CN103571180A - High-temperature-resistant nylon 66 and preparation method thereof - Google Patents
High-temperature-resistant nylon 66 and preparation method thereof Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention provides high-temperature-resistant nylon 66 and a preparation method thereof. The high-temperature-resistant nylon 66 comprises the following components in percentage by mass: 60-70% of polyphenyl diamide, 20-30% of glass fiber, 0.2-1.0% of antioxidant, 3-5% of toughening agent and 1-5% of silicon compound. The preparation method comprises the following steps: carrying out a prepolymerization reaction, namely in percentage by mass, mixing and stirring 60-70% of polyphenyl diamide, 20-30% of glass fiber, 0.2-1.0% of antioxidant, 3-5% of toughening agent and 1-5% of silicon compound to obtain a prepolymer, wherein a reaction temperature is 18-28 DEG C, and reaction time is 5-15 minutes; carrying out extrusion moulding on the prepolymer by virtue of a double screw extruder. By adopting the preparation method of the high-temperature-resistant nylon 66, strength and dimensional stability of the high-temperature-resistant nylon 66 can be improved, and more environment-friendly high-temperature-resistant nylon 66 can be produced.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to a kind of high temperature resistant nylon 66 and preparation method thereof.
Background technology
At present, polymeric amide (being commonly called as nylon 66) has great potentiality at electric, building materials and electronic industry, and the emerging parts such as building materials heat insulating strip have had very large growth to the demand of nylon 66 especially now.Due to the increase of the parts development trends such as building materials heat insulating strip, the temperature of electric, building materials and electronic industry element can rise quite highly, therefore needs nylon 66 to have resistant to elevated temperatures function.Nylon 66 of the prior art, conventionally by adding toughness reinforcing high temperature resistant dose, is realized the toughness reinforcing resistant to elevated temperatures performance of composite nylon 66.Yet toughness reinforcing high temperature resistant dose is easily caused certain pollution to environment, and it is poor in prior art, to be added with intensity and the dimensional stability of nylon 66 of toughness reinforcing high temperature resistant dose, has limited the application more widely of nylon 66.
In view of this, how designing a kind of high temperature resistant nylon 66 and preparation method thereof, to promote intensity and the dimensional stability of nylon 66, and reduce the pollution to environment, is the problem that insider needs solution badly.
Summary of the invention
In prior art, by adding the nylon 66 of the toughness reinforcing resistance to elevated temperatures of toughness reinforcing high temperature resistant dose of realization, easily environment is caused to certain pollution, and intensity and poor this defect of dimensional stability of being added with the nylon 66 of toughness reinforcing high temperature resistant dose, the invention provides a kind of high temperature resistant nylon 66 and preparation method thereof.
According to an aspect of the present invention, provide a kind of high temperature resistant nylon 66, wherein, by percentage to the quality, having comprised:
60～70% polyphenyl diamide;
20～30% glass fibre;
0.2～1.0% oxidation inhibitor;
3～5% toughner; And
1～5% silicide.
Preferably, described glass fibre is processed through silane coupling agent.
Preferably, the diameter of described glass fibre is 10～15 microns.
Preferably, the length of described glass fibre is 3～4 millimeters.
Preferably, described oxidation inhibitor is Switzerland's vapour bar irgasfos 168 or Switzerland's vapour bar antioxidant 1010.
Preferably, by percentage to the quality, more comprise:
0.1～1.0% anti-glass emergence on the surface agent; And
0.5～2.0% pentaerythritol resin.
According to another aspect of the present invention, proposed a kind of preparation method of above-mentioned high temperature resistant nylon 66, wherein, having comprised:
Prepolymerization reaction: by percentage to the quality, by the silicide mix and blend of 60～70% described polyphenyl diamide, 20～30% glass fibre, 0.2～1.0% oxidation inhibitor, 3～5% toughner and 1～5% to obtain prepolymer, temperature of reaction is 18～28 ℃, and the reaction times is 5～15 minutes; And
Described prepolymer is passed through to twin screw extruder extrusion moulding.
