CN106280081A - A kind of micro crystal graphite modified PVC pipeline and preparation method thereof - Google Patents

A kind of micro crystal graphite modified PVC pipeline and preparation method thereof Download PDF

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CN106280081A
CN106280081A CN201610639866.6A CN201610639866A CN106280081A CN 106280081 A CN106280081 A CN 106280081A CN 201610639866 A CN201610639866 A CN 201610639866A CN 106280081 A CN106280081 A CN 106280081A
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micro crystal
crystal graphite
carbon black
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陶如意
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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
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08L2205/03—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

Abstract

This invention relates to a kind of micro crystal graphite modified PVC pipeline, including following raw material components: PVC, modified polyacrylic acid isobutyl ester, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, modified carbon black, modified polyacrylic acid isobutyl ester is by polyisobutyl acrylate, Merlon, triethylene tetramine, polyacrylic acid and the reaction of 3 aminopropyltriethoxywerene werene prepare, micro crystal graphite is by wood powder, ammonium oxalate, powder of straw and phenol-formaldehyde resin modified reaction prepare, phenol-formaldehyde resin modified is by phenolic resin, methylolurea, N, the reaction of N dinitrosopentamethlyene tetramine prepares, modified carbon black is by sodium hexameta phosphate, white carbon black, hydrogen peroxide, sodium hydroxide, water and epichlorohydrin reaction prepare.This invention has the advantages such as the heat conductivity of excellence, heat stability, wearability, low free chlorine, impact strength, filler dispersibility, anti-flammability, mechanical property, resistance to ag(e)ing, oxidative resistance.

Description

A kind of micro crystal graphite modified PVC pipeline and preparation method thereof
Technical field
This invention relates to a kind of micro crystal graphite modified PVC pipeline and preparation method thereof.
Background technology
Pvc pipe has that the adhesive property of excellence, corrosion resistance, fluid resistance be little, watertightness, anti-gnaw, that price is low etc. is excellent Gesture.PVC plastic pipeline is widely used in municipal administration plumbing, industry plumbing, civilian plumbing, irrigation, vegetation are watered, chemical industry and Sanitary wastewater, chemicals, add hydrothermal solution and coolant, food, ultrarapture liquid, mud, gas, compressed air and vacuum system etc. neck Territory.
At present, PVC is material modified in heat conductivity, heat stability, wearability, low free chlorine, impact strength, filler dispersion The performance need such as property, anti-flammability, mechanical property, resistance to ag(e)ing, oxidative resistance promotes further.This invention uses PVC, modification poly- The raw materials such as Isobutyl 2-propenoate, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, modified carbon black By fundamental technology, being prepared for micro crystal graphite modified PVC pipeline, micro crystal graphite modified PVC pipeline prepared by the method has excellent Different heat conductivity, heat stability, wearability, low free chlorine, impact strength, filler dispersibility, anti-flammability, mechanical property, resistance to always The performances such as the property changed, oxidative resistance.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of micro crystal graphite modified PVC pipeline, and the method is by changing Reactant feed and technology mode, the pipeline of preparation has the heat conductivity of excellence, heat stability, wearability, low free chlorine, impact The performances such as intensity, filler dispersibility, anti-flammability, mechanical property, resistance to ag(e)ing, oxidative resistance.
To achieve these goals, the technical scheme of this invention is as follows.
