CN109054156A - A kind of preparation method of high heat resistance highstrenghtpiston masterbatch - Google Patents
A kind of preparation method of high heat resistance highstrenghtpiston masterbatch Download PDFInfo
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- CN109054156A CN109054156A CN201810798561.9A CN201810798561A CN109054156A CN 109054156 A CN109054156 A CN 109054156A CN 201810798561 A CN201810798561 A CN 201810798561A CN 109054156 A CN109054156 A CN 109054156A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- 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
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Abstract
The present invention relates to a kind of preparation methods of high heat resistance highstrenghtpiston masterbatch, belong to field of polymer material preparing technology.Graphite rod is electrolysed by the present invention first, oxidation, it is reacted again with kayexalate and sulfonated polyaniline and modified-reaction object is made, then using Poplar Powder as raw material, reaction product is made with benzyl chloride hybrid reaction, finally by modified-reaction object, reaction product, it is granulated in polymer and other reagent raw materials mixing investment dual-screw pelletizer and high heat resistance highstrenghtpiston masterbatch is made, nano-graphene material sheet sound construction generated is stablized, increasing specific surface area can be come into full contact with polymer, increase dispersion effect, modified nano-graphene material is scattered in masterbatch, it is improved masterbatch molecule high temperature resistance and mechanical performance, the present invention is modified Poplar Powder using benzyl chloride, can adhesive effect effectively be formed with molecules other in masterbatch, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high heat resistance highstrenghtpiston masterbatch, belong to high molecular material technology of preparing neck
Domain.
Background technique
China is the plastics big country in the world today, and plastic products annual output is answered extensively more than 21,000,000 tons
The every field for producing and living for people, the excellent performance such as plastics are light with its, waterproof, corrosion-resistant, intensity is big by
The favor of people.
Plastic matrix is that plastic additive super quantity is attached in resin and manufactured condensation product.In manufacture plastic products
When, it is not necessary to this kind of plastic additive is added, only need to be proportionally added into this masterbatch, its advantage is that: simple process, user
Just, it is easy to implement production automation, is raised labour productivity, and avoids environmental pollution.
With the rapid development of plastics industry, a kind of filling master batch not still added material can reduce plastic products
Production cost also has the certain physical properties for improving plastic products, such as reduces notch shrinking percentage, improves appearance and feel spy
Property and obtain the approval in market, it has also become indispensable raw material in certain plastic products.Currently, domestic plastic matrix is pressed
Material point is mainly include the following types: (1) PE filling master batch；(3) PP filling master batch；(3) filling parent material of calcium carbonate；(4) talcum powder
Filling master batch；(5) transparent filling master batch；(6) white master material.
Discoloration and embrittlement are easily decomposed when plastic matrix in the prior art meets high temperature, it is poor to exist simultaneously mechanical property,
Shock resistance is bad, it is difficult to natural decomposition, it is big to environmental hazard the defects of.
Therefore a kind of good mechanical performance is provided, it is heat-resisting, ageing-resistant performance is good, no pollution to the environment and low manufacture cost,
Simple plastic matrix of preparation method and preparation method thereof have become when business urgently.
