CN108530755A - A kind of preparation method of nano modification polypropylene board - Google Patents

A kind of preparation method of nano modification polypropylene board Download PDF

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CN108530755A
CN108530755A CN201810391179.6A CN201810391179A CN108530755A CN 108530755 A CN108530755 A CN 108530755A CN 201810391179 A CN201810391179 A CN 201810391179A CN 108530755 A CN108530755 A CN 108530755A
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mixed
nano
temperature
polypropylene
obtains
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沈春霞
杨明忠
张建初
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions 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
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • 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
    • C08K3/02—Elements
    • C08K2003/026—Phosphorus
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C08K2201/011—Nanostructured additives
    • 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

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to technical field of high-molecule composite preparation, and in particular to a kind of preparation method of nano modification polypropylene board.The present invention melts liquid as base material using modified polypropene, modified Nano mixed-powder dispersion liquid and treated basalt fiber are as modifying agent, and it is aided with maleic anhydride inoculated polypropylene, nano modification polypropylene board is prepared in calcium carbonate and citric acid etc., polypropylene is modified first, maleic anhydride inoculated polypropylene is added into polypropylene again, surface modification is carried out to basalt fibre using onium hydroxide solution, enhance its affinity with nano-particle, butyl titanate and absolute ethyl alcohol are mixed under the action of stabilizer, gel is obtained by the reaction, vegetation water is extracted from phoenix tree leaf, nano-zinc oxide powder is dispersed in non-polar substrate surface under polar adsorption, to reduce the uitraviolet intensity of direction of illumination, further increase the anti-aging of polypropylene board, it is with a wide range of applications.

Description

A kind of preparation method of nano modification polypropylene board
Technical field
The present invention relates to technical field of high-molecule composite preparation, and in particular to a kind of nano modification polypropylene board Preparation method.
Background technology
Polypropylene（PP）, prepared by being by propylene polymerization a kind of thermoplastic resin.Polypropylene（PP）Plank is PP resins Add the technical process such as various functions auxiliary agent is extruded, press polish, cooling, cutting and manufactured plastic plate.Polypropylene board without Smelly, nontoxic, tasteless to meet state health standards, density is small, is one kind most light in general-purpose plastics, can for a long time make at 100 DEG C With indeformable, while there is excellent electrical insulation capability and chemical stability, hardly absorbs water, with most chemical contacts It does not have an effect.Polypropylene board has been widely used in packagings and the daily lifes such as industry, agricultural, medical treatment, health at present Every field in, be a kind of product that dosage is maximum in current world's high molecular material, growth rate is most fast, mainly due to Its raw material sources is more, price is low, material property is excellent, electrical insulating property and chemical stability are good, while having again and being easily processed into The advantages of type.
Although polypropylene（PP）Plate advantage is more, but also has its deficiency：1, due to polypropylene at low ambient temperatures performance compared with Difference, it is each to uneven, poor plasticity is molded that plastic uptake when, has that crystallization causes, and plastic uptake is difficult；2, lower temperature resistance Difference, embrittlement under low temperature environment；3, since polypropylene is crystalline polymer, internal there is very big spherocrystals, cause polyacrylic Impact strength is low, poor toughness；4, ageing-resistant performance is poor, and molding shrinkage is big, easy firing, simultaneously because its is nonpolar Feature keeps it poor with the compatibility of other polar polymers, inorganic filler, to limit as injection molding, fiber, film etc. The raw material of product or the application of PP Pipe Compound；5, the case hardness of acrylic resin itself is not enough to cope with long-term friction, damage Deng.Currently, commonly used method be polypropylene is enhanced, is filled, alloying etc., but nonetheless, polypropylene board Wear-resisting and cutting resistance it is still barely satisfactory.
Therefore, developing a kind of polypropylene board that can solve above-mentioned performance issue is highly desirable.
