CN109265874A - The preparation method of high-intensitive resistance to combustion Corvic material - Google Patents
The preparation method of high-intensitive resistance to combustion Corvic material Download PDFInfo
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- CN109265874A CN109265874A CN201811144985.XA CN201811144985A CN109265874A CN 109265874 A CN109265874 A CN 109265874A CN 201811144985 A CN201811144985 A CN 201811144985A CN 109265874 A CN109265874 A CN 109265874A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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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
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a kind of preparation methods of the resistance to combustion Corvic material of high intensity, include the following steps: to prepare carbon nano tube dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanotube；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and nano hydrotalcite, obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Resistance to combustion component, calcium stearate, epoxidized soybean oil and triacetyl glycerine are mixed, the second mixture is obtained；High-speed stirred is carried out to the second mixture, obtains third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；And hot pressing and cold pressing are carried out to the Corvic sheet material after mill.
Description
Technical field
The present invention relates to high performance plastics technical fields, especially with regard to a kind of resistance to combustion Corvic material of high intensity
The preparation method of material.
Background technique
PVC product is divided into hard PVC and flexible PVC.Often contain about 10-15 parts of additive in every 100 parts of hard PVC,
Stabilizer, processing aid, anti-impact modifier, lubricant comprising 0.1-2% and for reducing the filler of cost.Flexible PVC
Often containing 40-60 parts of additive in every 100 parts, comprising the maximum plasticizer of component content, heat stabilizer, lubricant, filler,
Fire retardant etc..The performance of PVC product depend on the factors such as structure, molecular weight of resin itself and be added product auxiliary formula and
Its dosage.PVC has excellent processability and good mechanical performance, and fabricated product is easier to meet the need for product on the market
It asks.Polyvinyl chloride resin has excellent anti-flammability, smoke-suppressing, and limit oxygen index is up to 50-60%, and chemical stability is good, Ke Yinai
Sulfuric acid and concentration by hydrochloric acid, concentration lower than 90% are lower than 60% nitric acid and alkali, while its from a wealth of sources and side of synthesis
Method is simple, and price is also very cheap, therefore produces in enormous quantities and use.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The purpose of the present invention is to provide a kind of high intensity it is resistance to combustion Corvic material preparation method, can gram
Take the defect of the prior art.
To achieve the above object, the present invention provides a kind of high intensity it is resistance to combustion Corvic material preparation method,
Include the following steps: to prepare carbon nano tube dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；To being taken
The solid carbon nanotube obtained is dried；Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out first
Ball milling obtains modified solid carbon nanotube；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chlorinated polyvinyl chloride
Ethylene powder, polyvinyl chloride powder and nano hydrotalcite obtain the first mixture；Second ball milling is carried out to the first mixture,
Obtain resistance to combustion component；Resistance to combustion component, calcium stearate, epoxidized soybean oil and triacetyl glycerine are mixed, the second mixture is obtained；
High-speed stirred is carried out to the second mixture, obtains third mixture；Mill is carried out to third mixture, the polychlorostyrene after obtaining mill
Vinyl sheet material；And hot pressing and cold pressing are carried out to the Corvic sheet material after mill, it is poly- to obtain high-intensitive resistance to combustion
Vinyl chloride resin material.
In a preferred embodiment, carbon nano tube dispersion liquid is prepared to specifically comprise the following steps: carbon nanotube original
Material is put into silane coupler solution, wherein silane coupler solution concentration is 10-15wt%；To the silane of carbon nanotube
Coupling agent mixed liquor is stirred by ultrasonic, wherein ultrasonic agitation power is 400-500W, and the ultrasonic agitation time is 2-4h；It uses
Mixed liquor after microwave irradiation ultrasonic agitation, microwave power 100-150W, irradiation time 20-40s.
In a preferred embodiment, acquired solid carbon nanotube is dried specifically comprises the processes of: dry
Temperature is 70-80 DEG C, drying time 30-50h.
In a preferred embodiment, the mass ratio of the solid carbon nanotube after drying and four ammonia of triethylene is (50-
100): 1, the design parameter of the first ball milling are as follows: Ball-milling Time 10-20h, drum's speed of rotation 1000-1200rpm, ball milling temperature
Degree is 50-70 DEG C, and ratio of grinding media to material is (10-20): 1.
