CN106479172A - Halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite and preparation method thereof - Google Patents
Halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite and preparation method thereof Download PDFInfo
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- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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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Abstract
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite is it is characterised in that be made up of the component of following parts by weight：Nylon 6T 30 60, roving glass fiber 20 40, DOPO 13 18, antioxidant 0.5 1, compatilizer 5 10, triazine carbon forming agent 35, synergist 15, polypropene staple 35, potassium carbonate whisker 0.5 1, Pulvis Talci 24, carborundum 13, nucleator 0.5 1, viscosifier 14, microwax 0.5 1, dioctyl phthalate 13.Instant component is relatively simple, reasonable mixture ratio, by adding nucleator, viscosifier, polymer heterogeneous nucleation can be made, improve resistance to elevated temperatures, wearability and the processing characteristics of material, thus changing the intrinsic viscosity of polyester, fusing point and its molecular chain structure, improving the quality of PA6T melt, strengthening the bulk strength of PA6T material.
Description
Technical field
The present invention relates to halogen-free flame-retardant polymer technical field of composite materials is and in particular to a kind of halogen-free flameproof roving glass fiber increases
High temperature resistant PA6T composite and preparation method thereof by force.
Background technology
Nylon (polyamide) is a kind of current domestic and international application most widely thermoplastic engineering plastic, and it has tough resistance to
The excellent specific properties such as mill, impact resistance, endurance, corrosion-resistant, oil resistant, are widely used in auto-parts, electronic apparatus, machinery etc.
Industry, over 60 years, steady-state growth in the keen competition of engineering plastics, its demand occupies five large-engineering plastics so far always
First place.
At present, on market, the fire retardant of fiberglass reinforced PA 6T mainly has bromine antimony based flame retardant, red phosphorus combustion inhibitor, the resistance of phosphorus nitrogen system
Combustion agent etc..Although bromine antimony based flame retardant has preferable fire resistance and mechanical property, its environmental issue cannot overcome
Technical barrier；The storage of red phosphorus based flame retardant is difficult, and can only do dark product；Phosphorus-nitrogen containing flame retardant develops as current fire retardant
Direction, receive more concern.However, the phosphorus-nitrogen containing flame retardant on market has a decomposition temperature low, production cost height etc.
Problem, is extremely limited in the application of market.In prior art, have using MPP (tripolycyanamide phosphonate) flame-proof glass fibre
Strengthen the pertinent literature of PA6T, but it exists that decomposition temperature is low, plastic processing performance is poor, mechanical properties decrease is seriously etc. many
Technical problem.
Content of the invention
The technical problem to be solved is to provide a kind of mechanical property good, the high halogen-free flameproof roving glass fiber of intensity
Strengthen high temperature resistant PA6T composite.
The technical problem to be solved employs the following technical solutions to realize：
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite, is made up of the component of following parts by weight：Buddhist nun
Imperial 6T 30-60, roving glass fiber 20-40, DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) 13-18, antioxidant
0.5-1, compatilizer 5-10, triazine carbon forming agent 3-5, synergist 1-5, polypropene staple 3-5, potassium carbonate whisker 0.5-1, Talcum
Powder 2-4, carborundum 1-3, nucleator 0.5-1, viscosifier 1-4, microwax 0.5-1, dioctyl phthalate 1-3.
Described synergist selects quaternary alkylphosphonium salt intercalation modifying montmorillonite.
Irgasfos 168/1098 selected by described antioxidant.
Described triazine carbon forming agent selects CFA triazine carbon forming agent.
Described nucleator is selected in poly- 3- methyl butene -1, polyvinyl cyclosilane, polyvinyl cycloalkanes, poly- propane
The mixture of one or more.
Above-mentioned viscosifier are made up of the component of following weight：Ethylene glycol 80g, platinum compounds 2g, silane coupler 2g, benzene
Formic acid sodium salt 2g, Colophonium 5g, n-butyl acrylate 3g, lauryl mercaptan 3g, lac resin 4g, microwax 2g, nanoscale electricity
Gas stone powder body 3g, pure-acrylic emulsion 5g；This viscosifier is specifically designed for regeneration PA6T melt and is configured, and the speed of viscosity increasement is fast, and effect is good.