Invention content
The technical problems to be solved by the invention：Exist for common polypropylene board at present wear no resistance, shock resistance it is strong It is poor to spend low and ageing resistance, and easy firing, simultaneously because its nonpolar feature, makes it with other polar polymers, inorganic fills out The compatibility of material is poor, to limit its lacking as the raw material of the products such as injection molding, fiber, film or the application of PP Pipe Compound It falls into, provides a kind of preparation method of nano modification polypropylene board.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of nano modification polypropylene board, it is characterised in that specifically preparation process is：
（1）Weighing 75~85g polypropylene heat temperature raisings makes its softening, and 2~4g, tri- oxygen is sequentially added into the polypropylene after softening Change two antimony and 3~5g red phosphorus, continue heat preservation and be mixed, obtains modified polypropene melting liquid；
（2）It weighs 11~13g phoenix tree leafs to be placed in the beaker with 40~45mL deionized waters, and beaker is placed in ultrasonic wave and is shaken Ultrasonic extraction in device is swung, filtering removal filter residue collects filtrate, filtrate is evaporated under reduced pressure, obtains self-control plant extraction liquid, will Modified polypropene melts liquid and self-control plant extraction liquid mixing is placed in ultrasonic disperse in ultrasonic wave separating apparatus, obtains modified polypropene Dispersion liquid；
（3）16~20mL butyl titanates are measured to be dissolved in the beaker with 75~80mL absolute ethyl alcohols and 2~4mL acetylacetone,2,4-pentanediones, It is placed in magnetic stirrer and is mixed, obtain stirring liquid, then reaction is mixed in stirring liquid, hydrochloric acid and deionized water, After reaction, still aging, gel is obtained, continues gel being placed in drying in baking oven, xerogel is obtained, finally by xerogel It is placed in Muffle furnace, heat temperature raising, is sintered and keeps the temperature, cooled to room temperature, grinding discharging obtains nanometer titanium dioxide titanium valve End；
（4）It measures 35~45mL liquor zinci chloridis to pour into beaker, and beaker is placed in water-bath after stirring, then into beaker 30~32mL sodium hydroxide solutions are added dropwise, after completion of dropwise addition, continues insulated and stirred reaction, centrifuges, go after reaction Except supernatant, sediment is obtained, sediment is cleaned with deionized water, finally the sediment after cleaning is placed in baking oven and is dried, Cooled to room temperature, grinding discharging, obtains nano-zinc oxide powder, presses equal mass ratioes by nano-zinc oxide powder and nanometer two Titanium dioxide powder is mixed, and obtains a nanometer mixed-powder；
（5）It weighs 16~20g basalt fibres and is cut into 1~2cm length, obtain short basalt fibre, into short basalt fibre 4~6mL sodium hydroxide solutions are added, is mixed, obtains treated basalt fiber；
（6）It counts in parts by weight, weighs 35~45 parts of modified polypropene dispersion liquids, 4~6 parts of maleic anhydride grafting poly- third respectively Alkene, 12~16 parts of nanometer mixed-powders and 6~8 parts of treated basalt fiber mixing are placed in blender and stir, then add 1~3 Part absolute ethyl alcohol, 2~4 parts of calcium carbonate and 1~3 part of citric acid, continue to be mixed, obtain mixture, mixture are put into double Extrusion forming in Screw Extrusion sheet material machine, cooling discharging is to get nano modification polypropylene board.
Step（1）The heat temperature raising temperature is 165~175 DEG C, and continuation mixing time is 35~45min.
Step（2）The ultrasonic extraction temperature is 65~70 DEG C, and ultrasonic extraction frequency is 10~12kHz, ultrasonic extraction Time is 16~20min, and the vacuum distillation time is 8~10min, and modified polypropene melts liquid and makes the quality of plant extraction liquid by oneself Than being 3：1, ultrasonic disperse power is 85~100W, and ultrasonic disperse frequency is 4~6kHz, and the ultrasonic disperse time is 16~20min.
Step（3）The mixing time be 24~32min, stirring liquid, mass fraction be 20% hydrochloric acid and go from The volume ratio of sub- water is 5：1：2, it is 1~2h to be stirred to react the time, and the still aging time is 2~4h, and drying temperature is 75~80 DEG C, drying time is 16~20min, and finally heated warming temperature is 450~500 DEG C, and the sintered heat insulating time is 1~3h.
Step（4）A concentration of 0.7mol/L of the liquor zinci chloridi, whipping temp are 65~75 DEG C, and mixing time is 24~32min, a concentration of 0.6mol/L of sodium hydroxide solution, it is 16~20min to continue to be stirred to react the time, when centrifugation Between be 5~7min, wash number be 3~5 times, drying temperature be 70~85 DEG C, drying time be 45~60min, be mixed Time is 6~8min.
