CN104004270A - Low-halogen polypropylene flame-resistant materials and preparing method thereof - Google Patents
Low-halogen polypropylene flame-resistant materials and preparing 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
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
Abstract
The invention discloses low-halogen polypropylene flame-resistant materials and a preparing method thereof. The low-halogen polypropylene flame-resistant materials are obtained by the fact that homo-polypropylene, composite-prepared fire retardant, lubricating agents, antioxygen agents and inorganic filler are evenly mixed, and then extrusion pelleting is carried out through a double-screw extruder. The composite-prepared fire retardant is formed by mixing of phosphorus-containing fire retardant phenyl aluminum hypophosphite, bromine-containing fire retardant melamine hydrobromide or flame retardant TBC and flame retardant synergist 2,3-dimethyl-2,3-diphenylbutane. The antioxygen agents are formed by mixing of hindered phenol antioxygen agents 1010 and phosphite ester antioxygen agents 168. The phenyl aluminum hypophosphite is used as a foundation and is mixed with brominated flame retardant in a composite mode, through P-Br synergistic effect, flame retardant with the total adding amount not larger than 2wt% is used, flame-resistant PP with balanced comprehensive performance is obtained, the requirement for environment protecting is met, the flame resistance reaches American UL941.6mm V2, and the mechanical property and the electrical property are great.
Description
Technical field
The present invention relates to polypropylene (PP) flame retardant area, particularly relate to the technical field of phenyl phosphinic acid salt and bromide fire retardant compositional flame-retardant PP.
Background technology
PP molecular formula (C3H6) n is the universal thermoplastic resin of one of being prepared by propylene polycoordination.Nontoxic, light weight, mechanical property excellence, electrical insulating property is good, chemical resistance good.Because it is cheap, forming process is easy, so be widely used in the fields such as electronic apparatus, Communication Equipment, household electrical appliance, automobile, material of construction again.But PP oxygen index is only 17.4, and flame resistivity is poor, easily burning, and also combustion heating amount is large, very easily produces a large amount of melting drippages, initiation fire.Therefore the fire-retardant research of PP just becomes very important.
The more class methods of the fire-retardant application of PP are used to magnesium hydroxide (MDH) or this class hydrated metal compound fire retardant of aluminium hydroxide (ATH) exactly.For example US5583172, WO9810432 adopt respectively ATH, MDH are carried out to surface treatment, improve its flame retarding efficiency; Park, D.H etc. have studied ATH, MDH have been mixed to use, and study the cooperative flame retardant effect that may exist between ATH and MDH, shortcoming is that the addition of these hydrated metal compound fire retardants is large, the consistency of fire retardant and body material is poor, has had a strong impact on the processing characteristics of resin and the physical and mechanical property of final fire-retardant PP goods.
Halogen antimony cooperative flame retardant system is the fire-retardant a kind of effective ways of PP, and flame retarding efficiency is higher, and shortcoming is that halogen containing flame-retardant can react with some hindered amines stablizers, produces toxic smoke, contaminate environment.In the course of processing, also can produce sour gas corrosion equipment, increase difficulty of processing; Last goods also there will be the problem of frosting; This all requires halogen-antimony cooperative flame retardant PP system to improve.
Also rise in recent years the research that adopts the fire-retardant PP of expansion type flame retardant.Expansion type flame retardant (IFR) is made up of charcoal source, acid source and source of the gas, in the time of burning, acid source can be emitted mineral acid, make the polyvalent alcohol esterification in charcoal source, and then dehydration carbonization, under the effect of the small molecules volatile matter that the rare gas element that sticky carbonizing production discharges at source of the gas, the water vapour that reaction produces and polymer degradation produce, expand, form the charcoal layer of microvoid structure.That this charcoal layer has is heat insulation, oxygen barrier, without molten drop and make flame from the effect of putting out.For example US5204392,5204393,5484830 demonstrations are done acid source and source of the gas with APP, select pentaerthiyldichlorodiphosphite, urea-formaldehyde resin or melmac as char-forming agent, with the fire-retardant PP of this intumescent system, there is product to appear on the market at himont, clariant.US6921783 demonstration selects trimeric cyanamide phosphoric acid ester (MP) to do acid source and source of the gas, uses tetramethylolmethane and derivative thereof to carry out fire-retardant PP as char-forming agent, has also played the effect of expandable flame retardant.EP1516907 shows char-forming agent, the SiO with piperazine polyphosphate or trimeric cyanamide polyphosphate (MPP) and polyvalent alcohol and derivatives class thereof
2or the fire-retardant PP of metal oxide cooperation formation Intumscent Flame Retardant System, also obtain the flame retardant effect of expecting.US6632442 adopt the two spiro-phosphates (PEPA) of MPP and tetramethylolmethane separately add a small amount of organo montmorillonite carry out fire-retardant composite, addition 19wt%, 0.8wt% polynite just can reach fire-retardant PP UL-94V0.