Summary of the invention
The technical problems to be solved by the invention: discoloration and embrittlement are easily decomposed when meeting high temperature for current masterbatch, simultaneously
Poor mechanical property, the bad defect of shock resistance provide a kind of preparation method of high heat resistance highstrenghtpiston masterbatch.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of high heat resistance highstrenghtpiston masterbatch, it is characterised in that specific preparation step are as follows:
(1) the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution for weighing 400~500mL is put into beaker as electrolyte, will
Graphite rod immerses in 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution as the cathode and anode of electrode, in the item of supersonic oscillations
Be powered 2~3h of electrolysis under part, takes out graphite rod after electrolysis, product in beaker is filtered, obtain filter residue, successively use nothing
Water-ethanol and distilled water clean filter residue 4~8 times, and electrolysate is made；
(2) according to parts by weight, it is molten that 3~5 parts of above-mentioned electrolysates, 2.0~2.8 parts of potassium ferrates and 16~18 parts of sulfuric acid are weighed
In liquid mixing investment beaker, isothermal reaction in ice-water bath is placed the beaker, filter cake is obtained by filtration after reaction, filters wash with distilled water
It is cake 3~5 times, spare；
(3) according to parts by weight, 3~5 parts of above-mentioned filter cakes, 4~5 parts of kayexalates, 8~9 parts of sulfonated polyanilines are weighed
It is mixed to prepare mixed emulsion in 16~20 parts of acetone investment reaction kettles, mixed emulsion quality 5~8% is added dropwise into reaction kettle
Carbic anhydride is passed through 1~2h of hydrogen after completion of dropwise addition, modified filter residue is obtained by filtration, and modified filter residue is successively used anhydrous
Ethyl alcohol and distillation water washing 3~5 times are put into baking oven and dry obtained modified-reaction object, spare；
(4) Poplar Powder and sodium hydroxide solution 1:10 in mass ratio are stirred in investment beaker, place the beaker ultrasonic shake
It swings in instrument and shakes, filtered to obtain filter residue after concussion, be put into baking oven and dry after being washed with distilled water filter residue 3~5 times,
Desciccate is made；
(5) it will be uniformly mixed in above-mentioned desciccate and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask be placed in
Isothermal reaction in oil bath, reaction is placed on centrifugation in ultracentrifuge and obtains sediment, successively clear with dehydrated alcohol and distilled water
Wash 3~5 obtained reaction products；
(6) according to parts by weight, by 2~3 parts of spare modified-reaction objects, 3~5 parts of above-mentioned reaction products, 18~20 parts of adjacent benzene
It is mixed in diformazan dioctyl phthalate and 5~8 parts of γ-(methacryloxypropyl) propyl trimethoxy silicane investment two-dimensional mixing machines
Be made solidliquid mixture, according to parts by weight, by 8~10 parts of solidliquid mixtures, 4~6 parts of 6-caprolactones, 2~3 parts of paraffin, 3~
5 parts of calcium carbonate powders and 16~20 parts of polyethylene are sent into mixing granulator in dual-screw pelletizer after mixing, and high heat resistance is made
Highstrenghtpiston's masterbatch.
The mass fraction of 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution as described in step (1) is 12~15%, electricity
The DC voltage of pole is 50~60V, and supersonic oscillations frequency is 30~32kHz when electrolysis.
The mass fraction of sulfuric acid solution described in step (2) is 60~70%, in ice-water bath the isothermal reaction time be 30~
40min。
Temperature in reaction kettle described in step (3) is 35~40 DEG C, and speed of agitator is 200~240r/min, mixing
Mixing time is 30~40min.
The mass fraction of sodium hydroxide solution described in step (4) is 10~14%, the frequency of ultrasonic vibration instrument is 30~
32kHz, concussion time are 50~60min.
Oil bath temperature described in step (5) is 115~120 DEG C, and the isothermal reaction time is 60~70min in oil bath, is surpassed
The centrifugal rotational speed of fast centrifuge is 3900~4100r/min, and centrifugation time is 10~13min.
Mixing time in two-dimensional mixing machine described in step (6) is 30~40min.