Step（5）A concentration of 0.05mol/L of the sodium hydroxide solution, mixing time are 32~36min.
Step（6）The speed of agitator is 120~160r/min, and mixing time is 10~12min, continues speed of agitator For 240~320r/min, continuation mixing time is 45~60min, and extruding rotating speed is 85~100r/min, and it is 160 to squeeze temperature ~180 DEG C, squeeze pressure is 4~6MPa.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is using modified polypropene melting liquid as base material, modified Nano mixed-powder dispersion liquid and treated basalt fiber As modifying agent, and it is aided with maleic anhydride inoculated polypropylene, calcium carbonate and citric acid etc. and nano modification polypropylene board is prepared Material, first with anti-flammability antimony oxide and red phosphorus polypropylene is modified, due to antimony oxide and red phosphorus Unaffected to the polypropylene with heat resistance during decomposing when heated, these fire retardants are handed over polypropylene Connection reaction, generate layer of charcoal or foam-like covering, block air contact polypropylene surface, control volatilizable fuel into Enter air accelerated combustion, realize the effect for slowing down heat and mass, to improve the anti-flammability of polypropylene board, then to polypropylene Middle addition maleic anhydride inoculated polypropylene introduces highly polar side group on nonpolar polypropylene molecule main chain, enhances The cementability and compatibility of polar filler and non-polar polypropylene, while improving the dispersion of filler and polypropylene compatibility and filler Property, effectively dispersion of the reinforcing filler in polypropylene, to improve the impact strength of polypropylene board；
（2）The present invention carries out surface modification using sodium hydroxide solution to basalt fibre, due to basalt fibre surface relatively light Sliding, surface energy is relatively low, is cleaned to its surface, removes the greasy dirt on its surface, then carry out slight erosion to its surface, increases Its surface roughness to enhance its affinity with nano-particle, while accelerating nano-particle on basalt fibre surface The speed of deposition, and since basalt fibre is by silica, aluminium oxide, calcium oxide, magnesia, iron oxide and titanium dioxide The basalt building stones of equal oxides composition are after high-temperature fusion, made of bushing Defect, the presence of these oxides, It is filled in base material internal void so that the wearability of polypropylene board is improved；
（3）Butyl titanate and absolute ethyl alcohol are mixed under the action of stabilizer and gel are obtained by the reaction by the present invention, and will coagulate Glue sintering, grinding obtain nano titanium dioxide powder, itself and nano zine oxide are mixed to get a nanometer mixed-powder, wherein nanometer Titanium dioxide has very strong shielding action to ultraviolet light, and forms one layer with transparent, adhesive force is good in substrate surface Three-dimensional netted-oxide gel film, the ageing resistance for being conducive to polypropylene board is improved, then extracted from phoenix tree leaf Vegetation water wherein contains polar group in plant extraction liquid, is changed to base material using the plant extraction liquid containing polar group Property, make substrate surface be in polarity, it is in addition nano oxidized to improve the compatibility of polar nano mixed-powder and non-polar substrate Zinc powder is dispersed in non-polar substrate surface under polar adsorption, and the energy forbidden band of wherein nano-zinc oxide powder is wide Degree is 4.5eV, is equivalent to the energy of most of ultraviolet light, assigns its strong ultraviolet absorption ability, and nano zine oxide Particle size is much smaller than ultraviolet wavelength, assigns its excellent ultraviolet light scattering power, the ultraviolet light being radiated on nano zine oxide It can be scattered to all directions, to reduce the uitraviolet intensity of direction of illumination, further increase the anti-ageing of polypropylene board Change, is with a wide range of applications.
