CN109081984A - A kind of preparation method of titania modified polyethylene - Google Patents

A kind of preparation method of titania modified polyethylene Download PDF

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CN109081984A
CN109081984A CN201810709292.4A CN201810709292A CN109081984A CN 109081984 A CN109081984 A CN 109081984A CN 201810709292 A CN201810709292 A CN 201810709292A CN 109081984 A CN109081984 A CN 109081984A
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ethyl alcohol
titanium dioxide
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modified poly
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王尧尧
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04Homopolymers or copolymers of ethene
    • C08L23/06Polyethene
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • C09C1/3607Titanium dioxide
    • C09C1/3669Treatment with low-molecular organic compounds
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
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    • C08K3/22Oxides; Hydroxides of metals
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
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    • C08K2003/265Calcium, strontium or barium carbonate
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    • C08L2201/02Flame or fire retardant/resistant
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    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The invention is related to a kind of modified poly ethylene, including following raw material components: Lauxite modified poly ethylene, modifying titanium dioxide, silicon carbide, modified calcium carbonate and three [2, 4- di-tert-butyl-phenyl] phosphite ester, Lauxite modified poly ethylene pellet is by polyethylene pellet, Lauxite, ethyl alcohol, salicylic acid and the reaction of dichloromethyl triethoxysilane are made, modifying titanium dioxide is by ethyl phosphonic acid, 1,4-benzoquinone diimine, ethyl alcohol and titanium dioxide reaction are made, titanium dioxide is by tetraethyl titanate, water, isopropanol, ethyl alcohol, ammonium nitrate, three iso stearate isopropyl titanates and elaidin reaction are made, modified calcium carbonate is by calcium carbonate, ethyl alcohol, epoxychloropropane, sodium hydroxide and water reaction are made.The invention has the advantages such as excellent UV resistant, anti-flammability, filler dispersibility, filler compatibility, heat resistance, mechanical property, heating conduction, low volume shrinking percentage.

Description

A kind of preparation method of titania modified polyethylene
Technical field
The invention is related to a kind of modified poly ethylene and preparation method thereof.
Background technique
Polyethylene has excellent resistance to low temperature, and chemical stability is good, is resistant to the erosion of most of soda acids, water imbibition Small, electrical insulating property is excellent.Polyethylene can with squeeze out, injection, molding, blow molding and the molding of the methods of melt-spun, be widely used in film, The hollow containers such as sheet material, coating, bottle, tank, bucket tubing and electric wire, the insulation of cable and sheath.
Currently, polythene material is in UV resistant, anti-flammability, filler dispersibility, filler compatibility, heat resistance, mechanical property The performances such as energy, heating conduction need further to be promoted.The invention uses modified calcium carbonate, modifying titanium dioxide, Lauxite, carbon SiClx is prepared for modified poly ethylene, is prepared into various plastic products, party's legal system by techniques such as extrusion, injection molding, molding, blow moldings Standby modified polyethylene material has excellent UV resistant, anti-flammability, filler dispersibility, filler compatibility, heat resistance, mechanics The performances such as performance, heating conduction, low volume shrinking percentage.
Summary of the invention
A kind of preparation method for being designed to provide modified poly ethylene of the invention, this method is by changing reactant feed And technology mode, the material of preparation have excellent UV resistant, anti-flammability, filler dispersibility, filler compatibility, heat resistance, The performances such as mechanical property, heating conduction, low volume shrinking percentage.
To achieve the goals above, the technical solution of the invention is as follows.
