CN110204888A - A kind of low temperature resistant polyamide composite material and preparation method - Google Patents
A kind of low temperature resistant polyamide composite material and preparation method Download PDFInfo
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- CN110204888A CN110204888A CN201910546186.3A CN201910546186A CN110204888A CN 110204888 A CN110204888 A CN 110204888A CN 201910546186 A CN201910546186 A CN 201910546186A CN 110204888 A CN110204888 A CN 110204888A
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- 229920002647 polyamide Polymers 0.000 title claims abstract description 49
- 239000004952 Polyamide Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000463 material Substances 0.000 claims abstract description 45
- 230000002528 anti-freeze Effects 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 21
- 230000000996 additive effect Effects 0.000 claims abstract description 21
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 21
- 239000003921 oil Substances 0.000 claims abstract description 15
- 235000019198 oils Nutrition 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims abstract description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 6
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920001195 polyisoprene Polymers 0.000 claims abstract description 6
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 6
- 239000003549 soybean oil Substances 0.000 claims abstract description 6
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims abstract description 6
- 239000010457 zeolite Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 25
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000005543 nano-size silicon particle Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene chloride Substances ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- QMMBZOSZCYBCDC-UHFFFAOYSA-N NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC Chemical compound NCCNCCC[SiH](OC(OCC)(OCC)OCC)OC QMMBZOSZCYBCDC-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004807 desolvation Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 5
- 239000013067 intermediate product Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 claims description 5
- 229940094989 trimethylsilane Drugs 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 241000446313 Lamella Species 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 8
- 239000004677 Nylon Substances 0.000 description 5
- 229920001778 nylon Polymers 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 229910006124 SOCl2 Inorganic materials 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- 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
- C08L2207/06—Properties of polyethylene
- C08L2207/068—Ultra high molecular weight polyethylene
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of low temperature resistant polyamide composite material prepared by the present invention, is kneaded by following component with parts by weight: 50-70 parts of polyamide substrate, antifreeze mixing 10-15 parts, 5-7 parts of auxiliary material, 1-2 parts of antioxidant, 1-3 parts of additive;The antifreeze mixing is mixed by 10-15 parts of polyisoprene, 5-8 parts for kaolin, 3-5 parts of zeolite powders and 3-5 parts of modified manometer silicon dioxides；The auxiliary material is 3-5 parts of modified multiwalled carbon nanotubes, 6-10 parts of TiN, 5-8 parts of ultra-high molecular weight polyethylene powder, and the additive is 1-3 parts of epoxidized soybean oils, 1-3 parts of silane coupling agents, 1-2 modified silicon oil；The present invention prepares low temperature resistant polyamide composite material, and appointing under the conditions of subzero 50 DEG C has good intensity and toughness, and furthermore its flowing is good, facilitates later period material product to process, furthermore polyamide compoiste material appearance glossiness produced by the present invention is good.
Description
Technical field
The invention belongs to polyamide compoiste material field, specifically design be a kind of low temperature resistant polyamide composite material and its
Preparation method.
Background technique
Polyamide (nylon) has very strong vitality as most important kind maximum in engineering plastics, because nylon has
Have many characteristics, automobile, electrical equipment, Machinery Ministry structure, transportation equipment, weaving, in terms of obtain extensively
Using.With the miniaturization of automobile, the high performance of electronic electric equipment, the light-weighted progress faster of mechanical equipment, to nylon
Demand will more Gao Geng great.Especially nylon proposes its intensity, heat resistance, cold resistance etc. as structural material
Very high requirement.But it is poor with resistance to low temperature, is easy to happen embrittlement at low temperature, causes serious shadow to the performance of nylon
It rings.
Summary of the invention
In order to solve the above technical problems, the present invention proposes a kind of low temperature resistant polyamide composite material and preparation method, change
The resistance to low temperature of kind polyamide.
To achieve the above object, the technical solution adopted by the present invention are as follows: a kind of low temperature resistant polyamide composite material, by following
Ingredient is kneaded with parts by weight: 50-70 parts of polyamide substrate, antifreeze mixing 10-15 parts, and 5-7 parts of auxiliary material, antioxidant 1-
2 parts, 1-3 parts of additive;The antifreeze mixing by 10-15 parts of polyisoprene, 5-8 parts for kaolin, 3-5 parts of zeolite powders and
3-5 parts of modified manometer silicon dioxides mix；The auxiliary material is 3-5 parts of modified multiwalled carbon nanotubes, 6-10 parts TiN, 5-8 parts
Ultra-high molecular weight polyethylene powder, the additive are 1-3 parts of epoxidized soybean oils, 1-3 parts of silane coupling agents, 1-2 modified silicon oil.