Specific implementation mode
Weighing 75~85g polypropylene and being heated to 165~175 DEG C makes its softening, successively into the polypropylene after softening 2~4g antimony oxides and 3~5g red phosphorus is added, continues heat preservation and 35~45min is mixed, obtains modified polypropene melting Liquid；It weighs 11~13g phoenix tree leafs to be placed in the beaker with 40~45mL deionized waters, and beaker is placed in ultrasonic oscillator In, 16~20min of ultrasonic extraction under conditions of temperature is 65~70 DEG C, frequency is 10~12kHz, filtering removal filter residue is received Collect filtrate, filtrate is subjected to 8~10min of vacuum distillation, obtains self-control plant extraction liquid, be in mass ratio 3：1 by modification poly- third Alkene molten liquid and self-control plant extraction liquid mixing are placed in ultrasonic wave separating apparatus, power is 85~100W, frequency is 4~6kHz Under conditions of 16~20min of ultrasonic disperse, obtain modified polypropene dispersion liquid；16~20mL butyl titanates are measured to be dissolved in 75 In the beaker of~80mL absolute ethyl alcohols and 2~4mL acetylacetone,2,4-pentanediones, it is placed in 24~32min of mixing in magnetic stirrer, is obtained To stirring liquid, then will stir liquid, the hydrochloric acid that mass fraction is 20% and deionized water is 5 by volume：1：2 are mixed reaction 1 ~2h, after reaction, still aging 2~4h obtain gel, continue gel being placed in baking oven, are 75~80 DEG C in temperature 16~20min of lower drying, obtains xerogel, finally xerogel is placed in Muffle furnace, is heated to 450~500 DEG C, sintering And 1~3h is kept the temperature, cooled to room temperature, grinding discharging obtains nano titanium dioxide powder；It is a concentration of to measure 35~45mL The liquor zinci chloridi of 0.7mol/L pours into beaker, and beaker is placed in water-bath, and 24 are stirred at being 65~75 DEG C in temperature After~32min, then the sodium hydroxide solution of 30~32mL a concentration of 0.6mol/L is added dropwise into beaker, after completion of dropwise addition, after Continuation of insurance temperature is stirred to react 16~20min, centrifuges 5~7min after reaction, removes supernatant, obtains sediment, spend Ionized water cleans sediment 3~5 times, and finally the sediment after cleaning is placed in baking oven, is dried at being 70~85 DEG C in temperature 45~60min, cooled to room temperature, grinding discharging obtain nano-zinc oxide powder, press equal mass ratioes by nano zinc oxide powder 6~8min is mixed in end and nano titanium dioxide powder, obtains a nanometer mixed-powder；16~20g basalt fibres are weighed to cut At 1~2cm length, short basalt fibre is obtained, the hydrogen-oxygen of a concentration of 0.05mol/L of 4~6mL is added into short basalt fibre Change sodium solution, 32~36min is mixed, obtains treated basalt fiber；It counts in parts by weight, weighs 35~45 parts respectively and change Property polypropylene dispersion liquid, 4~6 parts of maleic anhydride inoculated polypropylenes, 12~16 parts of nanometer mixed-powders and 6~8 parts of modified Black Warriors The mixing of rock fiber is placed in blender, 10~12min is stirred under conditions of rotating speed is 120~160r/min, then add 1~3 Part absolute ethyl alcohol, 2~4 parts of calcium carbonate and 1~3 part of citric acid continue mixing under conditions of rotating speed is 240~320r/min and stir 45~60min is mixed, mixture is obtained, mixture is put into twin-screw extrusion sheet material machine, is 85~100r/min, temperature in rotating speed Degree for 160~180 DEG C and pressure be 4~6MPa under conditions of extrusion forming, cooling discharging is to get nano modification polypropylene board Material.
