CN106243550B - A kind of inorganic material-modified polyvinyl chloride and preparation method thereof - Google Patents
A kind of inorganic material-modified polyvinyl chloride and preparation method thereof Download PDFInfo
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- CN106243550B CN106243550B CN201610602873.9A CN201610602873A CN106243550B CN 106243550 B CN106243550 B CN 106243550B CN 201610602873 A CN201610602873 A CN 201610602873A CN 106243550 B CN106243550 B CN 106243550B
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- polyvinyl chloride
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 197
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 177
- 238000002360 preparation method Methods 0.000 title claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 122
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 229910001868 water Inorganic materials 0.000 claims abstract description 40
- 239000000835 fiber Substances 0.000 claims abstract description 39
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 36
- 239000004964 aerogel Substances 0.000 claims abstract description 35
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 17
- ATSGLBOJGVTHHC-UHFFFAOYSA-N bis(ethane-1,2-diamine)copper(2+) Chemical compound [Cu+2].NCCN.NCCN ATSGLBOJGVTHHC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 claims abstract description 17
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 17
- 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 17
- 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 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims abstract description 8
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 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
- 239000005033 polyvinylidene chloride Substances 0.000 claims abstract description 8
- MKWYFZFMAMBPQK-UHFFFAOYSA-J sodium feredetate Chemical compound [Na+].[Fe+3].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O MKWYFZFMAMBPQK-UHFFFAOYSA-J 0.000 claims abstract description 6
- 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 52
- 238000012423 maintenance Methods 0.000 claims description 39
- 238000005453 pelletization Methods 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- -1 aminopropyl Chemical group 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000008187 granular material Substances 0.000 claims description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 11
- 229910052791 calcium Inorganic materials 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 11
- 238000005292 vacuum distillation Methods 0.000 claims description 9
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229920001596 poly (chlorostyrenes) Polymers 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 6
- 229910052788 barium Inorganic materials 0.000 description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 14
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 11
- 125000003963 dichloro group Chemical group Cl* 0.000 description 11
- 238000001125 extrusion Methods 0.000 description 11
- 150000001805 chlorine compounds Chemical class 0.000 description 10
- 230000006837 decompression Effects 0.000 description 10
- 229940048820 edetates Drugs 0.000 description 10
- 150000004679 hydroxides Chemical class 0.000 description 10
- 239000011734 sodium Substances 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 10
- 229910021529 ammonia Inorganic materials 0.000 description 7
- 238000004821 distillation Methods 0.000 description 7
- 238000010025 steaming Methods 0.000 description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 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
- 239000007789 gas Substances 0.000 description 3
- 150000002926 oxygen Chemical class 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 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
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding 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
- 230000009467 reduction Effects 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- 150000001412 amines Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 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
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002649 leather substitute Substances 0.000 description 1
- 238000004519 manufacturing process 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
- 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
-
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—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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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- 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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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
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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, Ferric Sodium Edetate, 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 methods such as extrusion, injection, molding, blowings, be widely used in manufacture 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,
Various plastic products, inorganic material-modified polychlorostyrene prepared by this method are prepared into by techniques such as extrusion, injection, molding, blowings
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, which passes through, to be changed
Reactant feed and technology mode, the material of preparation has 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, Ferric Sodium Edetate, 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 vacuum distillations 2h, 105 DEG C of dry 2h, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, through 1L water washings 2 times, filtering, 120 DEG C of dry 2h, grinding obtains 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,
1~3h is reacted under the conditions of 45~63 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations 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, and 120 DEG C of dry 2h, grinding obtains 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
Speed is mixed for 72~95r/min, 1~3h is reacted under the conditions of 40~55 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h,
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, obtains 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, obtains inorganic material-modified polyvinyl chloride granules.