Further, the polyamide compoiste material also contains 1-3 parts of brighteners.
Further, 3-5 parts of TiC and 3-5 parts of silicate platelets are also contained in the antifreeze mixing.
Further, 1-1.5 parts of polytetrafluoroethylene (PTFE) are also contained in the auxiliary material.
Further, 1-2 parts of Cocoamidopropyl betaines are also contained in the additive.
Further, a kind of low temperature resistant polyamide composite material, preparation method includes the following steps:
One) modified manometer silicon dioxide, modified multiwalled carbon nanotube and modified silicon oil are prepared
Ethyl orthosilicate and dehydrated alcohol are added in the three-necked flask equipped with dropping funel, dripped while stirring under the conditions of 50 DEG C
The dehydrated alcohol and deionized water mixed liquor of the volume ratio 1:1 of HCl dropwise mistake is added nano-silicon dioxide particle and continues after dripping off
It stirs, the ratio of nano silica, ethyl orthosilicate, dehydrated alcohol and acidification dehydrated alcohol and deionized water mixed liquor is
After reacting 12h, 5% methacryloxy relative to nano-silicon dioxide particle quality is added in 1g:2ml:10ml:3ml
Oxypropyl trimethyl silane continues to be stirred to react 6 h at 50 °C, modified manometer silicon dioxide colloidal sol is obtained, then 50
It is dried in vacuo under the conditions of DEG C, obtains modified manometer silicon dioxide, it is spare；
(a), multi-walled carbon nanotube is added in concentrated nitric acid, the ratio of the two is 1g:30ml, after 120 DEG C of reflux for 24 hours, spend from
Sub- water dilution, washing, filtering, and dry；(b), by (a) step drying material be added SOCl2 in, the two ratio be 1g:50ml, 70 DEG C
It flows back after 24 h, centrifugation is washed with CH2Cl2 and dried under the conditions of 80 DEG C；(c), melting 18 is added in (b) step drying material
In amine, the two mass ratio is 1:5, reacts 24 h at 90 DEG C, is then centrifuged product, and washed with dehydrated alcohol, finally, 80
DEG C drying obtains modified multiwalled carbon nanotube, spare；
N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, four silicon of prestox ring for being first 1:15:3:2 by ratio
Oxygen alkane, hexamethyldisiloxane and tetramethyl hydrogenation ammonia are uniformly mixed, nitrogen protection, stirring, under the conditions of 110 DEG C, heat preservation 6-8h,
135 DEG C are then heated to, 0.5h is reacted, then low-boiling-point substance 0.5h is taken off in 135 DEG C, 60KPa vacuum, obtains intermediate product；In taking
Between product and active polyether isopropanol is added, proportions 2g:1g:50ml is stirred evenly, 80 DEG C of reaction 5h, finally, in
135 DEG C, the agent of 60KPa vacuum desolvation and low-boiling-point substance 0.5h, obtain modified silicon oil, spare；
Two) preparation of composite material
Polyamide substrate, antifreeze mixing, auxiliary material, antioxidant and additive are added in batch mixer according to the above ratio first, mixed
0.5h is closed, double screw extruder, screw speed 300-450r/min, extruder machine then is added in uniformly mixed mixture
Temperature setting in cylinder are as follows: 240 DEG C of an area, 255 DEG C of 2nd area, 263 DEG C of 3rd area, 260 DEG C of 4th area, mixture are made through extruder extrusion
Low temperature resistant polyamide composite material is made in grain.
Compared with prior art, the invention has the following advantages:
A kind of low temperature resistant polyamide composite material and preparation method prepared by the present invention, on the one hand it is under the conditions of subzero 50 DEG C
Appointing has good intensity and certain toughness, and on the other hand polyamide compoiste material flowing prepared by the present invention is good, convenient
The processing of later period material product, furthermore, the good effect of polyamide compoiste material appearance glossiness produced by the present invention.
Specific embodiment
Below with reference to the preferred embodiments of the present invention will be described in detail, so that advantages and features of the invention can be easier to
In being readily appreciated by one skilled in the art, so as to make a clearer definition of the protection scope of the present invention.