A kind of modified poly ethylene and preparation method thereof, specifically includes the following steps: (1), by calcium carbonate, ethyl alcohol, epoxy chlorine Propane, sodium hydroxide and water are that 100:70~100:13~27:2~5:3~6 are added in reactor according to mass parts ratio, Mixing speed is 120~140r/min, and 1~2h is reacted under the conditions of 55~70 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa It is evaporated under reduced pressure 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;(2), by tetraethyl titanate, water, isopropanol, ethyl alcohol, ammonium nitrate, Three iso stearate isopropyl titanates and oleic acid according to mass parts ratio 100:5~10:150~195:130~200:3~5:10~ 15:8~14 are added in reaction kettle, and mixing speed is 130~160r/min, anti-under the conditions of 40~60 DEG C of maintenance system temperature 2~5h is answered, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;(3), by second Base phosphoric acid, 1,4-benzoquinone diimine, ethyl alcohol and titanium dioxide add according to mass parts ratio 100:85~105:230~270:27~40 Enter into reaction kettle, at 145~160 DEG C of temperature, 1~3 h of reaction is under the conditions of mixing speed is 75~87r/min to get to changing Property titanium dioxide;(4), by polyethylene pellet, Lauxite, ethyl alcohol, salicylic acid and dichloromethyl triethoxysilane according to matter Amount portion rate 100:12~18:15~27:5~8:4~7 are added in open mill, mixed at 130~260 DEG C of temperature with open mill It closes 0.5~2h of reaction and obtains Lauxite modified poly ethylene pellet with extruder in 130~260 DEG C of extruding pelletizations of temperature; (5), by Lauxite modified poly ethylene, modifying titanium dioxide, silicon carbide, modified calcium carbonate and three [2,4- di-tert-butyl-phenyls] Phosphite ester is added in open mill according to mass parts ratio 100:2~7:5~8:8~12:1~3, with open mill in temperature 130~260 DEG C of 0.5~2h of hybrid reaction, with extruder 130~260 DEG C of temperature by modified poly ethylene extruding pelletization to get arriving Modified poly ethylene pellet.
The preparation method of modified poly ethylene described in the invention, including the following steps:
(1), by calcium carbonate, ethyl alcohol, epoxychloropropane, sodium hydroxide and water according to mass parts ratio be 100:70~100:13~ 27:2~5:3~6 are added in reactor, and mixing speed is 120~140r/min, 55~70 DEG C of conditions of maintenance system temperature 1~2h of lower reaction, through 90 DEG C, -0.08MPa is evaporated under reduced pressure 2h, and 120 DEG C of dry 2h obtain modified calcium carbonate;The hydroxide The epoxy group generation new for the reactivity and catalysis that improve epoxychloropropane of the purpose of sodium and water.
(2), by tetraethyl titanate, water, isopropanol, ethyl alcohol, ammonium nitrate, three iso stearate isopropyl titanates and oleic acid according to Mass parts ratio 100:5~10:150~195:130~200:3~5:10~15:8~14 are added in reaction kettle, stirring speed Degree is 130~160r/min, and 2~5h is reacted under the conditions of 40~60 DEG C of maintenance system temperature, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;The isopropanol and ethyl alcohol in order to improve material point Dissipate property, the purpose of the ammonium nitrate and oleic acid is in order to be catalyzed the hydrolysis of tetraethyl titanate.
(3), by ethyl phosphonic acid, 1,4-benzoquinone diimine, ethyl alcohol and titanium dioxide according to mass parts ratio 100:85~105: 230~270:27~40 are added in reaction kettle, and at 145~160 DEG C of temperature, mixing speed is anti-under the conditions of being 75~87r/min 1~3 h is answered to get modifying titanium dioxide is arrived;The purpose of the ethyl phosphonic acid and 1,4-benzoquinone diimine is in order to improve titanium dioxide The dispersibility of titanium and the anti-flammability of polyethylene.
(4), by polyethylene pellet, Lauxite, ethyl alcohol, salicylic acid and dichloromethyl triethoxysilane according to mass parts Number is added in open mill than 100:12~18:15~27:5~8:4~7, anti-in 130~260 DEG C of temperature mixing with open mill 0.5~2h is answered, with extruder in 130~260 DEG C of extruding pelletizations of temperature, obtains Lauxite modified poly ethylene pellet;Described The purpose of Lauxite is in order to improve the thermal stability of polyethylene.
(5), by Lauxite modified poly ethylene, modifying titanium dioxide, silicon carbide, modified calcium carbonate and three [2,4- bis- uncles Butyl phenyl] phosphite ester is added in open mill according to mass parts ratio 100:2~7:5~8:8~12:1~3, use mill Machine makes modified poly ethylene extrusion at 130~260 DEG C of temperature in 130~260 DEG C of 0.5~2h of hybrid reaction of temperature, with extruder Grain to get arrive modified poly ethylene pellet.
