or random arrangement, and then combining them with each other by mechanical, thermal bonding, chemical bonding, and the like. The non-woven fabric has the advantages of flexibility, lightness, thinness, low price, recycling and the like, and is widely used by various industries.
The nonwoven fabric may be classified into spunlace nonwoven fabric, heat-seal nonwoven fabric, wet-process nonwoven fabric, spunbond nonwoven fabric, melt-blown nonwoven fabric, stitch-bonded nonwoven fabric, and the like. The spun-bonded non-woven fabric is an important non-woven fabric and is prepared by the following steps: the polymer is extruded and stretched to form a thread; laying the silk threads into a fiber web; the fiber web is then subjected to self-bonding, thermal bonding, chemical bonding or mechanical consolidation to form a nonwoven fabric.
The polypropylene is the main raw material of the spun-bonded non-woven fabric due to the characteristics of light weight, stable performance, high cost performance, no odor, no toxicity and the like; however, the polypropylene spun-bonded non-woven fabric has poor hydrophilicity, which limits the application of the polypropylene spun-bonded non-woven fabric in the fields of disposable sanitary products (such as paper diapers) and the like.
Disclosure of Invention
In order to improve the hydrophilicity of the spun-bonded non-woven fabric made of polypropylene, the application provides a hydrophilic spun-bonded non-woven fabric, a preparation method thereof and hydrophilic threads.
In a first aspect, a hydrophilic spun-bonded nonwoven fabric is provided, which adopts the following technical scheme:
the hydrophilic spun-bonded non-woven fabric is made of hydrophilic threads, and the hydrophilic threads comprise hydrophilic polypropylene;
the hydrophilic polypropylene is obtained by copolymerizing propylene and oleic acid under the action of a metallocene catalyst.
By adopting the technical scheme, the oleic acid has better hydrophilicity, and the hydrophilicity of the copolymerization product of the oleic acid and the propylene can be improved through the synergistic cooperation of the oleic acid and the propylene, so that the silk threads made of the copolymerization product and the spun-bonded non-woven fabric have good hydrophilicity. Meanwhile, as the oleic acid is combined with the propylene in a polymerization mode, in the molecular chain of the copolymerization product of the oleic acid and the propylene, the oleic acid unit and the propylene unit are firmly combined, and the hydrophilicity durability of the obtained spun-bonded non-woven fabric is improved.
In a particular possible embodiment, the hydrophilic polypropylene is in particular made by the following process:
p1, introducing propylene into an oxygen-free reaction vessel;
p2, adding an inert solvent, dimethylsilylbis (cyclopentadienyl) zirconium dichloride, methylaluminoxane and oleic acid into a reaction vessel;
p3, raising the temperature of the reaction vessel to at least 60 ℃ and preserving the temperature to ensure that the propylene and the oleic acid have copolymerization reaction;
p4, introducing a hydrochloric acid-ethanol solution to terminate the copolymerization reaction;
p5, filtering and washing to obtain the hydrophilic polypropylene.
By adopting the technical scheme, the preparation process of the hydrophilic polypropylene is optimized, so that the spun-bonded non-woven fabric with better hydrophilic performance is obtained.
In a specific embodiment, the mass ratio of propylene to oleic acid is 1: (0.7-2.1).
By adopting the technical scheme, the proportion of the propylene and the oleic acid is optimized, so that the spun-bonded non-woven fabric prepared from the polymerization products of the propylene and the oleic acid has good hydrophilicity and also has mechanical properties.
In a specific possible embodiment, in said P2, the concentration of said dimethylsilylbis (cyclopentadienyl) zirconium dichloride in the reaction vessel is from 2 to 3 mmol/L.
By adopting the technical scheme, the adding amount of the dimethyl silicon-based bis (cyclopentadienyl) zirconium dichloride serving as a catalyst in the copolymerization reaction of the oleic acid and the propylene is optimized, and the copolymerization reaction of the oleic acid and the propylene is favorably carried out smoothly, so that the propylene-oleic acid copolymer (hydrophilic polypropylene) with a more stable structure can be obtained, and the spunbonded nonwoven fabric with better performance can be obtained.