Embodiment 1
A kind of low temperature resistant polyamide composite material is kneaded by following component with parts by weight: 50 parts of polyamide substrate, antifreeze
10 parts of mixing, 5 parts of auxiliary material, 1 part of antioxidant, 1 part of additive;The antifreeze mixing is by 10 parts of polyisoprene, 5 parts
Kaolin, 3 parts of zeolite powders and 3 parts of modified manometer silicon dioxides mix；The auxiliary material is 3 parts of modified multiwalled carbon nanotubes, 6
Part TiN, 5 parts of ultra-high molecular weight polyethylene powder, the additive are 1 part of epoxidized soybean oil, 1 part of silane coupling agent, 1 modified silicon
Oil.
Further, the polyamide compoiste material also contains 1 part of brightener.
Further, 3 parts of TiC and 3 part of silicate platelets are also contained in the antifreeze mixing.
Further, 1 part of polytetrafluoroethylene (PTFE) is also contained in the auxiliary material.
Further, 1 part of Cocoamidopropyl betaine is also contained in the additive.
Further, a kind of low temperature resistant polyamide composite material, preparation method includes the following steps:
One) modified manometer silicon dioxide, modified multiwalled carbon nanotube and modified silicon oil are prepared
Ethyl orthosilicate and dehydrated alcohol are added in the three-necked flask equipped with dropping funel, dripped while stirring under the conditions of 50 DEG C
The dehydrated alcohol and deionized water mixed liquor of the volume ratio 1:1 of HCl dropwise mistake is added nano-silicon dioxide particle and continues after dripping off
It stirs, the ratio of nano silica, ethyl orthosilicate, dehydrated alcohol and acidification dehydrated alcohol and deionized water mixed liquor is
After reacting 12h, 5% methacryloxy relative to nano-silicon dioxide particle quality is added in 1g:2ml:10ml:3ml
Oxypropyl trimethyl silane continues to be stirred to react 6 h at 50 °C, modified manometer silicon dioxide colloidal sol is obtained, then 50
It is dried in vacuo under the conditions of DEG C, obtains modified manometer silicon dioxide, it is spare；
(a), multi-walled carbon nanotube is added in concentrated nitric acid, the ratio of the two is 1g:30ml, after 120 DEG C of reflux for 24 hours, spend from
Sub- water dilution, washing, filtering, and dry；(b), by (a) step drying material be added SOCl2 in, the two ratio be 1g:50ml, 70 DEG C
It flows back after 24 h, centrifugation is washed with CH2Cl2 and dried under the conditions of 80 DEG C；(c), melting 18 is added in (b) step drying material
In amine, the two mass ratio is 1:5, reacts 24 h at 90 DEG C, is then centrifuged product, and washed with dehydrated alcohol, finally, 80
DEG C drying obtains modified multiwalled carbon nanotube, spare；
N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, four silicon of prestox ring for being first 1:15:3:2 by ratio
Oxygen alkane, hexamethyldisiloxane and tetramethyl hydrogenation ammonia are uniformly mixed, nitrogen protection, stirring, under the conditions of 110 DEG C, heat preservation 6-8h,
135 DEG C are then heated to, 0.5h is reacted, then low-boiling-point substance 0.5h is taken off in 135 DEG C, 60KPa vacuum, obtains intermediate product；In taking
Between product and active polyether isopropanol is added, proportions 2g:1g:50ml is stirred evenly, 80 DEG C of reaction 5h, finally, in
135 DEG C, the agent of 60KPa vacuum desolvation and low-boiling-point substance 0.5h, obtain modified silicon oil, spare；
Two) preparation of composite material
Polyamide substrate, antifreeze mixing, auxiliary material, antioxidant and additive are added in batch mixer according to the above ratio first, mixed
0.5h is closed, double screw extruder, screw speed 300-450r/min, extruder machine then is added in uniformly mixed mixture
Temperature setting in cylinder are as follows: 240 DEG C of an area, 255 DEG C of 2nd area, 263 DEG C of 3rd area, 260 DEG C of 4th area, mixture are made through extruder extrusion
Low temperature resistant polyamide composite material is made in grain.
Embodiment 2
A kind of low temperature resistant polyamide composite material is kneaded by following component with parts by weight: 60 parts of polyamide substrate, antifreeze
13 parts of mixing, 6 parts of auxiliary material, 1.5 parts of antioxidant, 2 parts of additive;The antifreeze mixing is by 12 parts of polyisoprene, 6 parts
It is mixed for kaolin, 4 parts of zeolite powders and 4 parts of modified manometer silicon dioxides；The auxiliary material is 4 parts of modified multi-wall carbon nano-tubes
Pipe, 8 parts of TiN, 6 parts of ultra-high molecular weight polyethylene powder, the additive are 2 parts of epoxidized soybean oils, 2 parts of silane coupling agents, and 1 is modified
Silicone oil.
