CN103265725B - Low-smoke aluminum hypophosphite compounded fire retardant and preparation method thereof - Google Patents

Low-smoke aluminum hypophosphite compounded fire retardant and preparation method thereof Download PDF

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Publication number
CN103265725B
CN103265725B CN201310232062.0A CN201310232062A CN103265725B CN 103265725 B CN103265725 B CN 103265725B CN 201310232062 A CN201310232062 A CN 201310232062A CN 103265725 B CN103265725 B CN 103265725B
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hypo
coupling agent
aluminum orthophosphate
mixing
fire retardant
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CN201310232062.0A
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CN103265725A (en
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张良
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Yangcheng Institute of Technology
Yancheng Institute of Technology
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Yangcheng Institute of Technology
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Abstract

The invention belongs to the field of chemical industry, and aims at providing a low-smoke aluminum hypophosphite compounded fire retardant with excellent fire resistance and smoke suppression performance, and a preparation method thereof. The fire retardant is formed by 30-60 parts by weight of aluminum hypophosphite, 20-40 parts by weight of hydrotalcite, 20-40 parts by weight of zinc borate, 5-10 parts by weight of diatomite, 5-10 parts by weight of magnesium oxide and 1-3 parts of coupling agent in a manner of mixing and screening. The coupling agent is a tetrabutyl titanate coupling agent or an aluminate coupling agent. The fire retardant has excellent fire resistance and smoke suppression performance, and after the compounded fire retardant is added, the mechanical property of polymers is not obliviously reduced.

