CN105111584A - Intumescent flame retardant masterbatch with polyphenyl silicone oil and preparation method thereof - Google Patents
Intumescent flame retardant masterbatch with polyphenyl silicone oil and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides an intumescent flame retardant masterbatch with polyphenyl silicone oil and a preparation method thereof, relating to flame retardant masterbatches and preparation methods thereof. The flame retardant masterbatch is characterized by comprising the following raw materials in parts by weight: 15-69.7 parts of polyolefin carrier resin, 0.2-2 parts of polyphenyl silicone oil, 26-75 parts of halogen-free flame retardant, 3-5 parts of dispersing agent and 0.1-1 part of antioxidant. Silicone oil with higher phenyl content and the flame retardant have certain synergistic effects, so that the flame retardant effects of the flame retardant masterbatch in flame retardant products can be effectively improved in the case of a certain additive amount. The problems of difficulty in extrusion molding of the flame retardant masterbatch, rough surface, solution fracture, dark luster, and the like can be improved by adding a small amount of polyphenyl silicone oil in the masterbatch preparation process.
Description
Technical field
The present invention relates to a kind of fire-retardant master granule and preparation method thereof, particularly relate to a kind of expansion type flame-retarding master batch with many phenyl silicone oil and preparation method thereof.
Background technology
Along with polymer modification industry develops to multifunctional direction, master-batch techniques becomes the development trend of polymer modification industry.By preparing fire-retardant master granule; the thermal histories of modified resin can be reduced; available protecting flame retardant constituent; improve the dispersiveness of fire retardant in resin simultaneously; reduce fire retardant addition; reduce the impact adding the mechanical property on resin of fire retardant, reduce difficulty of processing and tooling cost, improve shopwork environment.
Fire retardant kind is more, also different to the fire retardant mechanism of goods, fire-retardant for polypropylene, should select different fire retardant systems according to polypropylene environment for use and performance requriements.Also suitable fire retardant should be selected according to the service requirements of flame-retarded resin and physicochemical property in the preparation process of fire-retardant master granule, and select corresponding vector resin, lubricating system, dispersion system according to the mechanism characteristic etc. of fire retardant, consider the coupling between resin, fire retardant, auxiliary agent three, reduce the impact of each auxiliary agent on flame-retardant system flame retardant properties.
But expansion type flame retardant has the following disadvantages: 1. the polarity spectrum of expansion type flame retardant and polymkeric substance causes very greatly its poor compatibility, the electrical property of polymkeric substance and insulating property are declined to some extent, especially mechanical property such as intensity and toughness significantly declines; 2. expansion type flame retardant water absorbability is strong.As APP/PER/MA Intumescent Retardant System, the not only easy moisture absorption of poly-hydroxy PER, and easily there is alcoholysis between each composition, cause flame-retardant polymer poor water resistance; 3. usual, the relative molecular mass of expansion type flame retardant is little, easily migrates to polymer surfaces, thus causes the poor mechanical property of flame retardant products, and especially aesthetic appearance is poor; 4. processing difficulties, expanding fire retardant small molecules is more, poor heat stability, is heated and easily decomposes, add and NH3 can be made man-hour to decompose out, cause tie rod surfaces of tacky, not easily process.
In fire-retardant master granule process of manufacture, screw speed is excessively slow, has a strong impact on fire-retardant production efficiency, and meanwhile, fire retardant is overstand in screw rod, also will produce larger damage to the flame retarding efficiency of fire retardant.Therefore, under existing experiment condition, become production formula by adjustment production technique, add the processing aids such as lubricant, improve the processing fluidity of fire-retardant master granule melt, reduce master batch difficulty of processing, improve extrusion capacity, have great importance.
Along with the increase of phenyl molar fraction, the high thermal resistance of silicone oil, oilness and solvability in organic solvent all increase, but lower temperature resistance declines.Phenyl silicone oil high-low temperature resistant, the photograph of resistance to good fortune, and there is good oilness.Literature research shows, polysiloxane can be used as the synergist of expansion type flame retardant, has good fire retardation to polypropylene.Hydroxyl oil of bay, chlorination siloxanes etc. all Zeng Zuowei synergistic flame retardant use, and the fire-retardant rare report of phenyl silicone oil synergistic.