Expansion type flame retardant has been got rid of adding of halogen from source, reduced issuable corrodibility poison gas in combustion processes, has adapted in recent years to the non-halogen requirement of fire retardant; But in example above, the addition of fire retardant is all that 20wt% is between 35wt%, and processing difficulties, the mechanical property of goods is also affected, fire retardant joins not resistance to migration in addition in PP, easily separate out the problem of material surface, the Intumescent Retardant System of APP series also can cause moisture absorption problem, and this all requires further to improve the even development of new char-forming agent of formulating of recipe of Intumscent Flame Retardant System.
Summary of the invention
Addition is large when overcoming the fire-retardant PP of hydrated metal compound and the fire-retardant PP of expansion type flame retardant, has a strong impact on the processing characteristics of PP goods and the shortcoming of physicals, and retains the defect of halogen antimony cooperative flame retardant system because of halogen containing flame-retardant contaminate environment.The invention provides a kind of low halogen polypropylene flameretardant material.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of low halogen polypropylene flameretardant material, it is characterized in that, it is by homo-polypropylene (abbreviation homopolymerization PP) 97-99wt%, compound flame redundant 0.8-2wt%, lubricant 0.1-0.3wt%, oxidation inhibitor 0.1-0.4wt%, mineral filler 0-0.3wt%, after evenly mixing, obtain through twin screw extruder extruding pelletization.
Described PP is commercially available PP.
Described compound flame redundant is mainly mixed by three kinds of components, main component is phosphonium flame retardant phenyl hypo-aluminum orthophosphate (FR006), brominated flame-retardant trimeric cyanamide hydrobromate or three (2,3-dibromopropyl) isocyanuric acid ester, fire retarding synergist 2,3-dimethyl-2,3-diphenyl butane (DMDPB); Three kinds of compositions phenyl hypo-aluminum orthophosphate by weight: brominated flame-retardant: DMDPB=1:0.1-2:0.05-0.25.
Described lubricant is EBS, chemical name: ethylenebisstearamide.
Described oxidation inhibitor, by Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168, mixes by weight 1010:168=1:1-1:2; 1010 chemical names are: four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester; 168 chemical names are: three (2,4-di-tert-butyl-phenyl) phosphorous acid ester;
Described mineral filler is titanium dioxide or magnesium hydroxide.
Low halogen polypropylene flameretardant material preparation method of the present invention is, take raw material by described weight percentage, each component is stirred in high-speed mixer, after mixing, through twin screw extruder, at temperature range 190-220 DEG C, under screw speed 300-400rpm condition, extruding pelletization obtains fire-retardant PP material.
The present invention has announced taking phenyl phosphinic acid aluminium as basis, composite with bromide fire retardant, act synergistically by P-Br, be not more than the fire retardant of 2wt% with total addition level, obtain over-all properties equilibrium, meet environmental requirement, flame retardant resistance reaches U.S. UL941.6mm V2, mechanical property, the good fire-retardant PP of electric property; This material can partly substitute the materials such as flame-proof ABS, PC, PBT.And reduce the addition of fire retardant, reduce because fire retardant add the impact on the PP course of processing.
Embodiment
Below in conjunction with 16 embodiment, the invention will be further described; specific embodiment is below just in order better to explain formula technique of the present invention and complete processing; but do not limit the scope of the invention, therefore adopt this patent mentality of designing, change embodiment that similar surrogate reaches PP flame retardant effect equally in the protection domain of this patent.
Wherein in following each embodiment,
PP resin is ExxonMobil PP1013H1, provided by LyondellBasell, MIF (melting index) 7.5g/10min (230 DEG C/2.16kg, ISO1133).
The preparation of FROO6 (phenyl hypo-aluminum orthophosphate) Qingdao Fu Silin Chemical Industry Science Co., Ltd, median size (D50%) is 3m, the particle diameter of D98% is less than 10m.
TBC (three (2,3-dibromopropyl) isocyanuric acid ester): Shandong Province of China Zibo Sheng Yu plastics company limited, fusing point (MP): 105-115 DEG C, bromine content at least 65%.
MHB (trimeric cyanamide hydrobromate): company limited provides by the fire-retardant BACN of Chinese Shifang Tai Feng, white powder, median size (D50%) is 5m.
DMDPB (2,3-dimethyl-2,3-diphenyl butane): San Heyuan Chemical Co., Ltd. provides by Heze.
Lubricate EBS (N, N'-ethylene bis stearamide) plastifies company limited by mountain one to be provided.
