CN106751751A - A kind of hydrophobic enhancing nylon composite materials - Google Patents
A kind of hydrophobic enhancing nylon composite materials Download PDFInfo
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- CN106751751A CN106751751A CN201611030218.7A CN201611030218A CN106751751A CN 106751751 A CN106751751 A CN 106751751A CN 201611030218 A CN201611030218 A CN 201611030218A CN 106751751 A CN106751751 A CN 106751751A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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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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- 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
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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
- C08L2312/00—Crosslinking
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- Chemical Kinetics & Catalysis (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention discloses a kind of hydrophobic enhancing nylon composite materials, its preparation process is as follows：Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- 3h of ultrasonic reaction 2 of constant temperature；Step 2, adds dispersant and ammonium persulfate, and sealed extruded reacts 3 5h after stirring, and obtains mixed resin liquid；Step 3, pressurization 3 6h of revolving are carried out by mixed resin liquid, obtain concentrate；Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and the 7h of HTHP banburying 3 is carried out after stirring；Step 5, inorganic filler is put into reactor, carries out the 2h of micro-current catalytic reaction 1；Step 6, after reaction terminates, 1 2h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.The inventive method is easy, and process conditions are gentle, low production cost, material structure stabilization, and without high temperature, cross-linking effect is good, property retention stabilization.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of hydrophobic enhancing nylon composite materials.
Background technology
Nylon is the important thermoplastic resin of a class.Nylon with the water-wet behavior for reducing can have less moisture absorption
Property, relatively low coefficient of friction and the enhanced property of softening and hydrophobicity.Modified, the common method in this area for nylon material
It is to be mixed into filler to be mixed into nylon matrix by the method for physics, chemistry.Generally, hydrophilic filler is used to improve nylon
Hydrophily, hydrophobic filler is used to be lifted the hydrophobicity of nylon.Hydrophobic siloxanes fluids are the common rear additives of nylon,
To reduce the hydrophily of siloxanes, even if they are more hydrophobic.However, by siloxanes fluids, such as dimethyl silicone polymer is added to
When in nylon, during conventional melt blending, siloxanes can be migrated in nylon matrix so that siloxanes is in matrix content
Easily formed and reunited, negatively affected some physical properties.
The content of the invention
It is an object of the invention to provide a kind of hydrophobic enhancing nylon composite materials, the inventive method is easy, process conditions temperature
With, low production cost, material structure stabilization, without high temperature, cross-linking effect is good, property retention stabilization.
A kind of hydrophobic enhancing nylon composite materials, its preparation process is as follows：
Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- ultrasonic reaction 2-3h of constant temperature；
Step 2, adds dispersant and ammonium persulfate, and sealed extruded reaction 3-5h, obtains mixed resin liquid after stirring；
Step 3, pressurization revolving 3-6h is carried out by mixed resin liquid, obtains concentrate；
Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and HTHP banburying is carried out after stirring
3-7h；
Step 5, inorganic filler is put into reactor, carries out micro-current catalytic reaction 1-2h；
Step 6, after reaction terminates, 1-2h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.
The formula of the material is as follows:
Organic siliconresin 11-13 parts, tetrafluoroethene 15-18 parts, water 20-25 parts, dispersant 2-4 parts, ammonium persulfate 4-6 parts, draw
1-3 parts, crosslinking agent 2-4 parts, nylon 20-25 parts, inorganic filler 8-12 parts of agent of hair.
The dispersant uses polyvinylpyrrolidone.
The initiator uses di-isopropyl peroxydicarbonate or di-cyclohexylperoxy di-carbonate.
The crosslinking agent uses cumyl peroxide.
The inorganic filler uses nano silicon or glass fibre.
Thermostat temperature is 40-60 DEG C in the step 1, and the reaction uses constant temperature water bath, the supersonic frequency of micro- ultrasound
Rate is 1.3-3.7kHz.
The reaction pressure of the sealed extruded reaction in the step 2 is 0.3-0.7MPa, and reaction temperature is 50-70 DEG C.
Moulding pressure in the step 3 is 2-13MPa, and the revolving temperature is 100-110 DEG C, and the concentrate is mixed
The 30-50% of resin liquid.
The step 4 high temperature temperature is 150-250 DEG C, and the high-pressure is 0.7-1.1MPa.
The micro-current reaction of the step 5 is reacted using stirring circulation, and the battery lead plate spacing of the micro-current reaction is
1.5-3.0cm, the pressure of the micro-current reaction is 1.3-3.3V, and the electric current of the micro-current reaction is 20-35mA.