Weighing 75g polypropylene and being heated to 165 DEG C makes its softening, and tri- oxygen of 2g is sequentially added into the polypropylene after softening Change two antimony and 3g red phosphorus, continue heat preservation and 35min is mixed, obtains modified polypropene melting liquid；It weighs 11g phoenix tree leafs and is placed in band In the beaker for there are 40mL deionized waters, and beaker is placed in ultrasonic oscillator, temperature is 65 DEG C, frequency is 10kHz's Under the conditions of ultrasonic extraction 16min, filtering removal filter residue, collect filtrate, filtrate is subjected to vacuum distillation 8min, obtain self-control plant Extracting solution is in mass ratio 3：Modified polypropene melting liquid and self-control plant extraction liquid are mixed and are placed in ultrasonic wave separating apparatus by 1, Ultrasonic disperse 16min under conditions of power is 85W, frequency is 4kHz, obtains modified polypropene dispersion liquid；Measure 16mL metatitanic acids Butyl ester is dissolved in the beaker with 75mL absolute ethyl alcohols and 2mL acetylacetone,2,4-pentanediones, is placed in magnetic stirrer and is mixed 24min obtains stirring liquid, then will stir liquid, the hydrochloric acid that mass fraction is 20% and deionized water is 5 by volume：1：2 mixing It is stirred to react 1h, after reaction, still aging 2h obtains gel, continues gel being placed in baking oven, in the case where temperature is 75 DEG C Dry 16min, obtains xerogel, finally xerogel is placed in Muffle furnace, be heated to 450 DEG C, be sintered and keep the temperature 1h, from It is so cooled to room temperature, grinding discharging obtains nano titanium dioxide powder；Measure the liquor zinci chloridi of a concentration of 0.7mol/L of 35mL It pours into beaker, and beaker is placed in water-bath, at being 65 DEG C in temperature after stirring 24min, then 30mL is added dropwise into beaker The sodium hydroxide solution of a concentration of 0.6mol/L, after completion of dropwise addition, continue insulated and stirred react 16min, after reaction from The heart detaches 5min, removes supernatant, obtains sediment, sediment is cleaned 3 times with deionized water, finally by the sediment after cleaning It is placed in baking oven, 45min, cooled to room temperature is dried at being 70 DEG C in temperature, grinding discharging obtains nano zinc oxide powder End obtains a nanometer mixed-powder by waiting mass ratioes that 6min is mixed in nano-zinc oxide powder and nano titanium dioxide powder； It weighs 16g basalt fibres and is cut into 1cm length, obtain short basalt fibre, it is a concentration of that 4mL is added into short basalt fibre The sodium hydroxide solution of 0.05mol/L is mixed 32min, obtains treated basalt fiber；It counts, claims respectively in parts by weight Take 35 parts of modified polypropene dispersion liquids, 4 parts of maleic anhydride inoculated polypropylenes, 12 parts of nanometer mixed-powders and 6 parts of modified basalt Fiber mixing be placed in blender, rotating speed be 120r/min under conditions of stir 10min, then add 1 part of absolute ethyl alcohol, 2 parts Calcium carbonate and 1 part of citric acid continue that 45min is mixed under conditions of rotating speed is 240r/min, obtain mixture, will mix In material input twin-screw extrusion sheet material machine, squeezed under conditions of rotating speed is 85r/min, temperature is 160 DEG C and pressure is 4MPa Molding, cooling discharging is to get nano modification polypropylene board.
Weighing 80g polypropylene and being heated to 170 DEG C makes its softening, and tri- oxygen of 3g is sequentially added into the polypropylene after softening Change two antimony and 4g red phosphorus, continue heat preservation and 40min is mixed, obtains modified polypropene melting liquid；It weighs 12g phoenix tree leafs and is placed in band In the beaker for there are 43mL deionized waters, and beaker is placed in ultrasonic oscillator, temperature is 68 DEG C, frequency is 11kHz's Under the conditions of ultrasonic extraction 18min, filtering removal filter residue, collect filtrate, filtrate is subjected to vacuum distillation 9min, obtain self-control plant Extracting solution is in mass ratio 3：Modified polypropene melting liquid and self-control plant extraction liquid are mixed and are placed in ultrasonic wave separating apparatus by 1, Ultrasonic disperse 18min under conditions of power is 93W, frequency is 5kHz, obtains modified polypropene dispersion liquid；Measure 18mL metatitanic acids Butyl ester is dissolved in the beaker with 77mL absolute ethyl alcohols and 3mL acetylacetone,2,4-pentanediones, is placed in magnetic stirrer and is mixed 28min obtains stirring liquid, then will stir liquid, the hydrochloric acid that mass fraction is 20% and deionized water is 5 by volume：1：2 mixing It is stirred to react 1.5h, after reaction, still aging 3h obtains gel, continues gel being placed in baking oven, is 78 DEG C in temperature Lower dry 18min, obtains xerogel, finally xerogel is placed in Muffle furnace, is heated to 475 DEG C, is sintered and keeps the temperature 2h, Cooled to room temperature, grinding discharging, obtains nano titanium dioxide powder；The zinc chloride for measuring a concentration of 0.7mol/L of 40mL is molten Liquid pours into beaker, and