CN102241889A - Halloysite composite flame retardant masterbatch - Google Patents
Halloysite composite flame retardant masterbatch Download PDFInfo
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- CN102241889A CN102241889A CN2010102896985A CN201010289698A CN102241889A CN 102241889 A CN102241889 A CN 102241889A CN 2010102896985 A CN2010102896985 A CN 2010102896985A CN 201010289698 A CN201010289698 A CN 201010289698A CN 102241889 A CN102241889 A CN 102241889A
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Abstract
The invention provides a halloysite composite flame retardant masterbatch. The flame retardant masterbatch is prepared by the processes of mixing halloysite powder of 100 to 10000 meshes and a compound agent to obtain a halloysite composite flame retardant, mixing the halloysite composite flame retardant and one or more thermoplastic resins, and carrying out an extrusion process on the mixture to obtain a halloysite composite flame retardant masterbatch. Cellular structures of micro- or nano-tubes of halloysite have a strong sorption effect on gas and a strong heat insulation performance, can block a thermal transmission, have a good water absorption performance and a water retention performance, can produce water vapour for blocking oxygen and enable products obtained form a high-temperature calcination process to cover on the surface of a polymer and to play a role in oxygen blocking, thus halloysite has a good flame retardant performance, when halloysite are used in combination with a compound agent, flame retardant effects of halloysite are further improved due to a synergistic effect of halloysite and the compound agent. Compared with other flame retardants, halloysite has the advantages of no volatilization, long effecting time, low price, no smoke and no toxicity, thus a flame retardant masterbatch prepared form halloysite as a main additive is an ideal environment-friendly type flame retardant masterbatch.
Description
Technical field
The present invention relates to a kind of halloysite composite flame-proof master batch.
Background technology
Halloysite claims halloysite again, but halloysite and kaolin are distinguishing on crystalline structure, the one, and tubular structure, the one, schistose structure.The halloysite clay exquisiteness, impurity is low.Can be used for the production of high-grade ceramic, electroceramics, crucible and refractory materials.Here said moisture, be meant the water molecules of some fixed qties and other molecule component that combines, such material also is called hydrate.Halloysite looks like a very closely knit soil block, and under electron microscope, it is made up of countless fine tubuloses or fibrous crystals, belongs to nanometer-submicron mineral.Halloysite density low (2.1-2.6), (being generally white) of light color can not have a strong impact on its weight and the transparency with polymer after compound.
Halloysite generally is used for water treatment, support of the catalyst and fertilizer compounding technology as additive, with its application as fire-retardant master granule, does not appear in the newspapers as yet.
Fire retardant is a kind of auxiliary agent that can stop material to ignite or suppress propagation of flame, and to be the 1950's grow up with the demand of macromolecular material for it.Traditional fire retardant, mainly based on bromide fire retardant, though its flame retardant effect is fine, it can produce poisonous in fire-retardant process, deleterious gas, a lot of countries have limited its use.Mineral-type environmental type fire retardant is paid close attention to widely, produces because its burning is low cigarette, nontoxic, no obnoxious flavour, has obtained a large amount of application in American-European and Japan, accounts for the share in fire-retardant market 50%.The mineral-type fire retardant mainly is magnesium hydroxide and aluminium hydroxide, yet its price is expensive, has increased production cost.In addition, fly upward easily when interpolation of inorganic powder fire retardant and mixing, to be influenced operator's health after the human body suction, and be made into following advantage is arranged behind the fire-retardant master granule: the cleaning that can keep environment, easy to use, more convenient accurate in the metering, can not adhere to during mixing on the container, also more even with mixing of resin.
The microvoid structure of the micro-nano pipe of halloysite, gas there is strong adsorption, strong heat insulation heat-insulating property, and can block hot transmission, simultaneously because its good suction and water retention property, at high temperature can produce water vapor blocking-up oxygen, the product after the high-temperature calcination can cover the blocking oxygen that polymer surfaces plays a part, and makes it have good flame retardancy, halloysite itself is non-volatile, effect is lasting, and is cheap, smokeless, nontoxic, with fire-retardant, pressing down the function of cigarette and reduction toxic gas, is the fire-retardant master granule of main body additive with the halloysite therefore, is a kind of ideal green environmental-protection flame-retardant master batch.
