CN104693485A - Halogen-free intumescent compound flame retardant and application thereof in high-density polyethylene - Google Patents
Halogen-free intumescent compound flame retardant and application thereof in high-density polyethylene Download PDFInfo
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Abstract
The invention relates to a halogen-free intumescent compound flame retardant which is prepared by mixing the following components in weight percentage at high speed by means of a high mixing machine: 55-65 wt% of acid source, 18-28% of carbon source, 2-12% of gas source and 5-15% of synergist; the acid source is one or a mixture of ammonium polyphosphate, melamine phosphate and melamine polyphosphate; the carbon source is one or a mixture of dipentaerythritol, pentaerythritol phosphate and triazine char-forming agent; the gas source is melamine or melamine cyanurate or a mixture thereof; and the synergist is one or a mixture of hypophosphite, pyrophosphate, phosphate, silicon dioxide and lanthanum oxide. The halogen-free intumescent compound flame retardant is high in flame retardant efficient, low in cost, good in compatibility with matrixes and simple in preparation process; when the halogen-free intumescent compound flame retardant is applied to LDPE (Low-density Polyethylene), the obtained LDPE material has excellent flame retardant performance and is capable of maintaining mechanical property and effectively controlling molten drops.
Description
Technical field
the invention belongs to technical field of flame retardant, be specifically related to a kind of halogen-free expansible compound flame retardant and the application in high density polyethylene(HDPE) thereof.
Background technology
at present, be applied to the fire retardant mainly additive flame retardant of plastic applications, namely adopt additive flame retardant and resin matrix to melt extrude blended method and prepare flame retarded polymeric material.Conventional additive flame retardant has following a few class: metal hydroxides, comprises magnesium hydroxide, aluminium hydroxide etc.; Halogenated flame retardant, composite based on halogen antimony; Inorganic phosphorus flame retardant, is mainly red phosphorus; Organic phosphorus flame retardant, as phenoxy group ring phosphonitrile, alkyl phosphate etc.; A class is also had to be exactly expansion type flame retardant in addition.The shortcoming of metal hydroxide combustion inhibitor is that flame retarding efficiency is low, and addition is large, with the poor compatibility of resin matrix, larger to material mechanical performance infringement; Although halogenated flame retardant flame retarding efficiency is high, cost is low, the hazardous and noxious substances serious harm human health that its burning produces and contaminate environment, in today that environmental protection cry grows to even greater heights, halogenated flame retardant application is on a declining curve year by year; Red phosphorus has higher flame retarding efficiency, but its distinctive redness greatly limit its application; Organic phosphorus flame retardant flame retarding efficiency is higher, but cost is also very high, and actual application value is little; Expansion type flame retardant because of its flame retarding efficiency higher, addition is relatively less, and application prospect is had an optimistic view of, but at present halogen-free expansion fire retardant is used for still there is cost higher problem when polyolefine material is fire-retardant, makes its application be subject to a definite limitation.
high density polyethylene(HDPE) (high density polyethylene, i.e. HDPE) resin is white granular that is nontoxic, tasteless, odorless, fusing point is about 130 DEG C, relative density is 0.941 ~ 0.960, it has good thermotolerance and winter hardiness, and chemical stability is good, also has higher rigidity and toughness, physical strength is high, and dielectric properties, environmental stress cracking resistance are good.High density polyethylene(HDPE) because of its good over-all properties of many uses, common for extruding packaging film, rope, woven bag, water pipe and fishing net, injection moulding low-grade daily necessities, non-load member, glue case and Turnover Box, extrusion-blown modling container, hollow piece are as bottle etc.But because high density polyethylene(HDPE) is inflammable, combustionvelocity is fast and with producing a large amount of molten drops, thus brings larger disaster hidden-trouble, does not also have highly effective halogen-free flameproof, melt-drip resistant inflaming retarding agent at present for HDPE material.
Summary of the invention
the present invention is intended to overcome the deficiencies in the prior art, provides the halogen-free expansible compound flame retardant that a kind of flame retarding efficiency is higher, cost is lower.
another object of the present invention is applied in high-density polyethylene material by above-mentioned halogen-free expansible compound flame retardant, obtains that a kind of cost is lower, flame retardant effect is better and has the Flame-retardant Hdpe material of anti-dropping effect.