A kind of micro crystal graphite modified PVC pipeline and preparation method thereof, specifically includes following steps: (1), by hexa metaphosphoric acid Sodium, white carbon black, hydrogen peroxide, sodium hydroxide, water and epoxychloropropane are 10:105～140:17～25:1～5:2 according to portion rate ～9:12～25 joins in reactor, mixing speed is 46～63r/min, anti-under the conditions of maintenance system temperature 51～68 DEG C Answer 1～3h, in 70 DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；(2), by phenolic resin, methylolurea, N, N-bis- Nitroso-group five methine tetramine joins in reactor according to portion rate 100:2～20:10～17, and reaction temperature is 20～35 DEG C, mixing speed is 35～40r/min reactions 0.2～0.8h, obtains phenol-formaldehyde resin modified；(3), by wood powder, ammonium oxalate, straw Powder and phenol-formaldehyde resin modified join in reactor according to portion rate 100:90～120:70～95:18～32, and reaction temperature is 85～120 DEG C, mixing speed is 38～50r/min reactions 0.3～0.8h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat Process 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtain micro crystal graphite；(4), will be poly- Isobutyl 2-propenoate, Merlon, triethylene tetramine, polyacrylic acid and APTES are according to portion rate 100:20～27:7～18:6～12:2～5 joins in reactor, and reaction temperature is 55～70 DEG C, mixing speed be 45～ 60r/min reaction 0.5～1h, obtains modified polyacrylic acid isobutyl ester；(5), by PVC, modified polyacrylic acid isobutyl ester, hydroboration Sodium, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, modified carbon black according to portion rate 100:10～21:5～ 10:11～23:13～26:8～15:7～17:1～6 joins in mill, with mill in temperature 150～210 DEG C of mixing Reaction 0.3～1h, with extruder at temperature 150～210 DEG C of extruding pelletizations, i.e. obtains micro crystal graphite modified PVC pipeline.
The preparation method of the micro crystal graphite modified PVC pipeline described in this invention, comprises the following steps:
(1) it is, 10:105 by sodium hexameta phosphate, white carbon black, hydrogen peroxide, sodium hydroxide, water and epoxychloropropane according to portion rate ～140:17～25:1～5:2～9:12～25 joins in reactor, mixing speed is 46～63r/min, maintenance system temperature React 1～3h under the conditions of spending 51～68 DEG C, in 70 DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；Described six are inclined The purpose of sodium phosphate in order to improve dispersibility and the stability of white carbon black, described hydrogen peroxide and the purpose of epoxychloropropane in order to Modify carbon blacksurface.
(2), by phenolic resin, methylolurea, N, N-dinitrosopentamethlyene tetramine is according to portion rate 100:2～20: 10～17 join in reactor, and reaction temperature is 20～35 DEG C, and mixing speed is 35～40r/min reactions 0.2～0.8h, To phenol-formaldehyde resin modified；The purpose of described N, N-dinitrosopentamethlyene tetramine is in order to improve the frothing percentage of phenolic resin.
(3), by wood powder, ammonium oxalate, powder of straw and phenol-formaldehyde resin modified according to portion rate 100:90～120:70～95:18 ～32 join in reactor, reaction temperature is 85～120 DEG C, and mixing speed is 38～50r/min reactions 0.3～0.8h, will Material is in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatment 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C Heat treatment 2h, obtains micro crystal graphite；The purpose of described ammonium oxalate is for the hole of wood powder, powder of straw and phenol-formaldehyde resin modified Rate, it is ensured that the abundant carbonization of raw material.
(4), by polyisobutyl acrylate, Merlon, triethylene tetramine, polyacrylic acid and 3-aminopropyl triethoxy Silane joins in reactor according to portion rate 100:20～27:7～18:6～12:2～5, and reaction temperature is 55～70 DEG C, stirs Mixing speed is 45～60r/min reactions 0.5～1h, obtains modified polyacrylic acid isobutyl ester；Described polyisobutyl acrylate Purpose in order to improve the compatibility of PVC and raw material, the purpose of described Merlon in order to improve the rigidity of PVC, described three The purpose of ethylene tetramine in order to improve the chemical crosslinking density of PVC, mechanical strength, chemical stability and absorbing hydrogen chloride gas, Described polyacrylic purpose is in order to improve the chemical stability of triethylene tetramine.