Preferably, in described prepolymerization reaction, can also add mass percent is the pentaerythritol resin that 0.1～1.0% anti-glass emergence on the surface agent and mass percent are 0.5～2.0%.
Preferably, before described prepolymerization reaction, more comprise: polyphenyl diamide described in drying treatment, so that the mass percent of water is 0～0.6% in described polyphenyl diamide.
Preferably, the temperature of described twin screw extruder is 290～300 ℃, and rotating speed is 280～300 revs/min.
Advantage of the present invention is: by polyphenyl diamide, glass fibre, irgasfos 168 or antioxidant 1010, toughner and silicide are mixed and produce high temperature resistant nylon 66, the chemical resistant properties and the easy advantage of processing that make high temperature resistant nylon 66 not only keep other nylon 66 to have, and under the effect of glass fibre and irgasfos 168 or antioxidant 1010, improved intensity and the dimensional stability of high temperature resistant nylon 66.In addition, owing to adopting toughner and silicide to realize the toughness reinforcing high-temperature resistant result of high temperature resistant nylon 66, and can produce the high temperature resistant nylon 66 of environmental protection more, high temperature resistant nylon 66 can be more widely used.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 shows the schema according to the preparation method of high temperature resistant nylon 66 of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Fig. 1 shows the schema according to the preparation method of high temperature resistant nylon 66 of the present invention.With reference to Fig. 1, the preparation method of high temperature resistant nylon 66 comprises the following steps:
Step S1: polyphenyl diamide, glass fibre, oxidation inhibitor, toughner and silicide are mixed in proportion and stir to obtain prepolymer.First, by percentage to the quality, 60～70% polyphenyl diamide, 20～30% glass fibre, 0.2～1.0% oxidation inhibitor, 3～5% toughner and 1～5% silicide are added in reactor, mix and blend, temperature of reaction is 18～28 ℃, reaction times is 5～15 minutes, after above-mentioned reactant reaction, forms prepolymer.Wherein, oxidation inhibitor can adopt Switzerland's vapour bar irgasfos 168 or Switzerland's vapour bar antioxidant 1010.Certainly, can also be that polyphenyl diamide, 20～30% glass fibre, 0.2～1.0% oxidation inhibitor, 3～5% toughner and 1～5% the silicide of 0.1～1.0% anti-glass emergence on the surface agent and the mass percent pentaerythritol resin that is 0.5～2.0% and 60～70% is mixed together stirring to adding mass percent in reactor, and reaction prepolymer.
Step S2: prepolymer is passed through to twin screw extruder extrusion moulding.Then, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 290～300 ℃, and rotating speed is 280～300 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
In addition, before step S1, can also carry out drying treatment by first p-poly-phenyl diamide, making the mass percent that in polyphenyl diamide, water accounts for is 0～0.6%.