Further, the polyamide compoiste material also contains 2 parts of brighteners.
Further, 4 parts of TiC and 4 part of silicate platelets are also contained in the antifreeze mixing.
Further, 1 part of polytetrafluoroethylene (PTFE) is also contained in the auxiliary material.
Further, 1.5 parts of Cocoamidopropyl betaines are also contained in the additive.
Further, a kind of low temperature resistant polyamide composite material, preparation method includes the following steps:
One) modified manometer silicon dioxide, modified multiwalled carbon nanotube and modified silicon oil are prepared
Ethyl orthosilicate and dehydrated alcohol are added in the three-necked flask equipped with dropping funel, dripped while stirring under the conditions of 50 DEG C
The dehydrated alcohol and deionized water mixed liquor of the volume ratio 1:1 of HCl dropwise mistake is added nano-silicon dioxide particle and continues after dripping off
It stirs, the ratio of nano silica, ethyl orthosilicate, dehydrated alcohol and acidification dehydrated alcohol and deionized water mixed liquor is
After reacting 12h, 5% methacryloxy relative to nano-silicon dioxide particle quality is added in 1g:2ml:10ml:3ml
Oxypropyl trimethyl silane continues to be stirred to react 6 h at 50 °C, modified manometer silicon dioxide colloidal sol is obtained, then 50
It is dried in vacuo under the conditions of DEG C, obtains modified manometer silicon dioxide, it is spare；
(a), multi-walled carbon nanotube is added in concentrated nitric acid, the ratio of the two is 1g:30ml, after 120 DEG C of reflux for 24 hours, spend from
Sub- water dilution, washing, filtering, and dry；(b), by (a) step drying material be added SOCl2 in, the two ratio be 1g:50ml, 70 DEG C
It flows back after 24 h, centrifugation is washed with CH2Cl2 and dried under the conditions of 80 DEG C；(c), melting 18 is added in (b) step drying material
In amine, the two mass ratio is 1:5, reacts 24 h at 90 DEG C, is then centrifuged product, and washed with dehydrated alcohol, finally, 80
DEG C drying obtains modified multiwalled carbon nanotube, spare；
N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, four silicon of prestox ring for being first 1:15:3:2 by ratio
Oxygen alkane, hexamethyldisiloxane and tetramethyl hydrogenation ammonia are uniformly mixed, nitrogen protection, stirring, under the conditions of 110 DEG C, heat preservation 6-8h,
135 DEG C are then heated to, 0.5h is reacted, then low-boiling-point substance 0.5h is taken off in 135 DEG C, 60KPa vacuum, obtains intermediate product；In taking
Between product and active polyether isopropanol is added, proportions 2g:1g:50ml is stirred evenly, 80 DEG C of reaction 5h, finally, in
135 DEG C, the agent of 60KPa vacuum desolvation and low-boiling-point substance 0.5h, obtain modified silicon oil, spare；
Two) preparation of composite material
Polyamide substrate, antifreeze mixing, auxiliary material, antioxidant and additive are added in batch mixer according to the above ratio first, mixed
0.5h is closed, double screw extruder, screw speed 300-450r/min, extruder machine then is added in uniformly mixed mixture
Temperature setting in cylinder are as follows: 240 DEG C of an area, 255 DEG C of 2nd area, 263 DEG C of 3rd area, 260 DEG C of 4th area, mixture are made through extruder extrusion
Low temperature resistant polyamide composite material is made in grain.
Embodiment 3
A kind of low temperature resistant polyamide composite material is kneaded by following component with parts by weight: 70 parts of polyamide substrate, antifreeze
15 parts of mixing, 7 parts of auxiliary material, 2 parts of antioxidant, 3 parts of additive;The antifreeze mixing is by 15 parts of polyisoprene, 8 parts
Kaolin, 5 parts of zeolite powders and 5 parts of modified manometer silicon dioxides mix；The auxiliary material be 5 parts of modified multiwalled carbon nanotubes,
10 parts of TiN, 8 parts of ultra-high molecular weight polyethylene powder, the additive are 3 parts of epoxidized soybean oils, 3 parts of silane coupling agents, 2 modified silicons
Oil.
Further, the polyamide compoiste material also contains 3 parts of brighteners.
Further, 5 parts of TiC and 5 part of silicate platelets are also contained in the antifreeze mixing.