In a preferred embodiment, in the first mixture, in parts by weight, modified solid carbon nanotube is accounted for
10-20 parts, dibutyl tin dilaurate account for 3-7 parts, chliorinated polyvinyl chloride powder account for 20-40 parts, polyvinyl chloride powder account for 100-
150 parts and nano hydrotalcite account for 2-5 parts.
In a preferred embodiment, the design parameter of the second ball milling is carried out to the first mixture are as follows: Ball-milling Time is
10-20h, drum's speed of rotation 1300-1500rpm, ball milling temperature are 50-70 DEG C, and ratio of grinding media to material is (20-25): 1.
In a preferred embodiment, in the first mixture, in parts by weight, resistance to combustion component account for 100-150 parts, it is hard
Resin acid calcium accounts for 1-1.2 parts, epoxidized soybean oil accounts for 3-6 parts and triacetyl glycerine accounts for 1-2 parts.
In a preferred embodiment, the design parameter of high-speed stirred is carried out to the second mixture are as follows: whipping temp is
60-80 DEG C, blender revolving speed is 400-800rpm, mixing time 10-20min.
In a preferred embodiment, the design parameter of mill is carried out to third mixture are as follows: open mill temperature is
185-190 DEG C, the mill time is 10-20min, the Corvic sheet material after mill with a thickness of 2-4mm.
In a preferred embodiment, the specific of hot pressing and cold pressing is carried out to the Corvic sheet material after mill
Parameter are as follows: hot pressing temperature is 170-180 DEG C, hot pressing pressure 5-10MPa, and the sheet thickness after hot pressing is 0.5-1mm, cold pressing
Temperature is 30-50 DEG C, cold pressing pressure 3-6MPa.
Compared with prior art, the preparation method of the resistance to combustion Corvic material of high intensity of the invention has following excellent
Point: polyvinyl chloride is a kind of very outstanding resin material, but polyvinyl chloride still has some aspects to be improved, example
Such as the application for meeting some special occasions, the limit oxygen index of the polyvinyl chloride of public offering currently on the market still compared with
Low, tensile strength is lower, will occur at a lower temperature it is significant weightless (this explanation in burning, current polyvinyl chloride material
Material will release a large amount of poisonous and harmful substance), this causes the applicable situation of polyvinyl chloride to be limited by very large.At present
The prior art proposes the hybrid resin system for mixing chliorinated polyvinyl chloride with polyvinyl chloride, this resin system heat resistance compared with
Well, mechanical property is also good.But chliorinated polyvinyl chloride price be higher than polyvinyl chloride, for annual capacity reach it is millions of so that
For tens million of large chemical plants, a large amount of cost allowances that may cause hundreds of thousands of members using chliorinated polyvinyl chloride.For
Problem of the prior art, it is of the invention the invention proposes a kind of preparation method of the novel Corvic of resistance to combustion material
Method reduces the dosage of chliorinated polyvinyl chloride, reduces production cost, and the present invention develops further increase polychlorostyrene second simultaneously
The method of alkene material thermal resistance and mechanical property.The modified polyvinyl chloride mechanical property prepared using preparation method of the invention
Good, heat resistance is high, while thermal weight loss is less at high temperature, and use is very safe, can satisfy the application of a variety of occasions.
Detailed description of the invention
Fig. 1 is the method flow diagram of the preparation method of the resistance to combustion Corvic material of high intensity according to the present invention.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change
Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members
Part or other component parts.
Fig. 1 is the method flow diagram of the preparation method of the resistance to combustion Corvic material of high intensity according to the present invention.Such as
Shown in figure, preparation method of the invention includes the following steps:
Step 101: preparing carbon nano tube dispersion liquid；
Step 102: solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；
Step 103: acquired solid carbon nanotube is dried；
Step 104: the solid carbon nanotube after drying being mixed with four ammonia of triethylene, and carries out the first ball milling, is obtained
Modified solid carbon nanotube；
Step 105: mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polychlorostyrene
Ethylene powder and nano hydrotalcite obtain the first mixture；
Step 106: the second ball milling being carried out to the first mixture, obtains resistance to combustion component；
Step 107: the resistance to combustion component of mixing, calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixing
Object；
Step 108: high-speed stirred being carried out to the second mixture, obtains third mixture；
Step 109: mill being carried out to third mixture, the Corvic sheet material after obtaining mill；And
Step 110: hot pressing and cold pressing being carried out to the Corvic sheet material after mill, obtain high-intensitive resistance to combustion polychlorostyrene
Vinyl resinous material.