Summary of the invention
The invention provides good, the nontoxic and with low cost halloysite composite flame-proof master batch of a kind of flame retardant properties, for realizing the purpose of foregoing invention, the present invention solves by the following technical solutions:
A kind of halloysite composite flame-proof master batch is characterized in that: described halloysite composite flame-proof master batch be by halloysite composite flame-retardant agent and thermoplastics by 70-80: the 30-20 mass ratio mixes to extrude and forms.
Preferably, described halloysite composite flame-retardant agent comprises that halloysite powder and composite dose are with 10: 0.1-1: 1 is compound, and described composite dose is in magnesium hydroxide, aluminium hydroxide, kaolin, polynite, red phosphorus, phosphoric acid dihydro amine, boric acid or the trimeric cyanamide one or more.
Preferably, described halloysite powder is the 100-10000 order.
Preferably, adopt surface-modifying agent that halloysite is carried out surface treatment, the consumption of surface-modifying agent accounts for the 0.1-5% of halloysite weight.
Preferably, described surface-modifying agent is one or more in employing silane coupling agent, titanate coupling agent, the aluminate coupling agent.
Preferably, described silane coupling agent is one or more in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane or the γ-methacryloxypropyl triethoxyl silane.
Preferably, described thermoplastics comprises one or more in polyethylene (PE), polypropylene (PP), polystyrene (PS), acrylonitrile-butadiene-styrene copolymer general-purpose plastics such as (ABS) and polyamide (PA), the thermoplastic polyester engineering plastics such as (PBT, PET).
A kind of preparation method of halloysite composite flame-proof master batch, the preparation method of halloysite composite flame-proof master batch may further comprise the steps:
(1), natural halloysite is pulverized, make the halloysite powder;
(2), with halloysite powder, composite dose and surface-modifying agent premix in moderate-speed mixers, and then add thermo-stabilizer, lubricant, thermoplastic resin and mix;
(3), raw materials mixed is placed dual-screw-stem machine, through melt extruding granulation.
Preferably, halloysite in the described step (2), composite dose and surface-modifying agent are done time in advance in moderate-speed mixers and are 1-5 minute.
Preferably, add behind thermo-stabilizer, lubricant, the thermoplastic resin remix 5-15 minute in the described step (2).
Preferably, middle dual-screw-stem machine one district temperature 80-100 ℃ of described step (3), two district temperature 170-280 ℃, three district temperature 180-290 ℃, four district temperature 190-300 ℃; In barrel residence time 2-5 minute, melt pressure was 15-25MPa.
The present invention compared with prior art has the following advantages:
1, the present invention mixes by a certain percentage with natural halloysite and composite dose, because the microvoid structure of halloysite, gas there is strong adsorption, strong heat insulation heat-insulating property, and can block hot transmission, simultaneously because its good suction and water retention property, at high temperature can produce water vapor blocking-up oxygen, product after the high-temperature calcination can cover the blocking oxygen that polymer surfaces plays a part, make it have good flame retardancy, halloysite itself is non-volatile, and effect is lasting, cheap, smokelessly, nontoxic, with fire-retardant, the function that presses down cigarette and reduction toxic gas, therefore being the fire-retardant master granule of main body additive with the halloysite, is a kind of ideal green environmental-protection flame-retardant master batch.
2, technology of the present invention is simple, and cost is low, is the desirable fire-retardant master granule of plastic prod, has broad application prospects.
Embodiment
Below in conjunction with example and embodiment by experiment the present invention is set forth, yet protection scope of the present invention is not only to be confined to following examples.The person of an ordinary skill in the technical field all can realize purpose of the present invention according to content disclosed by the invention.