Further, 1.5 parts of polytetrafluoroethylene (PTFE) are also contained in the auxiliary material.
Further, 2 parts of Cocoamidopropyl betaines are also contained in the additive.
Further, a kind of low temperature resistant polyamide composite material, preparation method includes the following steps:
One) modified manometer silicon dioxide, modified multiwalled carbon nanotube and modified silicon oil are prepared
Ethyl orthosilicate and dehydrated alcohol are added in the three-necked flask equipped with dropping funel, dripped while stirring under the conditions of 50 DEG C
The dehydrated alcohol and deionized water mixed liquor of the volume ratio 1:1 of HCl dropwise mistake is added nano-silicon dioxide particle and continues after dripping off
It stirs, the ratio of nano silica, ethyl orthosilicate, dehydrated alcohol and acidification dehydrated alcohol and deionized water mixed liquor is
After reacting 12h, 5% methacryloxy relative to nano-silicon dioxide particle quality is added in 1g:2ml:10ml:3ml
Oxypropyl trimethyl silane continues to be stirred to react 6 h at 50 °C, modified manometer silicon dioxide colloidal sol is obtained, then 50
It is dried in vacuo under the conditions of DEG C, obtains modified manometer silicon dioxide, it is spare；
(a), multi-walled carbon nanotube is added in concentrated nitric acid, the ratio of the two is 1g:30ml, after 120 DEG C of reflux for 24 hours, spend from
Sub- water dilution, washing, filtering, and dry；(b), by (a) step drying material be added SOCl2 in, the two ratio be 1g:50ml, 70 DEG C
It flows back after 24 h, centrifugation is washed with CH2Cl2 and dried under the conditions of 80 DEG C；(c), melting 18 is added in (b) step drying material
In amine, the two mass ratio is 1:5, reacts 24 h at 90 DEG C, is then centrifuged product, and washed with dehydrated alcohol, finally, 80
DEG C drying obtains modified multiwalled carbon nanotube, spare；
N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, four silicon of prestox ring for being first 1:15:3:2 by ratio
Oxygen alkane, hexamethyldisiloxane and tetramethyl hydrogenation ammonia are uniformly mixed, nitrogen protection, stirring, under the conditions of 110 DEG C, heat preservation 6-8h,
135 DEG C are then heated to, 0.5h is reacted, then low-boiling-point substance 0.5h is taken off in 135 DEG C, 60KPa vacuum, obtains intermediate product；In taking
Between product and active polyether isopropanol is added, proportions 2g:1g:50ml is stirred evenly, 80 DEG C of reaction 5h, finally, in
135 DEG C, the agent of 60KPa vacuum desolvation and low-boiling-point substance 0.5h, obtain modified silicon oil, spare；
Two) preparation of composite material
Polyamide substrate, antifreeze mixing, auxiliary material, antioxidant and additive are added in batch mixer according to the above ratio first, mixed
0.5h is closed, double screw extruder, screw speed 300-450r/min, extruder machine then is added in uniformly mixed mixture
Temperature setting in cylinder are as follows: 240 DEG C of an area, 255 DEG C of 2nd area, 263 DEG C of 3rd area, 260 DEG C of 4th area, mixture are made through extruder extrusion
Low temperature resistant polyamide composite material is made in grain.
A specific embodiment of the invention, but scope of protection of the present invention is not limited thereto, it is any to be familiar with this field
Within the technical scope disclosed by the invention, changes or replacements that can be thought of without creative work should all be contained technical staff
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be to protect model defined by claims
Subject to enclosing.
Claims (6)
1. a kind of low temperature resistant polyamide composite material, it is characterised in that: be kneaded by following component with parts by weight: polyamide-based
50-70 parts of body, antifreeze mixing 10-15 parts, 5-7 parts of auxiliary material, 1-2 parts of antioxidant, 1-3 parts of additive;The antifreeze mixing by
10-15 parts of polyisoprene, 5-8 parts mix for kaolin, 3-5 parts of zeolite powders and 3-5 parts of modified manometer silicon dioxides；Institute
Auxiliary material is stated to form for 3-5 parts of modified multiwalled carbon nanotubes, 6-10 parts of TiN, 5-8 parts of ultra-high molecular weight polyethylene powder, it is described additional
Agent is 1-3 parts of epoxidized soybean oils, 1-3 parts of silane coupling agents, 1-2 modified silicon oil composition.