The silicone oil that phenyl content is higher and fire retardant have certain synergistic effect, when certain addition, effectively can improve the flame retardant effect of fire-retardant master granule in the right goods of resistance.Simultaneously by adding a small amount of many phenyl silicone oil in master batch preparation process, fire-retardant master granule extrusion moulding difficulty can be improved, the problem such as surface irregularity, solution break, dull.
Summary of the invention
The object of the present invention is to provide a kind of expansion type flame-retarding master batch with many phenyl silicone oil and preparation method thereof, the present invention effectively can improve the flame retardant effect of fire-retardant master granule in the right goods of resistance.Simultaneously by adding a small amount of many phenyl silicone oil in master batch preparation process, fire-retardant master granule extrusion moulding difficulty can be improved, the problem such as surface irregularity, solution break, dull.
The object of the invention is to be achieved through the following technical solutions:
Have an expansion type flame-retarding master batch for many phenyl silicone oil, this fire-retardant master granule is made up of according to mass parts following raw materials according:
Polyolefin carrier resin 15 ~ 69.7 parts;
Many phenyl silicone oil 0.2-2 part;
Halogen-free flame retardants 26 ~ 75 parts;
Dispersion agent 3 ~ 5 parts;
Oxidation inhibitor 0.1 ~ 1;
Polyolefin carrier is any one or both in LDPE, propylene-based elastomeric with arbitrarily than mixing; Dispersion agent is the mixture of one or more in polyethylene wax, Poly Propylene Wax, EVA wax, OP wax, TAS-2A; Oxidation inhibitor is the compound of the positive octadecanol ester of antioxidant 1076 propionic acid and irgasfos 168 phosphorous acid ester; Halogen-free flame retardants is phosphor-nitrogen expansion type combustion inhibitor, and it is made up of according to arbitrary proportion mixing acid source, source of the gas, charcoal source, and the ratio between acid source, source of the gas, charcoal source can not make a significant impact effect of the present invention, therefore can mix by arbitrary proportion; Acid source is one of ammonium polyphosphate, phosphoric acid, Vanadium Pentoxide in FLAKES, boric acid; Described source of the gas is any one in trimeric cyanamide, Dyhard RU 100, ammonium polyphosphate, amine borate, Dyhard RU 100 formaldehyde resin; Described charcoal source is any one in tetramethylolmethane, sorbyl alcohol, Mierocrystalline cellulose.
Have a preparation method for the expansion type flame-retarding master batch of many phenyl silicone oil, described method comprises following preparation process:
1) vector resin and many phenyl vinyl silicone oil are by proportioning high-speed mixer normal temperature mixing 1-5min, and the rotating speed of homogenizer is 500 revs/min;
2) fire retardant and other interpolation auxiliary agent is then added, mixing 3-8min; The rotating speed of homogenizer is 800 revs/min;
3) by twin screw extruder extruding pelletization, fire-retardant master granule is obtained and injection moulding.
Described a kind of preparation method with the expansion type flame-retarding master batch of many phenyl silicone oil, described many phenyl silicone oil synthetic method is as follows:
Multi-vinyl silicone oil is (3-5) with the massfraction ratio of tetraphenyl cyclopentadienyl ketone: 1, and in α-chloronaphthalene solvent, in 230 DEG C-250 DEG C under nitrogen atmosphere protection, 8-20h, Diels-Alder reaction occurs, reflux; Methanol wash, drying, obtain tetraphenyl phenyl vinyl silicone oil.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
The present invention synthesizes a kind of expansion type flame-retarding master batch with many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according: PP resin 35 parts, phenyl silicone oil 0.1 part, polyethylene wax 3 parts, fire retardant IFR20 part, antioxidant 1076 and irgasfos 168 compound 0.2 part.
Prepare many phenyl-vinyl silicon oils: vinyl silicone oil 20 parts, tetraphenyl cyclopentadienyl ketone 6 parts, in 100 parts of α-chloronaphthalene solvent, in 230 DEG C-250 DEG C under nitrogen atmosphere protection, there is Diels-Alder reaction, reflux in 8-20h.Methanol wash, drying, obtain tetraphenyl phenyl vinyl silicone oil.
Agglomerate preparation method: 1) PP vector resin and many phenyl silicone oil are by proportioning high-speed mixer normal temperature mixing 1-5min, and the rotating speed of homogenizer is 500 revs/min.
2) fire retardant and other additive is added, mixing about 3-8min.The rotating speed of homogenizer 800 revs/min.