(5), by PVC, modified polyacrylic acid isobutyl ester, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, Micro crystal graphite, modified carbon black add according to portion rate 100:10～21:5～10:11～23:13～26:8～15:7～17:1～6 Enter in mill, with mill in temperature 150～210 DEG C of hybrid reactions 0.3～1h, with extruder temperature 150～210 DEG C Extruding pelletization, i.e. obtains micro crystal graphite modified PVC pipeline；The purpose of described sodium borohydride is in order to improve the chemically stable of PVC Property, resistance to ag(e)ing and degraded, described polyurethane resin in order to improve mechanical strength and the impact strength of PVC, described crystallite The purpose of graphite is in order to improve heat conductivity and the wearability of PVC.
This beneficial effect of the invention is:
1, sodium hexameta phosphate has preferable peptizaiton, can in PVC preferable disperse black carbon；Hydrogen peroxide, hydroxide Sodium and epoxychloropropane can be modified to carbon blacksurface, give carbon blacksurface and have abundant hydroxyl and epoxide group, can make White carbon black is grafted in PVC molecular structure, improves white carbon black chemical stability in PVC and dispersibility.
2, when solidification, by phenolic resin, methylolurea, N, the phenolic aldehyde tree prepared by N-dinitrosopentamethlyene tetramine Fat binding agent, can reach higher porosity, can be with high degree of dispersion wood powder and powder of straw.
3, ammonium oxalate is heated and easily decomposes, and it is higher that the gas of generation can give wood powder, powder of straw and phenol-formaldehyde resin modified Porosity and bigger specific surface area, finally, it is ensured that the abundant carbonization of raw material, and change to micro crystal graphite.
4, polyisobutyl acrylate and polymer have the compatibility of excellence, can improve the compatibility of PVC and raw material；Poly- Carbonic ester can give the rigidity that PVC is higher；Triethylene tetramine can use as curable urethane resin agent, in processing and forming During, triethylene tetramine and curable urethane resin, the network structure of formation can improve the mechanical property of PVC, chemistry is handed over While connection density, chemical stability, it is also possible to absorb the hydrogen chloride gas produced during PVC processing and use, one Determine in degree, to solve the environmental issue produced because of hydrogen chloride；Polyacrylic acid can provide the chemical stability of triethylene tetramine.
5, sodium borohydride has stronger reducing property, can reduce the series of problems that PVC is caused because of oxidative phenomena, And the chemical stability of PVC, resistance to ag(e)ing can be improved and reduce degraded；Polyurethane resin has impact strength and the power of excellence Learn intensity, can give PVC excellent mechanical strength and impact strength；Cardanol has preferable reducing property, Ke Yiti The oxidative resistance of high PVC and ageing-resistant performance；Micro crystal graphite has heat conductivity and the wearability of excellence, can improve leading of PVC Hot and wearability.
Detailed description of the invention
Below in conjunction with embodiment, the detailed description of the invention of this invention is described, in order to be better understood from this invention.