Embodiment 1
First p-poly-phenyl diamide drying treatment, making the mass percent that in polyphenyl diamide, water accounts for is 0.6%.Then, by percentage to the quality, 65% polyphenyl diamide, 30% glass fibre, Switzerland's vapour bar irgasfos 168 of 1.0%, 3% toughner and 1% silicide are added in reactor, mix and blend, and temperature of reaction is 18 ℃, reaction times is 15 minutes, after above-mentioned reactant reaction, forms prepolymer.Finally, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 290 ℃, and rotating speed is 300 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
Embodiment 2
First p-poly-phenyl diamide drying treatment, making the mass percent that in polyphenyl diamide, water accounts for is 0.4%.Then, by percentage to the quality, 60% polyphenyl diamide, 35% glass fibre, Switzerland's vapour bar antioxidant 1010 of 1.0%, 3% toughner and 1% silicide are added in reactor, mix and blend, and temperature of reaction is 24 ℃, reaction times is 10 minutes, after above-mentioned reactant reaction, forms prepolymer.Finally, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 295 ℃, and rotating speed is 290 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
Embodiment 3
First p-poly-phenyl diamide drying treatment, making the mass percent that in polyphenyl diamide, water accounts for is 0.6%.Then, by percentage to the quality, 70% polyphenyl diamide, 25% glass fibre, Switzerland's vapour bar irgasfos 168 of 1.0%, 3% toughner and 1% silicide are added in reactor, mix and blend, and temperature of reaction is 28 ℃, reaction times is 5 minutes, after above-mentioned reactant reaction, forms prepolymer.Finally, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 300 ℃, and rotating speed is 280 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
Embodiment 4
First p-poly-phenyl diamide drying treatment, making the mass percent that in polyphenyl diamide, water accounts for is 0.6%.Then, by percentage to the quality, 62% polyphenyl diamide, 25% glass fibre, Switzerland's vapour bar antioxidant 1010 of 0.2%, 5% toughner, 5% silicide, 1.0% anti-glass emergence on the surface agent and 1.8% pentaerythritol resin are added in reactor, mix and blend, and temperature of reaction is 28 ℃, reaction times is 5 minutes, after above-mentioned reactant reaction, forms prepolymer.Finally, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 300 ℃, and rotating speed is 280 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
Embodiment 5
First p-poly-phenyl diamide drying treatment, making the mass percent that in polyphenyl diamide, water accounts for is 0.4%.Then, by percentage to the quality, 70% polyphenyl diamide, 20% glass fibre, Switzerland's vapour bar irgasfos 168 of 0.6%, 4% toughner, 3% silicide, 0.4% anti-glass emergence on the surface agent and 2.0% pentaerythritol resin are added in reactor, mix and blend, and temperature of reaction is 24 ℃, reaction times is 15 minutes, after above-mentioned reactant reaction, forms prepolymer.Finally, prepolymer is passed into twin screw extruder and squeeze, the temperature of twin screw extruder is 292 ℃, and rotating speed is 290 revs/min, and prepolymer is through twin screw extruder extrusion moulding.
Advantage of the present invention is: by polyphenyl diamide, glass fibre, irgasfos 168 or antioxidant 1010, toughner and silicide are mixed and produce high temperature resistant nylon 66, the chemical resistant properties and the easy advantage of processing that make high temperature resistant nylon 66 not only keep other nylon 66 to have, and under the effect of glass fibre and irgasfos 168 or antioxidant 1010, improved intensity and the dimensional stability of high temperature resistant nylon 66.In addition, owing to adopting toughner and silicide to realize the toughness reinforcing high-temperature resistant result of high temperature resistant nylon 66, and can produce the high temperature resistant nylon 66 of environmental protection more, high temperature resistant nylon 66 can be more widely used.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. a high temperature resistant nylon 66, is characterized in that, by percentage to the quality, comprising:
60～70% polyphenyl diamide;
20～30% glass fibre;
0.2～1.0% oxidation inhibitor;
3～5% toughner; And
1～5% silicide.
2. high temperature resistant nylon 66 as claimed in claim 1, is characterized in that, described glass fibre is processed through silane coupling agent.
3. high temperature resistant nylon 66 as claimed in claim 1, is characterized in that, the diameter of described glass fibre is 10～15 microns.
4. high temperature resistant nylon 66 as claimed in claim 1, is characterized in that, the length of described glass fibre is 3～4 millimeters.
5. the high temperature resistant nylon 66 as described in claim 1 to 4 any one, is characterized in that, described oxidation inhibitor is Switzerland's vapour bar irgasfos 168 or Switzerland's vapour bar antioxidant 1010.
6. high temperature resistant nylon 66 as claimed in claim 5, is characterized in that, by percentage to the quality, more comprises:
0.1～1.0% anti-glass emergence on the surface agent; And
0.5～2.0% pentaerythritol resin.
7. a preparation method for the high temperature resistant nylon 66 as described in claim 1 to 5 any one, is characterized in that, comprising:
Prepolymerization reaction: by percentage to the quality, by the silicide mix and blend of 60～70% described polyphenyl diamide, 20～30% glass fibre, 0.2～1.0% oxidation inhibitor, 3～5% toughner and 1～5% to obtain prepolymer, temperature of reaction is 18～28 ℃, and the reaction times is 5～15 minutes; And
Described prepolymer is passed through to twin screw extruder extrusion moulding.