for solving above technical problem, the technical scheme that the present invention takes is:
a kind of halogen-free expansible compound flame retardant, by weight percentage, described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by following component: 55% ~ 65% acid source, 18% ~ 28% charcoal source, 2% ~ 12% source of the gas and 5% ~ 15% synergist; Wherein, described acid source is the combination of one or more in ammonium polyphosphate, melamine phosphate and melamine polyphosphate; Described charcoal source is one or more the combination in dipentaerythritol (DPER), pentaerythritol phosphate (PEPA) and triazine char-forming agent; Described source of the gas is trimeric cyanamide or melamine cyanurate or both mixing; Described synergist is the combination of one or more in hypophosphite, pyrophosphate salt, phosphoric acid salt, silicon-dioxide and lanthanum trioxide.
preferably, by weight percentage, described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by following component: 60% ~ 65% ammonium polyphosphate, 20% ~ 25% pentaerythritol phosphate, 2% ~ 7% melamine cyanurate and 8% ~ 12% hypophosphite.
a kind of Flame-retardant Hdpe material, containing above-mentioned halogen-free expansible compound flame retardant in feed composition, by weight percentage, the composition of raw materials of described Flame-retardant Hdpe material comprises following component: 53% ~ 59% high-density polyethylene resin, 10% ~ 20% weighting agent, 25% ~ 30% halogen-free expansible compound flame retardant, 0.3% ~ 0.6% oxidation inhibitor, 0.2% ~ 0.5% lubricant, 0.3% ~ 0.5% coupling agent and 0.2% ~ 0.4% dispersion agent; Described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by the component of following weight percent: 55% ~ 65% acid source, 18% ~ 28% charcoal source, 2% ~ 12% source of the gas and 5% ~ 15% synergist; Wherein, described acid source is the combination of one or more in ammonium polyphosphate, melamine phosphate and melamine polyphosphate; Described charcoal source is one or more the combination in dipentaerythritol, pentaerythritol phosphate and triazine char-forming agent; Described source of the gas is trimeric cyanamide or melamine cyanurate or both mixing; Described synergist is the combination of one or more in hypophosphite, pyrophosphate salt, phosphoric acid salt, silicon-dioxide and lanthanum trioxide.
preferably, described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by the component of following weight percent: 60% ~ 65% ammonium polyphosphate, 20% ~ 25% pentaerythritol phosphate, 2% ~ 7% melamine cyanurate and 8% ~ 12% hypophosphite.
preferably, described weighting agent is talcum powder.
preferably, described oxidation inhibitor is the combination of one or more in irgasfos 168, oxidation inhibitor 628 and antioxidant 1010.
preferably, described lubricant is the combination of one or more in calcium stearate, Magnesium Stearate, Zinic stearas, polyethylene wax, amide waxe and pentaerythritol ester series lubricant agent.
preferably, described coupling agent is silane coupling agent, as KH550, KH560 or KH570 etc.
preferably, described dispersion agent is silicone powder.
due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
halogen-free expansible compound flame retardant of the present invention has that flame retarding efficiency is high, cost is low, with the plurality of advantages such as matrix phase capacitive is good, halogen-free environmental, preparation technology are simple; Flame-retardant Hdpe material of the present invention have good flame-retardance can while can keep its mechanical property well, and can effectively control combustion time molten drop phenomenon, cost is also cheaper compared with similar flame retardant products.
Embodiment
below in conjunction with each embodiment, the present invention is described in more detail, but is not limited to these embodiments.
embodiment 1
(1) by mass percentage, to prepare the formula of halogen-free expansible compound flame retardant as follows for the present embodiment: 60% ammonium polyphosphate, 18%DPER, 5% triazine char-forming agent, 7% melamine cyanurate, 10% hypophosphite; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, namely obtain the halogen-free expansible compound flame retardant of the present embodiment;
(2) composition of raw materials that by mass percentage, the present embodiment prepares Flame-retardant Hdpe material comprises following component: halogen-free expansible compound flame retardant, 0.2% irgasfos 168,0.1% antioxidant 1010,0.5% calcium stearate, 0.3% silicone powder that 58.5%HDPE resin, 10% talcum powder, 30% step (1) prepare; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, then take 0.4% coupling agent KH550, add in high mixer and continue to mix; Then mixing gained material is added melt blending in twin screw extruder, extruding pelletization, namely obtain the Flame-retardant Hdpe material of the present embodiment.