The method have the benefit that:
(1) graphite rod is electrolysed by the present invention first, and electrolysate is aoxidized, after oxidation with kayexalate
It is reacted with sulfonated polyaniline and modified-reaction object is made, then pre-processed in alkaline solution using Poplar Powder as raw material, it will be pre-
Reaction product is made in the Poplar Powder of processing and benzyl chloride hybrid reaction, finally by modified-reaction object, reaction product, polymer and
It is granulated in other reagent raw materials mixing investment dual-screw pelletizers and high heat resistance highstrenghtpiston masterbatch is made, the present invention is by graphite rod
As the anode and cathode of electrode, cell reaction is carried out in glyoxaline ion liquid, electrolytically generated grapheme material passes through miaow
After azole ionic liquid carries out surface-active modification, structure, laminated structure are secured in the form of sheets for nano-graphene material generated
Stablize, can come into full contact with increasing specific surface area with polymer, increase dispersion effect, to increase connecing for graphene and polymer
Contacting surface product, improves reaction efficiency, while the relative molecular mass of kayexalate and sulfonated polyaniline is lower, and modification is made to receive
The relative molecular mass of rice graphene reduces, and effectively improves the dispersion effect of graphene, modified nano-graphene material tool
There is the chemical bondings energy such as ionic bond, covalent bond, graphene molecules are scattered in masterbatch, and filling connection is played in masterbatch molecule and is made
With bonding other molecules in masterbatch material is improved masterbatch molecule high temperature resistance and mechanical performance；
(2) present invention is modified it using benzyl chloride using Poplar Powder as raw material, has lignin and fiber in Poplar Powder
Element has the functional groups such as hydroxyl, carboxyl in lignin, effectively can form adhesive effect with molecules other in masterbatch, utilize chlorine
Change benzyl to Poplar Powder carry out it is Benzylation modified, in non-polar group is introduced in polar plant fiber, make lignin and
Plant fiber is preferably dissolved in polymer solution, improves the mechanical property, shock resistance and heat resistance of masterbatch, has
Wide application prospect.
Specific embodiment
The 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution that 400~500mL mass fraction is 12~15% is weighed to be put into
It is used as electrolyte in beaker, immerses 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution for graphite rod as the cathode and anode of electrode
In, it is 50~60V in DC voltage, under conditions of ultrasonic frequency is 30~32kHz, ultrasonic vibration, which is powered, is electrolysed 2~3h,
Graphite rod is taken out after electrolysis, product in beaker is filtered, and is obtained filter residue, is successively cleaned with dehydrated alcohol and distilled water
Filter residue 4~8 times, electrolysate is made；According to parts by weight, 3~5 parts of above-mentioned electrolysates, 2.0~2.8 parts of ferric acid are weighed
In the sulfuric acid solution mixing investment beaker that potassium and 16~18 parts of mass fractions are 60~70%, place the beaker in ice-water bath, constant temperature
30~40min is reacted, filter cake is obtained by filtration after reaction, filter cake 3~5 times, spare wash with distilled water；According to parts by weight, claim
Take 3~5 parts of above-mentioned filter cakes, 4~5 parts of kayexalates, 8~9 parts of sulfonated polyanilines and 16~20 parts of acetone investment reactions
It is mixed in kettle, is 35~40 DEG C in temperature, 30~40min system is mixed under conditions of being 200~240r/min in speed of agitator
Mixed emulsion is obtained, the carbic anhydride of mixed emulsion quality 5~8% is added dropwise into reaction kettle, is passed through hydrogen after completion of dropwise addition
Modified filter residue is obtained by filtration in 1~2h, and modified filter residue is successively used dehydrated alcohol and distillation water washing 3~5 times, is put into baking oven
It dries and modified-reaction object is made, it is spare；The sodium hydroxide solution 1:10 in mass ratio for being 10~14% by Poplar Powder and mass fraction
Be stirred investment beaker in, place the beaker in ultrasonic vibration instrument, frequency be 30~32kHz under conditions of concussion 50~
60min is filtered to obtain filter residue after concussion, is put into baking oven and is dried after being washed with distilled water filter residue 3~5 times, is made
Desciccate；It will be uniformly mixed in above-mentioned desciccate and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask set
It is after 60~70min of isothermal reaction, to be placed in ultracentrifuge and be in 115~120 DEG C of oil bath in temperature in centrifugal rotational speed
It is centrifuged 10~13min under conditions of 3900~4100r/min, obtains sediment, successively 3 are cleaned with dehydrated alcohol and distilled water~
5 obtained reaction products；According to parts by weight, by 2~3 parts of spare modified-reaction objects, 3~5 parts of above-mentioned reaction products, 18~
20 parts of dioctyl phthalates and 5~8 parts of γ-(methacryloxypropyl) propyl trimethoxy silicanes put into two-dimensional mixing machine
In, 30~40min is mixed, solidliquid mixture is made, according to parts by weight, by 8~10 parts of solidliquid mixtures, 4~6 parts of ε-
Caprolactone, 2~3 parts of paraffin, 3~5 parts of calcium carbonate powders and 16~20 parts of polyethylene are sent into dual-screw pelletizer after mixing
High heat resistance highstrenghtpiston masterbatch is made in middle mixing granulator.
