CN102363671A - Flame-retardant master batch for nylon carrier and preparation method thereof - Google Patents
Flame-retardant master batch for nylon carrier and preparation method thereof Download PDFInfo
- Publication number
- CN102363671A CN102363671A CN201110182306XA CN201110182306A CN102363671A CN 102363671 A CN102363671 A CN 102363671A CN 201110182306X A CN201110182306X A CN 201110182306XA CN 201110182306 A CN201110182306 A CN 201110182306A CN 102363671 A CN102363671 A CN 102363671A
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- retardant master
- mca
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- temperature
- flame
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Classifications
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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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- 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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a flame-retardant master batch for a nylon carrier and a preparation method thereof. The flame-retardant master batch comprises the following components in percentage by weight: 9.4-49.6 percent of polycaprolactam powder, 50-90 percent of MCA (Melamine Cyanurate) and 0.4-0.6 percent of antioxidant. The preparation method comprises the following steps: weighting the components according to the weight percent; adding the weighted components into a high-speed mixer, mixing for 20-30 minutes and controlling a temperature in a range of 160-180 DEG C; and cooling the mixed components, adding the cooled components into a hopper of a double-screw extruder, performing fusion reaction, extruding and pelletizing. The flame-retardant master batch for the nylon carrier prepared according to the preparation method is excellent in flame-retardant property; the additive amount of the MCA in nylon is increased; and the production cost is reduced.
Description
[technical field]
The present invention relates to polymeric material field, relate in particular to a kind of nylon carrier fire-retardant master granule and preparation method thereof.
[background technology]
The halogen-free flame retardants that is used as halogen-free nylon at present in the world is mainly MCA (melamine cyanurate), and MCA is a kind of nitrogen system bittern-free fire retardant of excellent property, also is the lubricant of good plastics simultaneously.Compare with phosphorous, halogen-containing flame retardant; MCA has advantages such as toxicity is low, flame retarding efficiency is high, suitability is strong, low price; MCA is nontoxic environment-friendly product, and heat resistance is high, Heat stability is good; After MCA adds synthetic resins, can not faded, the product of non-blooming, electrical property and superior; MCA is specially adapted to the fire-retardant of not filled polymeric amide, and flame retardant properties can reach the V0 level.But MCA is a powder, its particle diameter≤2.0 micron, tap density 450-550kg/m3; Explain that the MCA powder is very thin; When producing halogen-free nylon with twin screw extruder, be difficult to blanking, the MCA powder can form at material feed opening place and build bridge, and causes the unsettled normally blanking of material; Disconnected bar is produced in screw rod idle running.The MCA addition is 8～12% in the halogen-free nylon at present, and addition is very low.
[summary of the invention]
The invention provides a kind of nylon carrier fire-retardant master granule and preparation method thereof, this nylon carrier fire-retardant master granule can improve the addition of MCA in nylon, reduces production costs.
Technical scheme of the present invention is:
A kind of nylon carrier fire-retardant master granule, by weight percentage, composed of the following components:
Polycaprolactam powder 9.4-49.6%;
MCA 50-90％；
Oxidation inhibitor 0.4-0.6%;
Wherein, the fineness of polycaprolactam powder is the 100-600 order, is that the employing molecular weight is the polycaprolactam polyimide resin of 17000-30000, pulverizes with Lowtemperaturepulverizer to form.
A kind of preparation method of nylon carrier fire-retardant master granule may further comprise the steps:
Step 1, take by weighing each component by above-mentioned described weight percent;
Step 2, each component that will take by weighing add combination treatment 20-30min in the high-speed mixer, and temperature is controlled at 160-180 ℃;
Step 3, with the cooling of mixed material, cooled material joins in the hopper of twin screw extruder, through frit reaction, extruding pelletization; The twin screw extruder processing condition are: twin screw extruder one district temperature 180-190 ℃, two district temperature 190-220 ℃, three district temperature 210-220 ℃, four district temperature 215-220 ℃, five district temperature 210-220 ℃, residence time 2-3min, pressure are 12-18Mpa.