Embodiment 1
The preparation method of the resistance to combustion Corvic material of high intensity of the invention includes the following steps: to prepare carbon nanotube
Dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanometer
Pipe；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and
Nano hydrotalcite obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Mix resistance to combustion component,
Calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；To poly- after mill
Vinyl chloride resin sheet material carries out hot pressing and cold pressing, obtains high-intensitive resistance to combustion Corvic material.Prepare carbon nanotube point
Dispersion liquid specifically comprises the following steps: for carbon nanotube raw material to be put into silane coupler solution, wherein silane coupler solution
Concentration is 10wt%；The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein power, which is stirred by ultrasonic, is
400W, ultrasonic agitation time are 2h；Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 100W, irradiation time
Acquired solid carbon nanotube is dried for 20s specifically comprises the processes of: drying temperature is 70 DEG C, drying time 30h
The mass ratio of solid carbon nanotube and four ammonia of triethylene after drying is 50:1, the design parameter of the first ball milling are as follows: when ball milling
Between be 10h, drum's speed of rotation 1000rpm, ball milling temperature be 50 DEG C, ratio of grinding media to material be 10:1 in the first mixture, with weight
Part meter, modified solid carbon nanotube account for 10 parts, dibutyl tin dilaurate account for 3 parts, chliorinated polyvinyl chloride powder account for 20 parts, it is poly-
Vinyl chloride powder accounts for 100 parts and nano hydrotalcite accounts for 2 parts of design parameters that the second ball milling is carried out to the first mixture are as follows: ball milling
Time is 10h, and drum's speed of rotation 1300rpm, ball milling temperature is 50 DEG C, and ratio of grinding media to material is 20:1 in the first mixture, with weight
Measure part meter, resistance to combustion component accounts for 100 parts, calcium stearate accounts for 1 part, epoxidized soybean oil accounts for 3 parts and triacetyl glycerine accounts for 1 part to the
The design parameter of two mixtures progress high-speed stirred are as follows: whipping temp is 60 DEG C, and blender revolving speed is 400rpm, and mixing time is
10min carries out the design parameter of mill to third mixture are as follows: open mill temperature is 185 DEG C, and the mill time is 10min, mill
The tool for carrying out hot pressing and cold pressing to the Corvic sheet material after mill with a thickness of 2mm of Corvic sheet material afterwards
Body parameter are as follows: hot pressing temperature is 170 DEG C, hot pressing pressure 5MPa, and the sheet thickness after hot pressing is 0.5mm, and temperature of colding pressing is
30 DEG C, cold pressing pressure 3MPa.
Embodiment 2
The preparation method of the resistance to combustion Corvic material of high intensity of the invention includes the following steps: to prepare carbon nanotube
Dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanometer
Pipe；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and
Nano hydrotalcite obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Mix resistance to combustion component,
Calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；To poly- after mill
Vinyl chloride resin sheet material carries out hot pressing and cold pressing, obtains high-intensitive resistance to combustion Corvic material.Prepare carbon nanotube point
Dispersion liquid specifically comprises the following steps: for carbon nanotube raw material to be put into silane coupler solution, wherein silane coupler solution
Concentration is 15wt%；The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein power, which is stirred by ultrasonic, is
500W, ultrasonic agitation time are 4h；Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 150W, irradiation time
Acquired solid carbon nanotube is dried for 40s specifically comprises the processes of: drying temperature is 80 DEG C, drying time 50h
The mass ratio of solid carbon nanotube and four ammonia of triethylene after drying is 100:1, the design parameter of the first ball milling are as follows: when ball milling
Between be 20h, drum's speed of rotation 1200rpm, ball milling temperature be 70 DEG C, ratio of grinding media to material be 20:1 in the first mixture, with weight
Part meter, modified solid carbon nanotube account for 20 parts, dibutyl tin dilaurate account for 7 parts, chliorinated polyvinyl chloride powder account for 40 parts, it is poly-
Vinyl chloride powder accounts for 150 parts and nano hydrotalcite accounts for 5 parts of design parameters that the second ball milling is carried out to the first mixture are as follows: ball milling
Time is 20h, and drum's speed of rotation 1500rpm, ball milling temperature is 70 DEG C, and ratio of grinding media to material is 25:1 in the first mixture, with weight
Measure part meter, resistance to combustion component account for 150 parts, calcium stearate account for 1.2 parts, epoxidized soybean oil account for 6 parts and triacetyl glycerine account for 2 parts it is right
The design parameter of second mixture progress high-speed stirred are as follows: whipping temp is 80 DEG C, and blender revolving speed is 800rpm, mixing time
The design parameter of mill is carried out to third mixture for 20min are as follows: open mill temperature is 190 DEG C, and the mill time is 20min, is opened
Corvic sheet material after refining carries out hot pressing and cold pressing to the Corvic sheet material after mill with a thickness of 4mm
Design parameter are as follows: hot pressing temperature is 180 DEG C, hot pressing pressure 10MPa, and the sheet thickness after hot pressing is 1mm, and temperature of colding pressing is
