CN110358288A - A kind of preparation method of Low temperature-resistanflexible flexible nylon material - Google Patents
A kind of preparation method of Low temperature-resistanflexible flexible nylon material Download PDFInfo
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- CN110358288A CN110358288A CN201910506101.9A CN201910506101A CN110358288A CN 110358288 A CN110358288 A CN 110358288A CN 201910506101 A CN201910506101 A CN 201910506101A CN 110358288 A CN110358288 A CN 110358288A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
Abstract
The present invention relates to a kind of preparation methods of Low temperature-resistanflexible flexible nylon material, belong to new material technology field.Silane coupling agent is as a kind of macromolecule surface inorganic agent in the present invention, and the long-term weatherability of the Low temperature-resistanflexible flexible nylon material prepared, resistant to chemical etching is all improved water resistance；The present invention is using polyurethane as elastomer come toughening Low temperature-resistanflexible flexible nylon material, material is when being impacted, toughener elastomer particle had both been used as stress that center is concentrated to induce a large amount of crazings and shear band, it can control the development of crazing again and terminate crazing in time and destructive crackle will not be developed into, the stress field in crazing forward position, which occurs, can induce the generation of shear band, and shear band can slow down the growth of crazing simultaneously, in this change procedure, the development of crazing and shear band consumes a large amount of energy, to significantly improve the impact strength of composite material.
Description
Technical field
The present invention relates to a kind of preparation methods of Low temperature-resistanflexible flexible nylon material, belong to new material technology field.
Background technique
Currently, constantly being expanded with the application of plastics substitution natural material in the world, scientist all over the world passes through various
Test finds new high-performance thermoplastics actively to substitute metal and timber, and this also become enterprise strive for more families and
The important component extended volume growth.
The development of high temperature plastics makes industrial or agricultural and civilian installation lightweight and powerful chemical conversion be miniaturized more as can
Energy.High-temperature resistance plastice can bring higher heat resistance for certain components, or simply produce instead of raw material metal
These components.The device and component of novel device equally also useful high-temperature resistance plastice replace metal and thermosetting material trend.
These will all increase the demand to high-temperature resistance plastice material, to drive the market demand.
These high-temperature resistance plastice materials can be with resistance to 180 DEG C of continuous high temperature, and is also able to maintain good dimensional stability.
With excellent long-term and short-term hot property, can be resistant to caused by (IR) reflow ovens infrared used in pb-free solder process
High temperature, and identical intensity is provided in wet condition, brilliant chemical resistance.
With the crystallinity amorphous nylon resins that nylon 6, nylon66 fiber position represent, due to toughness, chemical resistance, electrical
The excellent properties such as characteristic and the property for being easy to melt molding processing, are widely used in fiber, engineering plastics etc..However
Further investigation revealed that these nylon are shown as under low temperature and dry state as brittleness, so that these nylon are in some pairs of toughness
Higher field, as the application in terms of tubing receives very big limitation.Long carbon chain nylon, such as nylon 11, nylon 12, due to have compared with
Long carbochain, compared with conventional nylon, water absorption rate is lower, flexibility is more preferable, after plasticization and modification, is widely used in motor vehicle
Fluid delivery tube road.But in existing market the high-temperature resistance plastice material of all kinds have the shortcomings that one it is common: impact
Lower, brittleness is obvious, and especially in sub-zero temperature environment, more biasing is crisp.This disadvantage is larger to limit high temperature plastics substitution
The application range of metal and timber.
