CN109735031A - A kind of multicomponent collaboration halogen-free flame-retardant system and its application - Google Patents
A kind of multicomponent collaboration halogen-free flame-retardant system and its application Download PDFInfo
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- CN109735031A CN109735031A CN201910025959.3A CN201910025959A CN109735031A CN 109735031 A CN109735031 A CN 109735031A CN 201910025959 A CN201910025959 A CN 201910025959A CN 109735031 A CN109735031 A CN 109735031A
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Abstract
The invention discloses a kind of multicomponent collaboration halogen-free flame-retardant system and its applications, and by weight percentage, it includes: piperazine pyrophosphate 10~60% which, which cooperates with halogen-free flame-retardant system raw material composition,；Melamine pyrophosphate 10~60%；Inorganic hypophosphites 1~30%；Zinc oxide 0.1~10%；Modified Teflon 0.01~1%.The novel multicomponent collaboration halogen-free flame-retardant system has the characteristics that high flame retarding efficiency, fire-retardant stability is good, adaptation range is wide, thermal stability is good, easy dispersion, can be applied in the materials such as polyolefin and TPE.
Description
Technical field
The present invention relates to the technical fields of halogen-free flame retardants, and specifically a kind of multicomponent cooperates with halogen-free flame-retardant system and its making
Application in standby Halogenless fire retarded polymer.
Background technique
Fire retardant is the function additive of high molecular material, assigns inflammable high molecular material certain flame retardant property, due to
Most high molecular material is inflammable, and more application need can be fire-retardant high molecular material, therefore fire retardant be using compared with
More a kind of function additives.Fire retardant includes the basic flame-retardant system of two classes at present: halogen system flame-retardant system and non-halogen fire-retardant body
System.Halogen system flame-retardant system is usually brominated flame-retardant collaboration antimony oxide, a large number of studies show that, added with bromide fire retardant
High molecular material can produce thick smoke and the harmful substances such as hydrogen bromide in burning, human body can be caused to suffocate.Therefore, exploitation safety,
Environmental protection, halogen-free flame-retardant system have become a hot topic of research.
Halogen-free flame retardants mainly includes two major classes primary structure: one kind is inorganic hydroxide system, including magnesium hydroxide
And aluminium hydroxide；Another kind of is phosphorus nitrogen systems.For inorganic hydroxide system, fire retardation is limited, various in order to reach
The requirement of codes and standards, usual additive amount is very high, and the 70% of sometime up to entire formula system, since inorganic hydroxide hinders
Agent and macromolecule matrix poor compatibility are fired, is to be scattered in matrix resin in a manner of a kind of filler, therefore, high filler loading capacity will be big
The big mechanical property for reducing material.And phosphorus nitrogen systems, due to efficient flame retardant property, additive amount is low, to other performances of material
Influence is smaller, is the emphasis of current flame retardant area research.
Phosphorus nitrogen flame-retardant system is divided into intumescent and cohesion facies pattern flame-retardant system according to its fire retardant mechanism, both mechanism are phases
Mutually conflict.Phosphorus nitrogen system flame-retardant system is usually multicomponent synergistic effect, could generate preferable flame retardant effect.Based on nitrogenous coke
Phosphate system is a kind of phosphorus nitrogen flame-retardant system of intumescent, basic composition is piperazine pyrophosphate and melamine pyrophosphoric
Salt has preferable flame retardant property, while having lower water solubility, will not cause the moisture absorption and migration in the polymer, can answer
For in polyolefin, TPE.But the system faces Railway Project in the application: (1) flame retardant property is viscous by the melt of polymeric matrix
Degree is affected, this is related with its fire retardant mechanism, since it belongs to intumescent system, the melt strength of matrix resin at high temperature
Seriously affect the effect of expansion.Melt strength is big, and the gas discharged in burning wants enough effects that could generate expansion；It is molten
Body intensity is low, and foaming is easy to cause to rupture during expansion, and expansion effect is deteriorated, and barriering effect is poor, and flame retardant property is caused to decline, because
This, even identical material since difference of flowability can all cause the variation of the flame-retardant system flame retardant property, or even does not hinder
Combustion, fire-retardant Stability and adaptability are low；(2) flame retardant property is affected by various auxiliary agents and additive, micro processing
Auxiliary agent may destroy the flame retardant property of system；(3) there are dispersion, especially some black products in some materials
In, it can be found that white point, influences the appearance of product；(4) thermal stability of flame-retardant system is insufficient, especially shearing force, from
Body easily decomposes and the generation of phosphoric acid, can destroy polymeric matrix, easily causes the decline of material discoloration and mechanical property；(5) needle
To certain polymer, such as polyvinyl, flame retarding efficiency is still lower, and additive amount is excessive, not only reduces the mechanics of material
Performance also increases the cost of material, using being restricted.