The nylon carrier fire-retardant master granule of the present invention's preparation, flame retardant properties is good, can improve the addition of MCA in nylon, reduces production costs.
[embodiment]
Below in conjunction with concrete embodiment the present invention is done a detailed elaboration.
In following each embodiment, oxidation inhibitor by [3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (such as Switzerland CIBA produce 1010) with tricresyl phosphite (2,4-di-t-butyl phenyl ester) (such as Switzerland CIBA product 168) composite forming; The fineness of polycaprolactam powder is the 100-600 order, is that the employing molecular weight is the polycaprolactam polyimide resin of 17000-30000, pulverizes with Lowtemperaturepulverizer to form.
Embodiment 1
The nylon carrier fire-retardant master granule of this embodiment, by weight percentage, composed of the following components:
Polycaprolactam powder 49.6%; MCA 50%; Antioxidant 1010 0.2%; Oxidation inhibitor 1680.2%.
Its preparation method is following:
Step 1, take by weighing polycaprolactam powder, MCA, antioxidant 1010, oxidation inhibitor 168 by above-mentioned described weight percent;
Step 2, the polycaprolactam powder that takes by weighing, MCA, antioxidant 1010, oxidation inhibitor 168 added combination treatment 20min in the high-speed mixers, temperature is controlled at 160 ℃;
Step 3, with the cooling of mixed material, cooled material joins in the hopper of twin screw extruder, through frit reaction, extruding pelletization; The twin screw extruder processing condition are: 180 ℃ of twin screw extruder one district's temperature, and 190 ℃ of two district's temperature, 210 ℃ of three district's temperature, 215 ℃ of four district's temperature, 210 ℃ of five district's temperature, residence time 2min, pressure are 12Mpa.
Embodiment 2
The nylon carrier fire-retardant master granule of this embodiment, by weight percentage, composed of the following components:
Polycaprolactam powder 29.6%; MCA 70%; Antioxidant 1010 0.2%; Oxidation inhibitor 1680.2%.
Its preparation method is following:
Step 1, take by weighing polycaprolactam powder, MCA, antioxidant 1010, oxidation inhibitor 168 by above-mentioned described weight percent;
Step 2, the polycaprolactam powder that takes by weighing, MCA, antioxidant 1010, oxidation inhibitor 168 added combination treatment 30min in the high-speed mixers, temperature is controlled at 180 ℃;
Step 3, with the cooling of mixed material, cooled material joins in the hopper of twin screw extruder, through frit reaction, extruding pelletization; The twin screw extruder processing condition are: 190 ℃ of twin screw extruder one district's temperature, and 220 ℃ of two district's temperature, 220 ℃ of three district's temperature, 220 ℃ of four district's temperature, 220 ℃ of five district's temperature, residence time 3min, pressure are 18Mpa.
Embodiment 3
The nylon carrier fire-retardant master granule of this embodiment, by weight percentage, composed of the following components:
Polycaprolactam powder 19.4%; MCA 80%; Antioxidant 1010 0.3%; Oxidation inhibitor 1680.3%.
Its preparation method is following:
Step 1, take by weighing polycaprolactam powder, MCA, antioxidant 1010, oxidation inhibitor 168 by above-mentioned described weight percent;
Step 2, the polycaprolactam powder that takes by weighing, MCA, antioxidant 1010, oxidation inhibitor 168 added combination treatment 25min in the high-speed mixers, temperature is controlled at 170 ℃;
Step 3, with the cooling of mixed material, cooled material joins in the hopper of twin screw extruder, through frit reaction, extruding pelletization; The twin screw extruder processing condition are: 185 ℃ of twin screw extruder one district's temperature, and 200 ℃ of two district's temperature, 215 ℃ of three district's temperature, 215 ℃ of four district's temperature, 220 ℃ of five district's temperature, residence time 3min, pressure are 15Mpa.
Embodiment 4
The nylon carrier fire-retardant master granule of this embodiment, by weight percentage, composed of the following components:
Polycaprolactam powder 9.4%; MCA 90%; Antioxidant 1010 0.3%; Oxidation inhibitor 1680.3%.
