CN107353647A - A kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof - Google Patents
A kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof Download PDFInfo
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- CN107353647A CN107353647A CN201610312491.2A CN201610312491A CN107353647A CN 107353647 A CN107353647 A CN 107353647A CN 201610312491 A CN201610312491 A CN 201610312491A CN 107353647 A CN107353647 A CN 107353647A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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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- Polymers & Plastics (AREA)
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- Fireproofing Substances (AREA)
Abstract
The invention discloses a kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof, it is by 50 85% parts of main flame retardant, synergistic flame retardant 5 30%, odor adsorption agent 1 5%, hyperbranched polyorganosiloxane 5 15%, silane coupler 0.5 1%, heat stabilizer 0.2 1%, lubricant 0.2 1% are made through banburying, extruding pelletization.Fire-retardant master granule versatility prepared by the present invention is wide, active ingredient is high, low without obvious smell, addition, and preparation method is simple, and can effectively reduce dust pollution, improves work situation.
Description
Technical field
The present invention relates to technical field of macromolecules, and in particular to a kind of low smell, low distributes carrier-free nano flame-proof agglomerate
And preparation method thereof.
Background technology
With modern fire-retardant the reach of science, cooperative effect technology is increasingly used widely, particularly in multi-functional resistance
In combustion system, this technology can not only significantly improve the flame retarding efficiency of system, and can reduce some valencys in flame-retardant system
Lattice are expensive or the content of rare component, to meet the increasingly strict flame-retardancy requirements in some fields.The particle diameter of powdery combustion inhibitor is general
In micron order, or even nanoscale, it can produce arch formation during production application, and more seriously it is using process
In can produce a large amount of dust pollution, seriously jeopardize health of human body.At present, master-batch techniques, which turn into, solves this problem effective means.And
Usual carrier model fire-retardant master granule, consistency problem, Yi Zao be present because of the characteristic of its vector resin, during other non-carrier resin alloys
Into the significantly decline of fire proofing physical and chemical performance, its application is restricted.
The content of the invention
It is an object of the invention to provide a kind of low smell, low distribute carrier-free nano flame-proof agglomerate and preparation method thereof.
In order to realize the purpose of the present invention, the invention provides a kind of low smell, it is low distribute carrier-free nano flame-proof agglomerate,
It is characterized in that：It is prepared by mass percentage by following components：
Main flame retardant 50-85%,
Synergistic flame retardant 5-30%,
Odor adsorption agent 1-5%,
Hyperbranched polyorganosiloxane 5-15%,
Silane coupler 0.5-1%,
Heat stabilizer 0.2-1%,
Lubricant 0.2-1%.
Further scheme, described main flame retardant are made up of aluminum diethylphosphinate and melamine cyanurate, wherein two
The mass percent of ethylphosphinic acid aluminium is 50-90%.
The synergistic flame retardant is nano-sized magnesium hydroxide of the surface through silane coupler activation process.
Described odor adsorption agent is made up of by weight percentage following components：Hydrophobicity diatomite 50-70%, needle-like boiling
Stone molecular sieve 15-45%, high molecular quaternary grafted silica 5-15%.
Described hyperbranched polyorganosiloxane is active branched polymer amount siloxanes, and its molecular weight is 40~800,000.
Described silane coupler is gamma-aminopropyl-triethoxy-silane (KH550) or γ-(methacryloxypropyl) propyl group
Trimethoxy silane (KH570).
Described heat stabilizer is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and three
The mixture of [2.4- di-tert-butyl-phenyls] phosphite ester.
Described lubricant is at least one of zinc stearate, Tissuemat E, paraffin, stearic amide.