Embodiment 1
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 127 parts of white carbon blacks, 21 parts of hydrogen peroxide, 3 parts of sodium hydroxide, 5 parts of water and 18 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 52r/min, reacts 1.5h, in 70 under the conditions of maintenance system temperature 63 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 9 parts of methylolureas, 14 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 30 DEG C, and mixing speed is that 37r/min reacts 0.5h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 107 parts of ammonium oxalate, 86 parts of powder of straw and 28 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 105 DEG C, and mixing speed is that 42r/min reacts 0.4h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 25 parts of Merlon, 13 parts of triethylene tetramines, 9 parts of polyacrylic acid and 3 parts, are weighed APTES joins in reactor, and reaction temperature is 61 DEG C, and mixing speed is 53r/min reaction 0.5h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 17 parts of modified polyacrylic acid isobutyl esters, 7 parts of sodium borohydrides, 18 parts of poly-toluic acid esters, 23 parts Polyurethane resin, 11 parts of Cardanol, 15 parts of micro crystal graphites, 4 parts of modified carbon blacks join in mill, with mill in temperature 165 DEG C of hybrid reactions 0.4h, with extruder at 165 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 2
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 105 parts of white carbon blacks, 17 parts of hydrogen peroxide, 1 part of sodium hydroxide, 2 parts of water and 12 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 46r/min, under the conditions of maintenance system temperature 51 DEG C react 1h, in 70 DEG C ,- 0.08MPa decompression distillation 2h, obtains modified carbon black；
(2), weigh 100 parts of phenolic resin, 2 parts of methylolureas, 10 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 20 DEG C, and mixing speed is that 35r/min reacts 0.2h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 90 parts of ammonium oxalate, 70 parts of powder of straw and 18 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 85 DEG C, and mixing speed is that 38r/min reacts 0.3h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 20 parts of Merlon, 7 parts of triethylene tetramines, 6 parts of polyacrylic acid and 2 parts of 3-, are weighed Aminopropyltriethoxywerene werene joins in reactor, and reaction temperature is 55 DEG C, and mixing speed is that 45r/min reacts 0.5h, Obtain modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 10 parts of modified polyacrylic acid isobutyl esters, 5 parts of sodium borohydrides, 11 parts of poly-toluic acid esters, 13 parts Polyurethane resin, 8 parts of Cardanol, 7 parts of micro crystal graphites, 1 part of modified carbon black join in mill, with mill in temperature 150 DEG C hybrid reaction 0.3h, with extruder at 150 DEG C of extruding pelletizations of temperature, i.e. obtains micro crystal graphite modified PVC pipeline.
Embodiment 3
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 140 parts of white carbon blacks, 25 parts of hydrogen peroxide, 5 parts of sodium hydroxide, 9 parts of water and 25 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 63r/min, under the conditions of maintenance system temperature 68 DEG C react 3h, in 70 DEG C ,- 0.08MPa decompression distillation 2h, obtains modified carbon black；
(2), weigh 100 parts of phenolic resin, 20 parts of methylolureas, 17 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 35 DEG C, and mixing speed is that 40r/min reacts 0.8h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 120 parts of ammonium oxalate, 95 parts of powder of straw and 32 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 120 DEG C, and mixing speed is that 50r/min reacts 0.8h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 27 parts of Merlon, 18 parts of triethylene tetramines, 12 parts of polyacrylic acid and 5 parts, are weighed APTES joins in reactor, and reaction temperature is 70 DEG C, and mixing speed is that 60r/min reacts 1h, Obtain modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 21 parts of modified polyacrylic acid isobutyl esters, 10 parts of sodium borohydrides, 23 parts of poly-toluic acid esters, 26 Part polyurethane resin, 15 parts of Cardanol, 17 parts of micro crystal graphites, 6 parts of modified carbon blacks join in mill, with mill in temperature 210 DEG C of hybrid reactions 1h, with extruder at 210 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 4
