CN107459740A - A kind of inorganic material changes polyvinyl chloride and preparation method thereof - Google Patents
A kind of inorganic material changes polyvinyl chloride and preparation method thereof Download PDFInfo
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- CN107459740A CN107459740A CN201710818901.5A CN201710818901A CN107459740A CN 107459740 A CN107459740 A CN 107459740A CN 201710818901 A CN201710818901 A CN 201710818901A CN 107459740 A CN107459740 A CN 107459740A
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- polyvinyl chloride
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- ethanol
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 191
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 171
- 238000002360 preparation method Methods 0.000 title claims description 29
- 229910010272 inorganic material Inorganic materials 0.000 title description 2
- 239000011147 inorganic material Substances 0.000 title description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 118
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 39
- 239000000835 fiber Substances 0.000 claims abstract description 37
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004964 aerogel Substances 0.000 claims abstract description 32
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 claims abstract description 22
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 19
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims abstract description 18
- 239000005033 polyvinylidene chloride Substances 0.000 claims abstract description 18
- XJECNSWAHCMYNZ-UHFFFAOYSA-N C=C.[Fe].[Na] Chemical group C=C.[Fe].[Na] XJECNSWAHCMYNZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 16
- XNJIKBGDNBEQME-UHFFFAOYSA-L barium(2+);dioxido(oxo)phosphanium Chemical compound [Ba+2].[O-][P+]([O-])=O.[O-][P+]([O-])=O XNJIKBGDNBEQME-UHFFFAOYSA-L 0.000 claims abstract description 16
- ATSGLBOJGVTHHC-UHFFFAOYSA-N bis(ethane-1,2-diamine)copper(2+) Chemical compound [Cu+2].NCCN.NCCN ATSGLBOJGVTHHC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 16
- NEUOBESLMIKJSB-UHFFFAOYSA-J tetrasodium;tetraacetate Chemical compound [Na+].[Na+].[Na+].[Na+].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O NEUOBESLMIKJSB-UHFFFAOYSA-J 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract 4
- 239000002994 raw material Substances 0.000 claims abstract 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- 238000001914 filtration Methods 0.000 claims description 39
- 238000012423 maintenance Methods 0.000 claims description 38
- 238000005453 pelletization Methods 0.000 claims description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 25
- 229910052788 barium Inorganic materials 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 238000005292 vacuum distillation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 7
- -1 silicane alkane Chemical class 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 2
- 229940068984 polyvinyl alcohol Drugs 0.000 claims 2
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 claims 1
- UWNVYVSFILLUSQ-UHFFFAOYSA-N [Na].[Cu].C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(CN)N Chemical compound [Na].[Cu].C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(C)(=O)O.C(CN)N UWNVYVSFILLUSQ-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 150000002926 oxygen Chemical class 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 6
- 235000011116 calcium hydroxide Nutrition 0.000 description 16
- 239000008187 granular material Substances 0.000 description 12
- 150000001242 acetic acid derivatives Chemical class 0.000 description 10
- 150000001805 chlorine compounds Chemical class 0.000 description 10
- 230000006837 decompression Effects 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 235000000396 iron Nutrition 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- XDTMVPXMIHGPRR-UHFFFAOYSA-K [Na+].[Cu++].CC([O-])=O.CC([O-])=O.CC([O-])=O Chemical compound [Na+].[Cu++].CC([O-])=O.CC([O-])=O.CC([O-])=O XDTMVPXMIHGPRR-UHFFFAOYSA-K 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/04—Ferrous oxide [FeO]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2268—Ferrous oxide (FeO)
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention is related to a kind of inorganic material-modified polyvinyl chloride, including following raw material components:Polyvinyl chloride long fibre modified polyvinyl chloride, modified polyvinyl chloride, polyvinylidene chloride, polyvinyl chloride long fibre modified polyvinyl chloride is by polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous iron, calcium hydroxide, barium metaphosphate and aminopropyl triethoxysilane reaction are made, modified polyvinyl chloride is by coppe ferrite, polyvinyl chloride, ferrous oxide, barium metaphosphate and aminopropyl triethoxysilane reaction are made, modified oxidized ferrous iron is by ferrous oxide, aminopropyl triethoxysilane and ethanol synthesis are made, ferrous oxide is by frerrous chloride, ammoniacal liquor, charcoal-aero gel, polyvinyl alcohol and ethanol synthesis are made, coppe ferrite is by cupric ethylene diamine tetraacetate sodium, sodium iron ethylene diamine tetra acetate, water, ethanol and charcoal-aero gel reaction are made.The invention has the advantages such as excellent mechanical property, hydrophobicity, self-cleaning property, anti-flammability, mould proof performance, resistance to ag(e)ing, low water vapor transmittance, compatibility.
Description
Technical field
The invention is related to a kind of inorganic material-modified polyvinyl chloride and preparation method thereof.