Invention has the beneficial effects that:
1, using epoxychloropropane to calcium carbonate surface modifying, compatibility of the calcium carbonate in polyethylene not only can be improved, and And calcium carbonate surface chemical activity can also be improved, it crosslinks and reacts with modified poly ethylene, calcium carbonate on the one hand can be improved Dispersibility and compatibility in polyethylene, the impact strength, tensile strength, bending that on the other hand can also improve polyethylene are strong The mechanical strengths such as degree;
2, in titanium dioxide preparation process, three iso stearate isopropyl titanates can not only provide titanium source, but also can be to titanium Sour tetra-ethyl ester carries out surface chemical modification.When being continuously added oleic acid and ammonium nitrate in system, reaction system is by initial oil-in-water While system transition is water-in-oil system, the hydrogen ion of oleic acid ionization generates in conjunction with the nitrate ion that ammonium nitrate ionizes Nitric acid, nitric acid can be catalyzed metatitanic acid ester hydrolysis, and as ethyl alcohol and isopropanol constantly volatilize, reaction system is gradually formed by colloidal sol Gel, gel generate nano-titanium dioxide after high-temperature process, and nano-titanium dioxide has excellent ultraviolet shielding effect, can To assign polyethylene excellent UV resistant performance;
3, ethyl phosphonic acid and 1,4-benzoquinone diimine not only can be very good dispersed titanium dioxide, and polycondensation reaction can also occur, raw At the ethyl phosphonic acid with high flame resistance -1,4-benzoquinone diimine polymer, it is excellent that this polymer can not only assign polyethylene Flame retardant property and heat resistance, dispersibility and compatibility of the titanium dioxide in polyethylene can also be improved;
4, due to crazing toughening mechanism, the mechanical strength and toughness of polyethylene is can be improved in modifying titanium dioxide;
5, Lauxite modified poly ethylene pellet, can be improved polyethylene and while modified filler compatibility, can also with change Property filler crosslink reaction, improve dispersibility of the modified filler in polyethylene, compatibility, chemical stability, heat resistance and Mechanical strength;
6, the thermal conductivity of silicon carbide fibre is preferable, and the thermal conductivity of polyethylene not only can be improved, and can also enhance the power of polyethylene Learn intensity.
Specific embodiment
It is described below with reference to specific embodiment of the embodiment to the invention, to better understand the invention.
Embodiment 1
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 86 parts of ethyl alcohol, 23 parts of epoxychloropropane, 3.6 parts of sodium hydroxides and 4.5 parts of water are weighed to be added to In reactor, mixing speed 130r/min reacts 1.5h under the conditions of 60 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 7 parts of water, 175 parts of isopropanols, 160 parts of ethyl alcohol, 4 parts of ammonium nitrate, 12 part three it is different hard Ester acid isopropyl titanate and 11 parts of oleic acid are added in reaction kettle, mixing speed 140r/min, 52 DEG C of items of maintenance system temperature 3h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 95 parts of 1,4-benzoquinone diimines, 250 parts of ethyl alcohol and 34 parts of titanium dioxide are weighed and are added to reaction In kettle, at 150 DEG C of temperature, mixing speed reacts 2 h to get modifying titanium dioxide is arrived under the conditions of being 80r/min;
(4), 100 parts of polyethylene pellets, 15 parts of Lauxites, 23 parts of ethyl alcohol, 6 parts of salicylic acids and 5 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 170 DEG C of hybrid reaction 1h of temperature, is squeezed out with extruder at 170 DEG C of temperature It is granulated, obtains Lauxite modified poly ethylene pellet;
(5), weigh 100 parts of Lauxite modified poly ethylenes, 4 parts of modifying titanium dioxides, 6 parts of silicon carbide, 9 parts of modified calcium carbonates and 2 part of three [2,4- di-tert-butyl-phenyl] phosphite ester is added in open mill, with open mill in 172 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 172 DEG C of temperature with extruder by 0.8h.