It weighs the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution that 400mL mass fraction is 12% and is put into conduct in beaker
Electrolyte immerses graphite rod as the cathode and anode of electrode in 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution, in direct current
Piezoelectric voltage is 50V, and under conditions of ultrasonic frequency is 30kHz, ultrasonic vibration, which is powered, is electrolysed 2h, takes out graphite after electrolysis
Product in beaker is filtered by stick, obtains filter residue, is successively cleaned filter residue 4 times with dehydrated alcohol and distilled water, and electrolysis is made and produces
Object；According to parts by weight, it is molten to weigh the sulfuric acid that 3 parts of above-mentioned electrolysates, 2.0 parts of potassium ferrates and 16 parts of mass fractions are 60%
In liquid mixing investment beaker, place the beaker in ice-water bath, isothermal reaction 30min is obtained by filtration filter cake after reaction, uses distilled water
Cleaning filter cake 3 times, it is spare；According to parts by weight, 3 parts of above-mentioned filter cakes, 4 parts of kayexalates, 8 parts of sulfonated polyanilines are weighed
It is mixed in 16 parts of acetone investment reaction kettles, is 35 DEG C in temperature, speed of agitator is mixed under conditions of being 200r/min
Mixed emulsion is made in 30min, and the carbic anhydride of mixed emulsion quality 5% is added dropwise into reaction kettle, is passed through after completion of dropwise addition
Modified filter residue is obtained by filtration in hydrogen 1h, and modified filter residue is successively used dehydrated alcohol and distillation water washing 3 times, is put into baking oven and dries
Drying modified-reaction object, it is spare；The sodium hydroxide solution 1:10 in mass ratio stirring for being 10% by Poplar Powder and mass fraction is mixed
It closes in investment beaker, places the beaker in ultrasonic vibration instrument, 50min is shaken under conditions of frequency is 30kHz, after concussion
It is filtered to obtain filter residue, is put into baking oven and dries after being washed with distilled water filter residue 3 times, desciccate is made；By above-mentioned drying
It is uniformly mixed in product and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask is placed in the oil bath that temperature is 115 DEG C
In, after isothermal reaction 60min, it is placed in ultracentrifuge and is centrifuged 10min under conditions of centrifugal rotational speed is 3900r/min, obtain
To sediment, 3 obtained reaction products successively are cleaned with dehydrated alcohol and distilled water；According to parts by weight, 2 parts spare are changed
Property reactant, 3 parts of above-mentioned reaction products, 18 parts of dioctyl phthalates and 5 parts of γ-(methacryloxypropyl) propyl trimethoxies
Base silane is put into two-dimensional mixing machine, and 30min is mixed, and solidliquid mixture is made and according to parts by weight mixes 8 parts of solid-liquids
It closes object, 4 parts of 6-caprolactones, 2 parts of paraffin, 3 parts of calcium carbonate powders and 16 parts of polyethylene and is sent into dual-screw pelletizer after mixing
High heat resistance highstrenghtpiston masterbatch is made in middle mixing granulator.