In a specific possible embodiment, in said P2, the molar ratio of said methylalumoxane to dimethylsilylbis (cyclopentadienyl) zirconium dichloride is (6-12): 1.
by adopting the technical scheme, the proportion of the catalyst methylaluminoxane and the dimethyl silicon-based bis (cyclopentadienyl) zirconium dichloride is optimized, the propylene-oleic acid copolymer is facilitated to obtain more ideal performance, and further the method has positive significance for obtaining the spunbonded non-woven fabric with ideal performance.
In a specific embodiment, the inert solvent in P2 is toluene or isopentane.
In a specific possible embodiment, in the P3, the temperature of the reaction vessel is 60-80 ℃, and the holding time is 30-90 min.
By adopting the technical scheme, the copolymerization temperature and time of oleic acid and propylene are optimized, and hydrophilic polypropylene and spun-bonded non-woven fabric with ideal performance are obtained.
In a specific possible embodiment, the material of the hydrophilic thread further comprises potassium perfluorooctanoate, and the mass ratio of the potassium perfluorooctanoate to the hydrophilic polypropylene is (0.05-0.2): 1.
by adopting the technical scheme, the addition of the potassium perfluorooctanoate is beneficial to further improving the hydrophilicity of the obtained silk threads, so that the hydrophilicity of the obtained spun-bonded non-woven fabric is further improved.
In a second aspect, a method for preparing the hydrophilic spun-bonded non-woven fabric is provided, and the following technical scheme is adopted:
a method of making a hydrophilic spunbond nonwoven comprising:
taking hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate, and carrying out melt spinning to prepare a hydrophilic silk thread, wherein the hydrophilic polypropylene is obtained by copolymerizing propylene and oleic acid under the action of a metallocene catalyst;
laying the hydrophilic threads into a net and bonding to obtain the hydrophilic spun-bonded non-woven fabric.
By adopting the technical scheme, the hydrophilic spun-bonded non-woven fabric is successfully prepared.
In a third aspect, a hydrophilic silk thread is provided, which adopts the following technical scheme:
the hydrophilic silk thread is prepared by melt spinning hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate;
the hydrophilic polypropylene is prepared by copolymerizing propylene and oleic acid under the action of a metallocene catalyst.
By adopting the technical scheme, the hydrophilic silk thread can be used in spun-bonded non-woven fabrics, other non-woven fabrics and woven fabrics, so that the obtained cloth has good hydrophilicity.
In summary, the present application has at least one of the following beneficial technical effects:
1. the penetration time of water drops of the spun-bonded non-woven fabric obtained by the application is below 1s, the reverse osmosis amount is less than 0.2g, and good hydrophilicity is shown.
2. According to the method, the good hydrophilicity of oleic acid is utilized through the synergistic cooperation of oleic acid and propylene, so that the obtained copolymerization product has good hydrophilicity, and the silk threads and the spun-bonded non-woven fabric made of the copolymerization product have good hydrophilicity. Meanwhile, in the molecular chain of the oleic acid-propylene copolymer, the oleic acid unit and the propylene unit are firmly combined through chemical bonds, so that the hydrophilicity of the obtained spun-bonded non-woven fabric has good durability.
3. The hydrophilicity of the obtained silk threads can be further improved by adding the potassium perfluorooctanoate, so that the hydrophilicity of the obtained spun-bonded non-woven fabric is further improved.
4. The hydrophilic silk threads obtained by the method have good hydrophilicity, can be used for spun-bonded non-woven fabrics, other non-woven fabrics and woven fabrics, and endow the obtained cloth with good hydrophilicity.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example 1
The preparation example discloses a preparation method of hydrophilic polypropylene, which specifically comprises the following steps:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.350g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1 mmmol), 0.348g of methylaluminoxane (6 mmol), and 0.536g of oleic acid were charged to the reaction vessel.
