CN104140673A - Preparation method of high-temperature-resistant halogen-free flame retardant polyamide - Google Patents
Preparation method of high-temperature-resistant halogen-free flame retardant polyamide Download PDFInfo
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- CN104140673A CN104140673A CN201410392740.4A CN201410392740A CN104140673A CN 104140673 A CN104140673 A CN 104140673A CN 201410392740 A CN201410392740 A CN 201410392740A CN 104140673 A CN104140673 A CN 104140673A
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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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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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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- 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
-
- 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
- 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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a preparation method of high-temperature-resistant halogen-free flame retardant polyamide and belongs to the technical field of preparation of high molecular materials. The preparation method comprises the following steps: self-preparing a macromolecular interface modifier; weighing and mixing 45-50 parts of nylon 66 resin, 30-35 parts of nylon 46 resin, 5-8 parts of the macromolecular interface modifier and 10-15 parts of magnesium hydroxide in a high speed mixer for 3 minutes to 5 minutes; then, adding 10-12 parts of chopped glass fibers, 0.5-0.8 part of an antioxidant and 1-2 parts of nano-zinc oxide, and continuously mixing for 5 minutes-8 minutes to obtain a granulated material; and putting the granulated material into a twin-screw extruder to be fused and extruded, and controlling the temperatures of regions I to XII of the twin-screw extruder to obtain the product, namely the high-temperature-resistant halogen-free flame retardant polyamide. The preparation method disclosed by the invention is simple and convenient to operate, and the product is low in density, halogen-free, green and environment-friendly and high in high-temperature resistance, can fully replace low-end halogen-containing flame retardant polyamide materials in the market at present, and has a very high market value.
Description
Background technology
The present invention relates to field of polymer material preparing technology, specifically, relate to a kind of preparation method of high temperature resistant halogen-free flame-retardant polymeric amide.
Background technology
Polymeric amide (PA is commonly called as nylon) is that in five large-engineering plastics, consumption is maximum, kind is maximum, the oldest a kind of engineering plastics of qualification, and output occupies first of five large general engineering plastic.Engineering plastics have good over-all properties with polymeric amide, intensity, higher than metal, has good mechanical property, thermotolerance, wearability, chemical resistant properties, flame retardant resistance and self lubricity, and easily processing, frictional coefficient is low, so be widely used in electronics-electric field.Because the flame retardant properties of polymeric amide itself generally can only reach UL94V-2 level, so be applied to the polymeric amide in electric field, need to improve its flame retardant properties through modification.
In order to make nylon material possess certain flame retardant resistance, thereby conventionally add halogen containing flame-retardant, thereby while causing burning, produce a large amount of toxic smogs, fact proved, in fire failure, what cause the massive loss of life is not big fire itself, but toxic smog makes to be choked to death by besieging personnel.Therefore, the environmental protection class material of halogen-free flameproof is future developing trend.
Through retrieval, Chinese patent ZL201210127324.2, denomination of invention: the preparation method of the nylon alloy material of modification, comprise the following steps: take by weight nylon 1212 resin 50-58 part, ethylene-octene resin 25-30 part, coupling agent 0.6-1.1 part and filler 25-36 part, and mix in input high-speed mixer, then drop into oxidation inhibitor 0.3-0.9 part, short glass fiber 30-38 part and the stearic amide 0.3-0.6 part taking by weight, and continue to mix, obtain granulation material; The granulation material obtaining is dropped in twin screw extruder and melt extruded, and control the temperature in Zhi Qi district, twin screw extruder Yi district, obtain the nylon alloy material of modification.Nylon alloy material in this patent has good toughness and has eliminated the situation of impacting cracking, but the filler of this nylon and gold copper-base alloy is calcium carbonate, and flame retardant properties is not fine.
Chinese patent ZL200710074664.2, polyamide resin of a kind of halogen-free phosphor-free environmental protection inflaming retarding and preparation method thereof is disclosed, although the polyamide resin in this patent has been realized halogen-free phosphorus-free inflaming retarding, the resistance to elevated temperatures of this product does not have digital proof, and resistance to elevated temperatures is also uncertain.
Summary of the invention
The technical problem that 1, will solve
The preparation method who the object of this invention is to provide a kind of polymeric amide, polymeric amide prepared by the method can improve high-temperature resistant result, embody environmental protection, and this product also possesses good mechanical and physical performance simultaneously.
2, technical scheme
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, comprises the following steps:
Step 1, the preparation of macromolecule interfacial modifier, polipropene 25-30 part, terpolymer EP rubber 15-25 part, ethylene group bis-stearamides 8-10 part, maleic anhydride inoculated polypropylene 5-8 part of taking weight part mix in high-speed mixer, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, Nylon 66 45-50 part, nylon 46 resin 30-35 part, macromolecule interfacial modifier 5-8 part and magnesium hydroxide 10-15 part of taking weight part are mixed 3-5min in high-speed mixer, add again short glass fiber 10-12 part, oxidation inhibitor 0.5-0.8 part and nano zine oxide 1-2 part, continue to mix 5-8min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
Further, the mixing machine mixing condition in described step 1 is, time 8-10min, and rotating speed 1500r/min-2000r/min, the mixing rotating speed in step 2 is 2500r/min-3000r/min.