A kind of halloysite composite flame-proof master batch, described halloysite composite flame-proof master batch comprises and is crushed to 100-10000 purpose halloysite powder and composite dose with 10: 0.1-1: 1 is compound, and composite flame-retardant agent and thermoplastics are by 70-80: the 30-20 weight ratio is mixed to extrude and is formed.Described composite dose is in magnesium hydroxide, aluminium hydroxide, kaolin, polynite, red phosphorus, phosphoric acid dihydro amine, boric acid or the trimeric cyanamide one or more.Described thermoplastics comprises one or more in polyethylene (PE), polypropylene (PP), polystyrene (PS), acrylonitrile-butadiene-styrene copolymer general-purpose plastics such as (ABS) and polyamide (PA), the thermoplastic polyester engineering plastics such as (PBT, PET).Adopt surface-modifying agent that halloysite is carried out surface treatment, the consumption of surface-modifying agent accounts for the 0.1-5% of halloysite weight.Described surface-modifying agent is to adopt silane coupling agent, titanate coupling agent or aluminate coupling agent.Described silane coupling agent is one or more in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane or the γ-methacryloxypropyl triethoxyl silane.
And a kind of preparation method of halloysite composite flame-proof master batch:
Embodiment 1:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, magnesium hydroxide and silane coupling agent premix 1 minute in moderate-speed mixers, obtain the halloysite compound flame retardant, wherein magnesium hydroxide is 2: 1 as the quality proportioning of composite dose and halloysite and magnesium hydroxide.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 70: 30 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
As the alternative of the foregoing description scheme, described silane coupling agent is one or more in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane or the γ-methacryloxypropyl triethoxyl silane.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 8 weight ratio with acrylic resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 26 combustionproperties
Embodiment 2:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, trimeric cyanamide and titanate coupling agent premix 3 minutes in moderate-speed mixers, promptly obtain the halloysite compound flame retardant, wherein trimeric cyanamide is 2: 1 as the quality proportioning of composite dose and halloysite and trimeric cyanamide.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 70: 30 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 10 weight ratio with acrylic resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 28 combustionproperties
Embodiment 3:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, red phosphorus and aluminate coupling agent premix 5 minutes in moderate-speed mixers, promptly obtain the halloysite compound flame retardant, wherein red phosphorus is 3: 2 as the quality proportioning of composite dose and halloysite and red phosphorus.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 70: 30 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 7 weight ratio with acrylic resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 30 combustionproperties
Embodiment 4:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, trimeric cyanamide, magnesium hydroxide and aluminate coupling agent premix 5 minutes in moderate-speed mixers, promptly obtain the halloysite compound flame retardant, wherein trimeric cyanamide, magnesium hydroxide are 2: 1: 1 as the quality proportioning of composite dose and halloysite, trimeric cyanamide, magnesium hydroxide.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 70: 30 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 8 weight ratio with acrylic resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 30 combustionproperties
Embodiment 5:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, trimeric cyanamide, magnesium hydroxide and aluminate coupling agent premix 5 minutes in moderate-speed mixers, promptly obtain the halloysite compound flame retardant, wherein trimeric cyanamide, magnesium hydroxide are 3: 1: 1 as the quality proportioning of composite dose and halloysite, trimeric cyanamide, magnesium hydroxide.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 80: 20 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 10 weight ratio with acrylic resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 28 combustionproperties
Embodiment 6:
(1), natural halloysite is crushed to 100-10000 order (granularity is 0.2-2.8um),
(2), with halloysite powder, trimeric cyanamide, magnesium hydroxide and aluminate coupling agent premix 5 minutes in moderate-speed mixers, promptly obtain the halloysite compound flame retardant, wherein trimeric cyanamide, magnesium hydroxide are 2: 2: 1 as the quality proportioning of composite dose and halloysite, trimeric cyanamide, magnesium hydroxide.
(3), the halloysite compound flame retardant is mixed with acrylic resin with 75: 25 weight ratio, carry out the melt blending granulation with twin screw extruder then, make halloysite composite flame-proof master batch.