beaker is placed in water-bath, at being 70 DEG C in temperature after stirring 28min, then is added dropwise into beaker The sodium hydroxide solution of a concentration of 0.6mol/L of 31mL continues insulated and stirred and reacts 18min, reaction terminates after completion of dropwise addition After centrifuge 6min, remove supernatant, obtain sediment, sediment clean 4 times with deionized water, finally will be after cleaning sink Starch is placed in baking oven, and 53min, cooled to room temperature are dried at being 78 DEG C in temperature, and grinding discharging obtains nano zine oxide Powder obtains a nanometer mixed powder by waiting mass ratioes that 7min is mixed in nano-zinc oxide powder and nano titanium dioxide powder End；It weighs 18g basalt fibres and is cut into 1.5cm length, obtain short basalt fibre, it is dense that 5mL is added into short basalt fibre Degree is the sodium hydroxide solution of 0.05mol/L, and 34min is mixed, obtains treated basalt fiber；It counts in parts by weight, point Also known as take 40 parts of modified polypropene dispersion liquids, 5 parts of maleic anhydride inoculated polypropylenes, 14 parts of nanometer mixed-powders and 7 parts of modifications profound The mixing of military rock fiber is placed in blender, and 11min is stirred under conditions of rotating speed is 140r/min, then add 2 parts of absolute ethyl alcohols, 3 parts of calcium carbonate and 2 parts of citric acids continue that 53min is mixed under conditions of rotating speed is 280r/min, obtain mixture, will Mixture is put into twin-screw extrusion sheet material machine, under conditions of rotating speed is 93r/min, temperature is 170 DEG C and pressure is 5MPa Extrusion forming, cooling discharging is to get nano modification polypropylene board.
Weighing 85g polypropylene and being heated to 175 DEG C makes its softening, and tri- oxygen of 4g is sequentially added into the polypropylene after softening Change two antimony and 5g red phosphorus, continue heat preservation and 45min is mixed, obtains modified polypropene melting liquid；It weighs 13g phoenix tree leafs and is placed in band In the beaker for there are 45mL deionized waters, and beaker is placed in ultrasonic oscillator, temperature is 70 DEG C, frequency is 12kHz's Under the conditions of ultrasonic extraction 20min, filtering removal filter residue, collect filtrate, filtrate is subjected to vacuum distillation 10min, obtain self-control plant Object extracting solution is in mass ratio 3：Modified polypropene melting liquid and self-control plant extraction liquid are mixed and are placed in ultrasonic wave separating apparatus by 1 In, ultrasonic disperse 20min under conditions of power is 100W, frequency is 6kHz obtains modified polypropene dispersion liquid；Measure 20mL Butyl titanate is dissolved in the beaker with 80mL absolute ethyl alcohols and 4mL acetylacetone,2,4-pentanediones, is placed in magnetic stirrer and is mixed 32min obtains stirring liquid, then will stir liquid, the hydrochloric acid that mass fraction is 20% and deionized water is 5 by volume：1：2 mixing It is stirred to react 2h, after reaction, still aging 4h obtains gel, continues gel being placed in baking oven, in the case where temperature is 80 DEG C Dry 20min, obtains xerogel, finally xerogel is placed in Muffle furnace, be heated to 500 DEG C, be sintered and keep the temperature 3h, from It is so cooled to room temperature, grinding discharging obtains nano titanium dioxide powder；Measure the liquor zinci chloridi of a concentration of 0.7mol/L of 45mL It pours into beaker, and beaker is placed in water-bath, at being 75 DEG C in temperature after stirring 32min, then 32mL is added dropwise into beaker The sodium hydroxide solution of a concentration of 0.6mol/L, after completion of dropwise addition, continue insulated and stirred react 20min, after reaction from The heart detaches 7min, removes supernatant, obtains sediment, sediment is cleaned 5 times with deionized water, finally by the sediment after cleaning It is placed in baking oven, 60min, cooled to room temperature is dried at being 85 DEG C in temperature, grinding discharging obtains nano zinc oxide powder End obtains a nanometer mixed-powder by waiting mass ratioes that 8min is mixed in nano-zinc oxide powder and nano titanium dioxide powder； It weighs 20g basalt fibres and is cut into 2cm length, obtain short basalt fibre, it is a concentration of that 6mL is added into short basalt fibre The sodium hydroxide solution of 0.05mol/L is mixed 36min, obtains treated basalt fiber；It counts, claims respectively in parts by weight Take 45 parts of modified polypropene dispersion liquids, 6 parts of maleic anhydride inoculated polypropylenes, 16 parts of nanometer mixed-powders and 8 parts of modified basalt Fiber mixing be placed in blender, rotating speed be 160r/min under conditions of stir 12min, then add 3 parts of absolute ethyl alcohols, 4 parts Calcium carbonate and 3 parts of citric acids continue that 60min is mixed under conditions of rotating speed is 320r/min, obtain mixture, will mix In material input twin-screw extrusion sheet material machine, squeezed under conditions of rotating speed is 100r/min, temperature is 180 DEG C and pressure is 6MPa Molding, cooling discharging is to get nano modification polypropylene board.