50 DEG C, cold pressing pressure 6MPa.
Embodiment 3
The preparation method of the resistance to combustion Corvic material of high intensity of the invention includes the following steps: to prepare carbon nanotube
Dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanometer
Pipe；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and
Nano hydrotalcite obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Mix resistance to combustion component,
Calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；To poly- after mill
Vinyl chloride resin sheet material carries out hot pressing and cold pressing, obtains high-intensitive resistance to combustion Corvic material.Prepare carbon nanotube point
Dispersion liquid specifically comprises the following steps: for carbon nanotube raw material to be put into silane coupler solution, wherein silane coupler solution
Concentration is 11wt%；The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein power, which is stirred by ultrasonic, is
420W, ultrasonic agitation time are 2.5h；Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 110W, when irradiation
Between acquired solid carbon nanotube is dried for 25s specifically comprises the processes of: drying temperature is 75 DEG C, and drying time is
The mass ratio of solid carbon nanotube and four ammonia of triethylene after 35h is dry is 70:1, the design parameter of the first ball milling are as follows: ball milling
Time is 12h, and drum's speed of rotation 1050rpm, ball milling temperature is 55 DEG C, and ratio of grinding media to material is 12:1 in the first mixture, with weight
Measure part meter, modified solid carbon nanotube account for 12 parts, dibutyl tin dilaurate account for 4 parts, chliorinated polyvinyl chloride powder account for 25 parts,
Polyvinyl chloride powder accounts for 110 parts and nano hydrotalcite accounts for 3 parts of design parameters that the second ball milling is carried out to the first mixture are as follows: ball
Time consuming is 12h, and drum's speed of rotation 1350rpm, ball milling temperature is 55 DEG C, and ratio of grinding media to material is 21:1 in the first mixture, with
Parts by weight meter, resistance to combustion component accounts for 110 parts, calcium stearate accounts for 1.1 parts, epoxidized soybean oil accounts for 4 parts and triacetyl glycerine accounts for 1.5
Part carries out the design parameter of high-speed stirred to the second mixture are as follows: whipping temp is 65 DEG C, and blender revolving speed is 500rpm, stirring
Time is the design parameter that 12min carries out mill to third mixture are as follows: open mill temperature is 187 DEG C, and the mill time is
15min, Corvic sheet material after mill with a thickness of 3mm to the Corvic sheet material after mill carry out hot pressing with
And the design parameter of cold pressing are as follows: hot pressing temperature is 172 DEG C, hot pressing pressure 7MPa, and the sheet thickness after hot pressing is 0.6mm,
Temperature of colding pressing is 35 DEG C, cold pressing pressure 4MPa.