Summary of the invention
The technical problems to be solved by the invention: lower for existing high-temperature resistance plastice material impact, brittleness is obvious, especially
It is in sub-zero temperature environment, the crisp problem of more biasing provides a kind of preparation method of Low temperature-resistanflexible flexible nylon material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) 1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, carbon fiber are added to mixed
It closes in solution, carries out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed and are stirred,
Up to reaction solution, the pH of reaction solution being adjusted to get suspending liquid A, filters to obtain filter residue, filter residue is placed in the baking that temperature is 60~80 DEG C
It dries to constant weight in case to get modified carbon fiber；
(2) it in mass ratio 1: 1 mountain flour and aluminium powder is uniformly mixed is coupled titanate esters to get mixed powder, in mass ratio 1: 5: 1
Agent, acetone and isopropanol are uniformly mixed to get modification liquid, mixed powder is added in modification liquid be stirred to get
Suspension B filters to obtain precipitating, and precipitating is placed in the baking oven that temperature is 60~80 DEG C and is dried to constant weight, grinding is to get modified mixed
Close powder；
(3) nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, polyurethane elastomer, modification
Carbon fiber and modified mixed powder are uniformly mixed to get presoma, be granulated processing for presoma to get Low temperature-resistanflexible flexible Buddhist nun
Imperial material.
The mass ratio of carbon fiber described in step (1) and mixed liquor is 1: 10.
Carbon fiber is added in mixed solution by step described in (1), carries out ultrasonic disperse and stir process step are as follows: will
Carbon fiber is added in mixed solution, is 200~300W in power, after frequency is 5~10min of ultrasonic disperse under 50~70kHz,
Low whipping speed is 20~30min of high-speed stirred under 4000~5000r/min.
KH-560 and dispersion liquid are mixed described in step (1) and are stirred step are as follows: in mass ratio 1: 20 by KH-
560 and dispersion liquid mixing, low whipping speed be 2000~2500r/min, temperature be 60~70 DEG C at stir 1~2h.
The step of pH of reaction solution is adjusted described in step (1) are as follows: adjust reaction with the oxalic acid solution that mass fraction is 1%
The pH value of liquid is 4~5.
The mass ratio of mixed powder described in step (2) and modification liquid is 1: 10.
The size of mountain flour described in step (2) and aluminium powder is respectively that mountain flour crosses 35~40 meshes, and aluminium powder crosses 100~200 mesh
Sieve.
Mixed powder is added in modification liquid described in step (2) and is stirred step are as follows: by mixed powder plus
Enter into modification liquid, low whipping speed is that 1~2h is stirred under 5000~6000r/min.
Nylon 6 described in step (3), polyurethane elastomer, modified carbon fiber, the ratio difference being modified between mixed powder
Are as follows: according to parts by weight, 40~50 parts of nylon, 6,6~12 parts of polyurethane elastomers, 3~7 parts of modified carbon fibers, 1 are weighed respectively
~5 parts of modified mixed powders.
Presoma is subjected to the step of being granulated processing described in step (3) are as follows: presoma is subjected to granulation processing, squeezes out temperature
240~270 DEG C, screw speed 350r/min of degree, pellet use injection molding machine sample preparation after 100~120 DEG C of dry 4h, and injection temperature is
255~285 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) silane coupling agent is generally all different containing two parts polarity as a kind of macromolecule surface inorganic agent in the present invention
Group, a kind of functional group can be well in conjunction with carbon fiber surfaces, and another functional group (can produce in conjunction with matrix resin well
Raw copolymerization), not only protect carbon fiber surface, but also greatly strengthen the bonding of carbon fiber and resin boundary surface, prevent hydrone or its
The intrusion of his hazardous medium, the weakness for reducing or eliminating interface improve interface state, effectively deliver stress, make carbon fiber
Can be formed between matrix resin one it is firm whole, it is the long-term weatherability for the Low temperature-resistanflexible flexible nylon material prepared, water-fast
Property, it is resistant to chemical etching all improved, mechanical mechanics property also improves；
(2) use mountain flour, aluminium powder and modified carbon fiber as reinforcing material, the jail of fibrous material and polymeric matrix in the present invention