And P3, raising the temperature of the reaction vessel to 60 ℃, and then keeping the temperature for 90min under the stirring of 80rpm, so that the propylene and the oleic acid have copolymerization reaction under the catalytic action of the dimethylsilyl bis (cyclopentadienyl) zirconium dichloride and the methylaluminoxane.
P4, the reaction mixture obtained in P3 was added to a hydrochloric acid-ethanol solution (hydrochloric acid content: 10 wt%) to terminate the copolymerization reaction, and at this time, a precipitate was precipitated.
P5, filtering the precipitate obtained in the P4, and washing the precipitate by ethanol and hot water at 50 ℃ to obtain the hydrophilic polypropylene.
Preparation example 2
This preparation is essentially the same as preparation 1, except that: the mass ratio of the propylene to the oleic acid is 1:1.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.350g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1 mmmol), 0.348g of methylaluminoxane (6 mmol), and 0.765g of oleic acid were charged to the reaction vessel.
Preparation example 3
This preparation is essentially the same as preparation 1, except that: the mass ratio of the propylene to the oleic acid is 1: 1.4.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.350g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1 mmmol), 0.348g of methylaluminoxane (6 mmol), and 1.07g of oleic acid were charged to the reaction vessel.
Preparation example 4
This preparation is essentially the same as preparation 1, except that: the mass ratio of the propylene to the oleic acid is 1: 1.8.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.350g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1 mmmol), 0.348g of methylaluminoxane (6 mmol) and 1.38g of oleic acid were charged to the reaction vessel.
Preparation example 5
This preparation is essentially the same as preparation 1, except that: the mass ratio of the propylene to the oleic acid is 1: 2.1.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.350g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1 mmmol), 0.348g of methylaluminoxane (6 mmol), and 1.61g of oleic acid were charged to the reaction vessel.
Preparation example 6
This preparation is essentially the same as preparation 3, except that: the concentration of dimethylsilylbis (cyclopentadienyl) zirconium dichloride in the reaction vessel (i.e. the amount of dimethylsilylbis (cyclopentadienyl) zirconium dichloride per volume of the reaction vessel) was 2.5 mmmol/L.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.438g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1.25 mmmol), 0.435g of methylaluminoxane (7.5 mmol) and 1.07g of oleic acid were charged to the reaction vessel.
Preparation example 7
This preparation is essentially the same as preparation 3, except that: the concentration of dimethylsilylbis (cyclopentadienyl) zirconium dichloride in the reaction vessel was 3 mmmol/L.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.525g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1.5 mmmol), 0.522g of methylaluminoxane (9 mmol) and 1.07g of oleic acid were charged to the reaction vessel.
Preparation example 8
This preparation is essentially the same as preparation 6, except that: the molar ratio of methylaluminoxane to dimethylsilylbis (cyclopentadienyl) zirconium dichloride is 9: 1.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.438g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1.25 mmmol), 0.653g of methylaluminoxane (11.25 mmol) and 1.07g of oleic acid were charged to the reaction vessel.
Preparation example 9
This preparation is essentially the same as preparation 6, except that: the molar ratio of methylaluminoxane to dimethylsilylbis (cyclopentadienyl) zirconium dichloride is 12: 1.
P1-P2 are specifically:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction vessel, then filling nitrogen, repeating for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of isopentane, 0.438g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1.25 mmmol), 0.870g of methylaluminoxane (15 mmol) and 1.07g of oleic acid were charged to the reaction vessel.
Preparation example 10
This preparation is essentially the same as preparation 8, except that: the process parameters of some steps are different.
The method specifically comprises the following steps:
p1, taking 1000mL of three-port reaction vessel; evacuating the gas in the reaction vessel, then filling nitrogen, repeating for three times; thereafter, 800mL of propylene (1.53 g) was introduced into the reaction vessel and the corresponding volume of nitrogen was purged to maintain the inside of the reaction vessel at normal pressure.
P2, 200mL of isopentane, 0.876g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (2.5 mmmol), 1.31g of methylaluminoxane (22.5 mmol) and 2.14g of oleic acid were charged to the reaction vessel.