Embodiment 4
The preparation method of the resistance to combustion Corvic material of high intensity of the invention includes the following steps: to prepare carbon nanotube
Dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanometer
Pipe；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and
Nano hydrotalcite obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Mix resistance to combustion component,
Calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；To poly- after mill
Vinyl chloride resin sheet material carries out hot pressing and cold pressing, obtains high-intensitive resistance to combustion Corvic material.Prepare carbon nanotube point
Dispersion liquid specifically comprises the following steps: for carbon nanotube raw material to be put into silane coupler solution, wherein silane coupler solution
Concentration is 13wt%；The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein power, which is stirred by ultrasonic, is
450W, ultrasonic agitation time are 3h；Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 130W, irradiation time
Acquired solid carbon nanotube is dried for 30s specifically comprises the processes of: drying temperature is 75 DEG C, drying time 40h
The mass ratio of solid carbon nanotube and four ammonia of triethylene after drying is 80:1, the design parameter of the first ball milling are as follows: when ball milling
Between be 15h, drum's speed of rotation 1100rpm, ball milling temperature be 60 DEG C, ratio of grinding media to material be 15:1 in the first mixture, with weight
Part meter, modified solid carbon nanotube account for 15 parts, dibutyl tin dilaurate account for 5 parts, chliorinated polyvinyl chloride powder account for 30 parts, it is poly-
Vinyl chloride powder accounts for 130 parts and nano hydrotalcite accounts for 4 parts of design parameters that the second ball milling is carried out to the first mixture are as follows: ball milling
Time is 15h, and drum's speed of rotation 1400rpm, ball milling temperature is 60 DEG C, and ratio of grinding media to material is 22:1 in the first mixture, with weight
Part meter is measured, resistance to combustion component accounts for 130 parts, calcium stearate accounts for 1.1 parts, epoxidized soybean oil accounts for 4 parts and triacetyl glycerine accounts for 1.5 parts
The design parameter of high-speed stirred is carried out to the second mixture are as follows: whipping temp is 70 DEG C, and blender revolving speed is 600rpm, when stirring
Between for 15min to third mixture carry out mill design parameter are as follows: open mill temperature be 188 DEG C, the mill time be 15min,
Corvic sheet material after mill carries out hot pressing and cold pressing to the Corvic sheet material after mill with a thickness of 3mm
Design parameter are as follows: hot pressing temperature is 175 DEG C, hot pressing pressure 7MPa, and sheet thickness after hot pressing is 0.8mm, cold pressing temperature
Degree is 40 DEG C, cold pressing pressure 5MPa.
Embodiment 5
The preparation method of the resistance to combustion Corvic material of high intensity of the invention includes the following steps: to prepare carbon nanotube
Dispersion liquid；Solid carbon nanotube is filtered to take to obtain from carbon nano tube dispersion liquid；Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon nanometer
Pipe；Mixed and modified solid carbon nanotube, dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder and
Nano hydrotalcite obtains the first mixture；Second ball milling is carried out to the first mixture, obtains resistance to combustion component；Mix resistance to combustion component,
Calcium stearate, epoxidized soybean oil and triacetyl glycerine obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain third mixture；Mill is carried out to third mixture, the Corvic sheet material after obtaining mill；To poly- after mill
Vinyl chloride resin sheet material carries out hot pressing and cold pressing, obtains high-intensitive resistance to combustion Corvic material.Prepare carbon nanotube point
Dispersion liquid specifically comprises the following steps: for carbon nanotube raw material to be put into silane coupler solution, wherein silane coupler solution
Concentration is 14wt%；The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein power, which is stirred by ultrasonic, is
450W, ultrasonic agitation time are 3.5h；Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 140W, when irradiation
Between acquired solid carbon nanotube is dried for 35s specifically comprises the processes of: drying temperature is 75 DEG C, and drying time is
The mass ratio of solid carbon nanotube and four ammonia of triethylene after 45h is dry is 90:1, the design parameter of the first ball milling are as follows: ball milling
Time is 18h, and drum's speed of rotation 1150rpm, ball milling temperature is 65 DEG C, and ratio of grinding media to material is 18:1 in the first mixture, with weight
Measure part meter, modified solid carbon nanotube account for 18 parts, dibutyl tin dilaurate account for 6 parts, chliorinated polyvinyl chloride powder account for 35 parts,
Polyvinyl chloride powder accounts for 140 parts and nano hydrotalcite accounts for 4 parts of design parameters that the second ball milling is carried out to the first mixture are as follows: ball
Time consuming is 18h, and drum's speed of rotation 1450rpm, ball milling temperature is 65 DEG C, and ratio of grinding media to material is 24:1 in the first mixture, with
Parts by weight meter, resistance to combustion component accounts for 140 parts, calcium stearate accounts for 1.1 parts, epoxidized soybean oil accounts for 5 parts and triacetyl glycerine accounts for 1.5
Part carries out the design parameter of high-speed stirred to the second mixture are as follows: whipping temp is 75 DEG C, and blender revolving speed is 700rpm, stirring
Time is the design parameter that 18min carries out mill to third mixture are as follows: open mill temperature is 188 DEG C, and the mill time is
18min, Corvic sheet material after mill carry out hot pressing to the Corvic sheet material after mill with a thickness of 3.5mm
And the design parameter of cold pressing are as follows: hot pressing temperature is 178 DEG C, hot pressing pressure 9MPa, and the sheet thickness after hot pressing is
0.9mm, temperature of colding pressing are 45 DEG C, cold pressing pressure 5MPa.
