CN106519428A - Carbon nanotube reinforced polymer composite material and preparation method thereof - Google Patents
Carbon nanotube reinforced polymer composite material and preparation method thereof Download PDFInfo
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- CN106519428A CN106519428A CN201610917935.5A CN201610917935A CN106519428A CN 106519428 A CN106519428 A CN 106519428A CN 201610917935 A CN201610917935 A CN 201610917935A CN 106519428 A CN106519428 A CN 106519428A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a carbon nanotube reinforced polymer composite material. The carbon nanotube reinforced polymer composite material is prepared from the following raw materials in parts by weight: 1 to 2 parts of antimony trioxide, 6 to 9 parts of carbon nanotube, 110 to 130 parts of high-density polypropylene, 2 to 3 parts of dihydration gypsum powder, 3 to 4 parts of diphenyl silanediol, 0.4 to 1 part of 2-mercapto benzimidazole, 3 to 5 parts of diethylene glycol dibenzoate, 1 to 2 parts of tetrabutylammonium bromide, 0.7 to 1 part of fatty acid diethanol amide, 1 to 2 parts of aluminum ammonium sulfate, 0.8 to 1 part of p-methylbenzene sulfonic acid, 0.5 to 1 part of ethoxylated alkylphenol ammonium sulfate, 0.4 to 1 part of methyl triethoxysilane, 2 to 3 parts of sodium myrastate and 0.1 to 0.2 part of ammonium ferrous sulfate. The finished product has very high mechanical performance, high surface hydrophobicity and superior comprehensive performance.
Description
Technical field
The invention belongs to Material Field, is related to the composite of polymer, more particularly to a kind of CNT reinforcement poly
Thing composite and preparation method thereof.
Background technology
Polypropylene is nontoxic, tasteless, and density is little, and intensity, rigidity, hardness heat resistance are superior to low-pressure polyethylene, can be at 100 DEG C
Left and right uses.Do not affected with good dielectric properties and high-frequency insulation and by humidity, but become fragile during low temperature, it is not wear-resisting, easy
It is aging.It is suitable to make common mechanical part, corrosion-resistant part and insulating part.The organic solvents such as common acid, alkali to it almost
Do not work, can be used for tableware；Then it is how that filler grain is preferably compatible with polypropylene, it is to determine composite material quality
Key factor, affects the main color of key factor of Polymer inorganic nanocomposite performance to include：Inorganic nano-particle be polymerized
Capacitive between thing matrix；Dispersity of the nano-particle in polymeric matrix；Between the two interface and interaction.However,
Due to the reuniting effect of nano-particle itself, which is caused in being difficult to be evenly dispersed in polymeric matrix, to form nano combined material
Material.Therefore, in order to improve dispersion of the inorganic nano-particle in polymeric matrix and interface Interaction Force, it usually needs right
Inorganic nano-particle surface carries out covalently or non-covalently key functional modification.Covalent bond functional modification be presently the most extensively,
Effectively method of modifying, is compared to non-covalent bond and is modified, and modifier molecules mainly pass through covalent bond effect and inorganic nano-particle
Son links together, its strong, Stability Analysis of Structures that interacts.Simultaneously can also be by covalent modification on inorganic nano-particle surface
Active function groups or site is introduced, polymer nanocomposites is prepared by grafting or in-situ polymerization further, favorably
In obtaining, good dispersion, interaction force be strong, excellent performance polymer nanocomposites.
The content of the invention
It is an object of the invention to improve filler grain dispersiveness in the polymer, the stability of finished product is improved, there is provided
A kind of CNT reinforcement polymer composite and preparation method thereof.
For achieving the above object, the present invention is employed the following technical solutions：
A kind of CNT reinforcement polymer composite, it is made up of the raw material of following weight parts：
Antimony oxide 1-2, CNT 6-9, high density poly propylene 110-130, dihydrate gypsum powder 2-3, diphenyl silicon
Glycol 3-4,2-mercaptobenzimidazole 0.4-1, diethylene glycol dibenzoate 3-5, TBAB 1-2, aliphatic acid diethanol
Acid amides 0.7-1, alum 1-2, p-methyl benzenesulfonic acid 0.8-1, ethoxylated alkylphenol ammonium sulfate 0.5-1, three ethoxy of methyl
Base silane 0.4-1, myristic acid soda soap 2-3, iron ammonium sulfate 0.1-0.2.