Generally speaking, it for current nitrogenous pyrophosphate system, needs to solve the application problem that the system is faced, and leads to
Some efficient collaboration components are crossed, the multicomponent based on nitrogenous pyrophosphate system is formed and cooperates with halogen-free flame-retardant system.
Summary of the invention
Present invention defect in view of the prior art provides a kind of novel multicomponent collaboration halogen-free flame-retardant system.Gained
The flame-retardant system arrived has the characteristics that high flame retarding efficiency, fire-retardant stability is good, adaptation range is wide, thermal stability is good, easy dispersion,
It can be applied in the materials such as polyolefin and TPE.
Specific technical solution is as follows:
A kind of multicomponent collaboration halogen-free flame-retardant system, by weight percentage, raw material composition includes:
The present invention is applied to various conducted in various polymer materials for nitrogenous pyrophosphate Intumescent Retardant System
Defect has made extensive and intensive studies.
In the Intumescent Retardant System be made of piperazine pyrophosphate and melamine pyrophosphate, piperazine pyrophosphate is played
The effects of at carbon, acid source, and melamine pyrophosphate then plays a part of gas source, acid source, due to a kind of component had both it is more
Kind effect, efficiency will reduce, and along with mechanism of intumescence is also influenced by the melt strength of matrix polymer, lead to this two groups
The window narrows of point collaboration ratio show as fire-retardant unstable to the bad adaptability of polymer, and flame retardant property is good sometimes, sometimes
Poor flame retardant properties, in addition it is not fire-retardant.
Inventor herein passes through the study found that the compound ligand formed in piperazine pyrophosphate and melamine pyrophosphate
Certain inorganic hypophosphites is compounded in system again, forms the flame-retardant system of pyrophosphate and the collaboration of inorganic hypophosphites, Yi Ji
In the presence of having zinc oxide and modified Teflon, fire-retardant stability, flame retarding efficiency, the heat of flame-retardant system can be improved
Stability and dispersibility, solve the defect of existing system, and reduce the additive amount of fire retardant, are conducive to the application of the system.
The general structure of the inorganic hypophosphites is shown below:
In formula, M is selected from metallic element, is chosen in particular from the metals such as Al, Zn, Ca, Mg or Ti.
Preferably, the inorganic hypophosphites is selected from hypo-aluminum orthophosphate.
Inorganic hypophosphites, phosphorus content is high, can be used as effective acid source, and water-soluble low, resistance to migration, is polyester, poly-
Effective fire retardant of the self-containeds carbon polymer such as amide generates fire retardation with condensed phase mechanism, but is not having self-contained carbon characteristic
Polymer, without flame retardant effect if in polyolefin.With the fire retardant mechanism and application field of piperazine pyrophosphate flame-retardant system
Difference also has no inorganic hypophosphites and piperazine pyrophosphate system synergistic application in non-self-contained carbon system.And from mechanism
Analysis, expansion type flame retardant needs foaming and intumescing, and condensed phase fire retardant is then not necessarily to foam, or even can reduce foaming, therefore two
The fire retardant of kind different mechanism is with will lead to negative effect together.But the present inventor is it is discovered by experiment that a small amount of is inorganic
Hypophosphites is added, and flame retarding efficiency can be improved, and improves flame-retardant system to the adaptability of polymer.This may and conventional flame retardant
The mechanism of action it is different, conventional flame retardant is to work in igniting for polymer, and inorganic hypophosphites polymerize with matrix
Object does not work, but can promote the decomposition of piperazine pyrophosphate at high temperature, i.e., acts on flame retardant compositions generation, this is quite
In improving the efficiency of fire retardant, but excessively high inorganic hypophosphites does not help the flame retardant property of system.
In addition, zinc oxide and modified Teflon can also be added other than inorganic hypophosphites facilitation, these groups
Divide the viscosity and melt strength of adjustable polymer, and cooperateed with inorganic hypophosphites, is conducive to the expansion resistance of flame-retardant system
Combustion engine system, forms mutual synergy, further improves the fire retardation of system.
Modified Teflon is hud typed polytetrafluorethylepowder powder, and shell is acrylic copolymer, energy and matrix
The compatibility that polymer has had, stratum nucleare are polytetrafluoroethylene (PTFE), and polytetrafluoroethylene content is 50% or so, and modified polytetrafluoroethyl-ne is added
The melt strength of polymeric matrix can be improved in alkene, is conducive to expansion effect when fire retardant is had an effect.
In addition, the partial size of fire retardant also will affect flame retardant property, migration performance and the flame retardant property of material, it is therefore preferable that
Ground, the average grain diameter D50 of the piperazine pyrophosphate, 1 μm < D50 < 40 μm；The average grain diameter of the melamine pyrophosphate
D50,1 μm < D50 < 40 μm；The average grain diameter D50 of the inorganic hypophosphites, 1 μm < D50 < 40 μm.