Description

Low cigarette type hypo-aluminum orthophosphate compound flame retardant and preparation method thereof
Technical field
The invention belongs to chemical field, relate to a kind of fire retardant, particularly relate to a kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant and preparation method thereof.
Background technology
Research shows, in a fire, cigarette produces at first and the most lethal factor.According to expert statistics, in the people of the death because of fire failure in the world, more than 80% is that not naked light burns body and dies because the smog of macromolecular material burning releasing and poisonous gas make people be choked to death.Macromolecular material produces more smog and toxic gas when burning, this aerosol gases is factor the most dangerous in fire, because their velocity of diffusion is much larger than the velocity of diffusion of flame, hampers withdrawing and putting out work of people in a fire, thus lives and properties are sustained losses severely.Therefore in fire-retardant research field, fire-retardant is two eternal topics with pressing down cigarette problem.
Plastics are application a kind of polymer materialss very widely in household electrical appliances instrument, electronics, automobile etc.Because plastics have inflammable feature, so usually need to carry out fire-retardant finish to it, whether the fire retardant of use is halogen-containing by can be divided into halogenated flame retardant and halogen-free flame-retardant system.Although tradition halogen containing flame-retardant flame retarding efficiency is high, its burning can produce poisonous, corrosive gases in a large number, and the development trend of current fire retardant is non-halogen.Hypo-aluminum orthophosphate is a kind of novel halogen-free flame retardants, and its phosphorus content is high, have the advantages such as Heat stability is good, water-soluble little, fire-retardant effect is large, and work in-process does not cause the decomposition of polymkeric substance, does not affect plastics moulding compound yet.But the smoke suppressing of hypo-aluminum orthophosphate needs to be improved further, therefore by compounded technology make hypo-aluminum orthophosphate have concurrently fire-retardant, press down hood, do not affect mechanical properties of polymer simultaneously, meet again environmental protection requirement and then can have good prospects for commercial application.
Summary of the invention
The object of the invention is to for existing performance not enough, provide a kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant with good fire-retardant and smoke suppressing and preparation method thereof.
To achieve these goals, present invention employs following technical scheme:
A kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant, this fire retardant is made up after mixing, screening of the coupling agent of the diatomite of the zinc borate of the hydrotalcite of the hypo-aluminum orthophosphate of 30-60 weight part, 20-40 part, 20-40 part, 5-10 part, the magnesium oxide of 5-10 part and 1-3 part.
As preferably, fire retardant is made up after mixing, screening of the coupling agent of the diatomite of the zinc borate of the hydrotalcite of the hypo-aluminum orthophosphate of 40-50 weight part, 25-35 part, 25-35 part, 6-8 part, the magnesium oxide of 6-8 part and 1-2 part.
Further, described coupling agent is tetrabutyl titanate coupling agent or aluminate coupling agent.
A preparation method for low cigarette type hypo-aluminum orthophosphate compound flame retardant, comprises the following steps successively:
S1. hypo-aluminum orthophosphate, hydrotalcite, zinc borate, diatomite, magnesium oxide and coupling agent is taken according to the parts by weight of each component of fire retardant;
S2. ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 40-80min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C.
S3. the mass transport after mixing tentatively is sieved to vibratory screening apparatus, then the mass transport of tentatively sieving is sieved further to centrifugal screen;
S4. the material sieving out from centrifugal screen is packed, obtain fire retardant finished product.
The vibratory screening apparatus used in preparation method of the present invention adopts the vibratory screening apparatus of ZS series, if model is the vibratory screening apparatus of ZS-650 type, and its motor 1.5kw, rotating speed 1370rpm; The model that centrifugal screen adopts is LXS-300 type.
In raw material of the present invention, hypo-aluminum orthophosphate is a kind of novel halogen-free flame retardants, and its Heat stability is good, water-soluble little, fire-retardant effect are large, and be applicable to PA, PS, HIPS, ABS, PC-ABS, PC etc., but smoke suppressing is not enough, composite rear smoke suppressing effect significantly improves; Hydrotalcite (LDHs) is the novel inorganic functional materials that a class has laminate structure, and general designation is layered di-hydroxyl composite metal oxidate, and LDHs is when being heated, and its water of constitution laminated sheet hydroxyl and interlayer ion are with hydration CO 2form remove, play and reduce combustion gases concentration, intercept O 2effect; The water of constitution of LDHs, laminate hydroxyl and interlayer ion depart from laminate in different temperature, thus in lower scope, (200-800 DEG C) can discharge fire retardant matter.In fire-retardant process, caloric receptivity is large, and the high temperature produced when being conducive to reducing burning, as Halogen height smoke inhibition fire retardant, can be widely used in the fields such as plastics, rubber, coating.Zinc borate is one of fire retardant used the earliest, is also important inorganic combustion inhibitor, its feature be Heat stability is good, toxicity low, eliminate smoke, composite respond well with other fire retardant, material combustion smoke density can be reduced after interpolation.Diatomite light weight and soft, easy grinding powder, has very strong adsorptive power and gas barrier property, uses can reduce material cost as filler.Magnesium oxide can use as fire retardant, and itself and hypo-aluminum orthophosphate have synergy, can suppress the generation of smog.
Advantage of the present invention is as follows:
1. the present invention adopts and has that to press down the hydrotalcite of hood, zinc borate and hypo-aluminum orthophosphate composite.Hydrotalcite in compound product, zinc borate have good fire-retardant and smoke suppressing.
2. to adopt diatomite to participate in composite in the present invention, and its adsorptive power and gas barrier property improve the fire-retardant and smoke suppressing of hypo-aluminum orthophosphate.
3. the present invention adopt there is the magnesium oxide of synergistic effect and hypo-aluminum orthophosphate composite.Magnesium oxide in compound product and hypo-aluminum orthophosphate are worked in coordination with and are suppressed smog to produce.
4. add coupling agent in all material mixing process and carry out organic modification, improve the consistency of compound product and organic polymer, the reduction of the mechanical properties of polymer caused because of Blending Processes can be reduced.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
A kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant, comprises following raw material:
Hypo-aluminum orthophosphate 25kg (main content more than 99%), hydrotalcite 10kg, zinc borate 10kg, diatomite 4kg, magnesium oxide 3kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method, comprises the following steps:
S1. low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material is taken:
S2. above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 40min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
S3. the mass transport after mixing tentatively is sieved to vibratory screening apparatus, remove the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
S4. the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 2:
Difference from Example 1 is: take low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 50kg (main content more than 99%), hydrotalcite 30kg, zinc borate 30kg, diatomite 8kg, magnesium oxide 8kg, tetrabutyl titanate coupling agent 3kg;
Its preparation method:
First above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 50min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
Secondly, the mass transport after mixing tentatively is sieved to vibratory screening apparatus, removes the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
Finally, the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 3:
Difference from Example 1 is: take low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 40kg (main content more than 99%), hydrotalcite 15kg, zinc borate 15kg, diatomite 6kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method is as follows:
First above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 60min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
Secondly, the mass transport after mixing tentatively is sieved to vibratory screening apparatus, removes the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
Finally, the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 4:
Difference from Example 1 is: take low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 45kg (main content more than 99%), hydrotalcite 30kg, zinc borate 30kg, diatomite 6kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 2kg;
Its preparation method is as follows:
First, above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 45min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
Secondly, the mass transport after mixing tentatively is sieved to vibratory screening apparatus, removes the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
Finally, the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 5:
Difference from Example 1 is: take low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 60kg (main content more than 99%), hydrotalcite 20kg, zinc borate 20kg, diatomite 8kg, magnesium oxide 6kg, tetrabutyl titanate coupling agent 3kg;
Its preparation method is as follows:
First, above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 60min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
Secondly, the mass transport after mixing tentatively is sieved to vibratory screening apparatus, removes the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
Finally, the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 6:
Difference from Example 1 is: take low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 30kg (main content more than 99%), hydrotalcite 15kg, zinc borate 15kg, diatomite 45kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method is as follows:
First, above-mentioned ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 50min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
Secondly, the mass transport after mixing tentatively is sieved to vibratory screening apparatus, removes the material of macrobead or caking, then the mass transport of tentatively sieving is carried out regrading to centrifugal screen; Vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; Centrifugal screen model is LXS-300.
Finally, the mass transport of sieving out from centrifugal screen is packed to pack-thread, obtain low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Product obtained by above example 1-3 is applied in HIPS, ABS material respectively, according to the performance of national standard test material, formula composition and the performance test results as follows:
Table 1:HIPS formula composition and the performance test results
Table 2:ABS formula composition and the performance test results
Shownly above be only preferred embodiment of the present invention, interest field of the present invention can not be limited with this, therefore according to the equivalent variations that the present patent application the scope of the claims is done, still belong to the scope that the present invention is contained.