Constant temperature mixing speed in the step 6 is 600-1000r/min, and thermostat temperature is 80-85 DEG C.
Compared with prior art, the invention has the advantages that：
1st, the inventive method is easy, and process conditions are gentle, low production cost, material structure stabilization, without high temperature, crosslinking
Effect is good, property retention stabilization.
2nd, the present invention is placed 1 year in the environment that temperature range is 25 DEG C, relative humidity is 40%, then uses OCAH200
Contact angle tester tests the wettability of the surface, as a result shows that the surface is not less than 150 ° with the contact angle of water, and roll angle is small
In 5 °.
3rd, the present invention increases the stagger ratio of composite using organic siliconresin and tetrafluoroethene cross-linking reaction, is crosslinked first
Resin material be crosslinked with nylon, increase three between bridging property, it is ensured that the Stability Analysis of Structures between three, finally using micro-
Electric current catalysis carries out interior cross-linking reaction, it is ensured that the stability of internal structure, stagger ratio is increased again, it is ensured that its hydrophobic performance is again
Secondary increase.
Specific embodiment
The present invention is described further with reference to embodiment：
Embodiment 1
A kind of hydrophobic enhancing nylon composite materials, its preparation process is as follows：
Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- ultrasonic reaction 2h of constant temperature；
Step 2, adds dispersant and ammonium persulfate, and sealed extruded reaction 3h, obtains mixed resin liquid after stirring；
Step 3, pressurization revolving 3h is carried out by mixed resin liquid, obtains concentrate；
Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and HTHP banburying is carried out after stirring
3h；
Step 5, inorganic filler is put into reactor, carries out micro-current catalytic reaction 1h；
Step 6, after reaction terminates, 1h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.
The formula of the material is as follows:
11 parts of organic siliconresin, 15 parts of tetrafluoroethene, 20 parts of water, 2 parts of dispersant, 4 parts of ammonium persulfate, 1 part of initiator, crosslinking agent
2 parts, 20 parts of nylon, 8 parts of inorganic filler.
The dispersant uses polyvinylpyrrolidone.
The initiator uses di-isopropyl peroxydicarbonate.
The crosslinking agent uses cumyl peroxide.
The inorganic filler uses nano silicon.
Thermostat temperature is 40 DEG C in the step 1, and the reaction uses constant temperature water bath, and micro- ultrasonic supersonic frequency is
1.3kHz。
The reaction pressure of the sealed extruded reaction in the step 2 is 0.3MPa, and reaction temperature is 50 DEG C.
Moulding pressure in the step 3 is 2MPa, and the revolving temperature is 100 DEG C, and the concentrate is hybrid resin
The 30% of liquid.
The step 4 high temperature temperature is 150 DEG C, and the high-pressure is 0.7MPa.
The micro-current reaction of the step 5 is reacted using stirring circulation, and the battery lead plate spacing of the micro-current reaction is
1.5cm, the pressure of the micro-current reaction is 1.3V, and the electric current of the micro-current reaction is 20mA.
Constant temperature mixing speed in the step 6 is 600r/min, and thermostat temperature is 80 DEG C.
Embodiment 2
A kind of hydrophobic enhancing nylon composite materials, its preparation process is as follows：
Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- ultrasonic reaction 3h of constant temperature；
Step 2, adds dispersant and ammonium persulfate, and sealed extruded reaction 5h, obtains mixed resin liquid after stirring；
Step 3, pressurization revolving 6h is carried out by mixed resin liquid, obtains concentrate；
Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and HTHP banburying is carried out after stirring
7h；
Step 5, inorganic filler is put into reactor, carries out micro-current catalytic reaction 2h；
Step 6, after reaction terminates, 2h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.
The formula of the material is as follows:
13 parts of organic siliconresin, 18 parts of tetrafluoroethene, 25 parts of water, 4 parts of dispersant, 6 parts of ammonium persulfate, 3 parts of initiator, crosslinking agent
4 parts, 25 parts of nylon, 12 parts of inorganic filler.
The dispersant uses polyvinylpyrrolidone.
The initiator uses di-cyclohexylperoxy di-carbonate.
The crosslinking agent uses cumyl peroxide.
The inorganic filler uses glass fibre.