Comparative example 1
Difference from example 1 is that: it does not include step " by the solid carbon nanotube and triethylene four after drying
Ammonia mixing, and carry out the first ball milling ".
Comparative example 2
Difference from example 1 is that: mixed and modified solid carbon nanotube, chliorinated polyvinyl chloride powder, polychlorostyrene
Ethylene powder and nano hydrotalcite obtain the first mixture.
Comparative example 3
Difference from example 1 is that: the silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic,
In, ultrasonic agitation power is 200W, and the ultrasonic agitation time is 1h.
Comparative example 4
Difference from example 1 is that: the mixed liquor after being stirred by ultrasonic without using microwave irradiation.
Comparative example 5
Difference from example 1 is that: the mass ratio of solid carbon nanotube and four ammonia of triethylene after dry is
200:1, the design parameter of the first ball milling are as follows: Ball-milling Time 25h, drum's speed of rotation 1500rpm, ball milling temperature are 30 DEG C,
Ratio of grinding media to material is 15:1
Comparative example 6a
Difference from example 1 is that: in the first mixture, in parts by weight, modified solid carbon nanotube
Account for 30 parts, dibutyl tin dilaurate accounts for 2 parts, chliorinated polyvinyl chloride powder accounts for 50 parts, polyvinyl chloride powder accounts for 100 parts and receive
Rice hydrotalcite accounts for 3 parts.
Comparative example 6b
Difference from example 1 is that: in the first mixture, in parts by weight, modified solid carbon nanotube
Account for 5 parts, dibutyl tin dilaurate accounts for 10 parts, chliorinated polyvinyl chloride powder accounts for 50 parts, polyvinyl chloride powder accounts for 50 parts and receive
Rice hydrotalcite accounts for 8 parts.
Comparative example 7
Difference from example 1 is that: the design parameter of the second ball milling is carried out to the first mixture are as follows: Ball-milling Time
For 25h, drum's speed of rotation 1000rpm, ball milling temperature is 30 DEG C, ratio of grinding media to material 30:1.
Comparative example 8
Difference from example 1 is that: in the first mixture, in parts by weight, resistance to combustion component account for 200 parts, it is hard
Resin acid calcium accounts for 0.5 part, epoxidized soybean oil accounts for 2 parts and triacetyl glycerine accounts for 0.5 part.
Comparative example 9
Difference from example 1 is that: the design parameter of high-speed stirred is carried out to the second mixture are as follows: whipping temp
It is 100 DEG C, blender revolving speed is 1000rpm, mixing time 5min.
Comparative example 10
Difference from example 1 is that: the design parameter of mill is carried out to third mixture are as follows: open mill temperature is
200 DEG C, the mill time is 5min, the Corvic sheet material after mill with a thickness of 2mm.
Comparative example 11a
Difference from example 1 is that: hot pressing and cold pressing are carried out to the Corvic sheet material after mill
Design parameter are as follows: hot pressing temperature is 200 DEG C, hot pressing pressure 3MPa, and the sheet thickness after hot pressing is 0.5mm, temperature of colding pressing
It is 60 DEG C, cold pressing pressure 1MPa.
Comparative example 11b
Difference from example 1 is that: hot pressing and cold pressing are carried out to the Corvic sheet material after mill
Design parameter are as follows: hot pressing temperature is 160 DEG C, hot pressing pressure 12MPa, and the sheet thickness after hot pressing is 0.5mm, temperature of colding pressing
It is 20 DEG C, cold pressing pressure 8MPa.
Limit oxygen index test, tensile strength test and thermogravimetric test are carried out to embodiment 1-5 and comparative example 1-11
(corresponding temperature (T when wherein thermogravimetric test is with weightlessness 5%0.05) characterize the heat resistance of material).It the results are shown in Table 1.