Background technology
Polyvinyl chloride has an excellent chemical resistance, mechanical strength, electric insulating quality, and it is excellent that flow resistance is small etc.
Gesture.Polyvinyl chloride can be molded with the methods of extrusion, injection, molding, blowing, be widely used in manufacturing artificial leather, cable, plastics
Bag, film, commodity and various tubing etc..
At present, pvc material is in mechanical property, hydrophobicity, self-cleaning property, anti-flammability, mould proof performance, ageing-resistant
Property, the performance such as low water vapor transmittance, compatibility, oxidative resistance need further lifting.The invention using polyvinyl chloride long fibre,
Polyvinyl chloride, coppe ferrite, polyvinylidene chloride, modified oxidized ferrous, calcium hydroxide are prepared for inorganic material-modified polyvinyl chloride,
By extruding, being molded, being molded, the technique such as being blow molded and be prepared into various plastic products, inorganic material-modified polychlorostyrene prepared by this method
Vinyl material has excellent mechanical property, hydrophobicity, self-cleaning property, anti-flammability, mould proof performance, resistance to ag(e)ing, low steam
The performances such as transmitance, compatibility, oxidative resistance.
The content of the invention
The purpose of the invention is to provide a kind of preparation method of inorganic material-modified polyvinyl chloride, and this method passes through change
Reactant feed and technology mode, the material of preparation have excellent mechanical property, hydrophobicity, self-cleaning property, anti-flammability, mould proof
The performances such as bacterium performance, resistance to ag(e)ing, low water vapor transmittance, compatibility, oxidative resistance.
To achieve these goals, the technical scheme of the invention is as follows.
A kind of inorganic material-modified polyvinyl chloride and preparation method thereof, specifically includes following steps:(1), by ethylenediamine tetraacetic
Copper acetate sodium, sodium iron ethylene diamine tetra acetate, water, ethanol and charcoal-aero gel are 100 according to quality parts ratio:80~90:51~62:
85~100:37~47 are added in reactor, and 0.5~2h is reacted under the conditions of 50~70 DEG C of maintenance system temperature, at 80 DEG C ,-
0.06MPa is evaporated under reduced pressure 2h, 105 DEG C of dry 2h, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C are calcined
3h, through 1L water washings 2 times, filtering, 120 DEG C of drys 2h, grind, obtain coppe ferrite;(2), by frerrous chloride, ammoniacal liquor, charcoal airsetting
Glue, polyvinyl alcohol and ethanol are according to quality parts ratio 100:25~45:33~46:13~22:46~55 are added in reactor,
Under the conditions of 45~63 DEG C of maintenance system temperature react 1~3h, under nitrogen protection, 80 DEG C, -0.06MPa be evaporated under reduced pressure 2h, 105
DEG C dry 2h, under nitrogen protection, in 200 DEG C be calcined 2h, 300 DEG C roasting 2h, 400 DEG C roasting 2h, 500 DEG C roasting 3h, through 1L
Water washing 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;(3), will oxidation
Ferrous, aminopropyl triethoxysilane and ethanol are according to quality parts ratio 10:15~20:30~70 are added in reactor, stir
It is 72~95r/min to mix speed, reacts 1~3h, filtered, 120 DEG C of dry 2h under the conditions of 40~55 DEG C of maintenance system temperature,
Obtain modified oxidized ferrous iron;(4), by coppe ferrite, polyvinyl chloride, ferrous oxide, barium metaphosphate and aminopropyl triethoxysilane
According to quality parts ratio 10:85~100:6~10:1~3:2~5 are added in mill, with mill in temperature 140~190
DEG C 0.5~1h of hybrid reaction, with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, obtain modified polyvinyl chloride;(5), will
Polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous iron, calcium hydroxide, barium metaphosphate and aminopropyl triethoxysilane are pressed
According to quality parts ratio 100:75~90:7~13:13~22:1~2:2~3 are added in mill, with mill in temperature 140
~190 DEG C of 0.5~1h of hybrid reaction, with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre
Modified polyvinyl chloride;(6), by polyvinyl chloride long fibre modified polyvinyl chloride, modified polyvinyl chloride, polyvinylidene chloride according to matter
Measure portion rate 100:14~20:7~15 are added in mill, with mill 140~190 DEG C of hybrid reactions 0.5 of temperature~
1h, with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, obtain inorganic material-modified polyvinyl chloride granules.
The preparation method of inorganic material-modified polyvinyl chloride described in the invention, comprises the following steps:
(1), it is according to quality parts ratio by cupric ethylene diamine tetraacetate sodium, sodium iron ethylene diamine tetra acetate, water, ethanol and charcoal-aero gel
100:80~90:51~62:85~100:37~47 are added in reactor, anti-under the conditions of 50~70 DEG C of maintenance system temperature
0.5~2h is answered, at 80 DEG C, -0.06MPa is evaporated under reduced pressure 2h, 105 DEG C of drys 2h, is calcined 2h in 200 DEG C, and 300 DEG C are calcined 2h, and 400
DEG C roasting 2h, 500 DEG C of roasting 3h, through 1L water washings 2 times, filtering, 120 DEG C of drys 2h, grinds, obtains coppe ferrite;Described charcoal
The purpose of aeroge is in order to improve the dispersiveness of cupric ethylene diamine tetraacetate sodium and sodium iron ethylene diamine tetra acetate and reduce coppe ferrite
Agglomeration.