Its preparation method is identical with embodiment 3.
Performance test and evaluation:
With the particle of accomplishing granulation among the foregoing description 1-4 in 130-150 ℃ convection oven dry 4-6 hour,, keep the mould temperature in the sample making course between 70-100 ℃ again with the injection moulding sample preparation on the 80T injection moulding machine of exsiccant particle.The flame retardant properties bar is according to the UL-94 standard, and thickness is 1.6 millimeters.Taking out granular attitude and outward appearance gets final product through thinking to observe.
When performance test data is as shown in table 1 below for the set of dispense of the fire-retardant master granule of embodiment 1-4 preparation:
| Form (%) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| The polycaprolactam powder | 49.6 | 29.6 | 19.6 | 9.4 |
| Fire retardant MCA | 50 | 70 | 80 | 90 |
| Oxidation inhibitor | 0.4 | 0.4 | 0.4 | 0.6 |
| Fire-retardant UL94 | V0 | V0 | V0 | V0 |
| Take out the material state | It is stable to take out grain | It is stable to take out grain | It is stable to take out grain | It is unstable to take out material |
| Outward appearance | Smooth | Smooth | Smooth | Particle is coarse slightly |
Table 1
From last table 1, can find out: the fire-retardant master granule of embodiment of the invention 1-4 can reach flame retardant effect V0 fully; And the MCA addition can be by 50% to 90%; Twin screw extruder can be stablized and takes out grain when the MCA addition is between 50%～80%; To take out grain unstable for material when MCA addition＞80%, and particle surface is coarse slightly.
This shows that fire-retardant master granule of the present invention phenomenons such as difficult blanking, blanking bridge formation can not occur again, and production is carried out continually and steadily.And owing to considering again that cutting stock problems reduce the fire retardant consumption,, in a disguised form improve the fire retardant usage quantity, can reduce the cost of material significantly so can improve the consumption of fire-retardant master granule.
Above-described embodiment of the present invention does not constitute the qualification to protection domain of the present invention.Any modification of within spirit of the present invention and principle, being done, be equal to replacement and improvement etc., all should be included within the claim protection domain of the present invention.
Claims (3)
1. nylon carrier fire-retardant master granule is characterized in that: by weight percentage, composed of the following components:
Polycaprolactam powder 9.4-49.6%;
MCA 50-90％；
Oxidation inhibitor 0.4-0.6%;
Wherein, the fineness of polycaprolactam powder is the 100-600 order, is that the employing molecular weight is the polycaprolactam polyimide resin of 17000-30000, pulverizes with Lowtemperaturepulverizer to form.
2. nylon carrier fire-retardant master granule according to claim 1 is characterized in that: said oxidation inhibitor is by four [3-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and composite the forming of tricresyl phosphite (2,4-di-t-butyl phenyl ester).