It is a further object to provide above-mentioned low smell, the low preparation side for distributing carrier-free nano flame-proof agglomerate
Method, comprise the following steps：
(1) nano-sized magnesium hydroxide and deionized water are added in activation pot, 60-80 DEG C is heated to, by nano-sized magnesium hydroxide
The 2-4% of quality adds the silane coupler dissolved, and insulated and stirred is surface-treated to nano-sized magnesium hydroxide, obtains synergistic resistance
Fire agent；
(2) main flame retardant, synergistic flame retardant, odor adsorption agent, hyperbranched polyorganosiloxane, silane idol are added in banbury
Join agent, heat stabilizer and lubricant, banburying is blocking to material, then the blocking material after banburying is added in screw extruder and carried out
It is granulated, low smell is made, low distributes carrier-free nano flame-proof agglomerate.
The nano-sized magnesium hydroxide slurries good in activation pot surface treated use pulverizer after filter press filters off water
Filter cake is smashed, dried, makes powder water content for≤0.5wt%, then crushing is carried out to it by airslide disintegrating mill and breaks up to obtain
The nano-sized magnesium hydroxide of surface active；
The area's temperature of double screw extruder one is 60-80 DEG C, and two area's temperature are 100-120 DEG C, and three area's temperature are 130-
160 DEG C, four area's temperature are 150-180 DEG C, and five area's temperature are 160-180 DEG C, and six area's temperature are 160-170 DEG C, and seven area's temperature are
160-170℃；Twin-screw engine speed is 30-60rpm.
Beneficial effects of the present invention：
1. the synergistic flame retardant nano-sized magnesium hydroxide that the present invention uses improves it in base resinite after overactivation
It is scattered, while its moisture absorption defect is further improved, so as to serve good flame retardant synergism, and be advantageous to improve the power of material
Performance is learned, material is kept higher combination property.
2. odor adsorption body agent of the present invention is hydrophobic type, the general volatile for significantly reducing carrier-free nano flame-proof agglomerate is organic
Thing TVOC, relatively low water absorption rate is also maintained while guarantee material low odor property；Base is added to as fire-retardant master granule
The moulding processability of matrix plastic is not interfered with body plastics then.
3. the versatility of carrier-free nano flame-proof agglomerate prepared by the present invention is wide, active ingredient is high, without obvious smell, addition
Measure low, and preparation method is simple, and can effectively reduce dust pollution, improves work situation.
Embodiment
Embodiment 1
(1) nano-sized magnesium hydroxide, deionized water are added in activation pot, 60 DEG C are heated to, by nano-sized magnesium hydroxide quality
2% add the silane coupler gamma-aminopropyl-triethoxy-silane that has dissolved, insulated and stirred 30min.What is be surface-treated receives
Rice magnesium hydroxide slurry filters off water through filter press, is smashed filter cake with pulverizer, drops to powder water content by drying
≤ 0.5%, then by airslide disintegrating mill crush and break up to obtain the nano-sized magnesium hydroxide of surface active.
(2) added in banbury 65% main flame retardant (aluminum diethylphosphinate 75%, melamine cyanurate 25%),
20% synergistic flame retardant (nano-sized magnesium hydroxide of surface active), 2% odor adsorption agent (hydrophobicity diatomite 60%, 30% pin
Shape zeolite molecular sieve, 10% high molecular quaternary grafted silica), 10% hyperbranched polyorganosiloxane, 1% silane coupler
Gamma-aminopropyl-triethoxy-silane, 0.5% antioxidant 1010,0.5% irgasfos 168,0.5% zinc stearate, 0.5% paraffin,
Banburying is blocking to material, then material after banburying is added in screw extruder and is granulated, and low smell is made, low distributes no-load
Body nano flame-proof agglomerate.Wherein the area's temperature of double screw extruder one is 70 DEG C, and two area's temperature are 110 DEG C, and three area's temperature are 140
DEG C, four area's temperature are 160 DEG C, and five area's temperature are 170 DEG C, and six area's temperature are 160 DEG C, and seven area's temperature are 160 DEG C；Twin-screw main frame
Rotating speed is 50rpm.