Knot is adhered, is transferred to load suffered by polymeric matrix on high tensile strength fibrous material, and will be by localized delivery to biggish range
Inside even composite material is whole；Mountain flour, aluminium powder and modified carbon fiber collaboration enhancing, give full play to respective in blending procedure
Advantage, while the opposite collection beam force weakened between reinforcing agent of the same race, therefore the Low temperature-resistanflexible flexible nylon material prepared not only has
High-intensitive, high-modulus, and its heat resistance is preferable, molding shrinkage is lower, while the processing performance of composite material is excellent；
(3) present invention using polyurethane as elastomer come toughening Low temperature-resistanflexible flexible nylon material, material when being impacted, increasing
Tough dose of elastomer particle had not only been used as stress that center is concentrated to induce a large amount of crazings and shear band, but also can control the development of crazing and make
Crazing terminates in time and will not develop into destructive crackle, and the stress field in crazing forward position, which occurs, can induce the life of shear band
At, and shear band can slow down the growth of crazing simultaneously, in this change procedure, the development of crazing and shear band is consumed largely
Energy, to significantly improve the impact strength of composite material；Thermoplastic polyurethane (TPU) elastomer has plastics and rubber concurrently
Characteristic, TPU are a kind of A-B type block copolymers, have not only contained flexible soft chain segment in molecule but also have contained rigid hard segment；Wherein A
Soft segment is represented, is made of long-chain polyhydric alcohol, soft segment determines some final performances of TPU, such as elasticity, cryogenic subduing flexibility, at certain
The expansion character of polymer and water-disintegrable is also determined in kind of degree；B represents hard section, by small molecule dihydric alcohol or diamine and isocyanide
Acid esters is constituted, and what hard segment was shown is then hardness, elasticity modulus, release property and high-temperature behavior (thermal stability)；Hard segment passes through
Intermolecular hydrogen bonding obtains strong physical crosslinking structure, micro phase separation structure is formed, so table not being chemically crosslinked structure
Reveal caoutchouc elasticity；Polyurethane can still keep preferable elasticity as elastomer in wider temperature range, have simultaneously
Good resistance to low temperature, and impact brittle temperature and be lower than -60 DEG C, it can be formed with nylon in certain performances good mutual
It mends.
Specific embodiment
1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, in mass ratio 1: 10 by carbon
Fiber is added in mixed solution, is 200~300W in power, after frequency is 5~10min of ultrasonic disperse under 50~70kHz,
Mixing speed is that 20~30min of high-speed stirred is under 4000~5000r/min to get dispersion liquid, and in mass ratio 1: 20 by KH-560
It is mixed with dispersion liquid, low whipping speed is 2000~2500r/min, and temperature is that 1~2h is stirred at 60~70 DEG C to get reaction
The pH value that the oxalic acid solution that liquid is 1% with mass fraction adjusts reaction solution is 4~5 to get suspending liquid A, filters to obtain filter residue, will filter
Slag is placed in the baking oven that temperature is 60~80 DEG C and dries to constant weight to get modified carbon fiber；The stone of 35~40 meshes was taken respectively
Powder and the aluminium powder for crossing 100~200 meshes, and in mass ratio 1: 1 mixing is to get mixed powder, in mass ratio 1: 5: 1 by titanate esters
Coupling agent, acetone and isopropanol are uniformly mixed and mixed powder are added in modification liquid to get modification liquid, in mass ratio 1: 10,
Low whipping speed is that 1~2h is stirred under 5000~6000r/min to get suspension B, filters to obtain precipitating, precipitating is placed in temperature
To be dried in 60~80 DEG C of baking ovens to constant weight, grinding is to get modified mixed powder；According to parts by weight, 40 are weighed respectively~
50 parts of nylon, 6,6~12 parts of polyurethane elastomers, 3~7 parts of modified carbon fibers, 1~5 part of modified mixed powder by nylon 6, gather
Urethane elastomer, modified carbon fiber and modified mixed powder are uniformly mixed to get presoma, and presoma is carried out granulation processing,
240~270 DEG C of extrusion temperature, screw speed 350r/min, pellet uses injection molding machine sample preparation, injection molding after 100~120 DEG C of dry 4h
Temperature is 255~285 DEG C to get Low temperature-resistanflexible flexible nylon material.