And P3, raising the temperature of the reaction vessel to 70 ℃, and then keeping the temperature for 60min under the stirring of 70rpm, so that the propylene and the oleic acid have copolymerization reaction under the catalytic action of the dimethylsilyl bis (cyclopentadienyl) zirconium dichloride and the methylaluminoxane.
P4, the reaction mixture obtained in P3 was added to a hydrochloric acid-ethanol solution (hydrochloric acid content: 10 wt%) to terminate the copolymerization reaction, and at this time, a precipitate was precipitated.
P5, filtering the precipitate obtained from P4, and washing twice with ethanol and hot water at 30 ℃ to obtain the hydrophilic polypropylene.
Preparation example 11
This preparation is substantially the same as preparation 8 except that: the process parameters of some steps are different.
The method specifically comprises the following steps:
p1, taking a 500mL three-port reaction vessel; evacuating the gas in the reaction container, then filling nitrogen, repeating the process for three times; the reaction vessel was then kept at atmospheric pressure by introducing 400mL of propylene (0.765 g) and by purging a corresponding volume of nitrogen.
P2, 100mL of toluene, 0.438g of dimethylsilylbis (cyclopentadienyl) zirconium dichloride (1.25 mmmol), 0.653g of methylaluminoxane (11.25 mmol) and 1.07g of oleic acid were charged to the reaction vessel.
And P3, raising the temperature of the reaction vessel to 80 ℃, and then keeping the temperature for 30min under the stirring of 60rpm, so that the propylene and the oleic acid have copolymerization reaction under the catalytic action of the dimethylsilyl bis (cyclopentadienyl) zirconium dichloride and the methylaluminoxane.
P4, the reaction mixture obtained in P3 was added to a hydrochloric acid-ethanol solution (hydrochloric acid content: 10 wt%) to terminate the copolymerization reaction, and at this time, a precipitate was precipitated.
P5, filtering the precipitate obtained in P4, and washing the precipitate twice with ethanol and hot water at 50 ℃ to obtain the hydrophilic polypropylene.
Example 1
The embodiment discloses a hydrophilic spun-bonded non-woven fabric which is made of hydrophilic silk threads made of hydrophilic polypropylene; wherein: hydrophilic polypropylene was obtained from preparation example 1.
The preparation method of the hydrophilic spun-bonded non-woven fabric comprises the following steps:
s1, taking the hydrophilic polypropylene obtained in the preparation example 1, carrying out melt extrusion on the hydrophilic polypropylene through a screw extruder, and quantitatively spraying blank filaments through a metering pump; the temperature in the extruder was controlled at 225 ℃ and 235 ℃.
And S2, drawing the blank filament obtained in the step S1 by using hot air to obtain the hydrophilic silk thread, wherein the temperature of the hot air is controlled to be 170 ℃, the wind speed of the hot air is 800m/min, and the drawing time is 12S.
S3, laying the hydrophilic silk threads obtained in the step S2 on a lapping machine to form a net; then the hydrophilic spun-bonded non-woven fabric is formed by heat seal through a hot rolling mill; and finally slitting and winding.
The embodiment also discloses a hydrophilic thread which is prepared from S1-S2 in the preparation method of the hydrophilic spun-bonded non-woven fabric. The hydrophilic silk thread can be used in spun-bonded non-woven fabrics, other non-woven fabrics and woven fabrics, and the obtained cloth has good hydrophilicity.
Examples 2 to 11
Examples 2-11 are essentially the same as example 1, except that: the source of the hydrophilic polypropylene varies. The details are shown in Table 1.
