CN103881366A - High temperature resistant nylon nano composite material and preparation method thereof - Google Patents
High temperature resistant nylon nano composite material and preparation method thereof Download PDFInfo
- Publication number
- CN103881366A CN103881366A CN201210559817.3A CN201210559817A CN103881366A CN 103881366 A CN103881366 A CN 103881366A CN 201210559817 A CN201210559817 A CN 201210559817A CN 103881366 A CN103881366 A CN 103881366A
- Authority
- CN
- China
- Prior art keywords
- nylon
- salt
- parts
- carbon nano
- tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
-
- 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
-
- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- 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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention belongs to the field of high temperature resistant nylon composite material, and relates to a high temperature resistant nylon nano composite material and a preparation method thereof. The material is composed of the following components in parts by weight: 100 parts of nylon salt, 0.1 to 5 parts of carboxylated carbon nanotube, 0.1 to 1 part of blocking agent, 0.1 to 0.6 part of catalyst, and 30 to 60 parts of deionized water. An in-situ polymerization method is adopted to solve the problem that carboxylated carbon nanotubes are easy to agglomerate in matrix, and thus the performance of the interface between the carboxylated carbon nanotubes and the nylon matrix is improved, so that the mechanical performance of the composite material is improved. The prepared enhanced high temperature resistant nylon nano composite material has a better mechanical performance than that of pure nylon matrix. The preparation method is easy and practicable, and is suitable for industrial mass production.
Description
Technical field
The invention belongs to high temperature resistant nylon composite material field, relate to a kind of Nylon Nanocomposite and preparation method thereof.
Technical background
The development of high temperature resistant nylon changes into as possibility the more microminiaturized lightweight of industrial or agricultural and civilian installation and powerful.High temperature resistant nylon can bring higher heat resistance for some parts, or simply having substituted raw material metal produces these parts.The device of novel appts and assembly also useful high temperature resistant nylon replace the trend of metal and thermosetting material.These all will strengthen the requirement to high temperature resistant nylon material, thereby drive the market requirement.
Prepare carboxylic carbon nano-tube enhancing high temperature resistant nylon composite material and comprise solution blending, melt blending and in-situ blending etc.Wherein solution blending need to expend a large amount of solvents, is unfavorable for industrial application; Although melt blending can meet the needs of scale operation, carbon nanotube is bad dispersibility in matrix; And in-situ blending had both been applicable to industrial application and can makes good being dispersed in matrix of carbon nanotube, and can improve the interface performance between carbon nanotube and matrix.
Chinese patent CN200710171820.7 has announced a kind of carboxylic carbon nano-tube reinforced nylon 66 matrix materials, in the case of adding a small amount of carboxylic carbon nano-tube, the performance of matrix material is significantly improved, but there is no research in the reinforced effects of high-content carbon nanotube to matrix material more.Patent CN200410084741.9 has announced one and has prepared carbon nanotube Reinforced Nylon 1010 matrix materials by situ aggregation method.Have not been reported and prepare carboxylic carbon nano-tube enhancing high temperature resistant nylon composite material by the method for in-situ polymerization.
Summary of the invention
The defect the object of the invention is to for overcoming prior art provides a kind of good dispersity, and consistency is good, the enhancing high temperature resistant nylon nano composite material that mechanical property is improved.
Another object of the present invention is to provide the preparation method of above-mentioned enhancing high temperature resistant nylon nano composite material.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of Nylon Nanocomposite, made by the component that comprises following weight part:
Described carboxylic carbon nano-tube is preferably 0.5-3 part.
Described end-capping reagent is preferably 0.3-0.5 part.
Described catalyzer is preferably preferred 0.2-0.5 part.
Described deionized water is preferably 40-50 part.
Described nylon salt is selected from one or more in nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt, nylon 12T salt, nylon 6I salt, nylon 7I salt, nylon 8 I salt, nylon 9 I salt, nylon 10I salt, nylon 11 I salt or nylon 12I salt.
Its caliber of described carboxylic carbon nano-tube is 5-20nm, preferably 10nm, and its length is 0.5-20 μ m, preferably 5 μ m.
Described end-capping reagent is phenylformic acid, acetic acid, propionic acid or Tetra hydro Phthalic anhydride, preferably phenylformic acid.
Described catalyzer is sodium phosphate, trimagnesium phosphate, calcium phosphate, sodium phosphite, phosphorous acid magnesium, phosphorous acid calcium, one or more in zinc phosphite, inferior sodium phosphate, ortho phosphorous acid magnesium, Lime Hypophosphate or ortho phosphorous acid zinc, preferably inferior sodium phosphate.