The preparation method of inorganic material-modified polyvinyl chloride described in the invention, comprises the following steps：
(1), by cupric ethylene diamine tetraacetate sodium, Ferric Sodium Edetate, water, ethanol and charcoal-aero gel according to mass fraction
Than for 100：80~90：51~62：85~100：37~47 are added in reactor, 50~70 DEG C of conditions of maintenance system temperature
0.5~2h of lower reaction, at 80 DEG C, -0.06MPa vacuum distillations 2h, 105 DEG C of dry 2h are calcined 2h, 300 DEG C of roastings in 200 DEG C
2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h, through 1L water washings 2 times, filtering, 120 DEG C of dry 2h, grinding obtains coppe ferrite；Institute
The purpose for the charcoal-aero gel stated is in order to improve the dispersiveness and reduction iron of cupric ethylene diamine tetraacetate sodium and Ferric Sodium Edetate
The agglomeration of sour copper.
(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 vacuum distillations 2h, 105 DEG C of dry 2h under nitrogen protection, 2h, 300 DEG C are calcined in 200 DEG C
2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h are calcined, 2 times, filtering, 120 DEG C are washed through 1L water washings 3 times, filtering, 500mL ethanol
2h is dried, grinding obtains ferrous oxide；The purpose of described charcoal-aero gel in order to improve frerrous chloride dispersiveness and reduction 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 1~3h of reaction, warp under the conditions of 72~95r/min, 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 compares 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, obtains modified polyvinyl chloride；The mesh of described coppe ferrite
The fungus resistance energy in order to improve 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 is strong for the mechanics for improving 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 compares 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 fixed cupric ethylene diamine tetraacetate sodium and second two
Amine tetraacethyl ferrisodium, after high-temperature heat treatment, obtains coppe ferrite and has excellent ratio surface, particle homogeneity, low-surface-energy, low
The performances such as reunion；
2nd, charcoal-aero gel has big specific surface area, can preferably disperse and fixed frerrous chloride, and polyvinyl alcohol can
Preferably to disperse the reaction rate of ammonia spirit, control ammoniacal liquor and frerrous chloride, the ferrous oxide of preparation has excellent ratio
The performances such as surface, particle homogeneity, low-surface-energy, low reunion；
3rd, coppe ferrite and ferrous oxide have excellent hydrophobicity, in Blending Processes, and coppe ferrite and ferrous oxide can be with
Assign polyvinyl chloride excellent hydrophobic performance, be unfavorable for dirty material absorption in polyvinyl chloride surface, so as to reach polyvinyl chloride table
The automatically cleaning effect in face；
4th, polyvinyl chloride can discharge hydrogen chloride gas, the hydrogen chloride of polyvinyl chloride release can during processing and use
With with calcium hydroxide reaction, form calcium chloride and water, calcium chloride acts not only as filler and used, and can also impart to polychlorostyrene second
While alkene fire resistance, the harm that polyvinyl chloride discharges hydrogen chloride is solved；
5th, polyvinyl chloride long fibre has excellent mechanical property, and has excellent compatibility with polyvinyl chloride, can be with
Assign polyvinyl chloride excellent tensile property, 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 comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 85 parts of Ferric Sodium Edetates, 57 parts of water, 93 parts of ethanol and
43 parts of charcoal-aero gels are added in reactor, react 1.3h under the conditions of 62 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 1.5h is reacted under the conditions of 53 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding 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,
Mixing speed is to react 1.6h under the conditions of 84r/min, 47 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 aminopropyls, are weighed
Triethoxysilane is added in mill, with mill in 170 DEG C of hybrid reaction 0.7h of temperature, with extruder in temperature 170
DEG C extruding pelletization, 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 hydroxides, are weighed
Calcium, 2 parts of barium metaphosphates and 2.5 parts of aminopropyl triethoxysilanes are added in mill, with mill in 170 DEG C of mixing of temperature
0.6h is reacted, with extruder in 170 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 17 parts of modified polyvinyl chlorides, 13 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 170 DEG C of hybrid reaction 0.5h of temperature, is made with extruder in 170 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 2
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 80 parts of Ferric Sodium Edetates, 51 parts of water, 85 parts of ethanol and
