CN104559151A - Halogen-free flame-retardant glass fiber reinforced nylon material and preparation method thereof - Google Patents
Halogen-free flame-retardant glass fiber reinforced nylon material and preparation method thereof Download PDFInfo
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- 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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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
- C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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- 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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- 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
- B29C2948/9259—Angular 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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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
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- 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
- 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
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- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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Abstract
The invention discloses a halogen-free flame-retardant glass fiber reinforced nylon material and a preparation method thereof. The halogen-free flame-retardant glass fiber reinforced nylon material comprises the following components in percentage by mass: 44-70% of PA6, 15-25% of a halogen-free flame retardant, 0.2-0.4% of a coupling agent, 0.2-0.4% of an antioxidant, 0.3-0.5% of a lubricating agent and 10-30% of glass fiber. The halogen-free flame-retardant glass fiber reinforced nylon material prepared by the preparation method has the advantages of good mechanical properties, excellent flame-retardant property, smoke suppression, high heat deformation temperature, no pollution and lower cost and meets the environment-friendly requirements.
Description
[technical field]
The present invention relates to engineering plastic modification technical field, particularly relate to a kind of halogen-free flame-retardant glass fiber enhanced nylon material and preparation method thereof.
[background technology]
Nylon 6 is engineering plastics of a kind of high comprehensive performance, the higher advantage such as mechanics of machinery intensity, wear resistance, self lubricity, weather resisteant, easily injection moulding had.Flame-retardant reinforced nylon 6 material is widely used in electronic enterprises, as switch, terminal, junctor, rly., connector etc. because having the advantages such as high rigidity, high strength, high heat resistance, good flame retardant resistance.
Flame-retardant reinforced nylon material domestic at present uses bromide fire retardant mostly, bromide fire retardant to human health and environmental hazard larger.Along with day by day improving of people's environmental consciousness and being gradually improved of the relevant environmental protection laws and regulations of country, the exploitation of the halogen-free flame-retardant nylon 6 material of environmental protection is more aobvious important and urgent.
[summary of the invention]
The technical problem to be solved in the present invention is to provide one and meets environmental requirement, lower-cost halogen-free flame-retardant glass fiber enhanced nylon material and preparation method thereof.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a kind of halogen-free flame-retardant glass fiber enhanced nylon material, composed of the following components by mass percentage:
Described halogen-free flame retardants is by hydrotalcite and the composite composite halogen-free fire retardant of red phosphorus.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, the relative viscosity of nylon 6 is 2.4-2.8.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, in composite halogen-free fire retardant, the mass ratio of hydrotalcite and red phosphorus is 1:1-2:1.Hydrotalcite is magnalium carbonate form hydrotalcite and/or zinc-magnesium aluminium carbonate form hydrotalcite.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, red phosphorus is microencapsulated powder oil master batch.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, coupling agent is γ-aminopropyl triethoxysilane.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, oxidation inhibitor is by Hinered phenols antioxidant four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] two (2,4-DTBP) pentaerythritol diphosphites of pentaerythritol ester and phosphite ester kind antioxidant mixes.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, lubricant is one or both in calcium stearate, positive N-N ' ethylene bis stearamide, silicone powder, pentaerythritol stearate.
Above-described halogen-free flame-retardant glass fiber enhanced nylon material, glass fibre is alkali free glass fibre, and diameter is 9-14 μm.
A preparation method for above-mentioned halogen-free flame-retardant glass fiber enhanced nylon material, comprises the following steps:
Step one, take each component by mass percentage according to claim 1, and the PA6 resin slicer dry 4-6 hour at 80-100 DEG C of temperature that will take, other component at 60-80 DEG C of temperature dry more than 2 hours;
Step 2, dried PA6 resin slicer, hydrotalcite and red phosphorus composite halogen-free fire retardant, coupling agent, oxidation inhibitor and lubricant are mixed in high-speed mixer, stirring required time is 10-15 minute;
Step 3, step 2 is mixed after material join in the hopper of twin screw extruder, the side spout of glass fibre from twin screw extruder is added, extrudes through high-temperature extruder melt blending, cools, air-dry, granulation;
Wherein, the temperature of twin screw extruder is set to: a district: 200-220 DEG C; 2nd district: 230-250 DEG C; 3rd district: 240-260 DEG C; 4th district: 240-265 DEG C; 5th district: 230-250 DEG C; 6th district: 230-245 DEG C; 7th district: 220-240 DEG C; 8th district: 210-230 DEG C; Head temperature: 220-230 DEG C; Screw speed controls at 250-350 rev/min.