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 110 parts of white carbon blacks, 20 parts of hydrogen peroxide, 4 parts of sodium hydroxide, 3 parts of water and 15 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 50r/min, reacts 1.2h, in 70 under the conditions of maintenance system temperature 55 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 10 parts of methylolureas, 15 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 25 DEG C, and mixing speed is that 36r/min reacts 0.5h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 100 parts of ammonium oxalate, 80 parts of powder of straw and 20 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 90 DEG C, and mixing speed is that 40r/min reacts 0.5h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 25 parts of Merlon, 10 parts of triethylene tetramines, 10 parts of polyacrylic acid and 4 parts, are weighed APTES joins in reactor, and reaction temperature is 60 DEG C, and mixing speed is 50r/min reaction 0.9h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 15 parts of modified polyacrylic acid isobutyl esters, 6 parts of sodium borohydrides, 15 parts of poly-toluic acid esters, 20 parts Polyurethane resin, 10 parts of Cardanol, 10 parts of micro crystal graphites, 5 parts of modified carbon blacks join in mill, with mill in temperature 155 DEG C of hybrid reactions 0.7h, with extruder at 155 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 5
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 120 parts of white carbon blacks, 19 parts of hydrogen peroxide, 2 parts of sodium hydroxide, 4 parts of water and 24 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 62r/min, reacts 1.3h, in 70 under the conditions of maintenance system temperature 53 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 19 parts of methylolureas, 12 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 34 DEG C, and mixing speed is that 39r/min reacts 0.3h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 110 parts of ammonium oxalate, 85 parts of powder of straw and 31 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 100 DEG C, and mixing speed is that 39r/min reacts 0.6h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 21 parts of Merlon, 8 parts of triethylene tetramines, 11 parts of polyacrylic acid and 2.3, are weighed Part APTES joins in reactor, and reaction temperature is 65 DEG C, and mixing speed is 55r/min reaction 0.6h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 20 parts of modified polyacrylic acid isobutyl esters, 6 parts of sodium borohydrides, 21 parts of poly-toluic acid esters, 24 parts Polyurethane resin, 9 parts of Cardanol, 14 parts of micro crystal graphites, 3 parts of modified carbon blacks join in mill, with mill in temperature 160 DEG C hybrid reaction 0.8h, with extruder at 160 DEG C of extruding pelletizations of temperature, i.e. obtains micro crystal graphite modified PVC pipeline.
Embodiment 6
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 130 parts of white carbon blacks, 18 parts of hydrogen peroxide, 4 parts of sodium hydroxide, 7 parts of water and 22 parts of epoxies, are weighed Chloropropane joins in reactor, and mixing speed is 48r/min, reacts 1.6h, in 70 under the conditions of maintenance system temperature 54 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 17 parts of methylolureas, 15 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 29 DEG C, and mixing speed is that 39r/min reacts 0.4h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 116 parts of ammonium oxalate, 93 parts of powder of straw and 29 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 89 DEG C, and mixing speed is that 41r/min reacts 0.4h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 25 parts of Merlon, 12 parts of triethylene tetramines, 7 parts of polyacrylic acid and 3.6, are weighed Part APTES joins in reactor, and reaction temperature is 57 DEG C, and mixing speed is 58r/min reaction 0.9h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 13 parts of modified polyacrylic acid isobutyl esters, 7 parts of sodium borohydrides, 20 parts of poly-toluic acid esters, 16 parts Polyurethane resin, 11 parts of Cardanol, 9 parts of micro crystal graphites, 5 parts of modified carbon blacks join in mill, with mill in temperature 173 DEG C hybrid reaction 0.6h, with extruder at 173 DEG C of extruding pelletizations of temperature, i.e. obtains micro crystal graphite modified PVC pipeline.
Embodiment 7
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 115 parts of white carbon blacks, 18 parts of hydrogen peroxide, 2.3 parts of sodium hydroxide, 6.7 parts of water and 22 parts, are weighed Epoxychloropropane joins in reactor, and mixing speed is 48r/min, reacts 2.8h under the conditions of maintenance system temperature 59 DEG C, in 70 DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 17 parts of methylolureas, 13 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 25 DEG C, and mixing speed is that 36r/min reacts 0.7h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 104 parts of ammonium oxalate, 83 parts of powder of straw and 27 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 99 DEG C, and mixing speed is that 41r/min reacts 0.7h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4), weigh 100 parts of polyisobutyl acrylates, 20 parts of Merlon, 11 parts of triethylene tetramines, 9.3 parts of polyacrylic acid and 4.2 parts of APTESs join in reactor, and reaction temperature is 62 DEG C, and mixing speed is that 51r/min is anti- Answer 0.7h, obtain modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 18 parts of modified polyacrylic acid isobutyl esters, 6 parts of sodium borohydrides, 15 parts of poly-toluic acid esters, 14 parts Polyurethane resin, 13 parts of Cardanol, 12 parts of micro crystal graphites, 1 part of modified carbon black join in mill, with mill in temperature 184 DEG C of hybrid reactions 0.7h, with extruder at 184 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 8