Claims (4)

1. one kind low cigarette type hypo-aluminum orthophosphate compound flame retardant, it is characterized in that: this fire retardant is made up after mixing, screening of the coupling agent of the diatomite of the zinc borate of the hydrotalcite of the hypo-aluminum orthophosphate of 30-60 weight part, 20-40 part, 20-40 part, 5-10 part, the magnesium oxide of 5-10 part and 1-3 part, and described coupling agent is tetrabutyl titanate coupling agent or aluminate coupling agent.
2. low cigarette type hypo-aluminum orthophosphate compound flame retardant according to claim 1, is characterized in that: this fire retardant is made up after mixing, screening of the coupling agent of the diatomite of the zinc borate of the hydrotalcite of the hypo-aluminum orthophosphate of 40-50 weight part, 25-35 part, 25-35 part, 6-8 part, the magnesium oxide of 6-8 part and 1-2 part.
3. a preparation method for low cigarette type hypo-aluminum orthophosphate compound flame retardant according to claim 1, is characterized in that: comprise the following steps successively:
S1. hypo-aluminum orthophosphate, hydrotalcite, zinc borate, diatomite, magnesium oxide and coupling agent is taken according to the parts by weight of each component of fire retardant;
S2. ready each component put in the high-speed mixer with water cooling function and mix, mixing time is 40-80min, and the temperature of charge controlled in mixing process in mixing machine is lower than 100 DEG C;
S3. the mass transport after mixing tentatively is sieved to vibratory screening apparatus, then the mass transport of tentatively sieving is sieved further to centrifugal screen;
S4. the material sieving out from centrifugal screen is packed, obtain fire retardant finished product.
4. preparation method according to claim 3, is characterized in that: in step S3, and vibratory screening apparatus adopts the vibratory screening apparatus of ZS series, and the model that centrifugal screen adopts is LXS-300 type.
CN201310232062.0A 2013-06-13 2013-06-13 Low-smoke aluminum hypophosphite compounded fire retardant and preparation method thereof Expired - Fee Related CN103265725B (en)

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CN103980544B (en) * 2014-04-15 2016-05-25 芜湖同达新材料科技有限公司 A kind of fire-retardant non-metallic powder
CN108410019A (en) * 2018-03-30 2018-08-17 潍坊万丰新材料科技有限公司 Compound fire-proof smoke suppressor
CN113980353A (en) * 2021-11-24 2022-01-28 湖北航云科技有限公司 Environment-friendly aluminum hypophosphite flame retardant

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