A kind of preparation method of CNT reinforcement polymer composite, comprises the following steps：
(1) above-mentioned CNT is added in the salpeter solution of 96-98%, soaks 1-2 hours, filtered, water will be precipitated
Wash 3-4 time, air drying, mix with above-mentioned p-methyl benzenesulfonic acid, be added in the deionized water of compound weight 10-13 times,
The insulated and stirred 40-50 minute at 57-60 DEG C, above-mentioned iron ammonium sulfate is added, stirring reaction 20-30 minute, is filtered, will precipitation
Washing 2-3 time, is vacuum dried 1-2 hours at 60-65 DEG C, obtains modified carbon nano-tube；
(2) above-mentioned 2-mercaptobenzimidazole is added in the absolute ethyl alcohol of its weight 10-14 times, is stirred, raised
Temperature is 65-70 DEG C, insulated and stirred 20-30 minute, adds above-mentioned fatty diglycollic amide, stirs to normal temperature, obtain amide alcohol
Dispersion liquid；
(3) above-mentioned alum, dihydrate gypsum powder are mixed, are added in the deionized water of compound weight 10-14 times,
The insulated and stirred 10-20 minute at 70-75 DEG C, ethoxylated alkylphenol ammonium sulfate is added, is stirred to normal temperature, with above-mentioned three oxidations
Two antimony mix, and send in baking oven, are dried complete, discharging cooling, mix with above-mentioned modified carbon nano-tube, ball milling, obtain modified
Filler；
(4) above-mentioned myristic acid soda soap is added in the absolute ethyl alcohol of its weight 30-40 times, liter high-temperature is 76-80
DEG C, amide alcohol dispersion liquid, adds above-mentioned diphenyl silanediol, MTES at insulated and stirred 3-5 minute, continues to protect
Warm stirring 10-15 minutes, above-mentioned modified filler is added, ultrasonic 10-13 minutes, is filtered, precipitation is washed 2-3 time, air drying,
Obtain silane-modified filler；
(5) above-mentioned silane-modified filler is mixed with remaining each raw material, is stirred, send into extruder, melting extrusion is cold
But, obtain final product the composite.
Advantages of the present invention：
The CNT that the present invention is added can effectively improve the intensity and toughness of finished composite material, of the invention by silicon
Alkanol liquid and the mixed and modified filler of amide alcohol dispersion liquid, can effectively improve filler grain dispersiveness in the polymer, carry
The stability_intensity of high finished product, the finished product of the present invention have good mechanical property, surface hydrophobic good, and combination property is superior.
Specific embodiment
Embodiment 1
A kind of CNT reinforcement polymer composite, it is made up of the raw material of following weight parts：
Antimony oxide 1, CNT 9, high density poly propylene 130, dihydrate gypsum powder 3, diphenyl silanediol 4,2- mercaptos
Base benzimidazole 0.4, diethylene glycol dibenzoate 5, TBAB 1, fatty diglycollic amide 0.7, alum 1,
P-methyl benzenesulfonic acid 0.8, ethoxylated alkylphenol ammonium sulfate 0.5, MTES 0.4, myristic acid soda soap 2, sulphur
Sour ferrous ammonium 0.2.
A kind of preparation method of CNT reinforcement polymer composite, comprises the following steps：
(1) above-mentioned CNT is added in the salpeter solution of 96-98%, is soaked 1 hour, filtered, by precipitation washing 3
Secondary, air drying is mixed with above-mentioned p-methyl benzenesulfonic acid, is added in the deionized water of 13 times of compound weight, at 60 DEG C
Insulated and stirred 50 minutes, adds above-mentioned iron ammonium sulfate, stirring reaction 30 minutes to filter, by precipitation washing 2 times, at 65 DEG C
Vacuum drying 2 hours, obtains modified carbon nano-tube；
(2) above-mentioned 2-mercaptobenzimidazole is added in the absolute ethyl alcohol of 14 times of its weight, is stirred, rise high-temperature
For 70 DEG C, insulated and stirred 20 minutes adds above-mentioned fatty diglycollic amide, stirs to normal temperature, obtain amide alcohol dispersion liquid；
(3) above-mentioned alum, dihydrate gypsum powder are mixed, is added in the deionized water of 14 times of compound weight,
Insulated and stirred 20 minutes at 75 DEG C, add ethoxylated alkylphenol ammonium sulfate, stir to normal temperature, mixed with above-mentioned antimony oxide
Close, send in baking oven, be dried complete, discharging cooling, mix with above-mentioned modified carbon nano-tube, ball milling obtains modified filler；
(4) above-mentioned myristic acid soda soap is added in the absolute ethyl alcohol of 40 times of its weight, it is 80 DEG C to rise high-temperature, is added
Above-mentioned amide alcohol dispersion liquid, insulated and stirred 3 minutes add above-mentioned diphenyl silanediol, MTES, continue insulation
Stirring 15 minutes, adds above-mentioned modified filler, ultrasound 13 minutes to filter, and by precipitation washing 2-3 time, air drying obtains silane and changes
Property filler；
(5) above-mentioned silane-modified filler is mixed with remaining each raw material, is stirred, send into extruder, melting extrusion is cold
But, obtain final product the composite.