(2), by frerrous chloride, ammoniacal liquor, charcoal-aero gel, polyvinyl alcohol and ethanol according to quality parts ratio 100:25~45:
33~46:13~22:46~55 are added in reactor, 1~3h are reacted under the conditions of 45~63 DEG C of maintenance system temperature, in nitrogen
Under gas shielded, 80 DEG C, -0.06MPa be evaporated under reduced pressure 2h, 105 DEG C of drys 2h, under nitrogen protection, in 200 DEG C roasting 2h, 300 DEG C
2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h are calcined, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, 120 DEG C
2h is dried, grinding, obtains ferrous oxide;The purpose of described charcoal-aero gel in order to improve frerrous chloride dispersiveness and reduce oxygen
Change ferrous agglomeration.
(3), by ferrous oxide, aminopropyl triethoxysilane and ethanol according to quality parts ratio 10:15~20:30~70
It is added in reactor, mixing speed is 72~95r/min, and 1~3h, warp are reacted under the conditions of 40~55 DEG C of maintenance system temperature
Filtering, 120 DEG C of dry 2h, obtain modified oxidized ferrous iron;The purpose of described phthalate coupling agent is in order to improve ferrous oxide
With the dispersiveness and compatibility of polyvinyl chloride.
(4), by coppe ferrite, polyvinyl chloride, ferrous oxide, barium metaphosphate and aminopropyl triethoxysilane according to mass parts
Number ratio 10:85~100:6~10:1~3:2~5 are added in mill, with mill in 140~190 DEG C of hybrid reactions of temperature
0.5~1h, with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, obtain modified polyvinyl chloride;The mesh of described coppe ferrite
In order to improve the fungus resistance energy of polyvinyl chloride, the purpose of described ferrous oxide is in order to improve the oxidative resistance of polyvinyl chloride
Energy and ageing-resistant performance.
(5), by polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous iron, calcium hydroxide, barium metaphosphate and aminopropyl
Triethoxysilane is according to quality parts ratio 100:75~90:7~13:13~22:1~2:2~3 are added in mill, use
Mill with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, is obtained in 140~190 DEG C of 0.5~1h of hybrid reaction of temperature
Polyvinyl chloride long fibre modified polyvinyl chloride, the long stapled purpose of described polyvinyl chloride are strong in order to improve the mechanics of polyvinyl chloride
Degree, the purpose of described calcium hydroxide is in order to neutralize the hydrogen chloride gas in polyvinyl chloride and improve the anti-flammability of polyvinyl chloride
Energy.
(6), by polyvinyl chloride long fibre modified polyvinyl chloride, modified polyvinyl chloride, polyvinylidene chloride according to mass parts
Number ratio 100:14~20:7~15 are added in mill, with mill in 140~190 DEG C of 0.5~1h of hybrid reaction of temperature, use
Extruder obtains inorganic material-modified polyvinyl chloride granules, described poly- inclined dichloro in 140~190 DEG C of extruding pelletizations of temperature
The purpose of ethene is in order to reduce the water vapor transmittance of polyvinyl chloride.
The beneficial effect of the invention is:
1st, charcoal-aero gel has big specific surface area, can preferably disperse and fix cupric ethylene diamine tetraacetate sodium and ethylenediamine tetraacetic
Acetic acid ferrisodium, after high-temperature heat treatment, obtaining coppe ferrite has excellent ratio surface, particle homogeneity, low-surface-energy, low reunion
Etc. performance;
2nd, charcoal-aero gel has big specific surface area, can preferably disperse and fix frerrous chloride, and polyvinyl alcohol can be more
Good scattered ammonia spirit, controls the reaction rate of ammoniacal liquor and frerrous chloride, the ferrous oxide of preparation have excellent ratio surface,
The performances such as particle homogeneity, low-surface-energy, low reunion;
3rd, coppe ferrite and ferrous oxide have excellent hydrophobicity, and in Blending Processes, coppe ferrite and ferrous oxide can assign
The excellent hydrophobic performance of polyvinyl chloride, it is unfavorable for dirty material absorption in polyvinyl chloride surface, so as to reach polyvinyl chloride surface
Automatically cleaning effect;
4th, polyvinyl chloride is during processing and use, can discharge hydrogen chloride gas, and the hydrogen chloride of polyvinyl chloride release can be with
Calcium hydroxide reaction, calcium chloride and water are formed, calcium chloride acts not only as filler use, can also impart to polyvinyl chloride resistance
While firing performance, solves the harm of polyvinyl chloride release hydrogen chloride;
5th, polyvinyl chloride long fibre has excellent mechanical property, and has excellent compatibility with polyvinyl chloride, can assign
The excellent tensile property of polyvinyl chloride, impact property and bending property;
6th, polyvinylidene chloride has relatively low water vapor transmittance, can assign polyvinyl chloride excellent low steam breathability energy.