Halogen-free flame-retardant glass fiber enhanced nylon material prepared by the present invention has that mechanical mechanics property is excellent, excellent flame retardancy, press down cigarette, heat-drawn wire high; And pollution-free, meet environmental requirement, cost is lower.
[embodiment]
Below by embodiment, the present invention is further detailed explanation.
Halogen-free flame-retardant glass fiber enhanced nylon material of the present invention, composed of the following components by mass percentage:
Wherein, PA6 is low isoviscous resin in being, relative viscosity scope 2.4-2.8.
Halogen-free flame retardants is that 6:4 (feasible proportioning is 1:1-2:1) is composite in mass ratio forms for surperficial treated hydrotalcite and microencapsulated powder oil.Wherein hydrotalcite is one or both in magnalium carbonate form hydrotalcite or zinc-magnesium aluminium carbonate form hydrotalcite; Hydrotalcite surface treatment agent is one or both in silane coupling agent, titanate coupling agent or aluminate coupling agent.Red phosphorus is microencapsulated powder oil master batch.
Coupling agent is γ-aminopropyl triethoxysilane.
Oxidation inhibitor is by Hinered phenols antioxidant four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] two (2,4-DTBP) pentaerythritol diphosphites of pentaerythritol ester and phosphite ester kind antioxidant in mass ratio 1:1 mix.
Lubricant can be one or both in calcium stearate, positive N-N ' ethylene bis stearamide, silicone powder, pentaerythritol stearate.
Alkali-free short fiber thought by glass fibre, and diameter is: 9-14 μm.
Halogen-free flame-retardant glass fiber of the present invention strengthens PA6 material and preparation method thereof, comprising:
Step one, take each component by mass percentage according to claim 1, and the PA6 resin slicer dry 4-6 hour at 80-100 DEG C of temperature that will take, other component at 60-80 DEG C of temperature dry more than 2 hours.
Step 2, dried PA6 resin slicer, surperficial treated hydrotalcite and red phosphorus composite halogen-free fire retardant, coupling agent, oxidation inhibitor and lubricant are mixed in high-speed mixer, stirring required time is 10-15 minute.
Step 3, step 2 is mixed after material join in the hopper of twin screw extruder, the side spout of glass fibre from twin screw extruder is added, extrudes through high-temperature extruder melt blending, cools, air-dry, granulation.
Wherein, the temperature of twin screw extruder is set to: a district: 200-220 DEG C; 2nd district: 230-250 DEG C; 3rd district: 240-260 DEG C; 4th district: 240-265 DEG C; 5th district: 230-250 DEG C; 6th district: 230-245 DEG C; 7th district: 220-240 DEG C; 8th district: 210-230 DEG C; Head temperature: 220-230 DEG C; Screw speed controls at 250-350r/ minute.
Below in conjunction with embodiment, one detailed elaboration is done to the present invention.Wherein in each embodiment following: the relative viscosity of Nylon 6 is 2.5, the trade mark: newly U.S.A can reach PA6M2500;
Hydrotalcite is magnalium carbonate form hydrotalcite, the order number 2000 order trade mark: Nantong Ai Dewang chemical industry M-3;
Red phosphorus is the microencapsulated powder oil master batch trade mark: Guangzhou silver moulds FRP-750;
Coupling agent is the γ-aminopropyl triethoxysilane trade mark: boiling point KH550;
Main anti-oxidant and auxiliary antioxidant are Switzerland's vapour bar 1010 and 626;
Lubricant is the pentaerythritol stearate trade mark: the peaceful PETS P861 of section;
Glass fibre is short fiber (Fibre diameter 9 μm, the chopped length 3mm) trade mark: the multiple material ECS301NF in Chongqing;
Embodiment 1
By PA6 resin under 90 DEG C of conditions dry 6 hours, remaining material under 70 DEG C of conditions dry 3 hours.Take PA6 resin 67kg, composite halogen-free fire retardant 22kg, coupling agent 0.2kg, oxidation inhibitor 0.4kg (wherein primary antioxidant 10100.2kg, auxiliary anti-oxidant 6260.2kg), lubricant 0.4kg (wherein TAF0.4kg); Then stir 10 minutes in high-speed mixer.Again the material after mixing is joined in the hopper of twin screw extruder, control each section of temperature and exist: a district: 220 DEG C; 2nd district: 250 DEG C; 3rd district: 260 DEG C; 4th district: 250 DEG C; 5th district: 250 DEG C; 6th district: 240 DEG C; 7th district: 240 DEG C; 8th district: 230 DEG C; Head temperature: 240 DEG C, screw speed 320r/ minute, the spout of 10kg glass fibre from twin screw stage casing is added, extrudes through melt blending, water-cooled, air-dry, pelletizing, oven dry, be finally packaged into bag and halogen-free flame-retardant glass fiber strengthens PA6 material.