37 parts of charcoal-aero gels are added in reactor, react 0.5h under the conditions of 50 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 1h is reacted under the conditions of 45 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, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 1h under the conditions of 72r/min, 40 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, obtains being modified oxygen
Change ferrous；
(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 aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 140 DEG C of hybrid reaction 0.5h of temperature, with extruder in 140 DEG C of temperature
Extruding pelletization, that is, obtain modified polyvinyl chloride；
(5) 100 parts of polyvinyl chloride long fibres, 75 parts of polyvinyl chloride, 7 parts of modified oxidized ferrous, 13 parts of hydroxides, are weighed
Calcium, 1 part of barium metaphosphate and 2 parts of aminopropyl triethoxysilanes are added in mill, anti-in 140 DEG C of mixing of temperature with mill
0.5h is answered, with extruder in 140 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 14 parts of modified polyvinyl chlorides, 7 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 140 DEG C of hybrid reaction 0.5h of temperature, is made with extruder in 140 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 3
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 90 parts of Ferric Sodium Edetates, 62 parts of water, 100 parts of ethanol and
47 parts of charcoal-aero gels are added in reactor, and 2h is reacted under the conditions of 70 DEG C of maintenance system temperature, in 80 DEG C, -0.06MPa decompressions
2h, 105 DEG C of dry 2h are distilled, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h are calcined in 200 DEG C, is washed through 1L
2 times, filtering are washed, 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 add
Enter into reactor, 3h is reacted under the conditions of 63 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, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 3h under the conditions of 95r/min, 55 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, obtains being modified oxygen
Change ferrous；
(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 aminopropyls, are weighed
Triethoxysilane is added in mill, with mill in 190 DEG C of hybrid reaction 1h of temperature, with extruder in 190 DEG C of temperature
Extruding pelletization, that is, obtain 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 hydroxides, are weighed
Calcium, 2 parts of barium metaphosphates and 3 parts of aminopropyl triethoxysilanes are added in mill, anti-in 190 DEG C of mixing of temperature with mill
1h is answered, with extruder in 190 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 20 parts of modified polyvinyl chlorides, 15 parts of poly- inclined dichloros, are weighed
Ethene 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,
Obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 4
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 81 parts of Ferric Sodium Edetates, 61 parts of water, 97 parts of ethanol and
39 parts of charcoal-aero gels are added in reactor, react 0.8h under the conditions of 56 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 1.2h is reacted under the conditions of 47 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding 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,
Mixing speed is to react 1.4h under the conditions of 75r/min, 43 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 147 DEG C of hybrid reaction 1.7h of temperature, with extruder in temperature
147 DEG C of extruding pelletizations, that is, obtain modified polyvinyl chloride；
(5) 100 parts of polyvinyl chloride long fibres, 88 parts of polyvinyl chloride, 12 parts of modified oxidized ferrous, 21 parts of hydroxides, are weighed
Calcium, 1.5 parts of barium metaphosphates and 2.7 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 147 DEG C in temperature with mill
Reaction 1.8h is closed, with extruder in 147 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 14 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 147 DEG C of hybrid reaction 0.9h of temperature, is made with extruder in 147 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 5
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 81 parts of Ferric Sodium Edetates, 55 parts of water, 88 parts of ethanol and
39 parts of charcoal-aero gels are added in reactor, and 1.2h is reacted under the conditions of 55 DEG C of maintenance system temperature, in 80 DEG C, -0.06MPa decompressions
2h, 105 DEG C of dry 2h are distilled, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h are calcined in 200 DEG C, is washed through 1L
2 times, filtering are washed, 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 add
Enter into reactor, 2.6h is reacted under the conditions of 60 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding 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,
Mixing speed is to react 2.7h under the conditions of 90r/min, 52 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 153 DEG C of hybrid reaction 1.9h of temperature, with extruder in temperature
153 DEG C of extruding pelletizations, 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 hydroxides, are weighed
Calcium, 1.8 parts of barium metaphosphates and 2.1 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 153 DEG C in temperature with mill