2. a kind of low temperature resistant polyamide composite material according to claim 1, it is characterised in that: the polyamide composite wood
Material also contains 1-3 parts of brighteners.
3. a kind of low temperature resistant polyamide composite material according to claim 1, it is characterised in that: in the antifreeze mixing also
Contain 3-5 parts of TiC and 3-5 parts of titanate lamellas.
4. a kind of low temperature resistant polyamide composite material according to claim 1, it is characterised in that: also contain in the auxiliary material
1-1.5 parts of polytetrafluoroethylene (PTFE).
5. a kind of low temperature resistant polyamide composite material according to claim 1, it is characterised in that: also contain in the additive
There are 1-2 parts of Cocoamidopropyl betaines.
6. a kind of low temperature resistant polyamide composite material described in -5 any one according to claim 1, it is characterised in that: described resistance to
The preparation method of low temperature polyamide compoiste material the following steps are included:
One) modified manometer silicon dioxide, modified multiwalled carbon nanotube and modified silicon oil are prepared
Ethyl orthosilicate and dehydrated alcohol are added in the three-necked flask equipped with dropping funel, dripped while stirring under the conditions of 50 DEG C
The dehydrated alcohol and deionized water mixed liquor of the volume ratio 1:1 of HCl dropwise mistake is added nano-silicon dioxide particle and continues after dripping off
It stirs, the ratio of nano silica, ethyl orthosilicate, dehydrated alcohol and acidification dehydrated alcohol and deionized water mixed liquor is
After reacting 12h, 5% methacryloxy relative to nano-silicon dioxide particle quality is added in 1g:2ml:10ml:3ml
Oxypropyl trimethyl silane continues to be stirred to react 6 h at 50 °C, modified manometer silicon dioxide colloidal sol is obtained, then 50
It is dried in vacuo under the conditions of DEG C, obtains modified manometer silicon dioxide, it is spare；
(a), multi-walled carbon nanotube is added in concentrated nitric acid, the ratio of the two is 1g:30ml, after 120 DEG C of reflux for 24 hours, spend from
Sub- water dilution, washing, filtering, and dry；(b), SOCl is added in (a) step drying material2In, the two ratio be 1g:50ml, 70 DEG C
It flows back after 24 h, is centrifuged, uses CH2Cl2It washs and is dried under the conditions of 80 DEG C；(c), melting 18 is added in (b) step drying material
In amine, the two mass ratio is 1:5, reacts 24 h at 90 DEG C, is then centrifuged product, and washed with dehydrated alcohol, finally, 80
DEG C drying obtains modified multiwalled carbon nanotube, spare；
N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, four silicon of prestox ring for being first 1:15:3:2 by ratio
Oxygen alkane, hexamethyldisiloxane and tetramethyl hydrogenation ammonia are uniformly mixed, nitrogen protection, stirring, under the conditions of 110 DEG C, heat preservation 6-8h,
135 DEG C are then heated to, 0.5h is reacted, then low-boiling-point substance 0.5h is taken off in 135 DEG C, 60KPa vacuum, obtains intermediate product；In taking
Between product and active polyether isopropanol is added, proportions 2g:1g:50ml is stirred evenly, 80 DEG C of reaction 5h, finally, in
135 DEG C, the agent of 60KPa vacuum desolvation and low-boiling-point substance 0.5h, obtain modified silicon oil, spare；
Two) preparation of composite material
Polyamide substrate, antifreeze mixing, auxiliary material, antioxidant and additive are added in batch mixer according to the above ratio first, mixed
0.5h is closed, double screw extruder, screw speed 300-450r/min, extruder machine then is added in uniformly mixed mixture
Temperature setting in cylinder are as follows: 240 DEG C of an area, 255 DEG C of 2nd area, 263 DEG C of 3rd area, 260 DEG C of 4th area, mixture are made through extruder extrusion
Low temperature resistant polyamide composite material is made in grain.
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| CN112679955A (en) * | 2020-12-29 | 2021-04-20 | 江苏中科聚合新材料产业技术研究院有限公司 | Low-temperature-resistant polyimide foam material, and preparation method and application thereof |
| CN113121995A (en) * | 2021-04-19 | 2021-07-16 | 江苏扬农化工集团有限公司 | Nylon composite material with wear-resisting and antistatic properties as well as preparation method and application thereof |
| CN115505937A (en) * | 2022-09-26 | 2022-12-23 | 江门市优彼思半导体材料有限公司 | Phosphorus-free oil removal powder and preparation method thereof |
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Application publication date: 20190906 |