The preparation method of above-mentioned viscosifier is as follows：
(1) weigh each component by above-mentioned formula ratio, first ethylene glycol, n-butyl acrylate and lauryl mercaptan are put into
In reactor, it is heated to 50-60 DEG C, in 120-135 rev/min of rotating speed, continuous stirring 5-10 minute, obtained solution a is stand-by；
(2) benzoic acid sodium salt, Colophonium, lac resin, microwax and nano-scale tourmaline powder are added in solution a,
Heat while stirring, reach 80-90 DEG C to temperature and be incubated 2 hours, obtained solution b is stand-by；
Above-mentioned mixing speed controls at 90-110 rev/min.
(3) pure-acrylic emulsion is put in solution b, stir, mixing speed is maintained at 1200 revs/min about, stirring
30 minutes, obtained solution c was stand-by；
(4) by the temperature control of solution c at 40-45 DEG C, it is subsequently adding platinum compounds and silane coupler, stirs,
It is cooled to room temperature, go out kettle and obtain viscosifier.
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite one-step preppn process, step is as follows：
(1) polypropene staple, potassium carbonate whisker, Pulvis Talci, carborundum and synergist are sent in rotary drum and mixed
Rotary drum is heated up to 80-120 DEG C by stirring simultaneously, and pressure, in 150-200Mpa, took out and obtained compound at 40 minutes the time；
(2) nylon 6T and dioctyl phthalate are mixed, conveyed by mouth mould after being plastified by single screw extrusion machine
To high-temperature fusant reactor, add compound, DOPO, antioxidant, compatilizer, triazine carbon forming agent, nucleator, viscosifier and crystallite
Wax, keeps kettle temperature under the conditions of 235～240 DEG C, pressure 2.0～2.5MPa, obtains blend melt；
(3) blend melt is sent to dipping head, the temperature of dipping head is set as 280-360 DEG C, roving glass fiber is led to
Cross dipping head die hole, after dipping, pulled out dipping head, cooling, pelletizing, the enhancing obtaining 8-15mm length is high temperature resistant
PA6T composite.
The invention has the beneficial effects as follows：Instant component is relatively simple, reasonable mixture ratio, by adding nucleator, viscosifier,
Polymer heterogeneous nucleation can be made, improve resistance to elevated temperatures, wearability and the processing characteristics of material, thus the characteristic changing polyester is glued
Degree, fusing point and its molecular chain structure, improve the quality of PA6T melt, strengthen the bulk strength of PA6T material.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention realizes are easy to understand, tie below
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite, is made up of the component of following weight：Nylon 6T
45kg, roving glass fiber 30kg, DOPO 15kg, antioxidant 0.8kg, compatilizer 7.5kg, triazine carbon forming agent 4kg, synergist 3.5kg,
Polypropene staple 4kg, potassium carbonate whisker 0.75kg, Pulvis Talci 3kg, carborundum 2kg, nucleator 0.75kg, viscosifier
2.5kg, microwax 0.75kg, dioctyl phthalate 2kg.
Described synergist selects quaternary alkylphosphonium salt intercalation modifying montmorillonite.
Irgasfos 168 selected by described antioxidant.
Described triazine carbon forming agent selects CFA triazine carbon forming agent.
Poly- 3- methyl butene -1 selected by described nucleator.
Above-mentioned viscosifier are made up of the component of following weight：Ethylene glycol 80g, platinum compounds 2g, silane coupler 2g, benzene
Formic acid sodium salt 2g, Colophonium 5g, n-butyl acrylate 3g, lauryl mercaptan 3g, lac resin 4g, microwax 2g, nanoscale electricity
Gas stone powder body 3g, pure-acrylic emulsion 5g；This viscosifier is specifically designed for regeneration PA6T melt and is configured, and the speed of viscosity increasement is fast, and effect is good.
The preparation method of above-mentioned viscosifier is as follows：
(1) weigh each component by above-mentioned formula ratio, first ethylene glycol, n-butyl acrylate and lauryl mercaptan are put into
In reactor, it is heated to 50-60 DEG C, in 120-135 rev/min of rotating speed, continuous stirring 5-10 minute, obtained solution a is stand-by；
(2) benzoic acid sodium salt, Colophonium, lac resin, microwax and nano-scale tourmaline powder are added in solution a,
Heat while stirring, reach 80-90 DEG C to temperature and be incubated 2 hours, obtained solution b is stand-by；
Above-mentioned mixing speed controls at 90-110 rev/min.