3) by twin screw extruder extruding pelletization, fire-retardant master granule is obtained and injection moulding.
Embodiment 2
The present invention synthesizes a kind of expansion type flame-retarding master batch with many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according: PP resin 35 parts, phenyl silicone oil 0.5 part, polyethylene wax 3 parts, fire retardant IFR20 part, antioxidant 1076 and irgasfos 168 compound 0.2 part.
The preparation method of phenyl-vinyl silicon oil and the preparation method of master batch are with embodiment 1.
Embodiment 3
The present invention synthesizes a kind of expansion type flame-retarding master batch with many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according: PP resin 35 parts, phenyl silicone oil 1 part, polyethylene wax 3 parts, fire retardant IFR20 part, antioxidant 1076 and irgasfos 168 compound 0.2 part.
The preparation method of phenyl-vinyl silicon oil and the preparation method of master batch are with embodiment 1.
Embodiment 4
The present invention synthesizes a kind of expansion type flame-retarding master batch with many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according: PP resin 35 parts, phenyl silicone oil 1.5 parts, polyethylene wax 3 parts, fire retardant IFR20 part, antioxidant 1076 and irgasfos 168 compound 0.2 part.
The preparation method of phenyl-vinyl silicon oil and the preparation method of master batch are with embodiment 1.
Comparative example 1
The present invention synthesizes a kind of expansion type flame-retarding master batch with many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according: PP resin 35 parts, polyethylene wax 3 parts, fire retardant IFR20 part, antioxidant 1076 and irgasfos 168 compound 0.2 part.
Agglomerate preparation method: 1) PP vector resin and many phenyl silicone oil are by proportioning high-speed mixer normal temperature mixing 1-5min, and the rotating speed of homogenizer is 500 revs/min.
2) fire retardant and other additive is added, mixing about 3-8min.Homogenizer transfer 800 revs/min to.
3) by twin screw extruder extruding pelletization, fire-retardant master granule is obtained and injection moulding.
By the fire-retardant master granule of above-described embodiment and comparative example according to 20% weight ratio add to respectively in PP resin, then mix, use twin screw extruder granulation, test.
Table 1 fire-retardant master granule joins the performance test in polypropylene articles
Known by upper table analysis, many phenyl silicone oil can improve the resistance toheat of polymkeric substance, improve the oxygen index adding the fire-retardant master granule PP resin that many phenyl silicone oil obtain, owing to there is synergistic effect between phenyl silicone oil and fire retardant, adding of phenyl silicone oil can promote that matrix becomes charcoal, contributes to flame retardance of polymer, promote that fire retardant decomposes, slow down heat release rate, promote into charcoal, therefore a small amount of many phenyl oil add the flame retardant effect that effectively can improve fire-retardant master granule.But the content of many phenyl silicone oil own has inflammable methyl group, therefore the addition of many phenyl silicone oil can not be excessive.Addition is too much, reduces the flame retardant properties of goods.
The content of phenyl silicone oil more than table 2 is on the impact of fire-retardant master granule extrusion moulding process bath surface form
As seen from the above table, along with the increase of phenyl molar fraction, the high thermal resistance of silicone oil, oilness and solvability in organic solvent all increase, the many phenyl-vinyl silicon oils of polymer processing aids add the coarse phenomenon of bath surface effectively improved in the fire-retardant master granule course of processing, reduce master batch difficulty of processing, improve master batch surface gloss simultaneously.
In fire-retardant master granule, the melt index of vector resin PP is larger, when adding the fire retardant of 60wt%, because powder addition is larger, powder is difficult to be uniformly dispersed in vector resin, now, the flow process major embodiment of master batch solution is the glutinous stream of molecular chain between vector resin, when adding a small amount of many phenyl-vinyl silicon oils, because many phenyl-vinyl silicon oils are conducive to promoting the dispersion between melt resin and fire retardant powder, now the flow process of polymer melt starts to show as the flowing between vector resin and fire retardant powder, simultaneously due to many phenyl-vinyl silicon oils itself cannot rapidly and resin or fire retardant better compatible, cause the constricted flow of fire-retardant master granule solution, melting index reduces.Along with many phenyl-vinyl silicon oils content increases further, when auxiliary agent reaches certain content, many phenyl-vinyl silicon oils just can play good lubrication between resin carrier and fire retardant powder, now, polymer melt melting index improves, until exceed melt index value when not adding processing aid.