Embodiment
The embodiment of the invention is described with reference to embodiment, to be better understood from the invention.
Embodiment 1
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 85 parts of sodium iron ethylene diamine tetra acetates, 57 parts of water, 93 parts of ethanol and 43 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 1.3h under the conditions of 62 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 38 parts of ammoniacal liquor, 41 parts of charcoal-aero gels, 18 parts of polyvinyl alcohol and 49 parts of ethanol, are weighed to be added to
In reactor, 1.5h is reacted under the conditions of 53 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations
2h, 105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C are calcined
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, 120 DEG C of drys 2h, grinds, obtains ferrous oxide;
(3) 10 parts of ferrous oxides, 18 parts of aminopropyl triethoxysilanes and 50 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 84r/min, and 1.6h is reacted under the conditions of 47 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 91 parts of polyvinyl chloride, 8 parts of ferrous oxides, 2.5 parts of barium metaphosphates and 3 parts of second of aminopropyl three, are weighed
TMOS is added in mill, with mill in 170 DEG C of hybrid reaction 0.7h of temperature, is squeezed for 170 DEG C in temperature with extruder
Go out to be granulated, that is, obtain modified polyvinyl chloride;
(5) 100 parts of polyvinyl chloride long fibres, 86 parts of polyvinyl chloride, 10 parts of modified oxidized ferrous, 18 parts of calcium hydroxides, 2, are weighed
Part barium metaphosphate and 2.5 parts of aminopropyl triethoxysilanes are added in mill, with mill in 170 DEG C of hybrid reactions of temperature
0.6h, with extruder in 170 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 17 parts of modified polyvinyl chlorides, 13 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 170 DEG C of hybrid reaction 0.5h of temperature, with extruder in 170 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 2
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 80 parts of sodium iron ethylene diamine tetra acetates, 51 parts of water, 85 parts of ethanol and 37 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 0.5h under the conditions of 50 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 25 parts of ammoniacal liquor, 33 parts of charcoal-aero gels, 13 parts of polyvinyl alcohol and 46 parts of ethanol, are weighed to be added to
In reactor, 1h is reacted under the conditions of 45 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 15 parts of aminopropyl triethoxysilanes and 30 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 72r/min, and 1h is reacted under the conditions of 40 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, obtains modified oxidized Asia
Iron;
(4) 10 parts of coppe ferrites, 85 parts of polyvinyl chloride, 6 parts of ferrous oxides, 1 part of barium metaphosphate and 2 parts of ethoxies of aminopropyl three, are weighed
Base silane is added in mill, with mill in 140 DEG C of hybrid reaction 0.5h of temperature, with extruder in 140 DEG C of extrusions of temperature
It is granulated, that is, obtains modified polyvinyl chloride;
(5), weigh 100 parts of polyvinyl chloride long fibres, 75 parts of polyvinyl chloride, 7 parts of modified oxidized ferrous irons, 13 parts of calcium hydroxides, 1 part
Barium metaphosphate and 2 parts of aminopropyl triethoxysilanes are added in mill, with mill in 140 DEG C of hybrid reactions of temperature
0.5h, with extruder in 140 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 14 parts of modified polyvinyl chlorides, 7 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 140 DEG C of hybrid reaction 0.5h of temperature, with extruder in 140 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 3
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 90 parts of sodium iron ethylene diamine tetra acetates, 62 parts of water, 100 parts of ethanol and 47 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 2h under the conditions of 70 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa is evaporated under reduced pressure
2h, 105 DEG C of dry 2h, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings 2 are calcined in 200 DEG C
Secondary, filtering, 120 DEG C of dry 2h, grinding, obtains coppe ferrite;
(2) 100 parts of frerrous chlorides, 45 parts of ammoniacal liquor, 46 parts of charcoal-aero gels, 22 parts of polyvinyl alcohol and 55 parts of ethanol, are weighed to be added to
In reactor, 3h is reacted under the conditions of 63 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 20 parts of aminopropyl triethoxysilanes and 70 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 95r/min, and 3h is reacted under the conditions of 55 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, obtains modified oxidized Asia
Iron;
(4) 10 parts of coppe ferrites, 100 parts of polyvinyl chloride, 10 parts of ferrous oxides, 3 parts of barium metaphosphates and 5 parts of second of aminopropyl three, are weighed
TMOS is added in mill, with mill in 190 DEG C of hybrid reaction 1h of temperature, with extruder in 190 DEG C of extrusions of temperature
It is granulated, that is, obtains modified polyvinyl chloride;
(5) 100 parts of polyvinyl chloride long fibres, 90 parts of polyvinyl chloride, 13 parts of modified oxidized ferrous, 22 parts of calcium hydroxides, 2, are weighed
Part barium metaphosphate and 3 parts of aminopropyl triethoxysilanes are added in mill, with mill in 190 DEG C of hybrid reactions of temperature
1h, with extruder in 190 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 20 parts of modified polyvinyl chlorides, 15 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 190 DEG C of hybrid reaction 1h of temperature, with extruder in 190 DEG C of extruding pelletizations of temperature, produces
To inorganic material-modified polyvinyl chloride granules.