TABLE 1 Source of hydrophilic Polypropylene in examples 2-11
| Item | Hydrophilic polypropylene | Item | Hydrophilic polypropylene |
| Example 2 | Preparation example 2 | Example 7 | Preparation example 7 |
| Example 3 | Preparation example 3 | Example 8 | Preparation example 8 |
| Example 4 | Preparation example 4 | Example 9 | Preparation example 9 |
| Example 5 | Preparation example 5 | Example 10 | Preparation example 10 |
| Example 6 | Preparation example 6 | Example 11 | Preparation example 11 |
Example 12
This embodiment is substantially the same as embodiment 10 except that: the hydrophilic silk thread is made of a mixture of hydrophilic polypropylene and potassium perfluorocaprylate, and the mass ratio of the hydrophilic polypropylene to the potassium perfluorocaprylate is 1: 0.05.
the preparation method of the hydrophilic spun-bonded non-woven fabric comprises the following steps:
s1, mixing the components in a mass ratio of 1: 0.05, uniformly mixing the hydrophilic polypropylene and the potassium perfluorooctanoate obtained in the preparation example 10, then carrying out melt extrusion by a screw extruder, and quantitatively spraying blank filaments by a metering pump; the temperature in the extruder was controlled at 225 ℃ and 235 ℃.
And S2, drawing the blank filament obtained in the step S1 by using hot air to obtain the hydrophilic silk thread, wherein the temperature of the hot air is controlled to be 170 ℃, the wind speed of the hot air is 800m/min, and the drawing time is 12S.
S3, laying the hydrophilic silk threads obtained in the step S2 on a lapping machine to form a net; then the hydrophilic spun-bonded non-woven fabric is formed by heat seal through a hot rolling mill; and finally slitting and winding.
Examples 13 to 15
Examples 13-15 are essentially the same as example 12, except that: the mass ratio of the hydrophilic polypropylene to the potassium perfluorooctanoate was different.
The method specifically comprises the following steps:
in example 13, the mass ratio of hydrophilic polypropylene to potassium perfluorooctanoate was 1: 0.1.
in example 14, the mass ratio of the hydrophilic polypropylene to the potassium perfluorooctanoate was 1: 0.15.
in example 15, the mass ratio of the hydrophilic polypropylene to the potassium perfluorooctanoate was 1: 0.2.
example 16
This example is substantially the same as example 14 except that: partial process parameters of the preparation method of the hydrophilic spun-bonded non-woven fabric are changed.
The method specifically comprises the following steps:
s1, mixing the components in a mass ratio of 1: 0.15, uniformly mixing the hydrophilic polypropylene and the potassium perfluorooctanoate obtained in the preparation example 10, and then carrying out melt extrusion by a screw extruder and quantitatively spraying blank filaments by a metering pump; the temperature in the extruder is controlled at 215 ℃ and 230 ℃.
And S2, drawing the blank filament obtained in the step S1 by using hot air to obtain the hydrophilic silk thread, wherein the temperature of the hot air is controlled to be 150 ℃, the wind speed of the hot air is 1200m/min, and the drawing time is 8S.
S3, laying the hydrophilic silk threads obtained in the step S2 on a lapping machine to form a net; then the hydrophilic spun-bonded non-woven fabric is formed by heat seal through a hot rolling mill; and finally slitting and winding.
Comparative example 1
This comparative example differs from example 1 in that: the spun-bonded nonwoven fabric was made from filaments of ordinary polypropylene (available from Ponkan plastics materials Co., Ltd., Dongguan).
Performance detection
The hydrophilic spunbonded nonwovens obtained in examples 1-16 and comparative example 1 were tested; the results are shown in Table 2.
1. Hydrophilicity test: the time of water penetrating through the cloth cover is used for representing; specific reference standards are as follows: EDANA 153.0; when tested, the temperature was 25 ℃, the humidity was 30%, and the thickness of the spunbond nonwoven was 0.5 mm.
2. Reverse osmosis amount test: reference standard: EDANA 154.0; when tested, the temperature was 25 ℃, the humidity was 30%, and the thickness of the spunbond nonwoven was 0.5 mm.
3. And (3) testing the breaking strength: reference standard: ASTM D5035, shear slitting method-1C, measuring the breaking strength in the warp direction; when tested, the temperature was 25 ℃, the humidity was 30%, the length of the spunbond nonwoven was 150mm, and the thickness was 0.5 mm.