Embodiment 2
(1) nano-sized magnesium hydroxide, deionized water are added in activation pot, 80 DEG C are heated to, by nano-sized magnesium hydroxide quality
4% adds silane coupler γ-(methacryloxypropyl) propyl trimethoxy silicane dissolved, is surface-treated, and is incubated
Stir 30min.The nano-sized magnesium hydroxide slurries being surface-treated filter off water through filter press, are smashed filter cake with pulverizer, warp
Crossing to dry makes powder water content drop to≤0.5%, then by airslide disintegrating mill crush and break up to obtain receiving for surface active
Rice magnesium hydroxide.
(2) added in banbury 50% main flame retardant (aluminum diethylphosphinate 90%, melamine cyanurate 10%),
30% synergistic flame retardant (nano-sized magnesium hydroxide of surface active), 4% odor adsorption agent (hydrophobicity diatomite 50%, 45% pin
Shape zeolite molecular sieve, 5% high molecular quaternary grafted silica), 15% hyperbranched polyorganosiloxane, 0.5% silane coupler
γ-(methacryloxypropyl) propyl trimethoxy silicane, 0.1% antioxidant 1010,0.1% irgasfos 168,0.2% polyethylene
Wax, 0.1% stearic amide, banburying is blocking to material, then the material after banburying is added in screw extruder and is granulated, and makes
Low smell, low distribute carrier-free nano flame-proof agglomerate.Wherein the area's temperature of double screw extruder one is 60 DEG C, and two area's temperature are
100 DEG C, three area's temperature are 130 DEG C, and four area's temperature are 150 DEG C, and five area's temperature are 160 DEG C, and six area's temperature are 170 DEG C, seven area's temperature
Spend for 170 DEG C；Twin-screw engine speed is 30rpm.
Embodiment 3
(1) nano-sized magnesium hydroxide, deionized water are added in activation pot, 70 DEG C are heated to, by nano-sized magnesium hydroxide quality
3% adds the silane coupler gamma-aminopropyl-triethoxy-silane dissolved, is surface-treated, insulated and stirred 30min.Table
The nano-sized magnesium hydroxide slurries that face is handled well filter off water through filter press, are smashed filter cake with pulverizer, make powder by drying
Water content drops to≤0.5%, then by airslide disintegrating mill crush and break up to obtain the nano-sized magnesium hydroxide of surface active.
(2) added in banbury 85% main flame retardant (aluminum diethylphosphinate 50%, melamine cyanurate 50%),
5% synergistic flame retardant (nano-sized magnesium hydroxide of surface active), 1% odor adsorption agent (hydrophobicity diatomite 70%, 15% needle-like
Zeolite molecular sieve, 15% high molecular quaternary grafted silica), 7.5% hyperbranched polyorganosiloxane, 0.7% silane coupler
Gamma-aminopropyl-triethoxy-silane, 0.2% antioxidant 1010,0.2% irgasfos 168,0.2% zinc stearate, 0.2% paraffin,
Banburying is blocking to material, then material after banburying is added in screw extruder and is granulated, and low smell is made, low distributes no-load
Body nano flame-proof agglomerate.
Wherein the area's temperature of double screw extruder one is 80 DEG C, and two area's temperature are 120 DEG C, and three area's temperature are 160 DEG C, four area's temperature
Spend for 180 DEG C, five area's temperature are 180 DEG C, and six area's temperature are 170 DEG C, and seven area's temperature are 170 DEG C；Twin-screw engine speed is
60rpm。
By the low smell made by above-described embodiment 1-3, it is low distribute carrier-free nano flame-proof agglomerate, effectively hindered according to equivalent
Combustion component substitutes powder fire retardant (activation nano-sized magnesium hydroxide) and is respectively applied in PBT, PA66, ABS, and fire-retardant change is carried out to it
Property embodiment 4-6 and comparative example 1-3 is made, material modified as shown in the table with when performance, wherein mechanical property uses
ASTM standard is detected, and oder levels, TVOC are detected using GMW standards, and fire resistance determines according to UL94 standards.