Further, the particle diameter of described magnesium hydroxide is 0.5-10 micron.
Further, described step 3 kind the temperature in Zhi Qi district, control twin screw extruder Yi district be: 255 ℃, a district, 260 ℃, 2nd district, 265 ℃, 3rd district, 270 ℃, 4th district, 275 ℃, 5th district, 270 ℃, 275 ℃He 7th district, 6th districts.
Further, described short glass fiber is that length is the alkali-free short glass fiber of 3mm.
3, beneficial effect:
Macromolecule interfacial modifier of the present invention can effectively increase the consistency of nylon and magnesium hydroxide, and increases its mechanical property; Daiamid composition prepared by the present invention has following performance index: tensile strength is greater than 110MPa, and flexural strength is greater than 210MPa, and flame retardant resistance reaches V-0 (UL-94-1.6mm), and heat resistance is higher than 230 ℃, density: 1.25g/cm
3; Preparation method of the present invention is simple, handled easily and product low density, Halogen, environmental protection, resistance to elevated temperatures is high, all can replace the Halogen Flameproof polyamide material of low side in the market completely, there is very high marketable value, can be applied in household electrical appliances, automobile etc. to heatproof and the fire-retardant field that has requirement, as electrical appliance kit, the interior electric elements of engine room etc.
Embodiment
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1
A preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, comprises the following steps:
Step 1, the preparation of macromolecule interfacial modifier, 5 parts of 8 parts of 15 parts of polipropene 25 part, terpolymer EP rubbers, ethylene group bis-stearamides, maleic anhydride inoculated polypropylenes taking weight part mix in high-speed mixer, time 8min, rotating speed 1500r/min, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, take 10 parts of 5 parts of 30 parts of 45 parts of Nylon 66s, nylon 46 resins, the macromolecule interfacial modifiers of weight part and magnesium hydroxides and in high-speed mixer, mix 3-5min, add again 1 part of 10 parts of short glass fibers, 0.5 part, oxidation inhibitor and nano zine oxide, continue to mix 5min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
Embodiment 2
A preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, comprises the following steps:
Step 1, the preparation of macromolecule interfacial modifier, 8 parts of 10 parts of 25 parts of 30 parts of polypropylene, terpolymer EP rubbers, ethylene group bis-stearamides, maleic anhydride inoculated polypropylenes taking weight part mix in high-speed mixer, time 10min, rotating speed 2000r/min, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, take 15 parts of 8 parts of 35 parts of 50 parts of Nylon 66s, nylon 46 resins, the macromolecule interfacial modifiers of weight part and magnesium hydroxides and in high-speed mixer, mix 5min, add again 2 parts of 12 parts of short glass fibers, 0.8 part, oxidation inhibitor and nano zine oxides, continue to mix 8min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
Embodiment 3
A preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, comprises the following steps:
Step 1, the preparation of macromolecule interfacial modifier, 6 parts of 9 parts of 15 parts of 30 parts of polypropylene, terpolymer EP rubbers, ethylene group bis-stearamides, maleic anhydride inoculated polypropylenes taking weight part mix in high-speed mixer, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, take 12 parts of 6 parts of 30 parts of 50 parts of Nylon 66s, nylon 46 resins, the macromolecule interfacial modifiers of weight part and magnesium hydroxides and in high-speed mixer, mix 4min, add again 1 part of 11 parts of short glass fibers, 0.6 part, oxidation inhibitor and nano zine oxide, continue to mix 7min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
Embodiment 4
A preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, comprises the following steps:
Step 1, the preparation of macromolecule interfacial modifier, 7 parts of 9 parts of 20 parts of 27 parts of polypropylene, terpolymer EP rubbers, ethylene group bis-stearamides, maleic anhydride inoculated polypropylenes taking weight part mix in high-speed mixer, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, take 12 parts of 7 parts of 32 parts of 47 parts of Nylon 66s, nylon 46 resins, the macromolecule interfacial modifiers of weight part and magnesium hydroxides and in high-speed mixer, mix 4min, add again 2 parts of 11 parts of short glass fibers, 0.7 part, oxidation inhibitor and nano zine oxides, continue to mix 6min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
The daiamid composition being obtained by above-described embodiment has the technique effect shown in following table after tested.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention.All any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a preparation method for high temperature resistant halogen-free flame-retardant polymeric amide, is characterized in that: comprise the following steps:
Step 1, the preparation of macromolecule interfacial modifier, polipropene 25-30 part, terpolymer EP rubber 15-25 part, ethylene group bis-stearamides 8-10 part, maleic anhydride inoculated polypropylene 5-8 part of taking weight part mix in high-speed mixer, be placed in again twin screw extruder extruding pelletization, obtain macromolecule interfacial modifier;
Step 2, preparation granulation material, Nylon 66 45-50 part, nylon 46 resin 30-35 part, macromolecule interfacial modifier 5-8 part and magnesium hydroxide 10-15 part of taking weight part are mixed 3-5min in high-speed mixer, add again short glass fiber 10-12 part, oxidation inhibitor 0.5-0.8 part and nano zine oxide 1-2 part, continue to mix 5-8min, obtain granulation material;
Step 3, granulation, drops into the granulation material being obtained by step 2 in twin screw extruder and melt extrudes, and controls the temperature in Zhi Qi district, twin screw extruder Yi district, obtains product.