Reaction 1.6h is closed, with extruder in 153 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 16 parts of modified polyvinyl chlorides, 11 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 153 DEG C of hybrid reaction 1.4h of temperature, is made with extruder in 153 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 6
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 83 parts of Ferric Sodium Edetates, 57 parts of water, 91 parts of ethanol and
41 parts of charcoal-aero gels are added in reactor, and 1.7h is reacted under the conditions of 58 DEG C of maintenance system temperature, in 80 DEG C, -0.06MPa decompressions
2h, 105 DEG C of dry 2h are distilled, 2h, 300 DEG C of roastings 2h, 400 DEG C of roastings 2h, 500 DEG C of roasting 3h are calcined in 200 DEG C, is washed through 1L
2 times, filtering are washed, 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 add
Enter into reactor, 2.4h is reacted under the conditions of 47 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 1.4h under the conditions of 92r/min, 51 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 158 DEG C of hybrid reaction 1.1h of temperature, with extruder in temperature
158 DEG C of extruding pelletizations, 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 hydroxides, are weighed
Calcium, 1.3 parts of barium metaphosphates and 2.8 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 158 DEG C in temperature with mill
Reaction 1.2h is closed, with extruder in 158 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 19 parts of modified polyvinyl chlorides, 12 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 158 DEG C of hybrid reaction 1.9h of temperature, is made with extruder in 158 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 7
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 84 parts of Ferric Sodium Edetates, 58 parts of water, 90 parts of ethanol and
44 parts of charcoal-aero gels are added in reactor, react 1.8h under the conditions of 66 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 2.2h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 1.3h under the conditions of 88r/min, 47 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 164 DEG C of hybrid reaction 1.7h of temperature, with extruder in temperature
164 DEG C of extruding pelletizations, that is, obtain modified polyvinyl chloride；
(5) 100 parts of polyvinyl chloride long fibres, 82 parts of polyvinyl chloride, 12 parts of modified oxidized ferrous, 17 parts of hydroxides, are weighed
Calcium, 1.7 parts of barium metaphosphates and 2.7 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 164 DEG C in temperature with mill
Reaction 1.4h is closed, with extruder in 164 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 9 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 164 DEG C of hybrid reaction 1.7h of temperature, is made with extruder in 164 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 8
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of Ferric Sodium Edetates, 54 parts of water, 93 parts of ethanol and
39 parts of charcoal-aero gels are added in reactor, react 1.7h under the conditions of 58 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 1.4h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 2.7h under the conditions of 92r/min, 54 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 172 DEG C of hybrid reaction 0.9h of temperature, with extruder in temperature
172 DEG C of extruding pelletizations, that is, obtain modified polyvinyl chloride；
(5) 100 parts of polyvinyl chloride long fibres, 85 parts of polyvinyl chloride, 11 parts of modified oxidized ferrous, 19 parts of hydroxides, are weighed
Calcium, 1.2 parts of barium metaphosphates and 2.5 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 172 DEG C in temperature with mill
Reaction 0.8h is closed, with extruder in 172 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 12 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 172 DEG C of hybrid reaction 0.8h of temperature, is made with extruder in 172 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 9
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of Ferric Sodium Edetates, 57 parts of water, 87 parts of ethanol and
42 parts of charcoal-aero gels are added in reactor, react 0.7h under the conditions of 59 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 2.3h is reacted under the conditions of 57 DEG C of maintenance system temperature, under nitrogen protection, 80 DEG C, -0.06MPa decompression steamings
2h, 105 DEG C of dry 2h are evaporated, under nitrogen protection, 2h, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding 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,
Mixing speed is to react 1.2h under the conditions of 83r/min, 51 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, is modified
Ferrous oxide；
(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 ammonia third, are weighed
Ethyl triethoxy silicane alkane is added in mill, with mill in 179 DEG C of hybrid reaction 0.9h of temperature, with extruder in temperature
179 DEG C of extruding pelletizations, that is, obtain modified polyvinyl chloride；