Oxidation inhibitor is three (2,4-di-tert-butyl-phenyl) phosphorous acid ester (abbreviation irgasfos 168), density 1.02-1.04g/cm3, pH value 5-7.
Hinered phenols antioxidant four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (abbreviation antioxidant 1010), density 1.15, fusing point 110-125 DEG C.
Titanium dioxide (TiO2) and magnesium hydroxide (MH) are bought from Jinan China Jin Yingtai chemical industry limited liability company.
Embodiment 1-8
Embodiment 1-8 is the flame retardant effect of FR-006 and MHB compositional flame-retardant PP.Each proportioning raw materials is in table one.Experimentation leads to method: take raw material by described weight percentage, each component is stirred in high-speed mixer, after mixing, through twin screw extruder, at temperature range 190-220 DEG C, under screw speed 300-400rpm condition, extruding pelletization obtains fire-retardant PP material.
Table one
Can find out from table one data analysis: embodiment 1-8 keeps DMDPB addition 0.1wt% constant, inquire into FR-006, MHB (trimeric cyanamide hydrobromate), DMDPB (2,3-dimethyl-2,3-diphenyl butane) the composite fire retardation to PP of three.Because DMDPB is used as radical initiator in PP is fire-retardant, it promotes PP molecular rupture, and then promotes molten drop drippage; Bromine can impel molten drop not fire, and reaches and promotes drippage, reaches fire-retardant effect; Wherein embodiment 1:FR-006, MHB, DMDPB total addition level are that 1.1wt% just can reach UL-941.6mm V2 level.Embodiment 5-8 has studied respectively mineral filler magnesium hydroxide (MH) and the coupling fire retardation of titanium dioxide (TiO2) with composite flame-retardant agent, result shows that mineral filler addition is between 0.1-0.2wt%, and fire-retardant PP also can reach UL-941.6mm V2 level.
Embodiment 9-16
Embodiment 9-16 is the flame retardant effect of FR-006 and TBC compositional flame-retardant PP, and each proportioning raw materials is in table two, and preparation process is identical with table one embodiment.
Table two
Can find out from table two data analysis, embodiment 9-16 keeps DMDPB addition 0.1wt% constant, research FR-006, three (2,3-dibromopropyl) isocyanuric acid ester (TBC), the composite fire retardation to PP of DMDPB three.The effect of DMDPB (2,3-dimethyl-2,3-diphenyl butane) in PP is fire-retardant is to exist as the effect of radical initiator.Wherein embodiment 15:FR-006, TBC, DMDPB total addition level are that 0.8wt% just can reach UL941.6mm V2 level; Maintain the addition of TBC0.3wt% in embodiment 13-14 time, add inorganic particulate magnesium hydroxide (MH), MH fire-retardant PP in the time of 0.1-0.2wt% can reach UL941.6mm V2 level, in embodiment 15-16, phenyl hypo-aluminum orthophosphate (FR006) adds 0.5wt%, add the inorganic particulate TiO2 of 0.1-0.2wt%, when TiO2 and compound flame redundant total addition level are 1-1.2wt%, fire-retardant PP has reached UL941.6mm V-2 level.
Claims (2)
1. a low halogen polypropylene flameretardant material, is characterized in that, it is by homo-polypropylene 97-99wt%, compound flame redundant 0.8-2wt%, lubricant 0.1-0.3wt%, oxidation inhibitor 0.1-0.4wt%, mineral filler 0-0.3wt%, after evenly mixing, obtains through twin screw extruder extruding pelletization;
Described compound flame redundant is by phosphonium flame retardant phenyl hypo-aluminum orthophosphate, brominated flame-retardant trimeric cyanamide hydrobromate or three (2,3-dibromopropyl) isocyanuric acid ester and fire retarding synergist 2,3-dimethyl-2,3-diphenyl butane mixes, blending ratio is: by weight, and phenyl hypo-aluminum orthophosphate: brominated flame-retardant: fire retarding synergist=1:(0.1-2): (0.05-0.25);
Described lubricant is ethylenebisstearamide;
Described oxidation inhibitor, by Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168, mixes by weight 1010:168=1:1-1:2;
Described mineral filler is titanium dioxide or magnesium hydroxide.