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 136 parts of white carbon blacks, 19 parts of hydrogen peroxide, 4.6 parts of sodium hydroxide, 5 parts of water and 14 parts of rings, are weighed Oxygen chloropropane joins in reactor, and mixing speed is 53r/min, reacts 1h, in 70 under the conditions of maintenance system temperature 62 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 11 parts of methylolureas, 16 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 28 DEG C, and mixing speed is that 38r/min reacts 0.3h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 98 parts of ammonium oxalate, 93 parts of powder of straw and 28 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 109 DEG C, and mixing speed is that 46r/min reacts 0.3h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 22 parts of Merlon, 15 parts of triethylene tetramines, 7 parts of polyacrylic acid and 3 parts, are weighed APTES joins in reactor, and reaction temperature is 61 DEG C, and mixing speed is 49r/min reaction 0.7h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 11 parts of modified polyacrylic acid isobutyl esters, 9 parts of sodium borohydrides, 16 parts of poly-toluic acid esters, 24 parts Polyurethane resin, 12 parts of Cardanol, 14 parts of micro crystal graphites, 2 parts of modified carbon blacks join in mill, with mill in temperature 190 DEG C of hybrid reactions 0.5h, with extruder at 190 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 9
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 129 parts of white carbon blacks, 19 parts of hydrogen peroxide, 3.9 parts of sodium hydroxide, 7.3 parts of water and 21 parts, are weighed Epoxychloropropane joins in reactor, and mixing speed is 58r/min, reacts 2.5h under the conditions of maintenance system temperature 67 DEG C, in 70 DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 16 parts of methylolureas, 14 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 33 DEG C, and mixing speed is that 37r/min reacts 0.6h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 113 parts of ammonium oxalate, 92 parts of powder of straw and 27 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 117 DEG C, and mixing speed is that 43r/min reacts 0.6h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 25 parts of Merlon, 17 parts of triethylene tetramines, 7 parts of polyacrylic acid and 4.8, are weighed Part APTES joins in reactor, and reaction temperature is 64 DEG C, and mixing speed is 57r/min reaction 0.6h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 16 parts of modified polyacrylic acid isobutyl esters, 7 parts of sodium borohydrides, 16 parts of poly-toluic acid esters, 18 parts Polyurethane resin, 11 parts of Cardanol, 14 parts of micro crystal graphites, 3 parts of modified carbon blacks join in mill, with mill in temperature 200 DEG C of hybrid reactions 0.3h, with extruder at 200 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
Embodiment 10
A kind of micro crystal graphite modified PVC pipeline, its preparation method comprises the following steps:
(1) 10 parts of sodium hexameta phosphate, 113 parts of white carbon blacks, 24 parts of hydrogen peroxide, 3.5 parts of sodium hydroxide, 6 parts of water and 17 parts of rings, are weighed Oxygen chloropropane joins in reactor, and mixing speed is 56r/min, reacts 2.7h, in 70 under the conditions of maintenance system temperature 64 DEG C DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black；
(2), weigh 100 parts of phenolic resin, 13 parts of methylolureas, 13 parts of N, N-dinitrosopentamethlyene tetramines join reaction In still, reaction temperature is 29 DEG C, and mixing speed is that 38r/min reacts 0.5h, obtains phenol-formaldehyde resin modified；
(3), weigh 100 parts of wood powders, 116 parts of ammonium oxalate, 87 parts of powder of straw and 26 parts of phenol-formaldehyde resin modifieds and join in reactor, Reaction temperature is 106 DEG C, and mixing speed is that 47r/min reacts 0.7h, by material in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatments 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C of heat treatment 2h, obtains micro crystal graphite；
(4) 100 parts of polyisobutyl acrylates, 23 parts of Merlon, 13 parts of triethylene tetramines, 8 parts of polyacrylic acid and 2.7, are weighed Part APTES joins in reactor, and reaction temperature is 67 DEG C, and mixing speed is 54r/min reaction 0.8h, obtains modified polyacrylic acid isobutyl ester；
(5), weigh 100 parts of PVC, 19 parts of modified polyacrylic acid isobutyl esters, 8 parts of sodium borohydrides, 16 parts of poly-toluic acid esters, 18 parts Polyurethane resin, 12 parts of Cardanol, 15 parts of micro crystal graphites, 3 parts of modified carbon blacks join in mill, with mill in temperature 178 DEG C of hybrid reactions 0.7h, with extruder at 178 DEG C of extruding pelletizations of temperature, i.e. obtain micro crystal graphite modified PVC pipeline.