(5) 100 parts of polyvinyl chloride long fibres, 88 parts of polyvinyl chloride, 11 parts of modified oxidized ferrous, 14 parts of hydroxides, are weighed
Calcium, 1.4 parts of barium metaphosphates and 2.9 parts of aminopropyl triethoxysilanes are added in mill, are mixed for 179 DEG C in temperature with mill
Reaction 0.8h is closed, with extruder in 179 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 18 parts of modified polyvinyl chlorides, 13 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 179 DEG C of hybrid reaction 0.8h of temperature, is made with extruder in 179 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
Embodiment 10
A kind of inorganic material-modified polyvinyl chloride, its preparation method comprises the following steps：
(1), weigh 100 parts of cupric ethylene diamine tetraacetate sodium, 87 parts of Ferric Sodium Edetates, 53 parts of water, 99 parts of ethanol and
46 parts of charcoal-aero gels are added in reactor, react 0.8h under the conditions of 56 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa subtracts
Pressure distillation 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 are calcined in 200 DEG C
Washing 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 add
Enter into reactor, 3h is reacted under the conditions of 59 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, 300 DEG C of roastings 2h, 400 DEG C of roasting 2h, 500 DEG C of roastings are calcined in 200 DEG C
3h, 2 times, filtering are washed through 1L water washings 3 times, filtering, 500mL ethanol, and 120 DEG C of dry 2h, grinding obtains 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,
Mixing speed is to react 2h under the conditions of 93r/min, 53 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, obtains being modified oxygen
Change ferrous；
(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 aminopropyls three, are weighed
Ethoxysilane is added in mill, with mill in 185 DEG C of hybrid reaction 0.9h of temperature, with extruder in 185 DEG C of temperature
Extruding pelletization, 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, 15 parts of hydroxides, are weighed
Calcium, 1 part of barium metaphosphate and 3 parts of aminopropyl triethoxysilanes are added in mill, anti-in 185 DEG C of mixing of temperature with mill
0.7h is answered, with extruder in 185 DEG C of extruding pelletizations of temperature, that is, polyvinyl chloride long fibre modified polyvinyl chloride is obtained；
(6) 100 parts of polyvinyl chloride long fibre modified polyvinyl chlorides, 19 parts of modified polyvinyl chlorides, 12 parts of poly- inclined dichloros, are weighed
Ethene is added in mill, with mill in 185 DEG C of hybrid reaction 0.6h of temperature, is made with extruder in 185 DEG C of extrusions of temperature
Grain, that is, obtain inorganic material-modified polyvinyl chloride granules.
The performance parameter of inorganic material-modified polyvinyl chloride made from the embodiment 1 of table 1
| Embodiment 1 | |
| Oxygen index (OI) % | 36 |
| Water vapor transmittance/g/（m2.24h.mm） | 0.2 |
| Tensile strength/MPa | 65 |
| Self-cleaning property | It is excellent |
Described above is the preferred embodiment of the invention, it is noted that for those skilled in the art
For, 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 protection domain of the invention.
Claims (2)
1. a kind of 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, the quality parts ratio of polyvinylidene chloride are 100：14~20：7~15, wherein, described polychlorostyrene second
Alkene long fibre modified polyvinyl chloride is by polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous iron, calcium hydroxide, barium metaphosphate
It is made with aminopropyl triethoxysilane reaction, described polyvinyl chloride long fibre, polyvinyl chloride, modified oxidized ferrous, hydrogen-oxygen
The quality parts ratio for changing calcium, barium metaphosphate and aminopropyl triethoxysilane is 100：75~90：7~13：13~22：1~2：2
~3, described modified polyvinyl chloride is by coppe ferrite, polyvinyl chloride, ferrous oxide, barium metaphosphate and aminopropyl triethoxysilane
Reaction is made, described coppe ferrite, polyvinyl chloride, ferrous oxide, the mass parts of barium metaphosphate and aminopropyl triethoxysilane
Number is than being 10：85~100：6~10：1~3：2~5, described modified oxidized ferrous iron is by ferrous oxide, aminopropyl-triethoxy
Silane and ethanol synthesis are made, and the quality parts ratio of described ferrous oxide, aminopropyl triethoxysilane and ethanol is 10：15
~20：30~70, described ferrous oxide is made by frerrous chloride, ammoniacal liquor, charcoal-aero gel, polyvinyl alcohol and ethanol synthesis, institute
The quality parts ratio of frerrous chloride, ammoniacal liquor, charcoal-aero gel, polyvinyl alcohol and the ethanol stated is 100：25~45：33~46：13~
22：46~55, described coppe ferrite is anti-by cupric ethylene diamine tetraacetate sodium, Ferric Sodium Edetate, water, ethanol and charcoal-aero gel
It should be made, described cupric ethylene diamine tetraacetate sodium, Ferric Sodium Edetate, water, the quality parts ratio of ethanol and charcoal-aero gel
For 100：80~90：51~62：85~100：37~47.