Embodiment 4
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 81 parts of sodium iron ethylene diamine tetra acetates, 61 parts of water, 97 parts of ethanol and 39 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 0.8h under the conditions of 56 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 27 parts of ammoniacal liquor, 39 parts of charcoal-aero gels, 15 parts of polyvinyl alcohol and 48 parts of ethanol, are weighed to be added to
In reactor, 1.2h is reacted under the conditions of 47 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations
2h, 105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C are calcined
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, 120 DEG C of drys 2h, grinds, obtains ferrous oxide;
(3) 10 parts of ferrous oxides, 18 parts of aminopropyl triethoxysilanes and 35 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 75r/min, and 1.4h is reacted under the conditions of 43 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 89 parts of polyvinyl chloride, 9 parts of ferrous oxides, 1.2 parts of barium metaphosphates and 2.5 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 147 DEG C of hybrid reaction 1.7h of temperature, with extruder in 147 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5), weigh 100 parts of polyvinyl chloride long fibres, 88 parts of polyvinyl chloride, 12 parts of modified oxidized ferrous irons, 21 parts of calcium hydroxides,
1.5 parts of barium metaphosphates and 2.7 parts of aminopropyl triethoxysilanes are added in mill, with mill in 147 DEG C of mixing of temperature
1.8h is reacted, with extruder in 147 DEG C of extruding pelletizations of temperature, that is, obtains polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 14 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 147 DEG C of hybrid reaction 0.9h of temperature, with extruder in 147 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 5
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 81 parts of sodium iron ethylene diamine tetra acetates, 55 parts of water, 88 parts of ethanol and 39 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 1.2h under the conditions of 55 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa is evaporated under reduced pressure
2h, 105 DEG C of dry 2h, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings 2 are calcined in 200 DEG C
Secondary, filtering, 120 DEG C of dry 2h, grinding, obtains coppe ferrite;
(2) 100 parts of frerrous chlorides, 35 parts of ammoniacal liquor, 43 parts of charcoal-aero gels, 20 parts of polyvinyl alcohol and 53 parts of ethanol, are weighed to be added to
In reactor, 2.6h is reacted under the conditions of 60 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations
2h, 105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C are calcined
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, 120 DEG C of drys 2h, grinds, obtains ferrous oxide;
(3) 10 parts of ferrous oxides, 18 parts of aminopropyl triethoxysilanes and 40 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 90r/min, and 2.7h is reacted under the conditions of 52 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 95 parts of polyvinyl chloride, 8 parts of ferrous oxides, 1.3 parts of barium metaphosphates and 3.2 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 153 DEG C of hybrid reaction 1.9h of temperature, with extruder in 153 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5) 100 parts of polyvinyl chloride long fibres, 78 parts of polyvinyl chloride, 9 parts of modified oxidized ferrous, 17 parts of calcium hydroxides, 1.8, are weighed
Part barium metaphosphate and 2.1 parts of aminopropyl triethoxysilanes are added in mill, with mill in 153 DEG C of hybrid reactions of temperature
1.6h, with extruder in 153 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 16 parts of modified polyvinyl chlorides, 11 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 153 DEG C of hybrid reaction 1.4h of temperature, with extruder in 153 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 6
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 83 parts of sodium iron ethylene diamine tetra acetates, 57 parts of water, 91 parts of ethanol and 41 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 1.7h under the conditions of 58 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa is evaporated under reduced pressure
2h, 105 DEG C of dry 2h, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings 2 are calcined in 200 DEG C
Secondary, filtering, 120 DEG C of dry 2h, grinding, obtains coppe ferrite;
(2) 100 parts of frerrous chlorides, 41 parts of ammoniacal liquor, 39 parts of charcoal-aero gels, 16 parts of polyvinyl alcohol and 48 parts of ethanol, are weighed to be added to
In reactor, 2.4h is reacted under the conditions of 47 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 19 parts of aminopropyl triethoxysilanes and 65 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 92r/min, and 1.4h is reacted under the conditions of 51 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 93 parts of polyvinyl chloride, 8 parts of ferrous oxides, 1.9 parts of barium metaphosphates and 4.3 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 158 DEG C of hybrid reaction 1.1h of temperature, with extruder in 158 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5) 100 parts of polyvinyl chloride long fibres, 79 parts of polyvinyl chloride, 8 parts of modified oxidized ferrous, 14 parts of calcium hydroxides, 1.3, are weighed