The performance parameter of the micro crystal graphite modified PVC pipeline that table 1 embodiment 1 prepares
Embodiment 1
Wearability Good
Oxygen index (OI) % 34
Tensile yield strength MPa 47
Falling weight impact test 3
Free chlorine Up to standard
The above is the preferred implementation of this invention, it is noted that for those skilled in the art, On the premise of without departing from this inventive principle, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as this Bright protection domain.

Claims (9)

1. a micro crystal graphite modified PVC pipeline, it is characterised in that: include that following raw material components: PVC, modified polyacrylic acid are different Butyl ester, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, modified carbon black, described PVC, modification Polyisobutyl acrylate, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, part of modified carbon black Number ratio is 100:10～21:5～10:11～23:13～26:8～15:7～17:1～6, wherein, described modified polyacrylic acid Isobutyl ester is anti-by polyisobutyl acrylate, Merlon, triethylene tetramine, polyacrylic acid and APTES Should prepare, described polyisobutyl acrylate, Merlon, triethylene tetramine, polyacrylic acid and 3-aminopropyl triethoxy The portion rate of silane is 100:20～27:7～18:6～12:2～5, and described micro crystal graphite is by wood powder, ammonium oxalate, powder of straw Preparing with phenol-formaldehyde resin modified reaction, the score ratio of described wood powder, ammonium oxalate, powder of straw and phenol-formaldehyde resin modified is 100:90 ～120:70～95:18～32, described phenol-formaldehyde resin modified is by phenolic resin, methylolurea, N, five first of N-dinitroso Urotropine reaction prepares, and described phenolic resin, methylolurea, the portion rate of N, N-dinitrosopentamethlyene tetramine are 100: 2～20:10～17, described modified carbon black is by sodium hexameta phosphate, white carbon black, hydrogen peroxide, sodium hydroxide, water and epoxychloropropane Reaction prepares, and the portion rate of described sodium hexameta phosphate, white carbon black, hydrogen peroxide, sodium hydroxide, water and epoxychloropropane is 10: 105～140:17～25:1～5:2～9:12～25.
2. a micro crystal graphite modified PVC pipeline, it is characterised in that: described micro crystal graphite modified PVC pipeline is by following system Preparation Method prepare: (1), by sodium hexameta phosphate, white carbon black, hydrogen peroxide, sodium hydroxide, water and epoxychloropropane according to portion rate Joining in reactor for 10:105～140:17～25:1～5:2～9:12～25, mixing speed is 46～63r/min, dimension React 1～3h under the conditions of holding system temperature 51～68 DEG C, in 70 DEG C ,-0.08MPa decompression distillation 2h, obtain modified carbon black； (2), by phenolic resin, methylolurea, N, N-dinitrosopentamethlyene tetramine adds according to portion rate 100:2～20:10～17 Entering in reactor, reaction temperature is 20～35 DEG C, and mixing speed is 35～40r/min reactions 0.2～0.8h, obtains modified phenol Urea formaldehyde；(3), by wood powder, ammonium oxalate, powder of straw and phenol-formaldehyde resin modified according to portion rate 100:90～120:70～95:18 ～32 join in reactor, reaction temperature is 85～120 DEG C, and mixing speed is 38～50r/min reactions 0.3～0.8h, will Material is in 200 DEG C of heat treatment 2h, in 400 DEG C of heat treatment 2h, in 600 DEG C of heat treatment 2h, in 800 DEG C of heat treatment 2h, in 1000 DEG C Heat treatment 2h, obtains micro crystal graphite；(4), by polyisobutyl acrylate, Merlon, triethylene tetramine, polyacrylic acid and 3-ammonia Base