TABLE 2 Properties of spunbonded nonwovens obtained in examples 1-16 and comparative example 1
| Item | First penetration time/s | Third time of penetration/s | Fifth penetration time/s | Reverse osmosis amount/g | Breaking strength/N |
| Example 1 | 0.82 | 0.87 | 0.92 | 0.19 | 30.5 |
| Example 2 | 0.75 | 0.81 | 0.85 | 0.18 | 28.1 |
| Example 3 | 0.62 | 0.68 | 0.73 | 0.17 | 25.4 |
| Example 4 | 0.57 | 0.63 | 0.67 | 0.17 | 22.8 |
| Example 5 | 0.42 | 0.47 | 0.52 | 0.16 | 20.3 |
| Example 6 | 0.61 | 0.65 | 0.69 | 0.16 | 25.6 |
| Example 7 | 0.61 | 0.65 | 0.68 | 0.16 | 25.3 |
| Example 8 | 0.60 | 0.61 | 0.64 | 0.16 | 25.5 |
| Example 9 | 0.60 | 0.61 | 0.63 | 0.16 | 25.4 |
| Example 10 | 0.52 | 0.52 | 0.54 | 0.15 | 25.9 |
| Example 11 | 0.58 | 0.60 | 0.62 | 0.17 | 25.0 |
| Example 12 | 0.43 | 0.44 | 0.45 | 0.15 | 25.4 |
| Example 13 | 0.35 | 0.36 | 0.38 | 0.14 | 25.0 |
| Example 14 | 0.32 | 0.33 | 0.32 | 0.14 | 24.9 |
| Example 15 | 0.30 | 0.31 | 0.33 | 0.15 | 24.6 |
| Example 16 | 0.34 | 0.35 | 0.37 | 0.16 | 25.1 |
| Comparative example 1 | 5.31 | 5.35 | 5.33 | 2.3 | 38.3 |
Referring to Table 2, it can be seen from the test results of examples 1-16 that: the spunbonded nonwovens obtained in the examples of the application have the water drop penetration time of less than 1s and the reverse osmosis amount of less than 0.2g, and show good hydrophilicity.
From the test results of examples 1 to 5 and comparative document 1, it was found that: with the increase of the addition of the oleic acid, the water drop penetration time and the reverse osmosis amount of the obtained spun-bonded non-woven fabric are in a descending trend, which shows that the hydrophilicity of the spun-bonded non-woven fabric is continuously improved. The reason is that oleic acid has good hydrophilicity, and the polypropylene composite material with good hydrophilicity can be obtained by compounding the oleic acid with propylene, so that the hydrophilicity of silk threads spun by the polypropylene composite material is improved, and the hydrophilicity of the spun-bonded non-woven fabric made of the silk threads is improved. In contrast, the spunbond nonwoven fabric made with conventional polypropylene filaments (comparative example 1) had a higher water droplet penetration time and reverse osmosis, indicating a less hydrophilic character. Of course, the addition of oleic acid can affect the mechanical properties of the final spunbonded nonwoven to some extent, since it can reduce the proportion of propylene in the polypropylene composite. Meanwhile, the detection results also show that the difference of the first penetration time, the third penetration time and the fifth penetration time of the water drops of the spun-bonded non-woven fabric is not large, which indicates that the hydrophilicity of the spun-bonded non-woven fabric has good durability; the oleic acid is combined with the propylene in a polymerization mode, so that in the molecular chain of the obtained propylene-oleic acid copolymer (polypropylene composite material), the oleic acid unit and the propylene unit are firmly combined; the resulting spunbond nonwoven is relatively hydrophilic.
From the test results of examples 3, 6 to 7, it was found that: with the increase of the addition of the dimethylsilyl bis (cyclopentadienyl) zirconium dichloride, the difference of the first penetration time, the third penetration time and the fifth penetration time of water drops of the finally obtained spun-bonded non-woven fabric becomes smaller, namely the durability of the hydrophilicity of the spun-bonded non-woven fabric tends to be improved; the reason is that when propylene and oleic acid are copolymerized, the addition of the dimethyl silicon-based bis (cyclopentadienyl) zirconium dichloride used as a catalyst is increased, which is beneficial to the copolymerization of the propylene and the oleic acid, so that the formed propylene-oleic acid copolymer has a more stable structure, and the final spun-bonded non-woven fabric can obtain more durable hydrophilicity.