Part barium metaphosphate and 2.8 parts of aminopropyl triethoxysilanes are added in mill, with mill in 158 DEG C of hybrid reactions of temperature
1.2h, with extruder in 158 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 19 parts of modified polyvinyl chlorides, 12 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 158 DEG C of hybrid reaction 1.9h of temperature, with extruder in 158 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 7
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 84 parts of sodium iron ethylene diamine tetra acetates, 58 parts of water, 90 parts of ethanol and 44 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 1.8h under the conditions of 66 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 43 parts of ammoniacal liquor, 40 parts of charcoal-aero gels, 15 parts of polyvinyl alcohol and 51 parts of ethanol, are weighed to be added to
In reactor, 2.2h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 18 parts of aminopropyl triethoxysilanes and 60 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 88r/min, and 1.3h is reacted under the conditions of 47 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 96 parts of polyvinyl chloride, 7 parts of ferrous oxides, 2.3 parts of barium metaphosphates and 4.2 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 164 DEG C of hybrid reaction 1.7h of temperature, with extruder in 164 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5), weigh 100 parts of polyvinyl chloride long fibres, 82 parts of polyvinyl chloride, 12 parts of modified oxidized ferrous irons, 17 parts of calcium hydroxides,
1.7 parts of barium metaphosphates and 2.7 parts of aminopropyl triethoxysilanes are added in mill, with mill in 164 DEG C of mixing of temperature
1.4h is reacted, with extruder in 164 DEG C of extruding pelletizations of temperature, that is, obtains polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 9 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 164 DEG C of hybrid reaction 1.7h of temperature, with extruder in 164 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 8
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of sodium iron ethylene diamine tetra acetates, 54 parts of water, 93 parts of ethanol and 39 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 1.7h under the conditions of 58 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 37 parts of ammoniacal liquor, 41 parts of charcoal-aero gels, 18 parts of polyvinyl alcohol and 50 parts of ethanol, are weighed to be added to
In reactor, 1.4h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 17 parts of aminopropyl triethoxysilanes and 55 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 92r/min, and 2.7h is reacted under the conditions of 54 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 93 parts of polyvinyl chloride, 8 parts of ferrous oxides, 1.4 parts of barium metaphosphates and 4.5 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 172 DEG C of hybrid reaction 0.9h of temperature, with extruder in 172 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5), weigh 100 parts of polyvinyl chloride long fibres, 85 parts of polyvinyl chloride, 11 parts of modified oxidized ferrous irons, 19 parts of calcium hydroxides,
1.2 parts of barium metaphosphates and 2.5 parts of aminopropyl triethoxysilanes are added in mill, with mill in 172 DEG C of mixing of temperature
0.8h is reacted, with extruder in 172 DEG C of extruding pelletizations of temperature, that is, obtains polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 12 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 172 DEG C of hybrid reaction 0.8h of temperature, with extruder in 172 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 9
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of sodium iron ethylene diamine tetra acetates, 57 parts of water, 87 parts of ethanol and 42 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 0.7h under the conditions of 59 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 28 parts of ammoniacal liquor, 37 parts of charcoal-aero gels, 19 parts of polyvinyl alcohol and 52 parts of ethanol, are weighed to be added to
In reactor, 2.3h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations
2h, 105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C are calcined
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, 120 DEG C of drys 2h, grinds, obtains ferrous oxide;
(3) 10 parts of ferrous oxides, 18 parts of aminopropyl triethoxysilanes and 45 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 83r/min, and 1.2h is reacted under the conditions of 51 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, is obtained modified oxidized
It is ferrous;
(4) 10 parts of coppe ferrites, 89 parts of polyvinyl chloride, 7 parts of ferrous oxides, 2.6 parts of barium metaphosphates and 3.6 parts of aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 179 DEG C of hybrid reaction 0.9h of temperature, with extruder in 179 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride;
(5), weigh 100 parts of polyvinyl chloride long fibres, 88 parts of polyvinyl chloride, 11 parts of modified oxidized ferrous irons, 14 parts of calcium hydroxides,