Embodiment 2
By PA6 resin under 90 DEG C of conditions dry 6 hours, remaining material under 70 DEG C of conditions dry 3 hours.Take PA6 resin 61kg, composite halogen-free fire retardant 18kg, coupling agent 0.2kg, oxidation inhibitor 0.4kg (wherein primary antioxidant 10100.2kg, auxiliary anti-oxidant 6260.2kg), lubricant 0.4kg (wherein TAF0.4kg); Then stir 10 minutes in high-speed mixer.Again the material after mixing is joined in the hopper of twin screw extruder, control each section of temperature and exist: a district: 220 DEG C; 2nd district: 250 DEG C; 3rd district: 260 DEG C; 4th district: 250 DEG C; 5th district: 250 DEG C; 6th district: 240 DEG C; 7th district: 240 DEG C; 8th district: 230 DEG C; Head temperature: 240 DEG C, screw speed 320r/ minute, the spout of 20kg glass fibre from twin screw stage casing is added, extrudes through melt blending, water-cooled, air-dry, pelletizing, oven dry, be finally packaged into bag and halogen-free flame-retardant glass fiber strengthens PA6 material.
Embodiment 3
By PA6 resin under 90 DEG C of conditions dry 6 hours, remaining material under 70 DEG C of conditions dry 3 hours.Take PA6 resin 54kg, composite halogen-free fire retardant 15kg, coupling agent 0.2kg, oxidation inhibitor 0.4kg (wherein primary antioxidant 10100.2kg, auxiliary anti-oxidant 6260.2kg), lubricant 0.4kg (wherein TAF0.4kg); Then stir 10 minutes in high-speed mixer.Again the material after mixing is joined in the hopper of twin screw extruder, control each section of temperature and exist: a district: 220 DEG C; 2nd district: 250 DEG C; 3rd district: 260 DEG C; 4th district: 250 DEG C; 5th district: 250 DEG C; 6th district: 240 DEG C; 7th district: 240 DEG C; 8th district: 230 DEG C; Head temperature: 240 DEG C, screw speed 320r/ minute, the spout of 30kg glass fibre from twin screw stage casing is added, extrudes through melt blending, water-cooled, air-dry, pelletizing, oven dry, be finally packaged into bag and halogen-free flame-retardant glass fiber strengthens PA6 material.
The halogen-free flame-retardant glass fiber of embodiment 1 to 3 is strengthened PA6 material injection and becomes standard testing batten, test performance is as shown in the table:
The treated hydrotalcite in surface that the above embodiment of the present invention adopts and red phosphorus composite fire retardant, not halogen-containing.Hydrotalcite (Layered Double Hydroxides, be called for short LDHs, typical LDHs compound is magnalium carbonate form hydrotalcite: Mg6Al2 (OH) 16 〃 4H2O) be the double-metal hydroxide that a class has laminate structure, it has had the advantage of magnesium hydroxide and aluminium hydroxide fire retardant concurrently, overcomes again their respective deficiency.And hydrotalcite and red phosphorus have extraordinary cooperative flame retardant effect, have fire-retardant, fill, eliminate smoke three kinds of functions.This composite flame-retardant agent is a kind of fire retardant of efficient, Halogen, nontoxic, low cigarette.
Halogen-free flame-retardant glass fiber enhanced nylon material prepared by the above embodiment of the present invention has that mechanical mechanics property is excellent, excellent flame retardancy, press down cigarette, heat-drawn wire high; And pollution-free, meet environmental requirement, cost is lower.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (9)
1. a halogen-free flame-retardant glass fiber enhanced nylon material, is characterized in that, composed of the following components by mass percentage:
Described halogen-free flame retardants is by hydrotalcite and the composite composite halogen-free fire retardant of red phosphorus.
2. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, the relative viscosity of nylon 6 is 2.4-2.8.
3. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, in composite halogen-free fire retardant, the mass ratio of hydrotalcite and red phosphorus is 1:1-2:1, and hydrotalcite is magnalium carbonate form hydrotalcite and/or zinc-magnesium aluminium carbonate form hydrotalcite.
4. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, red phosphorus is microencapsulated powder oil master batch.
5. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, coupling agent is γ-aminopropyl triethoxysilane.
6. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, it is characterized in that, oxidation inhibitor is by Hinered phenols antioxidant four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] two (2,4-DTBP) pentaerythritol diphosphites of pentaerythritol ester and phosphite ester kind antioxidant mixes.
7. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, lubricant is one or both in calcium stearate, positive N-N ' ethylene bis stearamide, silicone powder, pentaerythritol stearate.
8. halogen-free flame-retardant glass fiber enhanced nylon material according to claim 1, is characterized in that, glass fibre is alkali free glass fibre, and diameter is 9-14 μm.
9. a preparation method for the halogen-free flame-retardant glass fiber enhanced nylon material as described in claim arbitrary in claim 1 to 8, comprises the following steps:
Step one, take each component by mass percentage according to claim 1, and the PA6 resin slicer dry 4-6 hour at 80-100 DEG C of temperature that will take, other component at 60-80 DEG C of temperature dry more than 2 hours;
Step 2, dried PA6 resin slicer, hydrotalcite and red phosphorus composite halogen-free fire retardant, coupling agent, oxidation inhibitor and lubricant are mixed in high-speed mixer, stirring required time is 10-15 minute;
Step 3, step 2 is mixed after material join in the hopper of twin screw extruder, the side spout of glass fibre from twin screw extruder is added, extrudes through high-temperature extruder melt blending, cools, air-dry, granulation;
Wherein, the temperature of twin screw extruder is set to: a district: 200-220 DEG C; 2nd district: 230-250 DEG C; 3rd district: 240-260 DEG C; 4th district: 240-265 DEG C; 5th district: 230-250 DEG C; 6th district: 230-245 DEG C; 7th district: 220-240 DEG C; 8th district: 210-230 DEG C; Head temperature: 220-230 DEG C; Screw speed controls at 250-350 rev/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861644A (en) * | 2015-05-25 | 2015-08-26 | 江苏南瑞泰事达电气有限公司 | Recoverable flame-retardant insulating modified material, and preparation and application of insulating parts |
| CN105670280A (en) * | 2016-04-01 | 2016-06-15 | 青岛国恩科技股份有限公司 | Glass-fiber-reinforced polyamide 6 (PA6) material for vehicle lights and preparation method thereof |
| CN106854295A (en) * | 2016-12-05 | 2017-06-16 | 合肥杰事杰新材料股份有限公司 | A kind of whiteness red phosphorus, nylon distribute whiteness red phosphorus flame-retardant masterbatch and preparation method thereof with low smell is low |
| CN109233264A (en) * | 2017-07-10 | 2019-01-18 | 合肥杰事杰新材料股份有限公司 | A kind of halogen-free flame-retardant glass fiber enhancing nylon composite materials and preparation method thereof |
| CN109233271A (en) * | 2018-09-25 | 2019-01-18 | 福建锦江科技有限公司 | Utilize the short glass fiber reinforced nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production |
| CN109233266A (en) * | 2018-07-05 | 2019-01-18 | 常州市阿曼特医药科技有限公司 | A kind of short fine enhancing halogen-free flame-retardant nylon 6 composite material of glass |
| CN109486124A (en) * | 2018-10-10 | 2019-03-19 | 深圳市富恒新材料股份有限公司 | A kind of halogen-free flame-retardant glass fiber enhancing PBT material and preparation method thereof |
| CN110922518A (en) * | 2019-11-30 | 2020-03-27 | 华东理工大学 | Water-resistant intumescent flame retardant and preparation method and application thereof |
| CN111454569A (en) * | 2020-05-26 | 2020-07-28 | 苏州润佳工程塑料股份有限公司 | Preparation method of nylon material with flame retardant property |
| CN112759921A (en) * | 2019-11-05 | 2021-05-07 | 浙江伟星实业发展股份有限公司 | Modified nylon material capable of being dyed together with clothes, preparation method thereof and zipper product |
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