Table 1
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. a kind of preparation method of the resistance to combustion Corvic material of high intensity, it is characterised in that: the resistance to combustion polychlorostyrene of high intensity
The preparation method of vinyl resinous material includes the following steps:
Prepare carbon nano tube dispersion liquid；
Solid carbon nanotube is filtered to take to obtain from the carbon nano tube dispersion liquid；
Acquired solid carbon nanotube is dried；
Solid carbon nanotube after drying is mixed with four ammonia of triethylene, and carries out the first ball milling, obtains modified solid carbon
Nanotube；
Mix solid carbon nanotube, the dibutyl tin dilaurate, chliorinated polyvinyl chloride powder, polyvinyl chloride powder of the modification
And nano hydrotalcite, obtain the first mixture；
Second ball milling is carried out to first mixture, obtains resistance to combustion component；
The resistance to combustion component, calcium stearate, epoxidized soybean oil and triacetyl glycerine are mixed, the second mixture is obtained；
High-speed stirred is carried out to second mixture, obtains third mixture；
Mill is carried out to the third mixture, the Corvic sheet material after obtaining mill；And
Hot pressing and cold pressing are carried out to the Corvic sheet material after the mill, obtain the high-intensitive Corvic of resistance to combustion
Material.
2. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: prepare carbon
Nanotube dispersion liquid specifically comprises the following steps:
Carbon nanotube raw material are put into silane coupler solution, wherein the silane coupler solution concentration is 10-
15wt%；
The silane coupling agent mixed liquor of carbon nanotube is stirred by ultrasonic, wherein ultrasonic agitation power is 400-500W, ultrasound
Mixing time is 2-4h；
Mixed liquor after being stirred by ultrasonic using microwave irradiation, microwave power 100-150W, irradiation time 20-40s.
3. the preparation method of resistance to combustion Corvic material as described in claim 1 high-intensitive, it is characterised in that: to being taken
What the solid carbon nanotube obtained was dried specifically comprises the processes of: drying temperature is 70-80 DEG C, drying time 30-50h.
4. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: drying
The mass ratio of solid carbon nanotube and four ammonia of triethylene afterwards is (50-100): 1, the design parameter of the first ball milling are as follows: when ball milling
Between be 10-20h, drum's speed of rotation 1000-1200rpm, ball milling temperature be 50-70 DEG C, ratio of grinding media to material be (10-20): 1.
5. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: described
In first mixture, in parts by weight, the solid carbon nanotube of the modification account for 10-20 parts, dibutyl tin dilaurate account for 3-7
Part, chliorinated polyvinyl chloride powder accounts for 20-40 parts, polyvinyl chloride powder accounts for 100-150 parts and nano hydrotalcite accounts for 2-5 parts.
6. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: to described
First mixture carries out the design parameter of the second ball milling are as follows: Ball-milling Time 10-20h, drum's speed of rotation 1300-1500rpm,
Ball milling temperature is 50-70 DEG C, and ratio of grinding media to material is (20-25): 1.
7. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: described
In first mixture, in parts by weight, the resistance to combustion component account for 100-150 parts, calcium stearate account for 1-1.2 parts, epoxidized soybean oil
It accounts for 3-6 parts and triacetyl glycerine accounts for 1-2 parts.
8. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: to described
The design parameter of second mixture progress high-speed stirred are as follows: whipping temp is 60-80 DEG C, and blender revolving speed is 400-800rpm,
Mixing time is 10-20min.
9. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: to described
The design parameter of third mixture progress mill are as follows: open mill temperature is 185-190 DEG C, and the mill time is 10-20min, described
Corvic sheet material after mill with a thickness of 2-4mm.
10. the preparation method of high-intensitive resistance to combustion Corvic material as described in claim 1, it is characterised in that: to institute
Corvic sheet material after stating mill carries out the design parameter of hot pressing and cold pressing are as follows: hot pressing temperature is 170-180 DEG C, heat
Pressure pressure is 5-10MPa, and the sheet thickness after hot pressing is 0.5-1mm, and temperature of colding pressing is 30-50 DEG C, cold pressing pressure 3-
6MPa。
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| CN106084547A (en) * | 2016-06-22 | 2016-11-09 | 安徽电信器材贸易工业有限责任公司 | A kind of carbon nano-tube modification fire-retardant cable material and preparation method thereof |
| CN107641273A (en) * | 2017-11-13 | 2018-01-30 | 安徽省康利亚股份有限公司 | A kind of 50 degree of low-smoke non-halogen flame-retardant cold-resistant insulation material |
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Application publication date: 20190125 |