2. the preparation method of a low halogen polypropylene flameretardant material as claimed in claim 1, it is characterized in that, take raw material by described weight percentage, each component is stirred in high-speed mixer, after mixing, through twin screw extruder, at temperature range 190-220 DEG C, under screw speed 300-400rpm condition, extruding pelletization obtains low halogen polypropylene flameretardant material.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418047A (en) * | 2017-06-02 | 2017-12-01 | 中山康诺德新材料有限公司 | A kind of High glow wire halogen-free flame retardant polyolefin composition and preparation method |
| CN108659339A (en) * | 2018-05-22 | 2018-10-16 | 青岛科技大学 | A kind of anti-flaming polypropylene material and preparation method thereof with good photostability |
| CN108976593A (en) * | 2018-06-20 | 2018-12-11 | 金发科技股份有限公司 | A kind of flame retardant polyolefin compound and preparation method thereof |
| CN109135046A (en) * | 2018-06-20 | 2019-01-04 | 金发科技股份有限公司 | A kind of flame retardant polyolefin compound and preparation method thereof |
| CN112225985A (en) * | 2020-09-04 | 2021-01-15 | 万华化学（宁波）有限公司 | Flame-retardant PP composite material and preparation method thereof |
| CN112694643A (en) * | 2020-12-25 | 2021-04-23 | 广东宇星阻燃安全材料研究院有限公司 | Preparation method of low-halogen flame retardant and application of low-halogen flame retardant in polypropylene |
| CN112812459A (en) * | 2020-12-30 | 2021-05-18 | 江西博硕电子有限公司 | Antimony-free flame-retardant polyvinyl chloride cable material and preparation method and application thereof |
| CN113912938A (en) * | 2021-10-12 | 2022-01-11 | 厦门稀土材料研究所 | Ultraviolet aging resistant flame-retardant polypropylene material and preparation method thereof |
| CN114736453A (en) * | 2022-03-14 | 2022-07-12 | 金发科技股份有限公司 | Low-halogen flame-retardant PP material and preparation method and application thereof |
| CN115232352A (en) * | 2021-04-23 | 2022-10-25 | 中国石油化工股份有限公司 | Flame-retardant antibacterial polypropylene composition, polypropylene expanded bead, preparation method of polypropylene expanded bead and molded body |
| CN115558181A (en) * | 2022-09-29 | 2023-01-03 | 广东顺德科恩新材料有限公司 | Flame-retardant master batch and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418047A (en) * | 2017-06-02 | 2017-12-01 | 中山康诺德新材料有限公司 | A kind of High glow wire halogen-free flame retardant polyolefin composition and preparation method |
| CN108659339A (en) * | 2018-05-22 | 2018-10-16 | 青岛科技大学 | A kind of anti-flaming polypropylene material and preparation method thereof with good photostability |
| CN108659339B (en) * | 2018-05-22 | 2020-07-21 | 青岛科技大学 | Flame-retardant polypropylene material with good light stability and preparation method thereof |
| CN108976593A (en) * | 2018-06-20 | 2018-12-11 | 金发科技股份有限公司 | A kind of flame retardant polyolefin compound and preparation method thereof |
| CN109135046A (en) * | 2018-06-20 | 2019-01-04 | 金发科技股份有限公司 | A kind of flame retardant polyolefin compound and preparation method thereof |
| CN112225985B (en) * | 2020-09-04 | 2023-03-31 | 万华化学（宁波）有限公司 | Flame-retardant PP composite material and preparation method thereof |
| CN112225985A (en) * | 2020-09-04 | 2021-01-15 | 万华化学（宁波）有限公司 | Flame-retardant PP composite material and preparation method thereof |
| CN112694643A (en) * | 2020-12-25 | 2021-04-23 | 广东宇星阻燃安全材料研究院有限公司 | Preparation method of low-halogen flame retardant and application of low-halogen flame retardant in polypropylene |
| CN112812459A (en) * | 2020-12-30 | 2021-05-18 | 江西博硕电子有限公司 | Antimony-free flame-retardant polyvinyl chloride cable material and preparation method and application thereof |
| CN115232352A (en) * | 2021-04-23 | 2022-10-25 | 中国石油化工股份有限公司 | Flame-retardant antibacterial polypropylene composition, polypropylene expanded bead, preparation method of polypropylene expanded bead and molded body |
| CN113912938A (en) * | 2021-10-12 | 2022-01-11 | 厦门稀土材料研究所 | Ultraviolet aging resistant flame-retardant polypropylene material and preparation method thereof |
| CN114736453A (en) * | 2022-03-14 | 2022-07-12 | 金发科技股份有限公司 | Low-halogen flame-retardant PP material and preparation method and application thereof |
| CN114736453B (en) * | 2022-03-14 | 2023-09-26 | 金发科技股份有限公司 | Low-halogen flame-retardant PP material and preparation method and application thereof |
| CN115558181A (en) * | 2022-09-29 | 2023-01-03 | 广东顺德科恩新材料有限公司 | Flame-retardant master batch and preparation method and application thereof |
| CN115558181B (en) * | 2022-09-29 | 2024-03-19 | 广东顺德科恩新材料有限公司 | Flame-retardant master batch and preparation method and application thereof |
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