A preparation method for above-mentioned Nylon Nanocomposite, is to adopt the method for in-situ polymerization to be prepared, and comprises the following steps:
(1) take 100 parts of nylon salts, 0.1-1 part end-capping reagent, 0.1-0.6 part catalyzer by said ratio, and above component is joined in autoclave;
Take 30-60 part deionized water, 0.1-5 part carboxylic carbon nano-tube, and carboxylic carbon nano-tube is dissolved in deionized water, ultrasonic agitation, then joins in autoclave;
(2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150-300 DEG C, pressure reaches 1.5-3MPa, keeps pressure at 1.5-3MPa by the way of water vapour in release reaction still, and the constant voltage reaction times is 1-3 hour; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
In described step (1), the time of ultrasonic agitation is 1-4 hour; Because carboxylic carbon nano-tube is easily reunited, by carboxylic carbon nano-tube is inserted, deionized water for stirring is also ultrasonic is uniformly dispersed it.
The present invention, by home position polymerization reaction, can improve the consistency between carboxylic carbon nano-tube and nylon matrix.
Advantage of the present invention is to have solved the shortcoming that carboxylic carbon nano-tube is easily reunited, and has improved the consistency of nylon and carboxylic carbon nano-tube, has prepared and has had the nano composite material high temperature resistant, mechanical property is high.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details:
Comparative example 1
1) take the nylon 10T salt of 100 parts, the deionized water of 50 parts, the phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Comparative example 2
1) take 100 parts of nylon pellets prepared by comparative example 1, take 3 parts of carboxylic carbon nano-tubes, by both by high mixer mixing 5min, add in twin screw extruder barrel, by twin screw extruder by carboxylic carbon nano-tube and nylon pellet melt blending, tie rod, pelletizing; ;
2) each section of temperature of twin screw extruder is: 270 DEG C, a district, and two 285 DEG C, districts, three 295 DEG C, districts, four 300 DEG C, districts, five 300 DEG C, districts, six 295 DEG C, districts, 295 DEG C of heads, screw speed is 200r/min;
Embodiment 1
1) take the nylon 10T salt of 100 parts, 0.5 part of end-capping reagent phenylformic acid, 0.4 part of catalyzer inferior sodium phosphate, and above component is joined in autoclave;
Take the deionized water of 50 parts, 3 parts of calibers are 10nm, length is the carboxylic carbon nano-tube of 5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 2
1) take the nylon 10T salt of 100 parts, the end-capping reagent phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 0.1 part of caliber is 5nm, length is the carboxylic carbon nano-tube of 0.5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 3
1) take the nylon 10T salt of 100 parts, the phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 5 parts of calibers are 20nm, length is the carboxylic carbon nano-tube of 20 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 4
1) take the nylon 9 T salt of 100 parts, the phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 3 parts of calibers are 10nm, length is the carboxylic carbon nano-tube of 0.5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 5
1) take the nylon 10I salt of 100 parts, the phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 1.5 parts of calibers are 10nm, length is the carboxylic carbon nano-tube of 0.5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 6
1) take the nylon 9 I salt of 100 parts, the phenylformic acid of 0.5 part, the inferior sodium phosphate of 0.4 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 2 parts of calibers are 10nm, length is the carboxylic carbon nano-tube of 1 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 7
1) take the nylon 6T salt of 70 parts, the nylon 12T salt of 30 parts, 0.7 part of end-capping reagent acetic acid, the Lime Hypophosphate of 0.3 part, and above component is joined in autoclave;
Take the deionized water of 50 parts, 3 parts of calibers are 20nm, length is the carboxylic carbon nano-tube of 5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 8
1) take the nylon 6T salt of 70 parts, the nylon 12T salt of 30 parts, 0.8 part of end-capping reagent propionic acid, the ortho phosphorous acid zinc of 0.5 part, and above component is joined in autoclave;
Take the deionized water of 35 parts, 1.5 parts of calibers are 5nm, length is the carboxylic carbon nano-tube of 20 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150 DEG C, and in 50min, make pressure reach 2.5MPa, keep pressure at 2.5MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 2 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 9
1) take the nylon 6T salt of 70 parts, the nylon 12T salt of 30 parts, the acetic acid of 0.7 part, the Lime Hypophosphate of 0.3 part, and above component is joined in autoclave;
Take the deionized water of 40 parts, 2 parts of calibers are 15nm, length is the carboxylic carbon nano-tube of 5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 160 DEG C, and in 60min, make pressure reach 3MPa, keep pressure at 3MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 1.5 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 10