Embodiment 2
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 70 parts of ethyl alcohol, 13 parts of epoxychloropropane, 2 parts of sodium hydroxides and 3 parts of water are weighed and are added to reaction In device, mixing speed 120r/min reacts 1h under the conditions of 55 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa vacuum distillation 2h, 120 DEG C of dry 2h, obtains modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 5 parts of water, 150 parts of isopropanols, 130 parts of ethyl alcohol, 3 parts of ammonium nitrate, 10 part three it is different hard Ester acid isopropyl titanate and 8 parts of oleic acid are added in reaction kettle, mixing speed 130r/min, 40 DEG C of items of maintenance system temperature 2h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 85 parts of 1,4-benzoquinone diimines, 230 parts of ethyl alcohol and 27 parts of titanium dioxide are weighed and are added to reaction In kettle, at 145 DEG C of temperature, mixing speed reacts 1 h to get modifying titanium dioxide is arrived under the conditions of being 75r/min;
(4), 100 parts of polyethylene pellets, 12 parts of Lauxites, 15 parts of ethyl alcohol, 5 parts of salicylic acids and 4 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 130 DEG C of hybrid reaction 0.5h of temperature, is squeezed with extruder at 130 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), weigh 100 parts of Lauxite modified poly ethylenes, 2 parts of modifying titanium dioxides, 5 parts of silicon carbide, 8 parts of modified calcium carbonates and 1 part of three [2,4- di-tert-butyl-phenyl] phosphite ester is added in open mill, with open mill in 130 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 130 DEG C of temperature with extruder by 0.5h.
Embodiment 3
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 100 parts of ethyl alcohol, 27 parts of epoxychloropropane, 5 parts of sodium hydroxides and 6 parts of water are weighed and are added to reaction In device, mixing speed 140r/min reacts 2h under the conditions of 70 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa vacuum distillation 2h, 120 DEG C of dry 2h, obtains modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 10 parts of water, 195 parts of isopropanols, 200 parts of ethyl alcohol, 5 parts of ammonium nitrate, 15 part three it is different hard Ester acid isopropyl titanate and 14 parts of oleic acid are added in reaction kettle, mixing speed 160r/min, 60 DEG C of items of maintenance system temperature 5h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 105 parts of 1,4-benzoquinone diimines, 270 parts of ethyl alcohol and 40 parts of titanium dioxide are weighed and are added to reaction In kettle, at 160 DEG C of temperature, mixing speed reacts 3 h to get modifying titanium dioxide is arrived under the conditions of being 87r/min;
(4), 100 parts of polyethylene pellets, 18 parts of Lauxites, 27 parts of ethyl alcohol, 8 parts of salicylic acids and 7 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 260 DEG C of hybrid reaction 2h of temperature, is squeezed out with extruder at 260 DEG C of temperature It is granulated, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 7 parts of modifying titanium dioxides, 8 parts of silicon carbide, 12 parts of modified calcium carbonates are weighed It is added in open mill with 3 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 260 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 260 DEG C of temperature with extruder by 2h.
Embodiment 4
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 75 parts of ethyl alcohol, 17 parts of epoxychloropropane, 2.4 parts of sodium hydroxides and 3.7 parts of water are weighed to be added to In reactor, mixing speed 135r/min reacts 1.2h under the conditions of 63 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 7 parts of water, 167 parts of isopropanols, 143 parts of ethyl alcohol, 4 parts of ammonium nitrate, 13 part three it is different hard Ester acid isopropyl titanate and 9 parts of oleic acid are added in reaction kettle, mixing speed 140r/min, 45 DEG C of items of maintenance system temperature 4h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 90 parts of 1,4-benzoquinone diimines, 240 parts of ethyl alcohol and 28 parts of titanium dioxide are weighed and are added to reaction In kettle, at 150 DEG C of temperature, mixing speed reacts 2 h to get modifying titanium dioxide is arrived under the conditions of being 77r/min;
(4), 100 parts of polyethylene pellets, 14 parts of Lauxites, 17 parts of ethyl alcohol, 6 parts of salicylic acids and 5 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 140 DEG C of hybrid reaction 1.3h of temperature, is squeezed with extruder at 140 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 3 parts of modifying titanium dioxides, 7 parts of silicon carbide, 11 parts of modified calcium carbonates are weighed It is added in open mill with 1 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 145 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 145 DEG C of temperature with extruder by 1.6h.