Example 1
1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, it is molten that carbon fiber is added to mixing
In liquid, carry out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed be stirred to get
Reaction solution adjusts the pH of reaction solution to get suspending liquid A, filters to obtain filter residue, filter residue is placed in dry in the baking oven that temperature is 60 DEG C
To constant weight to get modified carbon fiber；In mass ratio 1: 1 is uniformly mixed mountain flour and aluminium powder to get mixed powder, in mass ratio 1:
Be uniformly mixed titanate coupling agent, acetone and isopropanol to get modification liquid at 5: 1, by mixed powder be added in modification liquid into
Row stir process filters to obtain precipitating, precipitating is placed in the baking oven that temperature is 60 DEG C and is dried to constant weight, is ground to get suspension B
Mill is to get modified mixed powder；Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, poly- ammonia
Ester elastomer, modified carbon fiber and modified mixed powder are uniformly mixed to get presoma, presoma are carried out granulation processing, i.e.,
Obtain Low temperature-resistanflexible flexible nylon material.The mass ratio of carbon fiber and mixed liquor is 1: 10.Carbon fiber is added in mixed solution, into
Row ultrasonic disperse and stir process step are as follows: carbon fiber is added in mixed solution, is 200W, frequency 50kHz in power
After lower ultrasonic disperse 5min, low whipping speed is high-speed stirred 20min under 4000r/min.KH-560 and dispersion liquid are mixed into
Row stir process step are as follows: in mass ratio 1: 20 mixes KH-560 and dispersion liquid, low whipping speed 2000r/min, temperature
It is to stir 1h at 60 DEG C.The step of adjusting the pH of reaction solution are as follows: the pH of reaction solution is adjusted with the oxalic acid solution that mass fraction is 1%
Value is 4.The mass ratio of mixed powder and modification liquid is 1: 10.The size of mountain flour and aluminium powder is respectively that mountain flour crosses 35 meshes, aluminium powder
It sieves with 100 mesh sieve.Mixed powder is added in modification liquid and is stirred step are as follows: mixed powder is added to modification liquid
In, low whipping speed is to stir 1h under 5000r/min.Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder it
Between ratio be respectively as follows: according to parts by weight, weigh 40 parts of nylon, 6,6 parts of polyurethane elastomers, 3 parts of modified carbon fibers, 1 respectively
The modified mixed powder of part.Presoma is subjected to the step of being granulated processing are as follows: presoma is subjected to granulation processing, extrusion temperature 240
DEG C, screw speed 350r/min, pellet uses injection molding machine sample preparation after 100 DEG C of dry 4h, and injection temperature is 255 DEG C.