Performance test：
Tensile strength 25.1MPa；
Elongation at break 354%.
Claims (2)
1. a kind of CNT reinforcement polymer composite, it is characterised in that it is made up of the raw material of following weight parts：
Antimony oxide 1-2, CNT 6-9, high density poly propylene 110-130, dihydrate gypsum powder 2-3, diphenyl silanediol
3-4,2-mercaptobenzimidazole 0.4-1, diethylene glycol dibenzoate 3-5, TBAB 1-2, fatty diglycollic amide
0.7-1, alum 1-2, p-methyl benzenesulfonic acid 0.8-1, ethoxylated alkylphenol ammonium sulfate 0.5-1, methyltriethoxy silane
Alkane 0.4-1, myristic acid soda soap 2-3, iron ammonium sulfate 0.1-0.2.
2. a kind of preparation method of CNT reinforcement polymer composite as claimed in claim 1, it is characterised in that bag
Include following steps：
(1) above-mentioned CNT is added in the salpeter solution of 96-98%, soaks 1-2 hours, filtered, by precipitation washing 3-4
Secondary, air drying is mixed with above-mentioned p-methyl benzenesulfonic acid, is added in the deionized water of compound weight 10-13 times, in 57-
Insulated and stirred 40-50 minute at 60 DEG C, above-mentioned iron ammonium sulfate is added, stirring reaction 20-30 minute, is filtered, by precipitation washing
2-3 time, 1-2 hours are vacuum dried at 60-65 DEG C, modified carbon nano-tube is obtained；
(2) above-mentioned 2-mercaptobenzimidazole is added in the absolute ethyl alcohol of its weight 10-14 times, is stirred, rise high-temperature
For 65-70 DEG C, insulated and stirred 20-30 minute, above-mentioned fatty diglycollic amide is added, is stirred to normal temperature, obtain amide alcohol dispersion
Liquid；
(3) above-mentioned alum, dihydrate gypsum powder are mixed, is added in the deionized water of compound weight 10-14 times,
Insulated and stirred 10-20 minute at 70-75 DEG C, ethoxylated alkylphenol ammonium sulfate is added, is stirred to normal temperature, with above-mentioned three oxidations two
Antimony mixes, and sends in baking oven, is dried complete, discharging cooling, mixes with above-mentioned modified carbon nano-tube, ball milling, must be modified and fill out
Material；
(4) above-mentioned myristic acid soda soap is added in the absolute ethyl alcohol of its weight 30-40 times, it is 76-80 DEG C to rise high-temperature, acyl
Amine alcohol dispersion liquid, insulated and stirred 3-5 minute, adds above-mentioned diphenyl silanediol, MTES, continues insulated and stirred
10-15 minutes, above-mentioned modified filler is added, ultrasonic 10-13 minutes, is filtered, by precipitation washing 2-3 time, air drying obtains silane
Modified filler；
(5) above-mentioned silane-modified filler is mixed with remaining each raw material, is stirred, send into extruder, melting extrusion is cooled down,
Obtain final product the composite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610917935.5A CN106519428A (en) | 2016-10-21 | 2016-10-21 | Carbon nanotube reinforced polymer composite material and preparation method thereof |
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| CN201610917935.5A CN106519428A (en) | 2016-10-21 | 2016-10-21 | Carbon nanotube reinforced polymer composite material and preparation method thereof |
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| CN106519428A true CN106519428A (en) | 2017-03-22 |
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| CN201610917935.5A Pending CN106519428A (en) | 2016-10-21 | 2016-10-21 | Carbon nanotube reinforced polymer composite material and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1643620A (en) * | 2002-03-18 | 2005-07-20 | 阿托菲纳研究公司 | Conductive polyolefins with good mechanical properties |
| CN1654528A (en) * | 2005-01-27 | 2005-08-17 | 中国石油化工股份有限公司 | Carbon nanotube/polypropylene composite materials and process for preparing same |
-
2016
- 2016-10-21 CN CN201610917935.5A patent/CN106519428A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1643620A (en) * | 2002-03-18 | 2005-07-20 | 阿托菲纳研究公司 | Conductive polyolefins with good mechanical properties |
| CN1654528A (en) * | 2005-01-27 | 2005-08-17 | 中国石油化工股份有限公司 | Carbon nanotube/polypropylene composite materials and process for preparing same |
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Application publication date: 20170322 |
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