Embodiment 5
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 76 parts of ethyl alcohol, 15 parts of epoxychloropropane, 3.2 parts of sodium hydroxides and 3.8 parts of water are weighed to be added to In reactor, mixing speed 128r/min reacts 1.5h under the conditions of 60 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), 100 parts of tetraethyl titanates, 5.7 parts of water, 165 parts of isopropanols, 150 parts of ethyl alcohol, 3.8 parts of ammonium nitrate, 12 part three are weighed Iso stearate isopropyl titanate and 10 parts of oleic acid are added in reaction kettle, mixing speed 150r/min, maintenance system temperature 44 2.5h is reacted under the conditions of DEG C, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide Titanium;
(3), 100 parts of ethyl phosphonic acids, 95 parts of 1,4-benzoquinone diimines, 240 parts of ethyl alcohol and 30 parts of titanium dioxide are weighed and are added to reaction In kettle, at 155 DEG C of temperature, mixing speed reacts 1.2 h to get modifying titanium dioxide is arrived under the conditions of being 80r/min;
(4), 100 parts of polyethylene pellets, 13 parts of Lauxites, 16 parts of ethyl alcohol, 7 parts of salicylic acids and 6 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 145 DEG C of hybrid reaction 1.8h of temperature, is squeezed with extruder at 145 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 4 parts of modifying titanium dioxides, 7 parts of silicon carbide, 10 parts of modified calcium carbonates are weighed It is added in open mill with 1.6 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 150 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 150 DEG C of temperature with extruder by 0.9h.
Embodiment 6
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 83 parts of ethyl alcohol, 18 parts of epoxychloropropane, 3.6 parts of sodium hydroxides and 4.7 parts of water are weighed to be added to In reactor, mixing speed 125r/min reacts 1.1h under the conditions of 66 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 7 parts of water, 185 parts of isopropanols, 190 parts of ethyl alcohol, 4 parts of ammonium nitrate, 14 part three it is different hard Ester acid isopropyl titanate and 13 parts of oleic acid are added in reaction kettle, mixing speed 140r/min, 53 DEG C of items of maintenance system temperature 3.5h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 88 parts of 1,4-benzoquinone diimines, 250 parts of ethyl alcohol and 34 parts of titanium dioxide are weighed and are added to reaction In kettle, at 149 DEG C of temperature, mixing speed reacts 2.1 h to get modifying titanium dioxide is arrived under the conditions of being 78r/min;
(4), 100 parts of polyethylene pellets, 16 parts of Lauxites, 19 parts of ethyl alcohol, 6 parts of salicylic acids and 4 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 150 DEG C of hybrid reaction 1.6h of temperature, is squeezed with extruder at 150 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 5 parts of modifying titanium dioxides, 7 parts of silicon carbide, 12 parts of modified calcium carbonates are weighed It is added in open mill with 1.8 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 156 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 156 DEG C of temperature with extruder by 1.4h.
Embodiment 7
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 93 parts of ethyl alcohol, 25 parts of epoxychloropropane, 4.3 parts of sodium hydroxides and 5.6 parts of water are weighed to be added to In reactor, mixing speed 134r/min reacts 1.4h under the conditions of 68 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), 100 parts of tetraethyl titanates, 8.5 parts of water, 176 parts of isopropanols, 185 parts of ethyl alcohol, 4.3 parts of ammonium nitrate, 13.6 parts are weighed Three iso stearate isopropyl titanates and 12.3 parts of oleic acid are added in reaction kettle, mixing speed 152r/min, maintenance system temperature 4.5h is reacted under the conditions of 56 DEG C of degree, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain two Titanium oxide;
(3), 100 parts of ethyl phosphonic acids, 93 parts of 1,4-benzoquinone diimines, 260 parts of ethyl alcohol and 39 parts of titanium dioxide are weighed and are added to reaction In kettle, at 147 DEG C of temperature, mixing speed reacts 2.6 h to get modifying titanium dioxide is arrived under the conditions of being 85r/min;
(4), 100 parts of polyethylene pellets, 17 parts of Lauxites, 26 parts of ethyl alcohol, 7 parts of salicylic acids and 6 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 157 DEG C of hybrid reaction 1.5h of temperature, is squeezed with extruder at 157 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), weigh 100 parts of Lauxite modified poly ethylenes, 6 parts of modifying titanium dioxides, 7 parts of silicon carbide, 9 parts of modified calcium carbonates and 3 part of three [2,4- di-tert-butyl-phenyl] phosphite ester is added in open mill, with open mill in 240 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 240 DEG C of temperature with extruder by 0.6h.