The addition of polymer processing aids is not the bigger the better.In fire-retardant master granule preparation process, if many phenyl vinyl silicone oil addition is excessive, melt can be caused in screw rod melt blending process to produce skidding, and threaded rod shear shear force cannot effectively transmit, and makes fire retardant be difficult to be uniformly dispersed in vector resin.
Dissolving in Blending Processes, the many phenyl-vinyl silicon oils of polymer processing aids can form layer protecting film at twin screw machine barrel and head surface, and polymer melt resistance in twin screw blending extrusion process is reduced, and extrusion capacity increases.But, many phenyl-vinyl silicon oils need certain process in the formation of twin screw machine barrel and head surface film structure, therefore, the addition of most phenyl-vinyl silicon oil can be added a little in the starting stage of processing, can after continous-stable extrudes certain hour, reduce processing aid content again, to maintain the running balance of many phenyl silicone oil oil at machine barrel internal surface content.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (3)
1. there is an expansion type flame-retarding master batch for many phenyl silicone oil, it is characterized in that this fire-retardant master granule is made up of according to mass parts following raw materials according:
Polyolefin carrier resin 15 ~ 69.7 parts;
Many phenyl silicone oil 0.2-2 part;
Halogen-free flame retardants 26 ~ 75 parts;
Dispersion agent 3 ~ 5 parts;
Oxidation inhibitor 0.1 ~ 1;
Polyolefin carrier is any one or both in LDPE, propylene-based elastomeric with arbitrarily than mixing; Dispersion agent is the mixture of one or more in polyethylene wax, Poly Propylene Wax, EVA wax, OP wax, TAS-2A; Oxidation inhibitor is the compound of the positive octadecanol ester of antioxidant 1076 propionic acid and irgasfos 168 phosphorous acid ester; Halogen-free flame retardants is phosphor-nitrogen expansion type combustion inhibitor, and it is made up of according to arbitrary proportion mixing acid source, source of the gas, charcoal source, and the ratio between acid source, source of the gas, charcoal source can not make a significant impact effect of the present invention, therefore can mix by arbitrary proportion; Acid source is one of ammonium polyphosphate, phosphoric acid, Vanadium Pentoxide in FLAKES, boric acid; Described source of the gas is any one in trimeric cyanamide, Dyhard RU 100, ammonium polyphosphate, amine borate, Dyhard RU 100 formaldehyde resin; Described charcoal source is any one in tetramethylolmethane, sorbyl alcohol, Mierocrystalline cellulose.
2. have a preparation method for the expansion type flame-retarding master batch of many phenyl silicone oil, it is characterized in that, described method comprises following preparation process:
1) vector resin and many phenyl vinyl silicone oil are by proportioning high-speed mixer normal temperature mixing 1-5min, and the rotating speed of homogenizer is 500 revs/min;
Then fire retardant and other interpolation auxiliary agent is added, mixing 3-8min; The rotating speed of homogenizer is 800 revs/min;
3) by twin screw extruder extruding pelletization, fire-retardant master granule is obtained and injection moulding.
3. a kind of preparation method with the expansion type flame-retarding master batch of many phenyl silicone oil according to claim 2, it is characterized in that, described many phenyl silicone oil synthetic method is as follows:
Multi-vinyl silicone oil is (3-5) with the massfraction ratio of tetraphenyl cyclopentadienyl ketone: 1, and in α-chloronaphthalene solvent, in 230 DEG C-250 DEG C under nitrogen atmosphere protection, 8-20h, Diels-Alder reaction occurs, reflux; Methanol wash, drying, obtain tetraphenyl phenyl vinyl silicone oil.
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Cited By (2)
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| CN105859767A (en) * | 2016-03-30 | 2016-08-17 | 沈阳化工大学 | Normal pressure synthetic method for polyphenyl cyclic siloxane containing three vinyl groups |
| 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 |
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| CN103254385A (en) * | 2012-02-17 | 2013-08-21 | 苏州井上高分子新材料有限公司 | Polyurethane foam composition used for airplane seats |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859767A (en) * | 2016-03-30 | 2016-08-17 | 沈阳化工大学 | Normal pressure synthetic method for polyphenyl cyclic siloxane containing three vinyl groups |
| 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 |
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Application publication date: 20151202 |