Thermostat temperature is 60 DEG C in the step 1, and the reaction uses constant temperature water bath, and micro- ultrasonic supersonic frequency is
3.7kHz。
The reaction pressure of the sealed extruded reaction in the step 2 is 0.7MPa, and reaction temperature is 70 DEG C.
Moulding pressure in the step 3 is 13MPa, and the revolving temperature is 110 DEG C, and the concentrate is hybrid resin
The 50% of liquid.
The step 4 high temperature temperature is 250 DEG C, and the high-pressure is 1.1MPa.
The micro-current reaction of the step 5 is reacted using stirring circulation, and the battery lead plate spacing of the micro-current reaction is
3.0cm, the pressure of the micro-current reaction is 3.3V, and the electric current of the micro-current reaction is 35mA.
Constant temperature mixing speed in the step 6 is 1000r/min, and thermostat temperature is 85 DEG C.
Embodiment 3
A kind of hydrophobic enhancing nylon composite materials, its preparation process is as follows：
Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- ultrasonic reaction 2h of constant temperature；
Step 2, adds dispersant and ammonium persulfate, and sealed extruded reaction 4h, obtains mixed resin liquid after stirring；
Step 3, pressurization revolving 5h is carried out by mixed resin liquid, obtains concentrate；
Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and HTHP banburying is carried out after stirring
5h；
Step 5, inorganic filler is put into reactor, carries out micro-current catalytic reaction 2h；
Step 6, after reaction terminates, 1h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.
The formula of the material is as follows:
12 parts of organic siliconresin, 17 parts of tetrafluoroethene, 23 parts of water, 3 parts of dispersant, 5 parts of ammonium persulfate, 2 parts of initiator, crosslinking agent
3 parts, 23 parts of nylon, 10 parts of inorganic filler.
The dispersant uses polyvinylpyrrolidone.
The initiator uses di-isopropyl peroxydicarbonate.
The crosslinking agent uses cumyl peroxide.
The inorganic filler uses nano silicon.
Thermostat temperature is 50 DEG C in the step 1, and the reaction uses constant temperature water bath, and micro- ultrasonic supersonic frequency is
2.7kHz。
The reaction pressure of the sealed extruded reaction in the step 2 is 0.5MPa, and reaction temperature is 60 DEG C.
Moulding pressure in the step 3 is 8MPa, and the revolving temperature is 105 DEG C, and the concentrate is hybrid resin
The 35% of liquid.
The step 4 high temperature temperature is 220 DEG C, and the high-pressure is 0.9MPa.
The micro-current reaction of the step 5 is reacted using stirring circulation, and the battery lead plate spacing of the micro-current reaction is
2.3cm, the pressure of the micro-current reaction is 3V, and the electric current of the micro-current reaction is 25mA.
Constant temperature mixing speed in the step 6 is 800r/min, and thermostat temperature is 80 DEG C.
The composite of embodiment 1-3 is tested
| Embodiment | Contact angle | Roll angle | Rate of change |
| Embodiment 1 | 153° | 4.7° | 10% |
| Embodiment 2 | 160° | 4.6° | 11% |
| Embodiment 3 | 165° | 4.7° | 15% |
One embodiment of the invention is the foregoing is only, the side of the present invention, all use equivalents or equivalent transformation is not intended to limit
The technical scheme that formula is obtained, all falls within protection scope of the present invention.
Claims (10)
1. a kind of hydrophobic enhancing nylon composite materials, it is characterised in that its preparation process is as follows：
Step 1, during organic siliconresin and tetrafluoroethene added into reactor, and adds water, the micro- ultrasonic reaction 2-3h of constant temperature；
Step 2, adds dispersant and ammonium persulfate, and sealed extruded reaction 3-5h, obtains mixed resin liquid after stirring；
Step 3, pressurization revolving 3-6h is carried out by mixed resin liquid, obtains concentrate；
Step 4, nylon is added into reactor, adds initiator and crosslinking agent, and HTHP banburying is carried out after stirring
3-7h；
Step 5, inorganic filler is put into reactor, carries out micro-current catalytic reaction 1-2h；
Step 6, after reaction terminates, 1-2h is placed in constant temperature stirring, and natural cooling is that can obtain hydrophobic enhancing nylon composite materials.
2. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that the formula of the material is such as
Under:
Organic siliconresin 11-13 parts, tetrafluoroethene 15-18 parts, water 20-25 parts, dispersant 2-4 parts, ammonium persulfate 4-6 parts, draw
1-3 parts, crosslinking agent 2-4 parts, nylon 20-25 parts, inorganic filler 8-12 parts of agent of hair.