From the test results of examples 6, 8 to 9, it was found that: when propylene and oleic acid are copolymerized, the addition of methylaluminoxane is increased, and the copolymerization of the propylene and the oleic acid is facilitated, so that a propylene-oleic acid copolymer with a more stable structure can be formed, and the hydrophilicity durability of the obtained spun-bonded non-woven fabric is facilitated to be improved.
The results of the tests of examples 10,12 to 16 were analyzed to find that: with the addition of potassium perfluorooctanoate, the hydrophilicity of the spunbond nonwoven fabric made from the resulting filaments tends to increase; this is due to: the potassium perfluorooctanoate contributes to further improving the hydrophilicity of the resulting filaments, and thus the hydrophilicity of the spunbond nonwoven fabric is further improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A hydrophilic spunbond nonwoven characterized by: the fabric is made of hydrophilic silk threads, and the material of the hydrophilic silk threads comprises hydrophilic polypropylene;
the hydrophilic polypropylene is obtained by copolymerizing propylene and oleic acid under the action of a metallocene catalyst.
2. A hydrophilic spunbond nonwoven as recited in claim 1, wherein: the hydrophilic polypropylene is prepared by the following steps:
p1, introducing propylene into an oxygen-free reaction vessel;
p2, adding an inert solvent, dimethylsilylbis (cyclopentadienyl) zirconium dichloride, methylaluminoxane and oleic acid into a reaction vessel;
p3, raising the temperature of the reaction vessel to at least 60 ℃ and preserving the temperature to ensure that the propylene and the oleic acid have copolymerization reaction;
p4, introducing hydrochloric acid-ethanol solution to terminate the copolymerization reaction;
p5, filtering and washing to obtain hydrophilic polypropylene.
3. A hydrophilic spunbond nonwoven as recited in claim 2, wherein: the mass ratio of the propylene to the oleic acid is 1: (0.7-2.1).
4. A hydrophilic spunbond nonwoven as recited in claim 2, wherein: in the P2, the concentration of the dimethylsilylbis (cyclopentadienyl) zirconium dichloride in the reaction vessel is 2-3 mmol/L.
5. The hydrophilic spunbond nonwoven of claim 4, wherein: in the P2, the molar ratio of the methylaluminoxane to the dimethylsilylbis (cyclopentadienyl) zirconium dichloride is (6-12): 1.
6. a hydrophilic spunbond nonwoven as recited in claim 2, wherein: in the P2, the inert solvent is toluene or isopentane.
7. A hydrophilic spunbond nonwoven as recited in claim 2, wherein: in the P3, the temperature of the reaction container is 60-80 ℃, and the heat preservation time is 30-90 min.
8. A hydrophilic spunbond nonwoven as recited in claim 1, wherein: the hydrophilic silk thread is made of potassium perfluorocaprylate, and the mass ratio of the potassium perfluorocaprylate to the hydrophilic polypropylene is (0.05-0.2): 1.
9. a method of making a hydrophilic spunbond nonwoven fabric as recited in any of claims 1-8, wherein: the method comprises the following steps:
taking hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate, and carrying out melt spinning to prepare a hydrophilic silk thread, wherein the hydrophilic polypropylene is obtained by copolymerizing propylene and oleic acid under the action of a metallocene catalyst;
laying the hydrophilic threads into a net and bonding to obtain the hydrophilic spun-bonded non-woven fabric.
10. A hydrophilic thread characterized by: the material is prepared by melting and spinning hydrophilic polypropylene or a mixture of the hydrophilic polypropylene and potassium perfluorooctanoate;
the hydrophilic polypropylene is prepared by copolymerizing propylene and oleic acid under the action of a metallocene catalyst.
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