(3) pure-acrylic emulsion is put in solution b, stir, mixing speed is maintained at 1200 revs/min about, stirring
30 minutes, obtained solution c was stand-by；
(4) by the temperature control of solution c at 40-45 DEG C, it is subsequently adding platinum compounds and silane coupler, stirs,
It is cooled to room temperature, go out kettle and obtain viscosifier.
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite one-step preppn process, step is as follows：
(1) polypropene staple, potassium carbonate whisker, Pulvis Talci, carborundum and synergist are sent in rotary drum and mixed
Rotary drum is heated up to 80-120 DEG C by stirring simultaneously, and pressure, in 150-200Mpa, took out and obtained compound at 40 minutes the time；
(2) nylon 6T and dioctyl phthalate are mixed, conveyed by mouth mould after being plastified by single screw extrusion machine
To high-temperature fusant reactor, add compound, DOPO, antioxidant, compatilizer, triazine carbon forming agent, nucleator, viscosifier and crystallite
Wax, keeps kettle temperature under the conditions of 235～240 DEG C, pressure 2.0～2.5MPa, obtains blend melt；
(3) blend melt is sent to dipping head, the temperature of dipping head is set as 280-360 DEG C, roving glass fiber is led to
Cross dipping head die hole, after dipping, pulled out dipping head, cooling, pelletizing, the enhancing obtaining 8-15mm length is high temperature resistant
PA6T composite.
Embodiment 2
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite, is made up of the component of following weight：Nylon 6T
60kg, roving glass fiber 20kg, DOPO 18kg, antioxidant 0.5kg, compatilizer 10kg, triazine carbon forming agent 3kg, synergist 5kg, poly- third
Alkene chopped fiber 3kg, potassium carbonate whisker 1kg, Pulvis Talci 2kg, carborundum 3kg, nucleator 0.5kg, viscosifier 4kg, microwax
0.5kg, dioctyl phthalate 3kg.
Described synergist selects quaternary alkylphosphonium salt intercalation modifying montmorillonite.
Antioxidant 1098 selected by described antioxidant.
Described triazine carbon forming agent selects CFA triazine carbon forming agent.
Polyvinyl cyclosilane selected by described nucleator.
Above-mentioned viscosifier are made up of the component of following weight：Ethylene glycol 80g, platinum compounds 2g, silane coupler 2g, benzene
Formic acid sodium salt 2g, Colophonium 5g, n-butyl acrylate 3g, lauryl mercaptan 3g, lac resin 4g, microwax 2g, nanoscale electricity
Gas stone powder body 3g, pure-acrylic emulsion 5g；This viscosifier is specifically designed for regeneration PA6 melt and is configured, and the speed of viscosity increasement is fast, and effect is good.
The preparation method of above-mentioned viscosifier is as follows：
(1) weigh each component by above-mentioned formula ratio, first ethylene glycol, n-butyl acrylate and lauryl mercaptan are put into
In reactor, it is heated to 50-60 DEG C, in 120-135 rev/min of rotating speed, continuous stirring 5-10 minute, obtained solution a is stand-by；
(2) benzoic acid sodium salt, Colophonium, lac resin, microwax and nano-scale tourmaline powder are added in solution a,
Heat while stirring, reach 80-90 DEG C to temperature and be incubated 2 hours, obtained solution b is stand-by；
Above-mentioned mixing speed controls at 90-110 rev/min.
(3) pure-acrylic emulsion is put in solution b, stir, mixing speed is maintained at 1200 revs/min about, stirring
30 minutes, obtained solution c was stand-by；
(4) by the temperature control of solution c at 40-45 DEG C, it is subsequently adding platinum compounds and silane coupler, stirs,
It is cooled to room temperature, go out kettle and obtain viscosifier.
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite one-step preppn process, step is as follows：
(1) polypropene staple, potassium carbonate whisker, Pulvis Talci, carborundum and synergist are sent in rotary drum and mixed
Rotary drum is heated up to 80-120 DEG C by stirring simultaneously, and pressure, in 150-200Mpa, took out and obtained compound at 40 minutes the time；
(2) nylon 6T and dioctyl phthalate are mixed, conveyed by mouth mould after being plastified by single screw extrusion machine
To high-temperature fusant reactor, add compound, DOPO, antioxidant, compatilizer, triazine carbon forming agent, nucleator, viscosifier and crystallite
Wax, keeps kettle temperature under the conditions of 235～240 DEG C, pressure 2.0～2.5MPa, obtains blend melt；
(3) blend melt is sent to dipping head, the temperature of dipping head is set as 280-360 DEG C, roving glass fiber is led to
Cross dipping head die hole, after dipping, pulled out dipping head, cooling, pelletizing, the enhancing obtaining 8-15mm length is high temperature resistant
PA6T composite.