2. the preparation method of a kind of high temperature resistant halogen-free flame-retardant polymeric amide as claimed in claim 1, it is characterized in that: the mixing machine mixing condition in described step 1 is, time 8-10min, rotating speed 1500r/min-2000r/min, the mixing rotating speed in step 2 is 2500r/min-3000r/min.
3. the preparation method of a kind of high temperature resistant halogen-free flame-retardant polymeric amide as claimed in claim 1, is characterized in that: the particle diameter of described magnesium hydroxide is 0.5-10 micron.
4. the preparation method of a kind of high temperature resistant halogen-free flame-retardant polymeric amide as claimed in claim 1, is characterized in that: described step 3 kind the temperature in Zhi Qi district, control twin screw extruder Yi district be: 255 ℃, a district, 260 ℃, 2nd district, 265 ℃, 3rd district, 270 ℃, 4th district, 275 ℃, 5th district, 270 ℃, 275 ℃He 7th district, 6th districts.
5. the preparation method of a kind of high temperature resistant halogen-free flame-retardant polymeric amide as claimed in claim 1, is characterized in that: described short glass fiber is that length is the alkali-free short glass fiber of 3mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592751A (en) * | 2014-12-10 | 2015-05-06 | 苏州博利迈新材料科技有限公司 | Halogen-free flame retardant reinforced nylon 612 composite material, preparation method and application thereof |
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| CN101423666A (en) * | 2008-10-31 | 2009-05-06 | 广东新会美达锦纶股分有限公司 | Halogen-free flame retardant polyamide 6 composition |
| CN102108208A (en) * | 2009-12-29 | 2011-06-29 | 合肥杰事杰新材料有限公司 | High-strength flame-retardant polyamide composite material and preparation method |
| CN102558855A (en) * | 2012-02-14 | 2012-07-11 | 株洲时代工程塑料制品有限责任公司 | Modified nylon resin composition |
| CN102993735A (en) * | 2012-08-22 | 2013-03-27 | 常熟市筑紫机械有限公司 | Preparation method of halogen-free flame-retardant nylon 610 and polypropylene alloy composite material |
| CN103113738A (en) * | 2013-02-03 | 2013-05-22 | 广东安帝斯智能家具组件有限公司 | Special engineering nylon material for environment-friendly furniture connecting piece and preparation method thereof |
| CN103540013A (en) * | 2012-07-16 | 2014-01-29 | 上海杰事杰新材料(集团)股份有限公司 | Nylon 6/polypropylene plastic alloy and preparation method thereof |
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2014
- 2014-08-11 CN CN201410392740.4A patent/CN104140673B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423666A (en) * | 2008-10-31 | 2009-05-06 | 广东新会美达锦纶股分有限公司 | Halogen-free flame retardant polyamide 6 composition |
| CN102108208A (en) * | 2009-12-29 | 2011-06-29 | 合肥杰事杰新材料有限公司 | High-strength flame-retardant polyamide composite material and preparation method |
| CN102558855A (en) * | 2012-02-14 | 2012-07-11 | 株洲时代工程塑料制品有限责任公司 | Modified nylon resin composition |
| CN103540013A (en) * | 2012-07-16 | 2014-01-29 | 上海杰事杰新材料(集团)股份有限公司 | Nylon 6/polypropylene plastic alloy and preparation method thereof |
| CN102993735A (en) * | 2012-08-22 | 2013-03-27 | 常熟市筑紫机械有限公司 | Preparation method of halogen-free flame-retardant nylon 610 and polypropylene alloy composite material |
| CN103113738A (en) * | 2013-02-03 | 2013-05-22 | 广东安帝斯智能家具组件有限公司 | Special engineering nylon material for environment-friendly furniture connecting piece and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592751A (en) * | 2014-12-10 | 2015-05-06 | 苏州博利迈新材料科技有限公司 | Halogen-free flame retardant reinforced nylon 612 composite material, preparation method and application thereof |
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