embodiment 2
(1) by mass percentage, to prepare the formula of halogen-free expansible compound flame retardant as follows for the present embodiment: 60% melamine phosphate, 15%PEPA, 8% triazine char-forming agent, 7% trimeric cyanamide, 10% pyrophosphate salt; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, namely obtain the halogen-free expansible compound flame retardant of the present embodiment;
(2) composition of raw materials that by mass percentage, the present embodiment prepares Flame-retardant Hdpe material comprises following component: halogen-free expansible compound flame retardant, 0.3% antioxidant 1010,0.5% polyethylene wax, 0.3% silicone powder that 58.5%HDPE resin, 10% talcum powder, 30% step (1) prepare; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, then take 0.4% coupling agent KH560, add in high mixer and continue to mix; Then mixing gained material is added melt blending in twin screw extruder, extruding pelletization, namely obtain the Flame-retardant Hdpe material of the present embodiment.
embodiment 3
(1) by mass percentage, to prepare the formula of halogen-free expansible compound flame retardant as follows for the present embodiment: 65% ammonium polyphosphate, 25%PEPA, 2% melamine cyanurate, 8% hypophosphite; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, namely obtain the halogen-free expansible compound flame retardant of the present embodiment;
(2) composition of raw materials that by mass percentage, the present embodiment prepares Flame-retardant Hdpe material comprises following component: halogen-free expansible compound flame retardant, 0.2% irgasfos 168,0.1% antioxidant 1010,0.5% Zinic stearas, 0.3% silicone powder that 58.5%HDPE resin, 10% talcum powder, 30% step (1) prepare; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, then take 0.4% coupling agent KH550, add in high mixer and continue to mix; Then mixing gained material is added melt blending in twin screw extruder, extruding pelletization, namely obtain the Flame-retardant Hdpe material of the present embodiment.
embodiment 4
(1) by mass percentage, to prepare the formula of halogen-free expansible compound flame retardant as follows for the present embodiment: 60% ammonium polyphosphate, 10%DPER, 10%PEPA, 3% triazine char-forming agent, 7% melamine cyanurate, 10% hypophosphite; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, namely obtain the halogen-free expansible compound flame retardant of the present embodiment;
(2) composition of raw materials that by mass percentage, the present embodiment prepares Flame-retardant Hdpe material comprises following component: halogen-free expansible compound flame retardant, 0.2% irgasfos 168,0.1% antioxidant 1010,0.5% calcium stearate, 0.3% silicone powder that 53.5%HDPE resin, 20% talcum powder, 25% step (1) prepare; Add high-speed mixer and mixing after taking corresponding raw material by above-mentioned formula even, then take 0.4% coupling agent KH550, add in high mixer and continue to mix; Then mixing gained material is added melt blending in twin screw extruder, extruding pelletization, namely obtain the Flame-retardant Hdpe material of the present embodiment.
triazine char-forming agent used in the present invention is the common commercial triazine char-forming agent that can obtain, as CFA etc.
embodiment 5
the flame retardant properties of the Flame-retardant Hdpe material prepared in embodiment 1 ~ 4 and mechanical property are tested, and contrast with pure HDPE material, reference standard and and test result as shown in Table-1.
table-1
as can be seen from table-1, use halogen-free expansible compound flame retardant of the present invention to carry out fire-retardant high-density polyethylene material LOI value to be significantly improved, UL-94 test all can reach V-0 rank, and when carrying out LOI and UL-94 test, by observing batten combustion case, all do not find molten drop phenomenon, this shows that the flame retardant properties of obtained flame-retardant HDPE material of the present invention is significantly improved and molten drop phenomenon have also been obtained effective control.
halogen-free expansible compound flame retardant of the present invention not only can be applicable to the fire-retardant of high-density polyethylene material, also can be applicable to the fire-retardant of the polyolefine material such as common polythene, polypropylene, can play the effect improving flame retarding efficiency, reduce fire-retardant cost equally.
above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (9)
1. a halogen-free expansible compound flame retardant, it is characterized in that: by weight percentage, described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by following component: 55% ~ 65% acid source, 18% ~ 28% charcoal source, 2% ~ 12% source of the gas and 5% ~ 15% synergist; Wherein, described acid source is the combination of one or more in ammonium polyphosphate, melamine phosphate and melamine polyphosphate; Described charcoal source is one or more the combination in dipentaerythritol, pentaerythritol phosphate and triazine char-forming agent; Described source of the gas is trimeric cyanamide or melamine cyanurate or both mixing; Described synergist is the combination of one or more in hypophosphite, pyrophosphate salt, phosphoric acid salt, silicon-dioxide and lanthanum trioxide.
2. halogen-free expansible compound flame retardant according to claim 1, it is characterized in that: by weight percentage, described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by following component: 60% ~ 65% ammonium polyphosphate, 20% ~ 25% pentaerythritol phosphate, 2% ~ 7% melamine cyanurate and 8% ~ 12% hypophosphite.