It can be seen by upper table 1, after carrier-free nano flame-proof agglomerate prepared by the present invention mixes with different resins matrix, it hinders
Combustion performance can reach UL94V-0 levels, and oder levels reach 6.5 grades, and the tensile strength of material, bending strength and thermal deformation
The performances such as temperature are superior to powder anti-flaming modified material, improve comprehensive mechanical property and the processing of fire proofing to a certain extent
Performance.
In addition, using the carrier-free nano flame-proof agglomerate of the present invention dust pollution can be reduced, improve environmental protection and to human body without
Evil；And compatibility is good between resin matrix, the physical and chemical performance of modified resin is also correspondingly improved.
The description of above embodiment is that the invention will be further described, but this is not the limit to the present invention
System, those skilled in the art according to the present invention basic thought, various modifications may be made or improve, but without departing from this
The basic thought of invention, within the scope of the present invention.
Claims (10)
1. a kind of low smell, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：Made by mass percentage by following components
It is standby to form：
Main flame retardant 50-85%,
Synergistic flame retardant 5-30%,
Odor adsorption agent 1-5%,
Hyperbranched polyorganosiloxane 5-15%,
Silane coupler 0.5-1%,
Heat stabilizer 0.2-1%,
Lubricant 0.2-1%.
2. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Main flame retardant be made up of aluminum diethylphosphinate and melamine cyanurate, the wherein mass percent of aluminum diethylphosphinate
For 50-90%.
3. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Synergistic flame retardant is nano-sized magnesium hydroxide of the surface through silane coupler activation process.
4. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Odor adsorption agent be made up of by weight percentage following components：Hydrophobicity diatomite 50-70%, needle-like zeolite molecular sieve 15-
45%th, high molecular quaternary grafted silica 5-15%.
5. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Hyperbranched polyorganosiloxane be active branched polymer amount siloxanes, its molecular weight is 40~800,000.
6. a kind of low smell according to claim 1 or 3, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：Institute
The silane coupler stated be gamma-aminopropyl-triethoxy-silane or γ-（Methacryloxypropyl）Propyl trimethoxy silicane.
7. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Heat stabilizer for four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester and three [2.4- di-t-butyls
Phenyl] phosphite ester mixture.
8. a kind of low smell according to claim 1, low distribute carrier-free nano flame-proof agglomerate, it is characterised in that：It is described
Lubricant be zinc stearate, Tissuemat E, paraffin, at least one of stearic amide.
9. a kind of low smell, the low preparation method for distributing carrier-free nano flame-proof agglomerate as claimed in claim 1, its feature exist
In：Comprise the following steps：
（1）Nano-sized magnesium hydroxide and deionized water are added in activation pot, 60-80 DEG C is heated to, by nano-sized magnesium hydroxide quality
2-4% add the silane coupler that has dissolved, insulated and stirred is surface-treated to nano-sized magnesium hydroxide, obtains synergistic flame retardant；
（2）Main flame retardant, synergistic flame retardant, odor adsorption agent, hyperbranched polyorganosiloxane, silane coupled is added in banbury
Agent, heat stabilizer and lubricant, banburying is blocking to material, then the blocking material after banburying is added in screw extruder and made
Grain, low smell is made, low distributes carrier-free nano flame-proof agglomerate.