Example 2
1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, it is molten that carbon fiber is added to mixing
In liquid, carry out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed be stirred to get
Reaction solution adjusts the pH of reaction solution to get suspending liquid A, filters to obtain filter residue, filter residue is placed in dry in the baking oven that temperature is 67 DEG C
To constant weight to get modified carbon fiber；In mass ratio 1: 1 is uniformly mixed mountain flour and aluminium powder to get mixed powder, in mass ratio 1:
Be uniformly mixed titanate coupling agent, acetone and isopropanol to get modification liquid at 5: 1, by mixed powder be added in modification liquid into
Row stir process filters to obtain precipitating, precipitating is placed in the baking oven that temperature is 67 DEG C and is dried to constant weight, is ground to get suspension B
Mill is to get modified mixed powder；Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, poly- ammonia
Ester elastomer, modified carbon fiber and modified mixed powder are uniformly mixed to get presoma, presoma are carried out granulation processing, i.e.,
Obtain Low temperature-resistanflexible flexible nylon material.The mass ratio of carbon fiber and mixed liquor is 1: 10.Carbon fiber is added in mixed solution, into
Row ultrasonic disperse and stir process step are as follows: carbon fiber is added in mixed solution, is 235W, frequency 57kHz in power
After lower ultrasonic disperse 7min, low whipping speed is high-speed stirred 23min under 4350r/min.KH-560 and dispersion liquid are mixed into
Row stir process step are as follows: in mass ratio 1: 20 mixes KH-560 and dispersion liquid, low whipping speed 2170r/min, temperature
It is to stir 1.3h at 63 DEG C.The step of adjusting the pH of reaction solution are as follows: adjust reaction solution with the oxalic acid solution that mass fraction is 1%
PH value is 4.3.The mass ratio of mixed powder and modification liquid is 1: 10.The size of mountain flour and aluminium powder is respectively that mountain flour crosses 36 meshes,
Aluminium powder crosses 135 meshes.Mixed powder is added in modification liquid and is stirred step are as follows: mixed powder is added to modification
In liquid, low whipping speed is to stir 1.3h under 5350r/min.Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder
Ratio between body is respectively as follows: according to parts by weight, weighs 43 parts of nylon, 6,8 parts of polyurethane elastomers, 4 parts of modified carbon fibers respectively
Dimension, 2 parts of modified mixed powders.Presoma is subjected to the step of being granulated processing are as follows: presoma is subjected to granulation processing, extrusion temperature
250 DEG C, screw speed 350r/min, pellet uses injection molding machine sample preparation after 107 DEG C of dry 4h, and injection temperature is 265 DEG C.
Example 3
1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, it is molten that carbon fiber is added to mixing
In liquid, carry out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed be stirred to get
Reaction solution adjusts the pH of reaction solution to get suspending liquid A, filters to obtain filter residue, filter residue is placed in dry in the baking oven that temperature is 73 DEG C
To constant weight to get modified carbon fiber；In mass ratio 1: 1 is uniformly mixed mountain flour and aluminium powder to get mixed powder, in mass ratio 1:
Be uniformly mixed titanate coupling agent, acetone and isopropanol to get modification liquid at 5: 1, by mixed powder be added in modification liquid into
Row stir process filters to obtain precipitating, precipitating is placed in the baking oven that temperature is 73 DEG C and is dried to constant weight, is ground to get suspension B
Mill is to get modified mixed powder；Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, poly- ammonia
Ester elastomer, modified carbon fiber and modified mixed powder are uniformly mixed to get presoma, presoma are carried out granulation processing, i.e.,
Obtain Low temperature-resistanflexible flexible nylon material.The mass ratio of carbon fiber and mixed liquor is 1: 10.Carbon fiber is added in mixed solution, into
Row ultrasonic disperse and stir process step are as follows: carbon fiber is added in mixed solution, is 265W, frequency 63kHz in power
After lower ultrasonic disperse 8min, low whipping speed is high-speed stirred 27min under 4700r/min.KH-560 and dispersion liquid are mixed into
Row stir process step are as follows: in mass ratio 1: 20 mixes KH-560 and dispersion liquid, low whipping speed 2350r/min, temperature
It is to stir 1.6h at 67 DEG C.The step of adjusting the pH of reaction solution are as follows: adjust reaction solution with the oxalic acid solution that mass fraction is 1%
PH value is 4.6.The mass ratio of mixed powder and modification liquid is 1: 10.The size of mountain flour and aluminium powder is respectively that mountain flour crosses 38 meshes,
Aluminium powder crosses 165 meshes.Mixed powder is added in modification liquid and is stirred step are as follows: mixed powder is added to modification
In liquid, low whipping speed is to stir 1.6h under 5650r/min.Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder
Ratio between body is respectively as follows: according to parts by weight, weighs 46 parts of nylon, 6,10 parts of polyurethane elastomers, 6 parts of carbon modifieds respectively
Fiber, 4 parts of modified mixed powders.Presoma is subjected to the step of being granulated processing are as follows: presoma is subjected to granulation processing, squeezes out temperature
260 DEG C, screw speed 350r/min of degree, pellet use injection molding machine sample preparation after 113 DEG C of dry 4h, and injection temperature is 275 DEG C.