3. a kind of hydrophobic enhancing nylon composite materials according to claim 2, it is characterised in that the dispersant is using poly-
Vinylpyrrolidone, the initiator uses di-isopropyl peroxydicarbonate or di-cyclohexylperoxy di-carbonate.
4. a kind of hydrophobic enhancing nylon composite materials according to claim 2, it is characterised in that the crosslinking agent was used
Oxidation diisopropylbenzene (DIPB), the inorganic filler uses nano silicon or glass fibre.
5. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that constant temperature in the step 1
Temperature is 40-60 DEG C, and the reaction uses constant temperature water bath, and the supersonic frequency of micro- ultrasound is 1.3-3.7kHz.
6. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that close in the step 2
The reaction pressure for sealing extruding reaction is 0.3-0.7MPa, and reaction temperature is 50-70 DEG C.
7. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that it is in the step 3 plus
Pressure pressure is 2-13MPa, and the revolving temperature is 100-110 DEG C, and the concentrate is the 30-50% of mixed resin liquid.
8. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that step 4 high temperature
Temperature is 150-250 DEG C, and the high-pressure is 0.7-1.1MPa.
9. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that micro- electricity of the step 5
Using stirring circulation reaction, the battery lead plate spacing of the micro-current reaction is 1.5-3.0cm for stream reaction, the micro-current reaction
Pressure is 1.3-3.3V, and the electric current of the micro-current reaction is 20-35mA.
10. a kind of hydrophobic enhancing nylon composite materials according to claim 1, it is characterised in that the perseverance in the step 6
Warm mixing speed is 600-1000r/min, and thermostat temperature is 80-85 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611030218.7A CN106751751A (en) | 2016-11-22 | 2016-11-22 | A kind of hydrophobic enhancing nylon composite materials |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611030218.7A CN106751751A (en) | 2016-11-22 | 2016-11-22 | A kind of hydrophobic enhancing nylon composite materials |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030078998A (en) * | 2002-04-01 | 2003-10-10 | 주식회사 코오롱 | Glass fiber reinforced polyamide resin composition with excellent wear resistance |
| CN1714118A (en) * | 2002-10-24 | 2005-12-28 | 陶氏康宁公司 | Siloxane based amide modified nylons |
| CN101386681A (en) * | 2008-09-24 | 2009-03-18 | 华东理工大学 | Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof |
| CN102065823A (en) * | 2008-05-16 | 2011-05-18 | 雅芳产品公司 | Compositions for imparting superhydrophobicity |
| CN104046009A (en) * | 2014-06-20 | 2014-09-17 | 浙江衢州万能达科技有限公司 | Nylon 6-polytetrafluoroethylene composition |
| CN104804570A (en) * | 2014-01-24 | 2015-07-29 | 程威军 | Nanometer waterproof coating and preparation method thereof |
-
2016
- 2016-11-22 CN CN201611030218.7A patent/CN106751751A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030078998A (en) * | 2002-04-01 | 2003-10-10 | 주식회사 코오롱 | Glass fiber reinforced polyamide resin composition with excellent wear resistance |
| CN1714118A (en) * | 2002-10-24 | 2005-12-28 | 陶氏康宁公司 | Siloxane based amide modified nylons |
| CN102065823A (en) * | 2008-05-16 | 2011-05-18 | 雅芳产品公司 | Compositions for imparting superhydrophobicity |
| CN101386681A (en) * | 2008-09-24 | 2009-03-18 | 华东理工大学 | Hydrophobic organosilicon/polyamide 6block copolymers and in situ preparation method thereof |
| CN104804570A (en) * | 2014-01-24 | 2015-07-29 | 程威军 | Nanometer waterproof coating and preparation method thereof |
| CN104046009A (en) * | 2014-06-20 | 2014-09-17 | 浙江衢州万能达科技有限公司 | Nylon 6-polytetrafluoroethylene composition |
Non-Patent Citations (3)
| Title |
|---|
| 吴超 等: "《微颗粒黏附与清除》", 31 January 2014, 冶金工业出版社 * |
| 李光亮: "《有机硅高分子化学》", 31 March 1998, 科学出版社 * |
| 许伟 等: "新型交联网状端环氧基聚硅氧烷织物整理剂的制备工艺探讨", 《陕西科技大学学报》 * |
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Application publication date: 20170531 |