1) take the nylon 7T salt of 50 parts, the nylon 7I salt of 50 parts, 0.1 part of end-capping reagent acetic acid, 0.6 part of catalyzer ortho phosphorous acid magnesium, and above component is joined in autoclave;
Take the deionized water of 30 parts, 1 part of caliber is 10nm, length is the carboxylic carbon nano-tube of 15 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 160 DEG C, and in 60min, make pressure reach 3MPa, keep pressure at 3MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 1.5 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
Embodiment 11
1) take the nylon 8 T salt of 40 parts, the nylon 8 I salt of 60 parts, the propionic acid of 1 part, 0.1 part of catalyzer Lime Hypophosphate, and above component is joined in autoclave;
Take the deionized water of 60 parts, 4 parts of calibers are 10nm, length is the carboxylic carbon nano-tube of 0.5 μ m and is dissolved in deionized water, is prepared into solution, preparation solution as for ultrasonic lower stirring 1-4 hour, then join in autoclave;
2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 160 DEG C, and in 60min, make pressure reach 3MPa, keep pressure at 3MPa by the way of water vapour in release reaction still, the constant voltage reaction times is 1.5 hours; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
The performance test results of high temperature resistant nylon/carboxylic carbon nano-tube matrix material that above-mentioned part embodiment and comparative example obtain sees the following form 1:
Table 1
As can be seen from the above table, add after carboxylic carbon nano-tube, tensile strength, flexural strength and the heat-drawn wire of nylon/carboxylic carbon nano-tube matrix material of preparing by melt-blending process are greatly improved, and nylon/carboxylic carbon nano-tube matrix material of preparing by situ aggregation method, its tensile strength, flexural strength and heat-drawn wire improve more obvious.Carboxylic carbon nano-tube good dispersity in nylon/carboxylic carbon nano-tube matrix material prepared by situ aggregation method is described, its consistency improves.Nylon/carboxylic carbon nano-tube matrix material has good mechanical property and thermotolerance, can be widely used in automotive industry and electric industry, especially needs in the field of high strength, high temperature material.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various amendments to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from improvement and the amendment that category of the present invention makes all should be within protection scope of the present invention.
Claims (8)
1. a Nylon Nanocomposite, is characterized in that: be made up of the component that comprises following weight part:
2. Nylon Nanocomposite according to claim 1, is characterized in that: described carboxylic carbon nano-tube is 0.5-3 part;
Or described end-capping reagent is 0.3-0.5 part;
Or described catalyzer is preferred 0.2-0.5 part;
Or described deionized water is 40-50 part.
3. Nylon Nanocomposite according to claim 1, is characterized in that: described nylon salt is selected from one or more in nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt, nylon 12T salt, nylon 6I salt, nylon 7I salt, nylon 8 I salt, nylon 9 I salt, nylon 10I salt, nylon 11 I salt or nylon 12I salt.
4. Nylon Nanocomposite according to claim 1, is characterized in that: its caliber of described carboxylic carbon nano-tube is 5-20nm, preferably 10nm; Its length is 0.5-20 μ m, preferably 5 μ m.
5. Nylon Nanocomposite according to claim 1, is characterized in that: described end-capping reagent is phenylformic acid, acetic acid, propionic acid or Tetra hydro Phthalic anhydride.
6. Nylon Nanocomposite according to claim 1, it is characterized in that: described catalyzer is sodium phosphate, trimagnesium phosphate, calcium phosphate, sodium phosphite, phosphorous acid magnesium, phosphorous acid calcium, one or more in zinc phosphite, inferior sodium phosphate, ortho phosphorous acid magnesium, Lime Hypophosphate or ortho phosphorous acid zinc.
7. a preparation method for arbitrary described Nylon Nanocomposite in the claims 1-6, is characterized in that: comprise the following steps:
(1) take 100 parts of nylon salts, 0.1-1 part end-capping reagent, 0.1-0.6 part catalyzer by proportioning claimed in claim 1, and above component is joined in autoclave;
Take 30-60 part deionized water, 0.1-5 part carboxylic carbon nano-tube, and carboxylic carbon nano-tube is dissolved in deionized water, ultrasonic agitation, then joins in autoclave;
(2) air in use nitrogen replacement autoclave at least three times, then passes into nitrogen as reaction protection gas; Be warming up to 150-300 DEG C, pressure reaches 1.5-3MPa, keeps pressure at 1.5-3MPa by the way of water vapour in release reaction still, and the constant voltage reaction times is 1-3 hour; Then by reacting kettle inner pressure pressure release to normal pressure, discharging, in reaction process, temperature in the kettle is no more than 330 DEG C.