It weighs the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution that 450mL mass fraction is 13% and is put into conduct in beaker
Electrolyte immerses graphite rod as the cathode and anode of electrode in 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution, in direct current
Piezoelectric voltage is 55V, and under conditions of ultrasonic frequency is 31kHz, ultrasonic vibration, which is powered, is electrolysed 2h, takes out graphite after electrolysis
Product in beaker is filtered by stick, obtains filter residue, is successively cleaned filter residue 6 times with dehydrated alcohol and distilled water, and electrolysis is made and produces
Object；According to parts by weight, it is molten to weigh the sulfuric acid that 4 parts of above-mentioned electrolysates, 2.4 parts of potassium ferrates and 17 parts of mass fractions are 65%
In liquid mixing investment beaker, place the beaker in ice-water bath, isothermal reaction 35min is obtained by filtration filter cake after reaction, uses distilled water
Cleaning filter cake 4 times, it is spare；According to parts by weight, 4 parts of above-mentioned filter cakes, 4 parts of kayexalates, 8 parts of sulfonated polyanilines are weighed
It is mixed in 18 parts of acetone investment reaction kettles, is 37 DEG C in temperature, speed of agitator is mixed under conditions of being 220r/min
Mixed emulsion is made in 35min, and the carbic anhydride of mixed emulsion quality 7% is added dropwise into reaction kettle, is passed through after completion of dropwise addition
Modified filter residue is obtained by filtration in hydrogen 1h, and modified filter residue is successively used dehydrated alcohol and distillation water washing 4 times, is put into baking oven and dries
Drying modified-reaction object, it is spare；The sodium hydroxide solution 1:10 in mass ratio stirring for being 12% by Poplar Powder and mass fraction is mixed
It closes in investment beaker, places the beaker in ultrasonic vibration instrument, 55min is shaken under conditions of frequency is 31kHz, after concussion
It is filtered to obtain filter residue, is put into baking oven and dries after being washed with distilled water filter residue 4 times, desciccate is made；By above-mentioned drying
It is uniformly mixed in product and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask is placed in the oil bath that temperature is 117 DEG C
In, after isothermal reaction 65min, it is placed in ultracentrifuge and is centrifuged 12min under conditions of centrifugal rotational speed is 4000r/min, obtain
To sediment, 4 obtained reaction products successively are cleaned with dehydrated alcohol and distilled water；According to parts by weight, 2 parts spare are changed
Property reactant, 4 parts of above-mentioned reaction products, 19 parts of dioctyl phthalates and 6 parts of γ-(methacryloxypropyl) propyl trimethoxies
Base silane is put into two-dimensional mixing machine, and 35min is mixed, and solidliquid mixture is made and according to parts by weight mixes 9 parts of solid-liquids
It closes object, 5 parts of 6-caprolactones, 2 parts of paraffin, 4 parts of calcium carbonate powders and 18 parts of polyethylene and is sent into dual-screw pelletizer after mixing
High heat resistance highstrenghtpiston masterbatch is made in middle mixing granulator.