On the basis of above-mentioned preferred raw material, by weight percentage, further preferred raw material composition includes:
The multicomponent collaboration halogen-free flame-retardant system is also disclosed in the present invention is preparing Halogenless fire retarded polymer or nothing
Application in the fire-retardant enhancing polymer of halogen.Specifically, it can be applied to prepare halogen-free anti-flaming polyolefin material, preparation process is as follows:
A) multicomponent collaboration halogen-free flame-retardant system is surface-treated using surface treating agent；
B) flame-retardant system after surface treatment is mixed with other auxiliary agents, is uniformly mixed under high velocity agitation；
C) mixing, plasticizing and the extruding pelletization of composition are completed in an extruder；
The halogen-free anti-flaming polyolefin material, including polypropylene, polyethylene, EVA and their blend.And the nothing
Halogen flame-retardant system weight ratio in halogen-free anti-flaming polyolefin material is 20-50%.
In step a), the surface treating agent is selected from least one of stearic acid, Aluminate, titanate esters, organosilicon；
The additive amount of the surface treating agent is the 2~5% of flame-retardant system weight.
Other auxiliary agents include lubricant, antioxidant, the steady agent of light, pigment, filler etc..
In step c), to guarantee that flame-retardant system is dispersed in substrate, then using double with fire retardant powder feed inlet
When extruding pelletization, the mixed material in step b) is added from fire retardant powder feed inlet for screw extruder.The twin-screw squeezes
The maximum temperature of machine is no more than 230 DEG C out, preferably at 200 DEG C or less.
Compared with prior art, the present invention has the advantage that
The invention discloses what is formed using inorganic hypophosphites raising piperazine pyrophosphate and melamine pyrophosphate
The flame retardant property of compound system and the adaptability of fire retardation, and it is viscous using zinc oxide and polytetrafluoroethylene (PTFE) regulation polymer melt
Degree and intensity promote flame-retardant system to play expandable flame retardant mechanism of action.The multicomponent of formation cooperates with halogen-free flame-retardant system, has resistance
Fire it is high-efficient, wide to the adaptability of polymer, not by the features such as other auxiliary agents are influenced, thermal stability is high, can be applied to polyene
In hydrocarbon material, there is higher flame retardant property and mechanical property.
Specific embodiment
Raw material:
(1) piperazine pyrophosphate: Japanese ADEKA company, D50=5 μm；
(2) melamine pyrophosphate, Japanese ADEKA company, D50=5 μm；
(3) hypo-aluminum orthophosphate, Nantong meaning is special, and D50=10 μm；
(4) zinc oxide, East China medicine；
(5) polyethylene (LDPE-1), 1C7AS (melting means 6.9g/10min), Yanshan Petrochemical；
(6) polyethylene (LDPE-2), 2426 (melting means 19g/10min), Ba Saier；
(7) antioxidant, 1010, BASF；
(8) antioxidant, 168, BASF；
(9) silicone, middle Lan Chenguang；
(10) polyethylene wax, Clariant；
(11) glass, Chongqing Polycomp International Co., Ltd；
(12) modified Teflon, 3M.
Embodiment 1
(1) surface treatment of flame-retardant system
Load weighted flame-retardant system each component, starting stirring in advance according to the ratio is added in kneader, and it is single to open heating
Material is warming up to 110 DEG C by member, keeps 10min, removes the moisture content in material, is then added at 2% surface of material gross weight
Agent is managed, mixed processing 20min obtains the uniformly mixed compounding flame retardant being surface-treated.
(2) mixture of flame-retardant system and other auxiliary agents
The compounding flame retardant each component and other auxiliary agents for being added in machine and weighing up in advance according to the ratio are stirred in height, starts high-speed stirring
It mixes, stirs 10min, complete the mixture of halogen-free flame-retardant system, discharge.
(3) extruding pelletization of material
Each area's temperature setting of double screw extruder in predetermined temperature, after temperature stablizes 20min, it is added from hopper poly-
Object is closed, halogen-free flame-retardant system is fed by powder charging aperture, is started host and feeder, is completed the extruding pelletization of material.It makes
The material of grain is sent into feed bin by blast system, and dries.
(4) application and test of material
Material after drying is molded by the standard sample of various testing standard defineds in injection molding machine, and carries out correlation
The test of material property.It is primarily upon following performance indicator:
A, fire-retardant
It is tested according to UL94V0 testing standard.
B, resistance to migration experiment
The fire-retardant poly polymer sample that will be prepared, is put into climatic chamber, is arranged 85 DEG C of temperature, relative humidity
85%, the state of specimen surface of the visual observations after 168 hours.