2. a kind of preparation method of inorganic material-modified polyvinyl chloride according to claim 1, it is characterised in that：Described
Inorganic material-modified polyvinyl chloride is as made from following preparation method：(1), by cupric ethylene diamine tetraacetate sodium, ethylenediamine tetrem
Sour ferrisodium, water, ethanol and charcoal-aero gel are 100 according to quality parts ratio：80~90：51~62：85~100：37~47 add
Into reactor, 0.5~2h is reacted under the conditions of 50~70 DEG C of maintenance system temperature, at 80 DEG C, -0.06MPa vacuum distillation 2h,
105 DEG C of dry 2h, 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 washings 2 times,
Filtering, 120 DEG C of dry 2h, grinding obtains coppe ferrite；(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, and maintenance system temperature 45~
1~3h, under nitrogen protection, 80 DEG C, -0.06MPa vacuum distillations 2h, 105 DEG C of dry 2h, in nitrogen are reacted under the conditions of 63 DEG C
Under 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 washings 3 times, filtering,
500mL ethanol washs 2 times, filtering, and 120 DEG C of dry 2h, grinding obtains ferrous oxide；(3), by ferrous oxide, the second of aminopropyl three
TMOS and ethanol are according to quality parts ratio 10：15~20：30~70 are added in reactor, and mixing speed is 72~95r/
1~3h is reacted under the conditions of min, 40~55 DEG C of maintenance system temperature, through filtering, 120 DEG C of dry 2h, modified oxidized ferrous iron is obtained；
(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 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, obtains modified polyvinyl chloride；(5), by polyvinyl chloride long fibre,
Polyvinyl chloride, modified oxidized ferrous iron, calcium hydroxide, barium metaphosphate and aminopropyl triethoxysilane are 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 hybrid reactions of temperature
0.5~1h, with extruder in 140~190 DEG C of extruding pelletizations of temperature, that is, obtains polyvinyl chloride long fibre modified polyvinyl chloride；
(6), by polyvinyl chloride long fibre modified polyvinyl chloride, modified polyvinyl chloride, polyvinylidene chloride according to quality parts 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, are existed with extruder
140~190 DEG C of extruding pelletizations of temperature, that is, obtain inorganic material-modified polyvinyl chloride granules.
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| CN201710819458.3A CN107501798A (en) | 2016-07-28 | 2016-07-28 | A kind of inorganic material polyvinyl chloride and preparation method thereof |
| CN201610602873.9A CN106243550B (en) | 2016-07-28 | 2016-07-28 | A kind of inorganic material-modified polyvinyl chloride and preparation method thereof |
| CN201710818999.4A CN107522978B (en) | 2016-07-28 | 2016-07-28 | A kind of modified inorganic material polyvinyl chloride and preparation method thereof |
| CN201710818901.5A CN107459740B (en) | 2016-07-28 | 2016-07-28 | A kind of inorganic material-modified polyvinyl chloride and preparation method thereof |
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| CN201710818999.4A Division CN107522978B (en) | 2016-07-28 | 2016-07-28 | A kind of modified inorganic material polyvinyl chloride and preparation method thereof |
| CN201710818901.5A Division CN107459740B (en) | 2016-07-28 | 2016-07-28 | A kind of inorganic material-modified polyvinyl chloride and preparation method thereof |
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