Embodiment 3
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite, is made up of the component of following weight：Nylon 6T
30kg, roving glass fiber 40kg, DOPO 13kg, antioxidant 1kg, compatilizer 5kg, triazine carbon forming agent 5kg, synergist 1kg, polypropylene
Chopped fiber 5kg, potassium carbonate whisker 0.5kg, Pulvis Talci 4kg, carborundum 1kg, nucleator 1kg, viscosifier 1kg, microwax 1kg,
Dioctyl phthalate 1kg.
Described synergist selects quaternary alkylphosphonium salt intercalation modifying montmorillonite.
Irgasfos 168 selected by described antioxidant.
Described triazine carbon forming agent selects CFA triazine carbon forming agent.
Poly- propane selected by described nucleator.
Above-mentioned viscosifier are made up of the component of following weight：Ethylene glycol 80g, platinum compounds 2g, silane coupler 2g, benzene
Formic acid sodium salt 2g, Colophonium 5g, n-butyl acrylate 3g, lauryl mercaptan 3g, lac resin 4g, microwax 2g, nanoscale electricity
Gas stone powder body 3g, pure-acrylic emulsion 5g；This viscosifier is specifically designed for regeneration PA6 melt and is configured, and the speed of viscosity increasement is fast, and effect is good.
The preparation method of above-mentioned viscosifier is as follows：
(1) weigh each component by above-mentioned formula ratio, first ethylene glycol, n-butyl acrylate and lauryl mercaptan are put into
In reactor, it is heated to 50-60 DEG C, in 120-135 rev/min of rotating speed, continuous stirring 5-10 minute, obtained solution a is stand-by；
(2) benzoic acid sodium salt, Colophonium, lac resin, microwax and nano-scale tourmaline powder are added in solution a,
Heat while stirring, reach 80-90 DEG C to temperature and be incubated 2 hours, obtained solution b is stand-by；
Above-mentioned mixing speed controls at 90-110 rev/min.
(3) pure-acrylic emulsion is put in solution b, stir, mixing speed is maintained at 1200 revs/min about, stirring
30 minutes, obtained solution c was stand-by；
(4) by the temperature control of solution c at 40-45 DEG C, it is subsequently adding platinum compounds and silane coupler, stirs,
It is cooled to room temperature, go out kettle and obtain viscosifier.
A kind of halogen-free flameproof long glass fiber reinforced is high temperature resistant PA6T composite one-step preppn process, step is as follows：
(1) polypropene staple, potassium carbonate whisker, Pulvis Talci, carborundum and synergist are sent in rotary drum and mixed
Rotary drum is heated up to 80-120 DEG C by stirring simultaneously, and pressure, in 150-200Mpa, took out and obtained compound at 40 minutes the time；
(2) nylon 6T and dioctyl phthalate are mixed, conveyed by mouth mould after being plastified by single screw extrusion machine
To high-temperature fusant reactor, add compound, DOPO, antioxidant, compatilizer, triazine carbon forming agent, nucleator, viscosifier and crystallite
Wax, keeps kettle temperature under the conditions of 235～240 DEG C, pressure 2.0～2.5MPa, obtains blend melt；
(3) blend melt is sent to dipping head, the temperature of dipping head is set as 280-360 DEG C, roving glass fiber is led to
Cross dipping head die hole, after dipping, pulled out dipping head, cooling, pelletizing, the enhancing obtaining 8-15mm length is high temperature resistant
PA6T composite.
To embodiment 1- embodiment 3 products obtained therefrom, using ASTM standard, its comprehensive mechanical property and fire resistance are carried out
Detection, including tensile strength, bending strength, bending moduluses, Izod notch impact strength and heat distortion temperature.Test result sees below
Table 1.
Table 1
| Test event | Method of testing | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Fire resistance (UL-94-1.6mm) | UL-94 | V-0 | V-0 | V-0 |
| Tensile strength (MPa) | ASTMD638 | 187 | 190 | 185 |
| Bending strength (MPa) | ASTMD790 | 210 | 190 | 195 |
| Bending moduluses (MPa) | ASTMD790 | 2510 | 3400 | 3150 |
| Izod notch impact strength (J/m) | ASTMD256 | 370 | 350 | 290 |
| Heat distortion temperature (DEG C) | ASTMD648 | 270 | 266 | 280 |
Ultimate principle and principal character and the advantages of the present invention of the present invention have been shown and described above.The technology of the industry
, it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description is originally for personnel
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and its
Equivalent thereof.