Embodiment 8
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 96 parts of ethyl alcohol, 23 parts of epoxychloropropane, 3.5 parts of sodium hydroxides and 5.2 parts of water are weighed to be added to In reactor, mixing speed 131r/min reacts 1.4h under the conditions of 62 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), 100 parts of tetraethyl titanates, 8.3 parts of water, 174 parts of isopropanols, 185 parts of ethyl alcohol, 3.3 parts of ammonium nitrate, 14.5 parts are weighed Three iso stearate isopropyl titanates and 10 parts of oleic acid are added in reaction kettle, mixing speed 140r/min, maintenance system temperature 3.2h is reacted under the conditions of 47 DEG C, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain dioxy Change titanium;
(3), 100 parts of ethyl phosphonic acids, 97 parts of 1,4-benzoquinone diimines, 250 parts of ethyl alcohol and 35 parts of titanium dioxide are weighed and are added to reaction In kettle, at 146 DEG C of temperature, mixing speed reacts 1.5 h to get modifying titanium dioxide is arrived under the conditions of being 83r/min;
(4), 100 parts of polyethylene pellets, 15 parts of Lauxites, 21 parts of ethyl alcohol, 6 parts of salicylic acids and 5 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 210 DEG C of hybrid reaction 0.8h of temperature, is squeezed with extruder at 210 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 4 parts of modifying titanium dioxides, 7 parts of silicon carbide, 11 parts of modified calcium carbonates are weighed It is added in open mill with 2 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 200 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 200 DEG C of temperature with extruder by 0.8h.
Embodiment 9
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 93 parts of ethyl alcohol, 20 parts of epoxychloropropane, 3.1 parts of sodium hydroxides and 4.2 parts of water are weighed to be added to In reactor, mixing speed 137r/min reacts 1.7h under the conditions of 61 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa subtracts Pressure distillation 2h, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), 100 parts of tetraethyl titanates, 8.5 parts of water, 172 parts of isopropanols, 186 parts of ethyl alcohol, 4.7 parts of ammonium nitrate, 13.2 parts are weighed Three iso stearate isopropyl titanates and 11.8 parts of oleic acid are added in reaction kettle, mixing speed 148r/min, maintenance system temperature 3.8h is reacted under the conditions of 47 DEG C of degree, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain two Titanium oxide;
(3), 100 parts of ethyl phosphonic acids, 100 parts of 1,4-benzoquinone diimines, 245 parts of ethyl alcohol and 37 parts of titanium dioxide are weighed and are added to reaction In kettle, at 151 DEG C of temperature, mixing speed reacts 2.3 h to get modifying titanium dioxide is arrived under the conditions of being 85r/min;
(4), 100 parts of polyethylene pellets, 14 parts of Lauxites, 25 parts of ethyl alcohol, 7 parts of salicylic acids and 6 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 190 DEG C of hybrid reaction 1.2h of temperature, is squeezed with extruder at 190 DEG C of temperature It is granulated out, obtains Lauxite modified poly ethylene pellet;
(5), weigh 100 parts of Lauxite modified poly ethylenes, 4 parts of modifying titanium dioxides, 7 parts of silicon carbide, 8 parts of modified calcium carbonates and 2.4 part of three [2,4- di-tert-butyl-phenyl] phosphite ester is added in open mill, with open mill in 190 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 190 DEG C of temperature with extruder by 0.9h.
Embodiment 10
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 83 parts of ethyl alcohol, 17 parts of epoxychloropropane, 3 parts of sodium hydroxides and 4 parts of water are weighed and are added to reaction In device, mixing speed 123r/min reacts 1.5h under the conditions of 66 DEG C of maintenance system temperature, and through 90 DEG C, -0.08MPa decompression is steamed 2h is evaporated, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 7 parts of water, 175 parts of isopropanols, 186 parts of ethyl alcohol, 4 parts of ammonium nitrate, 12 part three it is different hard Ester acid isopropyl titanate and 13 parts of oleic acid are added in reaction kettle, mixing speed 140r/min, 49 DEG C of items of maintenance system temperature 4h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 102 parts of 1,4-benzoquinone diimines, 253 parts of ethyl alcohol and 37 parts of titanium dioxide are weighed and are added to reaction In kettle, at 154 DEG C of temperature, mixing speed reacts 2.5 h to get modifying titanium dioxide is arrived under the conditions of being 85r/min;
(4), 100 parts of polyethylene pellets, 18 parts of Lauxites, 19 parts of ethyl alcohol, 7 parts of salicylic acids and 7 parts of three second of dichloromethyl are weighed Oxysilane is added in open mill, with open mill in 180 DEG C of hybrid reaction 1h of temperature, is squeezed out with extruder at 180 DEG C of temperature It is granulated, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 7 parts of modifying titanium dioxides, 6 parts of silicon carbide, 10 parts of modified calcium carbonates are weighed It is added in open mill with 1.7 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 185 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 185 DEG C of temperature with extruder by 1.4h.