3. the preparation method of a nylon carrier fire-retardant master granule is characterized in that, may further comprise the steps:
Step 1, take by weighing each component by the described weight percent of claim 1;
Step 2, each component that will take by weighing add combination treatment 20-30min in the high-speed mixer, and temperature is controlled at 160-180 ℃;
Step 3, with the cooling of mixed material, cooled material joins in the hopper of twin screw extruder, through frit reaction, extruding pelletization; The twin screw extruder processing condition are: twin screw extruder one district temperature 180-190 ℃, two district temperature 190-220 ℃, three district temperature 210-220 ℃, four district temperature 215-220 ℃, five district temperature 210-220 ℃, residence time 2-3min, pressure are 12-18Mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110182306XA CN102363671A (en) | 2011-06-30 | 2011-06-30 | Flame-retardant master batch for nylon carrier and preparation method thereof |
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| CN201110182306XA CN102363671A (en) | 2011-06-30 | 2011-06-30 | Flame-retardant master batch for nylon carrier and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073515A (en) * | 2012-12-03 | 2013-05-01 | 杭州捷尔思阻燃化工有限公司 | Large-particle-size melamine cyanurate, and preparation method and application thereof |
| CN104292818A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method of nano halogen-free flame retardant polyamide-6 |
| CN104387763A (en) * | 2014-11-26 | 2015-03-04 | 河南机电高等专科学校 | Flame-retardant sealing ring for lithium ion batteries |
| CN106118040A (en) * | 2016-07-08 | 2016-11-16 | 广州鑫昇工程塑料有限公司 | A kind of high-efficiency environment friendly halogen-free flame retardants master batch and preparation method thereof |
| CN107760116A (en) * | 2017-11-18 | 2018-03-06 | 安徽省神洲建材科技有限公司 | A kind of preparation method of thermal insulation inner-wall veneer coating |
| CN109679338A (en) * | 2018-12-23 | 2019-04-26 | 德力西电气有限公司 | A kind of halogen-free flame-retardant polyamide alloy material of low precipitation and preparation method thereof |
| CN111574828A (en) * | 2020-06-30 | 2020-08-25 | 上海芷燃新材料有限公司 | Nylon halogen-free flame-retardant master batch and preparation method thereof |
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| CN1810862A (en) * | 2006-02-23 | 2006-08-02 | 广州金发科技股份有限公司 | Continuous long fiber reinforced fire-retardant thermoplastic resin and its prepn |
| CN101074317A (en) * | 2007-06-25 | 2007-11-21 | 辽宁大学 | Production of trimeric-cyanamide cyanurate fire-retardant nylon material |
| CN101139747A (en) * | 2007-09-20 | 2008-03-12 | 东华大学 | Method for preparing flame-proof polyamide 6 fibre by employing composite fire retarding agent |
| CN101343410A (en) * | 2007-07-12 | 2009-01-14 | 上海化工研究院 | Halogen-free flame-proof reinforced polyamide composition |
| CN101358033A (en) * | 2008-09-28 | 2009-02-04 | 大连工业大学 | Halogen-free anti-dripping flame-retardant material for polyamide |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1810862A (en) * | 2006-02-23 | 2006-08-02 | 广州金发科技股份有限公司 | Continuous long fiber reinforced fire-retardant thermoplastic resin and its prepn |
| CN101074317A (en) * | 2007-06-25 | 2007-11-21 | 辽宁大学 | Production of trimeric-cyanamide cyanurate fire-retardant nylon material |
| CN101343410A (en) * | 2007-07-12 | 2009-01-14 | 上海化工研究院 | Halogen-free flame-proof reinforced polyamide composition |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073515A (en) * | 2012-12-03 | 2013-05-01 | 杭州捷尔思阻燃化工有限公司 | Large-particle-size melamine cyanurate, and preparation method and application thereof |
| CN104292818A (en) * | 2014-09-09 | 2015-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method of nano halogen-free flame retardant polyamide-6 |
| CN104292818B (en) * | 2014-09-09 | 2016-08-17 | 上海纳米技术及应用国家工程研究中心有限公司 | The method of nanometer halogen-free anti-flaming polyamide-6 |
| CN104387763A (en) * | 2014-11-26 | 2015-03-04 | 河南机电高等专科学校 | Flame-retardant sealing ring for lithium ion batteries |
| CN106118040A (en) * | 2016-07-08 | 2016-11-16 | 广州鑫昇工程塑料有限公司 | A kind of high-efficiency environment friendly halogen-free flame retardants master batch and preparation method thereof |
| CN107760116A (en) * | 2017-11-18 | 2018-03-06 | 安徽省神洲建材科技有限公司 | A kind of preparation method of thermal insulation inner-wall veneer coating |
| CN109679338A (en) * | 2018-12-23 | 2019-04-26 | 德力西电气有限公司 | A kind of halogen-free flame-retardant polyamide alloy material of low precipitation and preparation method thereof |
| CN111574828A (en) * | 2020-06-30 | 2020-08-25 | 上海芷燃新材料有限公司 | Nylon halogen-free flame-retardant master batch and preparation method thereof |
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Application publication date: 20120229 |