The combustionproperty test
Halloysite composite flame-proof master batch is mixed with 1: 7 weight ratio with acrylonitrile-butadiene-styrene copolymer (ABS) resin, carry out the melt blending granulation with twin screw extruder then, carry out injection moulding, obtain flame-retardant polypropylene composite material with injection moulding machine.It is as follows to measure its every flame retardant properties:
It is the UL94-V0 level that oxygen index can reach 28 combustionproperties
As the alternative of the foregoing description scheme, described composite dose is in magnesium hydroxide, aluminium hydroxide, kaolin, polynite, red phosphorus, phosphoric acid dihydro amine, boric acid or the trimeric cyanamide one or more.
More than the embodiment of the invention is described in detail, used specific case herein principle of the present invention and embodiment set forth, the explanation of above embodiment just is used for help understanding method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (11)
1. halloysite composite flame-proof master batch is characterized in that: described halloysite composite flame-proof master batch be by halloysite composite flame-retardant agent and thermoplastics by 70-80: the 30-20 mass ratio mixes to extrude and forms.
2. halloysite composite flame-proof master batch according to claim 1, it is characterized in that: described halloysite composite flame-retardant agent comprises that halloysite powder and composite dose are with 10: 0.1-1: 1 is compound, and described composite dose is in magnesium hydroxide, aluminium hydroxide, kaolin, polynite, red phosphorus, phosphoric acid dihydro amine, boric acid or the trimeric cyanamide one or more.
3. halloysite composite flame-proof master batch according to claim 2 is characterized in that: described halloysite powder is the 100-10000 order.
4. halloysite composite flame-proof master batch according to claim 2 is characterized in that: adopt surface-modifying agent that halloysite is carried out surface treatment, the consumption of surface-modifying agent accounts for the 0.1-5% of halloysite weight.
5. halloysite composite flame-proof master batch according to claim 4 is characterized in that: described surface-modifying agent is one or more in employing silane coupling agent, titanate coupling agent, the aluminate coupling agent.
6. halloysite composite flame-proof master batch according to claim 5 is characterized in that: described silane coupling agent is one or more in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane or the γ-methacryloxypropyl triethoxyl silane.
7. halloysite composite flame-proof master batch according to claim 1 is characterized in that: described thermoplastics comprises one or more in polyethylene (PE), polypropylene (PP), polystyrene (PS), acrylonitrile-butadiene-styrene copolymer general-purpose plastics such as (ABS) and polyamide (PA), the thermoplastic polyester engineering plastics such as (PBT, PET).
8. the preparation method of a halloysite composite flame-proof master batch, it is characterized in that: the preparation method of halloysite composite flame-proof master batch may further comprise the steps:
(1), natural halloysite is pulverized, make the halloysite powder;
(2), with halloysite powder, composite dose and surface-modifying agent premix in moderate-speed mixers, and then add thermo-stabilizer, lubricant, thermoplastic resin and mix;
(3), raw materials mixed is placed dual-screw-stem machine, through melt extruding granulation.
9. the preparation method of a kind of halloysite composite flame-proof master batch as claimed in claim 8 is characterized in that: halloysite in the described step (2), composite dose and surface-modifying agent are done time in advance in moderate-speed mixers and are 1-5 minute.
10. the preparation method of a kind of halloysite composite flame-proof master batch as claimed in claim 8 is characterized in that: added in the described step (2) behind thermo-stabilizer, lubricant, the thermoplastic resin remix 5-15 minute.
11. the preparation method of a kind of halloysite composite flame-proof master batch as claimed in claim 8 is characterized in that: middle dual-screw-stem machine one district temperature 80-100 ℃ of described step (3), two district temperature 170-280 ℃, three district temperature 180-290 ℃, four district temperature 190-300 ℃; In barrel residence time 2-5 minute, melt pressure was 15-25MPa.
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Application publication date: 20111116 |