Embodiment 11
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 90 parts of ethyl alcohol, 27 parts of epoxychloropropane, 2 parts of sodium hydroxides and 3.8 parts of water are weighed to be added to instead It answers in device, mixing speed 136r/min, reacts 1.3h under the conditions of 61 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa is depressurized 2h is distilled, 120 DEG C of dry 2h obtain modified calcium carbonate;
(2), 100 parts of tetraethyl titanates, 6.7 parts of water, 178 parts of isopropanols, 193 parts of ethyl alcohol, 4.6 parts of ammonium nitrate, 13.2 parts are weighed Three iso stearate isopropyl titanates and 9.6 parts of oleic acid are added in reaction kettle, mixing speed 157r/min, maintenance system temperature 3.4h is reacted under the conditions of 55 DEG C, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide Titanium;
(3), 100 parts of ethyl phosphonic acids, 99 parts of 1,4-benzoquinone diimines, 238 parts of ethyl alcohol and 29 parts of titanium dioxide are weighed and are added to reaction In kettle, at 153 DEG C of temperature, mixing speed reacts 2.2 h to get modifying titanium dioxide is arrived under the conditions of being 86r/min;
(4), 100 parts of polyethylene pellets, 17 parts of Lauxites, 22 parts of ethyl alcohol, 7 parts of salicylic acids and 5.6 parts of dichloromethyls three are weighed Ethoxysilane is added in open mill, with open mill in 186 DEG C of hybrid reaction 1.3h of temperature, with extruder at 186 DEG C of temperature Extruding pelletization obtains Lauxite modified poly ethylene pellet;
(5), weigh 100 parts of Lauxite modified poly ethylenes, 5 parts of modifying titanium dioxides, 6 parts of silicon carbide, 9 parts of modified calcium carbonates and 2.4 part of three [2,4- di-tert-butyl-phenyl] phosphite ester is added in open mill, with open mill in 190 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 190 DEG C of temperature with extruder by 1.1h.
Embodiment 12
A kind of modified poly ethylene, preparation method includes the following steps:
(1), 100 parts of calcium carbonate, 77 parts of ethyl alcohol, 24 parts of epoxychloropropane, 3 parts of sodium hydroxides and 4 parts of water are weighed and are added to reaction In device, mixing speed 130r/min reacts 2h under the conditions of 60 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa vacuum distillation 2h, 120 DEG C of dry 2h, obtains modified calcium carbonate;
(2), weigh 100 parts of tetraethyl titanates, 5 parts of water, 165 parts of isopropanols, 170 parts of ethyl alcohol, 5 parts of ammonium nitrate, 14 part three it is different hard Ester acid isopropyl titanate and 11 parts of oleic acid are added in reaction kettle, mixing speed 150r/min, 53 DEG C of items of maintenance system temperature 3h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h obtain titanium dioxide;
(3), 100 parts of ethyl phosphonic acids, 95 parts of 1,4-benzoquinone diimines, 260 parts of ethyl alcohol and 37 parts of titanium dioxide are weighed and are added to reaction In kettle, at 150 DEG C of temperature, mixing speed reacts 2 h to get modifying titanium dioxide is arrived under the conditions of being 77r/min;
(4), 100 parts of polyethylene pellets, 14 parts of Lauxites, 23 parts of ethyl alcohol, 6.4 parts of salicylic acids and 5.2 parts of dichloromethyls are weighed Triethoxysilane is added in open mill, with open mill in 188 DEG C of hybrid reaction 0.6h of temperature, with extruder in temperature 188 DEG C extruding pelletization, obtains Lauxite modified poly ethylene pellet;
(5), 100 parts of Lauxite modified poly ethylenes, 7 parts of modifying titanium dioxides, 6 parts of silicon carbide, 12 parts of modified calcium carbonates are weighed It is added in open mill with 2 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, with open mill in 185 DEG C of hybrid reactions of temperature Modified poly ethylene extruding pelletization is arrived modified poly ethylene pellet in 185 DEG C of temperature with extruder by 0.8h.