Claims (7)
1. a kind of high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced is it is characterised in that group by following parts by weight
Divide and make：Nylon 6T 30-60, roving glass fiber 20-40, DOPO 13-18, antioxidant 0.5-1, compatilizer 5-10, triazine carbon forming agent
3-5, synergist 1-5, polypropene staple 3-5, potassium carbonate whisker 0.5-1, Pulvis Talci 2-4, carborundum 1-3, nucleator 0.5-
1st, viscosifier 1-4, microwax 0.5-1, dioctyl phthalate 1-3.
2. the high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced according to claim 1 is it is characterised in that described
Synergist select quaternary alkylphosphonium salt intercalation modifying montmorillonite.
3. the high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced according to claim 1 is it is characterised in that described
Antioxidant select irgasfos 168/1098.
4. the high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced according to claim 1 is it is characterised in that described
Triazine carbon forming agent select CFA triazine carbon forming agent.
5. the high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced according to claim 1 is it is characterised in that described
Nucleator select one or more of poly- 3- methyl butene -1, polyvinyl cyclosilane, polyvinyl cycloalkanes, poly- propane
Mixture.
6. the high temperature resistant PA6T composite of halogen-free flameproof long glass fiber reinforced according to claim 1 is it is characterised in that above-mentioned
Viscosifier are made up of the component of following weight：Ethylene glycol 80g, platinum compounds 2g, silane coupler 2g, benzoic acid sodium salt 2g,
Colophonium 5g, n-butyl acrylate 3g, lauryl mercaptan 3g, lac resin 4g, microwax 2g, nano-scale tourmaline powder 3g,
Pure-acrylic emulsion 5g；
The preparation method of above-mentioned viscosifier is as follows：
(1) weigh each component by above-mentioned formula ratio, first ethylene glycol, n-butyl acrylate and lauryl mercaptan are put into reaction
In kettle, it is heated to 50-60 DEG C, in 120-135 rev/min of rotating speed, continuous stirring 5-10 minute, obtained solution a is stand-by；
(2) benzoic acid sodium salt, Colophonium, lac resin, microwax and nano-scale tourmaline powder are added in solution a, while stirring
Mix side heating, reach 80-90 DEG C to temperature and be incubated 2 hours, obtained solution b is stand-by；
Above-mentioned mixing speed controls at 90-110 rev/min.
(3) pure-acrylic emulsion is put in solution b, stir, mixing speed is maintained at 1200 revs/min about, stir 30 points
Clock, obtained solution c is stand-by；
(4) by the temperature control of solution c at 40-45 DEG C, it is subsequently adding platinum compounds and silane coupler, stirs, cooling
To room temperature, go out kettle and obtain viscosifier.
7. halogen-free flameproof long glass fiber reinforced high temperature resistant PA6T composite one-step method preparation described in a kind of any one of claim 1-6
Method is it is characterised in that step is as follows：
(1) polypropene staple, potassium carbonate whisker, Pulvis Talci, carborundum and synergist are sent in rotary drum and carry out mix and blend,
Rotary drum is heated up to 80-120 DEG C, pressure, in 150-200Mpa, took out and obtained compound at 40 minutes the time simultaneously；
(2) nylon 6T and dioctyl phthalate are mixed, after plastifying by single screw extrusion machine, height is transported to by mouth mould
Warm fusant reaction kettle, adds compound, DOPO, antioxidant, compatilizer, triazine carbon forming agent, nucleator, viscosifier and microwax,
Keep kettle temperature under the conditions of 235～240 DEG C, pressure 2.0～2.5MPa, obtain blend melt；
(3) blend melt is sent to dipping head, the temperature of dipping head is set as 280-360 DEG C, roving glass fiber is passed through leaching
Stain head nib, after dipping, is pulled out dipping head, cooling, pelletizing, the high temperature resistant PA6T of enhancing obtaining 8-15mm length is multiple
Condensation material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112375297A (en) * | 2020-11-27 | 2021-02-19 | 江苏金发科技新材料有限公司 | Glass fiber reinforced PP/PA66 composite material for water chamber of new energy automobile and preparation method thereof |
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