It weighs the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution that 500mL mass fraction is 15% and is put into conduct in beaker
Electrolyte immerses graphite rod as the cathode and anode of electrode in 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution, in direct current
Piezoelectric voltage is 60V, and under conditions of ultrasonic frequency is 32kHz, ultrasonic vibration, which is powered, is electrolysed 3h, takes out graphite after electrolysis
Product in beaker is filtered by stick, obtains filter residue, is successively cleaned filter residue 8 times with dehydrated alcohol and distilled water, and electrolysis is made and produces
Object；According to parts by weight, it is molten to weigh the sulfuric acid that 5 parts of above-mentioned electrolysates, 2.8 parts of potassium ferrates and 18 parts of mass fractions are 70%
In liquid mixing investment beaker, place the beaker in ice-water bath, isothermal reaction 40min is obtained by filtration filter cake after reaction, uses distilled water
Cleaning filter cake 5 times, it is spare；According to parts by weight, 5 parts of above-mentioned filter cakes, 5 parts of kayexalates, 9 parts of sulfonated polyanilines are weighed
It is mixed in 20 parts of acetone investment reaction kettles, is 40 DEG C in temperature, speed of agitator is mixed under conditions of being 240r/min
Mixed emulsion is made in 40min, and the carbic anhydride of mixed emulsion quality 8% is added dropwise into reaction kettle, is passed through after completion of dropwise addition
Modified filter residue is obtained by filtration in hydrogen 2h, and modified filter residue is successively used dehydrated alcohol and distillation water washing 5 times, is put into baking oven and dries
Drying modified-reaction object, it is spare；The sodium hydroxide solution 1:10 in mass ratio stirring for being 14% by Poplar Powder and mass fraction is mixed
It closes in investment beaker, places the beaker in ultrasonic vibration instrument, 60min is shaken under conditions of frequency is 32kHz, after concussion
It is filtered to obtain filter residue, is put into baking oven and dries after being washed with distilled water filter residue 5 times, desciccate is made；By above-mentioned drying
It is uniformly mixed in product and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask is placed in the oil bath that temperature is 120 DEG C
In, after isothermal reaction 70min, it is placed in ultracentrifuge and is centrifuged 13min under conditions of centrifugal rotational speed is 4100r/min, obtain
To sediment, 5 obtained reaction products successively are cleaned with dehydrated alcohol and distilled water；According to parts by weight, 3 parts spare are changed
Property reactant, 5 parts of above-mentioned reaction products, 20 parts of dioctyl phthalates and 8 parts of γ-(methacryloxypropyl) propyl trimethoxies
Base silane is put into two-dimensional mixing machine, and 40min is mixed, and solidliquid mixture is made and according to parts by weight mixes 10 parts of solid-liquids
It closes object, 6 parts of 6-caprolactones, 3 parts of paraffin, 5 parts of calcium carbonate powders and 20 parts of polyethylene and is sent into dual-screw pelletizer after mixing
High heat resistance highstrenghtpiston masterbatch is made in middle mixing granulator.
Comparative example is high-strength to high heat resistance produced by the present invention as a comparison case with the plastic matrix that company of Jinan City produces
Plastic matrix in degree plastic matrix and comparative example is detected through tabletting machine molding, and testing result is as shown in table 1:
Mechanics Performance Testing
It is tested using mechanical property tester.
Water resistance test is tested according to standard GB/T1034-2008, by high heat resistance high-strength plastic produced by the present invention
Plastic master tablet in material masterbatch piece and comparative example is divided into 4 groups, every group of 3 samples (50 × 50mm), 1h or 50 DEG C at 100 DEG C
Lower drying for 24 hours, weighs each sample (being accurate to 1mg), it is determined as m1.Then sample is immersed to the container for filling distilled water, water temperature
25 DEG C, for 24 hours after, sample is taken out from water and sucks the water on surface with clean dry cloth or filter paper, sample in taking-up 2min again
It weighs (quality m0), calculates to obtain water absorption rate.
Heat-resisting quantity test is simultaneously by the plastics in high heat resistance highstrenghtpiston masterbatch piece produced by the present invention and comparative example
Masterbatch piece is placed in the environment of temperature is 120 DEG C after 3h, observes sample.
1 performance measurement result of table
According to data in table 1 it is found that high heat resistance highstrenghtpiston masterbatch produced by the present invention, has intensity high, mechanical property is good,
The features such as heat-resisting ability is strong, and water-tolerant, will not generate pollution to environment, and excellent combination property has wide use
Prospect.