1.4 parts of barium metaphosphates and 2.9 parts of aminopropyl triethoxysilanes are added in mill, with mill in 179 DEG C of mixing of temperature
0.8h is reacted, with extruder in 179 DEG C of extruding pelletizations of temperature, that is, obtains polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 13 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 179 DEG C of hybrid reaction 0.8h of temperature, with extruder in 179 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 10
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprise the following steps:
(1) 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of sodium iron ethylene diamine tetra acetates, 53 parts of water, 99 parts of ethanol and 46 parts, are weighed
Charcoal-aero gel is added in reactor, reacts 0.8h under the conditions of 56 DEG C of maintenance system temperature, and at 80 DEG C, -0.06MPa decompressions are steamed
2h, 105 DEG C of dry 2h are evaporated, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings are calcined in 200 DEG C
2 times, filtering, 120 DEG C of dry 2h, grinding, obtain coppe ferrite;
(2) 100 parts of frerrous chlorides, 33 parts of ammoniacal liquor, 44 parts of charcoal-aero gels, 16 parts of polyvinyl alcohol and 47 parts of ethanol, are weighed to be added to
In reactor, 3h is reacted under the conditions of 59 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is passed through
1L water washings 3 times, filtering, 500mL ethanol wash 2 times, filtering, 120 DEG C of drys 2h, grind, obtain ferrous oxide;
(3) 10 parts of ferrous oxides, 19 parts of aminopropyl triethoxysilanes and 35 parts of ethanol, are weighed to be added in reactor, are stirred
Speed is 93r/min, and 2h is reacted under the conditions of 53 DEG C of maintenance system temperature, filtered, 120 DEG C of dry 2h, obtains modified oxidized Asia
Iron;
(4) 10 parts of coppe ferrites, 98 parts of polyvinyl chloride, 7 parts of ferrous oxides, 2 parts of barium metaphosphates and 5 parts of ethoxies of aminopropyl three, are weighed
Base silane is added in mill, with mill in 185 DEG C of hybrid reaction 0.9h of temperature, with extruder in 185 DEG C of extrusions of temperature
It is granulated, that is, obtains modified polyvinyl chloride;
(5) 100 parts of polyvinyl chloride long fibres, 86 parts of polyvinyl chloride, 10 parts of modified oxidized ferrous, 15 parts of calcium hydroxides, 1, are weighed
Part barium metaphosphate and 3 parts of aminopropyl triethoxysilanes are added in mill, with mill in 185 DEG C of hybrid reactions of temperature
0.7h, with extruder in 185 DEG C of extruding pelletizations of temperature, that is, obtain polyvinyl chloride long fibre modified polyvinyl chloride;
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 19 parts of modified polyvinyl chlorides, 12 parts of polyvinylidene chloride, are weighed
It is added in mill, with mill in 185 DEG C of hybrid reaction 0.6h of temperature, with extruder in 185 DEG C of extruding pelletizations of temperature, i.e.,
Obtain inorganic material-modified polyvinyl chloride granules.
Reference examples 1
In this reference examples, coppe ferrite is not added, other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, ferrous oxide is not added, other components and preparation method are same as Example 1.
Reference examples 3
In this reference examples, modified polyvinyl chloride is not added, other components and preparation method are same as Example 1.
Reference examples 4
In this reference examples, polyvinyl chloride long fibre modified polyvinyl chloride, other components and preparation method and the phase of embodiment 1 are not added
Together.
Reference examples 5
In this reference examples, polyvinylidene chloride is not added, other components and preparation method are same as Example 1.
Reference examples 6
In this reference examples, calcium hydroxide is not added, other components and preparation method are same as Example 1.
Reference examples 7
In this reference examples, the coppe ferrite selected in formula in common coppe ferrite alternate embodiment 1, other components and preparation method with
Embodiment 1 is identical.
Reference examples 8
In this reference examples, from the ferrous oxide in common ferrous oxide alternate embodiment 1, other components and preparation side in formula
Method is same as Example 1.
The performance parameter of inorganic material-modified polyvinyl chloride made from the embodiment 1 of table 1 and reference examples 1~8
Embodiment 1 | Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 | Reference examples 5 | Reference examples 6 | Reference examples 7 | Reference examples 8 | |
Oxygen index (OI) % | 36 | 33 | 35 | 31 | 34 | 32 | 26 | 33 | 35 |
Water vapor transmittance/g/(m2.24h.mm) | 0.2 | 0.25 | 0.26 | 0.21 | 0.24 | 0.38 | 0.23 | 0.24 | 0.25 |
Tensile strength/MPa | 65 | 62 | 60 | 63 | 41 | 62 | 63 | 62 | 63 |
Self-cleaning property | It is excellent | Typically | Difference | Difference | It is excellent | It is excellent | It is excellent | Difference | Difference |
Described above is the preferred embodiment of the invention, it is noted that for those skilled in the art,
On the premise of the inventive principle is not departed from, some improvements and modifications can also be made, these improvements and modifications are also considered as the hair
Bright protection domain.