Example 4
1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, it is molten that carbon fiber is added to mixing
In liquid, carry out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed be stirred to get
Reaction solution adjusts the pH of reaction solution to get suspending liquid A, filters to obtain filter residue, filter residue is placed in dry in the baking oven that temperature is 80 DEG C
To constant weight to get modified carbon fiber；In mass ratio 1: 1 is uniformly mixed mountain flour and aluminium powder to get mixed powder, in mass ratio 1:
Be uniformly mixed titanate coupling agent, acetone and isopropanol to get modification liquid at 5: 1, by mixed powder be added in modification liquid into
Row stir process filters to obtain precipitating, precipitating is placed in the baking oven that temperature is 80 DEG C and is dried to constant weight, is ground to get suspension B
Mill is to get modified mixed powder；Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, poly- ammonia
Ester elastomer, modified carbon fiber and modified mixed powder are uniformly mixed to get presoma, presoma are carried out granulation processing, i.e.,
Obtain Low temperature-resistanflexible flexible nylon material.The mass ratio of carbon fiber and mixed liquor is 1: 10.Carbon fiber is added in mixed solution, into
Row ultrasonic disperse and stir process step are as follows: carbon fiber is added in mixed solution, is 300W, frequency 70kHz in power
After lower ultrasonic disperse 10min, low whipping speed is high-speed stirred 30min under 5000r/min.KH-560 and dispersion liquid are mixed into
Row stir process step are as follows: in mass ratio 1: 20 mixes KH-560 and dispersion liquid, low whipping speed 2500r/min, temperature
It is to stir 2h at 70 DEG C.The step of adjusting the pH of reaction solution are as follows: the pH of reaction solution is adjusted with the oxalic acid solution that mass fraction is 1%
Value is 5.The mass ratio of mixed powder and modification liquid is 1: 10.The size of mountain flour and aluminium powder is respectively that mountain flour crosses 40 meshes, aluminium powder
Cross 200 meshes.Mixed powder is added in modification liquid and is stirred step are as follows: mixed powder is added to modification liquid
In, low whipping speed is to stir 2h under 6000r/min.Nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder it
Between ratio be respectively as follows: according to parts by weight, weigh respectively 50 parts of nylon, 6,12 parts of polyurethane elastomers, 7 parts of modified carbon fibers,
5 parts of modified mixed powders.Presoma is subjected to the step of being granulated processing are as follows: presoma is subjected to granulation processing, extrusion temperature 270
DEG C, screw speed 350r/min, pellet uses injection molding machine sample preparation after 120 DEG C of dry 4h, and injection temperature is 285 DEG C.
Low temperature-resistanflexible flexible nylon material prepared by the present invention and commercially available plastic material are detected, specific testing result
Such as following table table 1:
Detection method:
The Low temperature-resistanflexible flexible nylon material prepared according to example 1~3 can use at -20 to -40 DEG C；In identical item
Its impact strength (unit: kJ/m is tested under part2), thermal change type temperature (unit: DEG C), bending modulus (unit: MPa).
Impact strength is after it is freezed 4 hours at -40 DEG C, to test its impact strength；It is tested under conditions of 1.82Mpa
Its thermal change type temperature；Product is easy molding in the process not sticking to mould of injection molding.
1 Low temperature-resistanflexible flexible nylon material performance characterization of table
Low temperature-resistanflexible flexible nylon material prepared by the present invention as shown in Table 1, impact strength is high, and thermal change type temperature is high, lower temperature resistance
Can be excellent, it remains to show excellent bending modulus under cryogenic, has a vast market value and application prospect.