C, material mechanical performance
Impact strength is tested by ASTM D256, the addition of fire retardant would generally reduce the impact property of material, and additive amount is got over
Greatly, impact property is lower.
The stretching of material would generally be reduced by testing tensile strength and elongation at break, the addition of fire retardant by ASTM D638
Intensity and elongation at break, additive amount is bigger, and tensile strength is lower.
D, dispersibility
2% or so black masterbatch is added in material after the drying, prepares impact specimen, completes impact, passes through magnifying glass
Whether observation fracture surface of sample has white aggregate etc..
Each material and proportion are shown in Table 1 in embodiment, and obtained testing of materials the results are shown in Table 1.
Embodiment 2
Implementation process is same as Example 1, in addition to the amount for being scaling up compounding flame retardant.Other materials and proportion are shown in
Table 1, obtained material the results are shown in Table 1.
Embodiment 3
Implementation process is same as Example 1, in addition to polyethylene being changed into the higher trade mark of melting means.Other materials and proportion are shown in
Table 1, obtained material the results are shown in Table 1.
Embodiment 4
Implementation process is same as Example 1, in addition to lubricant polyethylene wax is changed into silicone.Other materials and proportion are shown in Table
1, obtained material the results are shown in Table 1.
Embodiment 5
Implementation process is same as Example 1, except the glass of addition 30% in system.Other materials and proportion are shown in Table 1, gained
To material the results are shown in Table 1.
Embodiment 6
Implementation process is same as Example 1, in addition to adjustment piperazine pyrophosphate and melamine pyrophosphate ratio, and protects
It is constant to hold flame retardance element total amount.Other materials and proportion are shown in Table 1, and obtained material the results are shown in Table 1.
Embodiment 7
Implementation process is same as Example 1, except adjustment hypo-aluminum orthophosphate, piperazine pyrophosphate and melamine pyrophosphate ratio
Exception, and keep flame retardance element total amount constant.Other materials and proportion are shown in Table 1, and obtained material the results are shown in Table 1.
Comparative example 1
Implementation process is same as Example 1, in addition to not using hypo-aluminum orthophosphate, and improves piperazine pyrophosphate and melamine
The ratio of pyrophosphate, so that material reaches the flame retardant rating of V0.Other materials and proportion are shown in Table 1, obtained material result
It is shown in Table 1.
Comparative example 2
Implementation process is identical as comparative example 1, other than the polyethylene trade mark that polyethylene is changed into high melting means.Other materials and
Proportion is shown in Table 1, and obtained material the results are shown in Table 1.
Comparative example 3
Implementation process is identical as comparative example 1, other than polyethylene wax is changed into silicone.Other materials and proportion are shown in Table 1, institute
Obtained material the results are shown in Table 1.
Comparative example 4
Implementation process is identical as comparative example 1, other than the glass of addition 30%.Other materials and proportion are shown in Table 1, acquired
Material the results are shown in Table 1.
Comparative example 5
Implementation process is same as Example 1, other than without using hypo-aluminum orthophosphate.Other materials and proportion are shown in Table 1, acquired
Material the results are shown in Table 1.
Comparative example 6
Implementation process is same as Example 1, other than without using zinc oxide and modified Teflon.Other materials and match
Than being shown in Table 1, obtained material the results are shown in Table 1.Table 1
Continued 1
。
Claims (10)
1. a kind of multicomponent cooperates with halogen-free flame-retardant system, which is characterized in that by weight percentage, raw material composition includes:
2. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that the piperazine pyrophosphate
Average grain diameter D50,1 μm < D50 < 40 μm.
3. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that the melamine pyrophosphoric
The average grain diameter D50 of salt, 1 μm < D50 < 40 μm.
4. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that the inorganic hypophosphites
General structure is shown below:
In formula, M is selected from metallic element.
5. the preparation method of halogen-free polypropylene flame redardant according to claim 4, which is characterized in that the M be selected from Al, Zn,
Ca, Mg or Ti.
6. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that the inorganic hypophosphites choosing
From hypo-aluminum orthophosphate.
7. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that the inorganic hypophosphites
Average grain diameter D50,1 μm < D50 < 40 μm.
8. multicomponent according to claim 1 cooperates with halogen-free flame-retardant system, which is characterized in that by weight percentage, former
Material forms
9. multicomponent according to claim 8 cooperates with halogen-free flame-retardant system, which is characterized in that the inorganic hypophosphites choosing
From hypo-aluminum orthophosphate.
10. a kind of multicomponent collaboration halogen-free flame-retardant system any according to claim 1~9 is preparing halogen-free flameproof polymerization
Application in object.
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| CN111662526A (en) * | 2020-06-24 | 2020-09-15 | 苏州通优新材料科技有限公司 | Halogen-free flame-retardant sheath material for thin cables with thickness of 0.13 square millimeter and below, and preparation method and application thereof |
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