Claims (2)
- A kind of 1. preparation method of inorganic material-modified polyvinyl chloride, it is characterised in that:Including following raw material components:Polyvinyl chloride Long fibre modified polyvinyl chloride, modified polyvinyl chloride, polyvinylidene chloride, described polyvinyl chloride long fibre modified polyvinyl chloride Alkene, modified polyvinyl chloride, polyvinylidene chloride are according to quality parts ratio 100:14~20:7~15 are added in mill, with opening Mill is in 140~190 DEG C of 0.5~1h of hybrid reaction of temperature, with extruder in 140~190 DEG C of extruding pelletizations of temperature;Wherein, institute The polyvinyl chloride long fibre modified polyvinyl chloride stated is by polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous, hydroxide Calcium, barium metaphosphate and aminopropyl triethoxysilane reaction are made, described polyvinyl chloride long fibre, polyvinyl chloride, modified oxygen Change ferrous iron, calcium hydroxide, barium metaphosphate and aminopropyl triethoxysilane according to quality parts ratio 100:75~90:7~13:13 ~22:1~2:2~3 are added in mill, with mill in 140~190 DEG C of 0.5~1h of hybrid reaction of temperature, use extruder In 140~190 DEG C of extruding pelletizations of temperature;Described modified polyvinyl chloride is by coppe ferrite, polyvinyl chloride, ferrous oxide, metaphosphoric acid Barium and aminopropyl triethoxysilane reaction are made, described coppe ferrite, polyvinyl chloride, ferrous oxide, barium metaphosphate and ammonia third Ethyl triethoxy silicane alkane is according to quality parts ratio 10:85~100:6~10:1~3:2~5 are added in mill, use mill In 140~190 DEG C of 0.5~1h of hybrid reaction of temperature, with extruder in 140~190 DEG C of extruding pelletizations of temperature;Described modification oxygen Change ferrous iron to be made by ferrous oxide, aminopropyl triethoxysilane and ethanol synthesis, described ferrous oxide, the ethoxy of aminopropyl three Base silane and ethanol are according to quality parts ratio 10:15~20:30~70 are added in reactor, and mixing speed is 72~95r/ Min, 1~3h, filtered, 120 DEG C of dry 2h are reacted under the conditions of 40~55 DEG C of maintenance system temperature;Described ferrous oxide by Frerrous chloride, ammoniacal liquor, charcoal-aero gel, polyvinyl alcohol and ethanol synthesis are made, described frerrous chloride, ammoniacal liquor, charcoal-aero gel, poly- Vinyl alcohol and ethanol are according to quality parts ratio 100:25~45:33~46:13~22:46~55 are added in reactor, maintain 1~3h is reacted under the conditions of 45~63 DEG C of system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations 2h, 105 DEG C dry Dry 2h, under nitrogen protection, 2h is calcined in 200 DEG C, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, is washed through 1L Wash 3 times, filter, 500mL ethanol washs 2 times, filtering, 120 DEG C of dry 2h, grinding;Described coppe ferrite is by ethylenediamine tetra-acetic acid Copper sodium, sodium iron ethylene diamine tetra acetate, water, ethanol and charcoal-aero gel reaction are made, described cupric ethylene diamine tetraacetate sodium, ethylenediamine Tetraacethyl ferrisodium, water, the quality parts ratio of ethanol and charcoal-aero gel are 100:80~90:51~62:85~100:37~47.
- A kind of 2. preparation method of inorganic material-modified polyvinyl chloride according to claim 1, it is characterised in that:Described Coppe ferrite is as made from following preparation method:By cupric ethylene diamine tetraacetate sodium, sodium iron ethylene diamine tetra acetate, water, ethanol and charcoal Aeroge is 100 according to quality parts ratio:80~90:51~62:85~100:37~47 are added in reactor, maintenance system 0.5~2h is reacted under the conditions of 50~70 DEG C of temperature, at 80 DEG C, -0.06MPa is evaporated under reduced pressure 2h, 105 DEG C of dry 2h, in 200 DEG C 2h is calcined, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, through 1L water washings 2 times, filtering, 120 DEG C of dry 2h, is ground Mill.
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- 2016-07-28 CN CN201710818901.5A patent/CN107459740B/en active Active
- 2016-07-28 CN CN201710819458.3A patent/CN107501798A/en not_active Withdrawn
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EP2298835A1 (en) * | 2009-04-15 | 2011-03-23 | Rohm And Haas Company | Stabilized polymer compositions |
CN103467883A (en) * | 2013-08-26 | 2013-12-25 | 晶锋集团股份有限公司 | Lead-free termite-proof polyvinyl chloride cable material and preparation method thereof |
CN103642109A (en) * | 2013-11-18 | 2014-03-19 | 西南科技大学 | Photo-thermal cooperatively controllably degradable high-molecular composite mater batch and preparation method thereof |
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CN108963944A (en) * | 2018-08-06 | 2018-12-07 | 宁夏三林管业有限公司 | Compound reinforcement plastic film pre-fabricated electric cables ditch pipeline and its manufacture craft |
CN108963944B (en) * | 2018-08-06 | 2020-11-20 | 宁夏三林管业有限公司 | Composite reinforced plastic film prefabricated cable trench pipeline and manufacturing process thereof |
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CN107522978A (en) | 2017-12-29 |
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CN106243550A (en) | 2016-12-21 |
CN106243550B (en) | 2017-10-31 |
CN107522978B (en) | 2018-06-15 |
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