8. the preparation method of high temperature resistant nylon 66 as claimed in claim 7, is characterized in that, in described prepolymerization reaction, can also add mass percent is the pentaerythritol resin that 0.1～1.0% anti-glass emergence on the surface agent and mass percent are 0.5～2.0%.
9. the preparation method of high temperature resistant nylon 66 as claimed in claim 7 or 8, is characterized in that, before described prepolymerization reaction, more comprises: polyphenyl diamide described in drying treatment, so that the mass percent of water is 0～0.6% in described polyphenyl diamide.
10. the preparation method of high temperature resistant nylon 66 as claimed in claim 9, is characterized in that, the temperature of described twin screw extruder is 290～300 ℃, and rotating speed is 280～300 revs/min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210285406.XA CN103571180A (en) | 2012-08-12 | 2012-08-12 | High-temperature-resistant nylon 66 and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210285406.XA CN103571180A (en) | 2012-08-12 | 2012-08-12 | High-temperature-resistant nylon 66 and preparation method thereof |
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| CN103571180A true CN103571180A (en) | 2014-02-12 |
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Citations (7)
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|---|---|---|---|---|
| CN1417257A (en) * | 2001-11-02 | 2003-05-14 | 上海杰事杰新材料股份有限公司 | Glass fiber reinforced blow molded nylon |
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| CN101724258A (en) * | 2008-10-31 | 2010-06-09 | 比亚迪股份有限公司 | Nylon composition, method for preparing same and application thereof |
| CN101781456A (en) * | 2010-03-17 | 2010-07-21 | 东莞劲胜精密组件股份有限公司 | Reinforced nylon material without floating fiber and preparation method thereof |
| CN101921474A (en) * | 2010-08-30 | 2010-12-22 | 青岛科柏利高性能聚合物有限公司 | Reinforced high-temperature nylon and preparation method thereof |
| US20110160378A1 (en) * | 2009-12-28 | 2011-06-30 | Cheil Industries Inc. | Polyamide Resin Composition with Good Reflectance, Impact Strength, Heat Resistance, and Water Resistance and Method of Preparing the Same |
| CN102482491A (en) * | 2009-07-17 | 2012-05-30 | 纳幕尔杜邦公司 | Semi aromatic polyamide resin compositions, processes for their manfacture and articles thereof |
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2012
- 2012-08-12 CN CN201210285406.XA patent/CN103571180A/en active Pending
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|---|---|---|---|---|
| CN1417257A (en) * | 2001-11-02 | 2003-05-14 | 上海杰事杰新材料股份有限公司 | Glass fiber reinforced blow molded nylon |
| CN1995142A (en) * | 2006-12-28 | 2007-07-11 | 深圳市科聚新材料有限公司 | Polyamide material and its preparing process |
| CN101724258A (en) * | 2008-10-31 | 2010-06-09 | 比亚迪股份有限公司 | Nylon composition, method for preparing same and application thereof |
| CN102482491A (en) * | 2009-07-17 | 2012-05-30 | 纳幕尔杜邦公司 | Semi aromatic polyamide resin compositions, processes for their manfacture and articles thereof |
| US20110160378A1 (en) * | 2009-12-28 | 2011-06-30 | Cheil Industries Inc. | Polyamide Resin Composition with Good Reflectance, Impact Strength, Heat Resistance, and Water Resistance and Method of Preparing the Same |
| CN101781456A (en) * | 2010-03-17 | 2010-07-21 | 东莞劲胜精密组件股份有限公司 | Reinforced nylon material without floating fiber and preparation method thereof |
| CN101921474A (en) * | 2010-08-30 | 2010-12-22 | 青岛科柏利高性能聚合物有限公司 | Reinforced high-temperature nylon and preparation method thereof |
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Application publication date: 20140212 |