10. preparation method according to claim 9, it is characterised in that：The nanometer good in activation pot surface treated
Magnesium hydroxide slurry smashes filter cake after filter press filters off water, with pulverizer, dries, make powder water content for≤
0.5wt%, then it is carried out to crush by airslide disintegrating mill and breaks up to obtain the nano-sized magnesium hydroxide of surface active；
The area's temperature of double screw extruder one is 60-80 DEG C, and two area's temperature are 100-120 DEG C, and three area's temperature are 130-160
DEG C, four area's temperature are 150-180 DEG C, and five area's temperature are 160-180 DEG C, and six area's temperature are 160-170 DEG C, and seven area's temperature are 160-
170℃；Twin-screw engine speed is 30-60rpm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107936604A (en) * | 2017-12-04 | 2018-04-20 | 王文广 | One kind removes VOC masterbatch |
| CN108676231A (en) * | 2018-05-24 | 2018-10-19 | 成都菲斯特新材料有限公司 | A kind of PE/PET, PE/PP bicomponent fibers flame-retardant master batch and preparation method |
| CN111117168A (en) * | 2018-10-30 | 2020-05-08 | 万华化学集团股份有限公司 | Flame-retardant master batch and aromatic polymer composition containing same |
| CN111363367A (en) * | 2020-04-01 | 2020-07-03 | 见喜新材料股份有限公司 | Low-temperature ceramic flame-retardant functional master batch and preparation method thereof |
| CN112759823A (en) * | 2020-12-29 | 2021-05-07 | 金发科技股份有限公司 | Irradiation crosslinking low-smoke halogen-free polyolefin cable material and preparation method and application thereof |
| CN113563663A (en) * | 2021-07-22 | 2021-10-29 | 广东聚石化学股份有限公司 | Fire-resistant low-smoke halogen-free soft material and preparation method thereof |
| CN114672099A (en) * | 2022-02-22 | 2022-06-28 | 金发科技股份有限公司 | Magnesium hydroxide master batch and preparation method and application thereof |
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| CN102558850A (en) * | 2011-12-13 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Flame-retardant functional masterbatch special for nylon 6 and preparation method for masterbatch |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102558850A (en) * | 2011-12-13 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | Flame-retardant functional masterbatch special for nylon 6 and preparation method for masterbatch |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107936604B (en) * | 2017-12-04 | 2022-09-02 | 王文广 | VOC (volatile organic compound) removing master batch |
| CN107936604A (en) * | 2017-12-04 | 2018-04-20 | 王文广 | One kind removes VOC masterbatch |
| CN108676231A (en) * | 2018-05-24 | 2018-10-19 | 成都菲斯特新材料有限公司 | A kind of PE/PET, PE/PP bicomponent fibers flame-retardant master batch and preparation method |
| CN108676231B (en) * | 2018-05-24 | 2021-05-18 | 成都菲斯特新材料有限公司 | Flame-retardant master batch for PE/PET (polyethylene/polyethylene terephthalate) and PE/PP (polyethylene/polypropylene) bicomponent fibers and preparation method thereof |
| CN111117168A (en) * | 2018-10-30 | 2020-05-08 | 万华化学集团股份有限公司 | Flame-retardant master batch and aromatic polymer composition containing same |
| CN111117168B (en) * | 2018-10-30 | 2022-03-11 | 万华化学集团股份有限公司 | Flame-retardant master batch and aromatic polymer composition containing same |
| CN111363367A (en) * | 2020-04-01 | 2020-07-03 | 见喜新材料股份有限公司 | Low-temperature ceramic flame-retardant functional master batch and preparation method thereof |
| CN111363367B (en) * | 2020-04-01 | 2022-03-08 | 见喜新材料股份有限公司 | Low-temperature ceramic flame-retardant functional master batch and preparation method thereof |
| CN112759823A (en) * | 2020-12-29 | 2021-05-07 | 金发科技股份有限公司 | Irradiation crosslinking low-smoke halogen-free polyolefin cable material and preparation method and application thereof |
| CN113563663A (en) * | 2021-07-22 | 2021-10-29 | 广东聚石化学股份有限公司 | Fire-resistant low-smoke halogen-free soft material and preparation method thereof |
| CN113563663B (en) * | 2021-07-22 | 2023-09-12 | 广东聚石化学股份有限公司 | Fireproof low-smoke halogen-free soft material and preparation method thereof |
| CN114672099A (en) * | 2022-02-22 | 2022-06-28 | 金发科技股份有限公司 | Magnesium hydroxide master batch and preparation method and application thereof |
| CN114672099B (en) * | 2022-02-22 | 2023-08-29 | 金发科技股份有限公司 | Magnesium hydroxide master batch and preparation method and application thereof |
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Application publication date: 20171117 |