Claims (10)
1. a kind of preparation method of Low temperature-resistanflexible flexible nylon material, it is characterised in that specific preparation step are as follows:
(1) 1: 3 deionized water and dehydrated alcohol are uniformly mixed by volume to get mixed solution, carbon fiber are added to mixed
It closes in solution, carries out ultrasonic disperse and stir process to get dispersion liquid, KH-560 and dispersion liquid are mixed and are stirred,
Up to reaction solution, the pH of reaction solution being adjusted to get suspending liquid A, filters to obtain filter residue, filter residue is placed in the baking that temperature is 60~80 DEG C
It dries to constant weight in case to get modified carbon fiber；
(2) it in mass ratio 1: 1 mountain flour and aluminium powder is uniformly mixed is coupled titanate esters to get mixed powder, in mass ratio 1: 5: 1
Agent, acetone and isopropanol are uniformly mixed to get modification liquid, mixed powder is added in modification liquid be stirred to get
Suspension B filters to obtain precipitating, and precipitating is placed in the baking oven that temperature is 60~80 DEG C and is dried to constant weight, grinding is to get modified mixed
Close powder；
(3) nylon 6, polyurethane elastomer, modified carbon fiber, modified mixed powder are taken, by nylon 6, polyurethane elastomer, modification
Carbon fiber and modified mixed powder are uniformly mixed to get presoma, be granulated processing for presoma to get Low temperature-resistanflexible flexible Buddhist nun
Imperial material.
2. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (1)
The mass ratio of the carbon fiber and mixed liquor is 1: 10.
3. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (1)
Described is added to carbon fiber in mixed solution, carries out ultrasonic disperse and stir process step are as follows: be added to carbon fiber mixed
It closes in solution, is 200~300W in power, frequency is under 50~70kHz after 5~10min of ultrasonic disperse, and low whipping speed is
20~30min of high-speed stirred under 4000~5000r/min.
4. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (1)
Described mix KH-560 and dispersion liquid is stirred step are as follows: in mass ratio 1: 20 mixes KH-560 and dispersion liquid
It closes, low whipping speed is 2000~2500r/min, and temperature is that 1~2h is stirred at 60~70 DEG C.
5. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (1)
The step of pH of the adjusting reaction solution are as follows: the pH value that the oxalic acid solution for being 1% with mass fraction adjusts reaction solution is 4~5.
6. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (2)
The mass ratio of the mixed powder and modification liquid is 1: 10.
7. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (2)
The size of the mountain flour and aluminium powder is respectively that mountain flour crosses 35~40 meshes, and aluminium powder crosses 100~200 meshes.
8. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (2)
Described mixed powder is added in modification liquid is stirred step are as follows: mixed powder be added in modification liquid,
Mixing speed is that 1~2h is stirred under 5000~6000r/min.
9. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (3)
The nylon 6, polyurethane elastomer, modified carbon fiber, the ratio between modified mixed powder are respectively as follows: in parts by weight
Meter weighs 40~50 parts of nylon, 6,6~12 parts of polyurethane elastomers, 3~7 parts of modified carbon fibers, 1~5 part of modified mixing respectively
Powder.
10. a kind of preparation method of Low temperature-resistanflexible flexible nylon material according to claim 1, it is characterised in that: step (3)
It is described that presoma is carried out to the step of being granulated processing are as follows: presoma is subjected to granulation processing, 240~270 DEG C of extrusion temperature, spiral shell
Bar revolving speed 350r/min, pellet use injection molding machine sample preparation after 100~120 DEG C of dry 4h, and injection temperature is 255~285 DEG C.
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| CN201910506101.9A CN110358288A (en) | 2019-06-12 | 2019-06-12 | A kind of preparation method of Low temperature-resistanflexible flexible nylon material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113667395A (en) * | 2021-09-02 | 2021-11-19 | 南京项多裕建筑科技有限公司 | Anti-fouling low-temperature-resistant synthetic resin and preparation method thereof |
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