The polypropylene board that comparative example is produced with Shanghai City company is as a comparison case
Polypropylene board in nano modification polypropylene board produced by the present invention and comparative example is detected, testing result is such as Shown in table 1：
Ageing resistance is tested
The nano modification polypropylene board and comparative example polypropylene board be prepared to Examples 1 to 3 carries out anti-aging property Test carries out artificially roughening according to thermo-oxidative ageing experimental standard GB/T7141-2008（90 DEG C, 500h）.
1 performance measurement result of table
From the data in table 1, it can be seen that nano modification polypropylene board produced by the present invention, have wearability it is good, it is excellent in cushion effect and Ageing resistance is good, and anti-flammability is strong, has good market prospects.

Claims (7)

1. a kind of preparation method of nano modification polypropylene board, it is characterised in that specifically preparation process is：
（1）Weighing 75~85g polypropylene heat temperature raisings makes its softening, and 2~4g, tri- oxygen is sequentially added into the polypropylene after softening Change two antimony and 3~5g red phosphorus, continue heat preservation and be mixed, obtains modified polypropene melting liquid；
（2）It weighs 11~13g phoenix tree leafs to be placed in the beaker with 40~45mL deionized waters, and beaker is placed in ultrasonic wave and is shaken Ultrasonic extraction in device is swung, filtering removal filter residue collects filtrate, filtrate is evaporated under reduced pressure, obtains self-control plant extraction liquid, will Modified polypropene melts liquid and self-control plant extraction liquid mixing is placed in ultrasonic disperse in ultrasonic wave separating apparatus, obtains modified polypropene Dispersion liquid；
（3）16~20mL butyl titanates are measured to be dissolved in the beaker with 75~80mL absolute ethyl alcohols and 2~4mL acetylacetone,2,4-pentanediones, It is placed in magnetic stirrer and is mixed, obtain stirring liquid, then reaction is mixed in stirring liquid, hydrochloric acid and deionized water, After reaction, still aging, gel is obtained, continues gel being placed in drying in baking oven, xerogel is obtained, finally by xerogel It is placed in Muffle furnace, heat temperature raising, is sintered and keeps the temperature, cooled to room temperature, grinding discharging obtains nanometer titanium dioxide titanium valve End；
（4）It measures 35~45mL liquor zinci chloridis to pour into beaker, and beaker is placed in water-bath after stirring, then into beaker 30~32mL sodium hydroxide solutions are added dropwise, after completion of dropwise addition, continues insulated and stirred reaction, centrifuges, go after reaction Except supernatant, sediment is obtained, sediment is cleaned with deionized water, finally the sediment after cleaning is placed in baking oven and is dried, Cooled to room temperature, grinding discharging, obtains nano-zinc oxide powder, presses equal mass ratioes by nano-zinc oxide powder and nanometer two Titanium dioxide powder is mixed, and obtains a nanometer mixed-powder；
（5）It weighs 16~20g basalt fibres and is cut into 1~2cm length, obtain short basalt fibre, into short basalt fibre 4~6mL sodium hydroxide solutions are added, is mixed, obtains treated basalt fiber；
（6）It counts in parts by weight, weighs 35~45 parts of modified polypropene dispersion liquids, 4~6 parts of maleic anhydride grafting poly- third respectively Alkene, 12~16 parts of nanometer mixed-powders and 6~8 parts of treated basalt fiber mixing are placed in blender and stir, then add 1~3 Part absolute ethyl alcohol, 2~4 parts of calcium carbonate and 1~3 part of citric acid, continue to be mixed, obtain mixture, mixture are put into double Extrusion forming in Screw Extrusion sheet material machine, cooling discharging is to get nano modification polypropylene board.
2. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（1） The heat temperature raising temperature is 165~175 DEG C, and continuation mixing time is 35~45min.
3. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（2） The ultrasonic extraction temperature is 65~70 DEG C, and ultrasonic extraction frequency is 10~12kHz, and the ultrasonic extraction time is 16~20min, The vacuum distillation time is 8~10min, and it is 3 that modified polypropene, which melts liquid and makes the mass ratio of plant extraction liquid by oneself,：1, ultrasonic disperse Power is 85~100W, and ultrasonic disperse frequency is 4~6kHz, and the ultrasonic disperse time is 16~20min.
4. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（3） The mixing time is 24~32min, and the volume ratio of stirring liquid, the hydrochloric acid that mass fraction is 20% and deionized water is 5：1：2, it is 1~2h to be stirred to react the time, and the still aging time is 2~4h, and drying temperature is 75~80 DEG C, drying time 16 ~20min, finally heated warming temperature are 450~500 DEG C, and the sintered heat insulating time is 1~3h.
5. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（4） A concentration of 0.7mol/L of the liquor zinci chloridi, whipping temp are 65~75 DEG C, and mixing time is 24~32min, hydrogen-oxygen A concentration of 0.6mol/L for changing sodium solution continues to be stirred to react the time as 16~20min, and the centrifugation time is 5~7min, clearly It is 3~5 times to wash number, and drying temperature is 70~85 DEG C, and drying time is 45~60min, and the mixing time is 6~8min.
6. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（5） A concentration of 0.05mol/L of the sodium hydroxide solution, mixing time are 32~36min.
7. a kind of preparation method of nano modification polypropylene board according to claim 1, it is characterised in that：Step（6） The speed of agitator is 120~160r/min, and mixing time is 10~12min, and continuation speed of agitator is 240~320r/ Min, continuation mixing time are 45~60min, and extruding rotating speed is 85~100r/min, and it is 160~180 DEG C to squeeze temperature, is squeezed Pressure is 4~6MPa.
CN201810391179.6A 2018-04-27 2018-04-27 A kind of preparation method of nano modification polypropylene board Withdrawn CN108530755A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109134899A (en) * 2018-09-20 2019-01-04 何治伟 A kind of preparation method of acid-alkali-corrosive-resisting wear-resisting type aluminum-plastic composite membrane
CN110922680A (en) * 2019-11-15 2020-03-27 江苏东方电缆材料有限公司 Basalt fiber reinforced and toughened polypropylene-based composite material and preparation method thereof
CN112300487A (en) * 2020-10-23 2021-02-02 无锡市锡山新材料科技有限公司 Preparation method of anti-aging polypropylene plate
CN115819879A (en) * 2022-10-31 2023-03-21 四川兴辉腾集团有限公司 Polypropylene and basalt composite pipe and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109134899A (en) * 2018-09-20 2019-01-04 何治伟 A kind of preparation method of acid-alkali-corrosive-resisting wear-resisting type aluminum-plastic composite membrane
CN110922680A (en) * 2019-11-15 2020-03-27 江苏东方电缆材料有限公司 Basalt fiber reinforced and toughened polypropylene-based composite material and preparation method thereof
CN112300487A (en) * 2020-10-23 2021-02-02 无锡市锡山新材料科技有限公司 Preparation method of anti-aging polypropylene plate
CN112300487B (en) * 2020-10-23 2023-02-28 无锡市锡山新材料科技有限公司 Preparation method of anti-aging polypropylene plate
CN115819879A (en) * 2022-10-31 2023-03-21 四川兴辉腾集团有限公司 Polypropylene and basalt composite pipe and preparation method thereof

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