The performance parameter of modified poly ethylene made from 1 embodiment 1 of table
Embodiment 1
Ultraviolet-shielding type It is excellent
Oxygen index (OI) % 38
Thermal coefficient/W/m.K 0.83
Tensile strength/MPa 45
Zero load maximum operation (service) temperature/DEG C 130
Molding shrinkage/% 1.3
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art, Under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as the hair Bright protection scope.

Claims (2)

1. a kind of preparation method of modified poly ethylene, it is characterised in that: including following raw material components: the modified poly- second of Lauxite Alkene, modifying titanium dioxide, silicon carbide, modified calcium carbonate and three [2,4- di-tert-butyl-phenyl] phosphite esters, the ureaformaldehyde tree The matter of rouge modified poly ethylene, modifying titanium dioxide, silicon carbide, modified calcium carbonate and three [2,4- di-tert-butyl-phenyl] phosphite esters Amount portion rate is that 100:2~7:5~8:8~12:1~3 are added in open mill, is mixed with open mill at 130~260 DEG C of temperature 0.5~2h is reacted, with extruder in 130~260 DEG C of temperature by modified poly ethylene extruding pelletization, wherein the Lauxite Modified poly ethylene pellet is reacted by polyethylene pellet, Lauxite, ethyl alcohol, salicylic acid and dichloromethyl triethoxysilane to be made , the polyethylene pellet, Lauxite, ethyl alcohol, salicylic acid and dichloromethyl triethoxysilane mass parts ratio be 100:12~18:15~27:5~8:4~7 are added in open mill, with open mill in 130~260 DEG C of hybrid reactions 0.5 of temperature ~2h, with extruder in 130~260 DEG C of extruding pelletizations of temperature, the modifying titanium dioxide is sub- by ethyl phosphonic acid, 1,4-benzoquinone two Amine, ethyl alcohol and titanium dioxide reaction are made, the mass parts of the ethyl phosphonic acid, 1,4-benzoquinone diimine, ethyl alcohol and titanium dioxide Number than be 100:85~105:230~270:27~40, the titanium dioxide by tetraethyl titanate, water, isopropanol, ethyl alcohol, Ammonium nitrate, three iso stearate isopropyl titanates and elaidin reaction are made, the tetraethyl titanate, water, isopropanol, ethyl alcohol, nitre The mass parts ratio of sour ammonium, three iso stearate isopropyl titanates and oleic acid be 100:5~10:150~195:130~200:3~ 5:10~15:8~14 are added in reaction kettle, and mixing speed is 130~160r/min, 40~60 DEG C of items of maintenance system temperature 2~5h is reacted under part, through filtering, 1L water washing 3 times, 500mL ethanol washing 2 times, 500 DEG C of roasting 3h, the modification carbonic acid Calcium is reacted by calcium carbonate, ethyl alcohol, epoxychloropropane, sodium hydroxide and water to be made, the calcium carbonate, ethyl alcohol, epoxychloropropane, The mass parts ratio of sodium hydroxide and water is that 100:70~100:13~27:2~5:3~6 are added in reactor, mixing speed For 120~140r/min, 1~2h is reacted under the conditions of 55~70 DEG C of maintenance system temperature, through 90 DEG C, -0.08MPa vacuum distillation 2h, 120 DEG C of dry 2h.
2. a kind of preparation method of modified poly ethylene according to claim 1, it is characterised in that: the modification titanium dioxide Titanium is as made from following preparation method: by ethyl phosphonic acid, 1,4-benzoquinone diimine, ethyl alcohol and titanium dioxide according to mass parts ratio 100:88~102:238~260:28~39 are added in reaction kettle, at 146~155 DEG C of temperature, mixing speed is 77~ 1.2~2.6 h are reacted under the conditions of 86r/min.
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