propyl-triethoxysilicane joins in reactor according to portion rate 100:20～27:7～18:6～12:2～5, reaction temperature Degree is 55～70 DEG C, and mixing speed is 45～60r/min reactions 0.5～1h, obtains modified polyacrylic acid isobutyl ester；(5), will PVC, modified polyacrylic acid isobutyl ester, sodium borohydride, poly-toluic acid ester, polyurethane resin, Cardanol, micro crystal graphite, modification White carbon black joins in mill according to portion rate 100:10～21:5～10:11～23:13～26:8～15:7～17:1～6, With mill in temperature 150～210 DEG C of hybrid reactions 0.3～1h, with extruder at temperature 150～210 DEG C of extruding pelletizations, to obtain final product To micro crystal graphite modified PVC pipeline.
3. a micro crystal graphite modified PVC pipeline, it is characterised in that: in the preparation process of described modified carbon black, treat white carbon black, mistake After hydrogen oxide, sodium hydroxide and water mix homogeneously, epoxychloropropane adds to reactor with the interpolation speed of 0.6mL/min.
4. a micro crystal graphite modified PVC pipeline, it is characterised in that: in the preparation process of described modified carbon black, hexa metaphosphoric acid Sodium finally adds to reactor.
5. a micro crystal graphite modified PVC pipeline, it is characterised in that: in the preparation process of described phenol-formaldehyde resin modified, hydroxyl first Base urea finally adds to reactor.
6. a micro crystal graphite modified PVC pipeline, it is characterised in that: in the preparation process of described micro crystal graphite, wood powder, oxalic acid After ammonium and powder of straw mix homogeneously, add to equipped with in the reactor of phenol-formaldehyde resin modified.
7. a micro crystal graphite modified PVC pipeline, it is characterised in that: the preparation process of described modified polyacrylic acid isobutyl ester In, triethylene tetramine finally adds to reactor.
8. a micro crystal graphite modified PVC pipeline, it is characterised in that: the preparation process of described micro crystal graphite modified PVC pipeline In, after sodium borohydride is first mixed homogeneously with Cardanol, then add to mill.
9. a micro crystal graphite modified PVC pipeline, it is characterised in that: described micro crystal graphite modified PVC pipeline can be applied Heat conductivity that municipal administration plumbing, industry plumbing, civilian plumbing, irrigation, vegetation are watered etc., heat stability, wearability, low trip From fields such as chlorine, impact strength, filler dispersibility, anti-flammability, mechanical property, resistance to ag(e)ing, oxidative resistances.
CN201610639866.6A 2016-08-08 2016-08-08 A kind of micro crystal graphite modified PVC pipeline and preparation method thereof Pending CN106280081A (en)

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CN1651505A (en) * 2004-02-07 2005-08-10 中国石化齐鲁股份有限公司 Heat resistant smoke inhibiting polyvinyl chloride composition and its preparation method
CN103254531A (en) * 2013-05-27 2013-08-21 常州大学 Flame-retardant PVC (polyvinyl chloride) composite material and preparation method thereof
CN105175949A (en) * 2015-10-31 2015-12-23 贵州同益塑料制品有限公司 Drain pipe and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1651505A (en) * 2004-02-07 2005-08-10 中国石化齐鲁股份有限公司 Heat resistant smoke inhibiting polyvinyl chloride composition and its preparation method
CN103254531A (en) * 2013-05-27 2013-08-21 常州大学 Flame-retardant PVC (polyvinyl chloride) composite material and preparation method thereof
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Application publication date: 20170104