8. preparation method according to claim 7, is characterized in that: in described step (1), the time of ultrasonic agitation is 1-4 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210559817.3A CN103881366A (en) | 2012-12-20 | 2012-12-20 | High temperature resistant nylon nano composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210559817.3A CN103881366A (en) | 2012-12-20 | 2012-12-20 | High temperature resistant nylon nano composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103881366A true CN103881366A (en) | 2014-06-25 |
Family
ID=50950514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210559817.3A Pending CN103881366A (en) | 2012-12-20 | 2012-12-20 | High temperature resistant nylon nano composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103881366A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669971A (en) * | 2016-04-08 | 2016-06-15 | 南京工业大学 | Preparation method of in-situ polymerized carbon nanotube modified nylon composite material |
| CN105885401A (en) * | 2016-04-20 | 2016-08-24 | 南京工业大学 | Graphene carbon nanotube bio-based nylon ternary composite material and preparation method thereof |
| CN105968804A (en) * | 2016-07-04 | 2016-09-28 | 黄河科技学院 | Flame-retardant and high-temperature-resistant nylon composite material and preparation method thereof |
| CN106118044A (en) * | 2016-07-04 | 2016-11-16 | 黄河科技学院 | Flame-resistant high-temperature-resistant Nylon Nanocomposite and preparation method thereof |
-
2012
- 2012-12-20 CN CN201210559817.3A patent/CN103881366A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669971A (en) * | 2016-04-08 | 2016-06-15 | 南京工业大学 | Preparation method of in-situ polymerized carbon nanotube modified nylon composite material |
| CN105669971B (en) * | 2016-04-08 | 2019-01-04 | 南京工业大学 | Preparation method of in-situ polymerized carbon nanotube modified nylon composite material |
| CN105885401A (en) * | 2016-04-20 | 2016-08-24 | 南京工业大学 | Graphene carbon nanotube bio-based nylon ternary composite material and preparation method thereof |
| CN105885401B (en) * | 2016-04-20 | 2018-08-17 | 南京工业大学 | Graphene carbon nanotube bio-based nylon ternary composite material and preparation method thereof |
| CN105968804A (en) * | 2016-07-04 | 2016-09-28 | 黄河科技学院 | Flame-retardant and high-temperature-resistant nylon composite material and preparation method thereof |
| CN106118044A (en) * | 2016-07-04 | 2016-11-16 | 黄河科技学院 | Flame-resistant high-temperature-resistant Nylon Nanocomposite and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1325556C (en) | Large hole nano-composite resin material and its preparation method | |
| CN103881366A (en) | High temperature resistant nylon nano composite material and preparation method thereof | |
| CN105085899A (en) | Graphene modified high-temperature-resisting nylon composite material | |
| CN102199265B (en) | Long carbon chain nylon modified phenolic resin and preparation method thereof | |
| CN1314749C (en) | Nano composite resin materials and method for preparing same | |
| CN107722595B (en) | Preparation method of fiber-graphene-thermoplastic polyarylether multi-scale composite material | |
| CN101195709B (en) | Method for producing high decentrality amido carbon nano-tube/nylon 66 composite material | |
| CN108912659B (en) | Preparation method of crosslinked three-dimensional carbon nano composite polyurethane material | |
| CN108250603B (en) | Carbon nano tube conductive modified polystyrene carrier tape material and preparation method thereof | |
| CN102311642A (en) | Calcium sulfate whisker modified nylon 66 composite material and preparation process thereof | |
| CN104371314B (en) | One kind is by graphene in-situ polymerization semi-aromatic polyamide resin and preparation method thereof | |
| CN102296279A (en) | Preparation method for carbon nanotube-aluminum oxide composite structure enhanced polyurethane based composite material | |
| CN101457019B (en) | Carbon nanotube/polysulfonamide nano composite material and preparation method thereof | |
| CN102617817A (en) | Organic complex composite phenolic resin of nickel and preparation method of organic complex composite phenolic resin | |
| CN105968804A (en) | Flame-retardant and high-temperature-resistant nylon composite material and preparation method thereof | |
| CN104804411A (en) | Low water absorption and high temperature resistance nylon composite material and preparation method thereof | |
| CN103160120A (en) | High-temperature-resistant nylon composite material and preparation method thereof | |
| CN103408927A (en) | Composite fiber modified nylon material and preparation method thereof | |
| CN101824200B (en) | Dendritic flame-retardant layered silicate and preparation method thereof | |
| CN103788624A (en) | Aramid fiber reinforced high temperature resistance nylon composite material and preparation method thereof | |
| CN103804893A (en) | Wear-resistant high-temperature resistant nylon nanocomposite | |
| CN101823000A (en) | Method for preparing poly(p-styrene) sulphonate grafted modified carbon nano tube | |
| CN104419363A (en) | Method for producing phenolic resin-nitrile rubber adhesive | |
| CN101565535A (en) | Heat resistant epoxide resin and preparation method thereof | |
| CN103804900A (en) | High-temperature-resistant semi-aromatic nylon nanocomposite and its preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140625 |