3. a Flame-retardant Hdpe material, it is characterized in that: by weight percentage, the composition of raw materials of described Flame-retardant Hdpe material comprises following component: 53% ~ 59% high-density polyethylene resin, 10% ~ 20% weighting agent, 25% ~ 30% halogen-free expansible compound flame retardant, 0.3% ~ 0.6% oxidation inhibitor, 0.2% ~ 0.5% lubricant, 0.3% ~ 0.5% coupling agent and 0.2% ~ 0.4% dispersion agent; Described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by the component of following weight percent: 55% ~ 65% acid source, 18% ~ 28% charcoal source, 2% ~ 12% source of the gas and 5% ~ 15% synergist; Wherein, described acid source is the combination of one or more in ammonium polyphosphate, melamine phosphate and melamine polyphosphate; Described charcoal source is one or more the combination in dipentaerythritol, pentaerythritol phosphate and triazine char-forming agent; Described source of the gas is trimeric cyanamide or melamine cyanurate or both mixing; Described synergist is the combination of one or more in hypophosphite, pyrophosphate salt, phosphoric acid salt, silicon-dioxide and lanthanum trioxide.
4. Flame-retardant Hdpe material according to claim 3, is characterized in that: described halogen-free expansible compound flame retardant is formed through high mixer high-speed mixing by the component of following weight percent: 60% ~ 65% ammonium polyphosphate, 20% ~ 25% pentaerythritol phosphate, 2% ~ 7% melamine cyanurate and 8% ~ 12% hypophosphite.
5. the Flame-retardant Hdpe material according to claim 3 or 4, is characterized in that: described weighting agent is talcum powder.
6. the Flame-retardant Hdpe material according to claim 3 or 4, is characterized in that: described oxidation inhibitor is the combination of one or more in irgasfos 168, oxidation inhibitor 628 and antioxidant 1010.
7. the Flame-retardant Hdpe material according to claim 3 or 4, is characterized in that: described lubricant is the combination of one or more in calcium stearate, Magnesium Stearate, Zinic stearas, polyethylene wax, amide waxe and pentaerythritol ester series lubricant agent.
8. the Flame-retardant Hdpe material according to claim 3 or 4, is characterized in that: described coupling agent is silane coupling agent.
9. the Flame-retardant Hdpe material according to claim 3 or 4, is characterized in that: described dispersion agent is silicone powder.
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| CN105273470A (en) * | 2015-11-24 | 2016-01-27 | 宁夏润龙包装新材料股份有限公司 | Halogen-free intumescent flame retardant and preparation method thereof |
| CN105419044A (en) * | 2015-11-27 | 2016-03-23 | 康平县塑编产业集群综合服务中心 | Halogen-free flame-retardant master batch for plastic woven bags |
| CN106349178A (en) * | 2016-08-12 | 2017-01-25 | 合肥光冉高分子材料科技有限公司 | Preparation method of macromolecular three-element-integrated low-smoke halogen-free intumescent flame retardant |
| CN106750893A (en) * | 2016-11-18 | 2017-05-31 | 中国科学院宁波材料技术与工程研究所 | A kind of bio-based source of the gas itself and constitute anti-flaming polyolefin composition |
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| CN105273470A (en) * | 2015-11-24 | 2016-01-27 | 宁夏润龙包装新材料股份有限公司 | Halogen-free intumescent flame retardant and preparation method thereof |
| CN105419044A (en) * | 2015-11-27 | 2016-03-23 | 康平县塑编产业集群综合服务中心 | Halogen-free flame-retardant master batch for plastic woven bags |
| CN106349178A (en) * | 2016-08-12 | 2017-01-25 | 合肥光冉高分子材料科技有限公司 | Preparation method of macromolecular three-element-integrated low-smoke halogen-free intumescent flame retardant |
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| CN106750893B (en) * | 2016-11-18 | 2019-10-11 | 中国科学院宁波材料技术与工程研究所 | A kind of anti-flaming polyolefin composition biology base gas source it and constituted |
| CN106930093A (en) * | 2016-12-16 | 2017-07-07 | 中山康诺德新材料有限公司 | A kind of fabric coating efficient halogen-free environmental protection fire retarding agent and preparation method thereof |
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| CN108178883A (en) * | 2018-02-01 | 2018-06-19 | 哈尔滨理工大学 | A kind of halogen-free flameproof polystyrene of fire retardant selective distribution and preparation method thereof |
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| CN111378245B (en) * | 2018-12-29 | 2021-04-20 | 北京化工大学 | Bendable epoxy resin fireproof plate and preparation method thereof |
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Application publication date: 20150610 |