Claims (7)
1. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch, it is characterised in that specific preparation step are as follows:
(1) the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution for weighing 400~500mL is put into beaker as electrolyte, will
Graphite rod immerses in 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution as the cathode and anode of electrode, in the item of supersonic oscillations
Be powered 2~3h of electrolysis under part, takes out graphite rod after electrolysis, product in beaker is filtered, obtain filter residue, successively use nothing
Water-ethanol and distilled water clean filter residue 4~8 times, and electrolysate is made；
(2) according to parts by weight, it is molten that 3~5 parts of above-mentioned electrolysates, 2.0~2.8 parts of potassium ferrates and 16~18 parts of sulfuric acid are weighed
In liquid mixing investment beaker, isothermal reaction in ice-water bath is placed the beaker, filter cake is obtained by filtration after reaction, filters wash with distilled water
It is cake 3~5 times, spare；
(3) according to parts by weight, 3~5 parts of above-mentioned filter cakes, 4~5 parts of kayexalates, 8~9 parts of sulfonated polyanilines are weighed
It is mixed to prepare mixed emulsion in 16~20 parts of acetone investment reaction kettles, mixed emulsion quality 5~8% is added dropwise into reaction kettle
Carbic anhydride is passed through 1~2h of hydrogen after completion of dropwise addition, modified filter residue is obtained by filtration, and modified filter residue is successively used anhydrous
Ethyl alcohol and distillation water washing 3~5 times are put into baking oven and dry obtained modified-reaction object, spare；
(4) Poplar Powder and sodium hydroxide solution 1:10 in mass ratio are stirred in investment beaker, place the beaker ultrasonic shake
It swings in instrument and shakes, filtered to obtain filter residue after concussion, be put into baking oven and dry after being washed with distilled water filter residue 3~5 times,
Desciccate is made；
(5) it will be uniformly mixed in above-mentioned desciccate and benzyl chloride 1:5 in mass ratio investment single-necked flask, single-necked flask be placed in
Isothermal reaction in oil bath, reaction is placed on centrifugation in ultracentrifuge and obtains sediment, successively clear with dehydrated alcohol and distilled water
Wash 3~5 obtained reaction products；
(6) according to parts by weight, by 2~3 parts of spare modified-reaction objects, 3~5 parts of above-mentioned reaction products, 18~20 parts of adjacent benzene
It is mixed in diformazan dioctyl phthalate and 5~8 parts of γ-(methacryloxypropyl) propyl trimethoxy silicane investment two-dimensional mixing machines
Be made solidliquid mixture, according to parts by weight, by 8~10 parts of solidliquid mixtures, 4~6 parts of 6-caprolactones, 2~3 parts of paraffin, 3~
5 parts of calcium carbonate powders and 16~20 parts of polyethylene are sent into mixing granulator in dual-screw pelletizer after mixing, and high heat resistance is made
Highstrenghtpiston's masterbatch.
2. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(1) mass fraction of the 1- ethyl-3-methylimidazole tetrafluoro boric acid sodium solution described in is 12~15%, the direct current electricity of electrode
Pressure is 50~60V, and supersonic oscillations frequency is 30~32kHz when electrolysis.
3. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(2) mass fraction of the sulfuric acid solution described in is 60~70%, and the isothermal reaction time is 30~40min in ice-water bath.
4. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(3) temperature in reaction kettle described in is 35~40 DEG C, and speed of agitator is 200~240r/min, mixing time 30
~40min.
5. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(4) mass fraction of the sodium hydroxide solution described in is 10~14%, and the frequency of ultrasonic vibration instrument is 30~32kHz, when concussion
Between be 50~60min.
6. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(5) oil bath temperature described in is 115~120 DEG C, and the isothermal reaction time is 60~70min in oil bath, ultracentrifuge from
Heart revolving speed is 3900~4100r/min, and centrifugation time is 10~13min.
7. a kind of preparation method of high heat resistance highstrenghtpiston masterbatch according to claim 1, it is characterised in that: step
(6) mixing time in two-dimensional mixing machine described in is 30~40min.
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| CN116162312A (en) * | 2022-12-26 | 2023-05-26 | 湖南工业职业技术学院 | High polymer material wear-resistant concrete conveying pipeline |
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