CN103265725A - 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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CN103265725A
CN103265725A CN2013102320620A CN201310232062A CN103265725A CN 103265725 A CN103265725 A CN 103265725A CN 2013102320620 A CN2013102320620 A CN 2013102320620A CN 201310232062 A CN201310232062 A CN 201310232062A CN 103265725 A CN103265725 A CN 103265725A
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hypo
coupling agent
aluminum orthophosphate
mixing
fire retardant
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CN103265725B (en
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张良
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Yangcheng Institute of Technology
Yancheng 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, related in particular to a kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant and preparation method thereof.
Background technology
Studies show that in fire, cigarette is to produce at first and the most deadly factor.According to expert statistics, in the world because of the dead philtrum of fire failure, be because smog and poisonous gas that the macromolecular material burning is emitted are choked to death the people more than 80%, be not naked light burns body and dies.Macromolecular material produces more smog and toxic gas when burning, this smog gas is factor the most dangerous in the fire, because what their velocity of diffusion, had hindered people much larger than the velocity of diffusion of flame in fire withdraws and puts out work, thereby lives and properties are sustained losses severely.Therefore in fire-retardant research field, fire-retardant is two eternal topics with pressing down the cigarette problem.
Plastics are to use a kind of polymer materials very widely at aspects such as household electrical appliances instrument, electronics, automobiles.Because plastics have inflammable characteristics, so need carry out fire-retardant finish to it usually, whether the fire retardant of use is halogen-containing by can be divided into halogenated flame retardant and halogen-free flame-retardant system.Though tradition halogen containing flame-retardant flame retarding efficiency height, its burning can produce poisonous, corrosive gases in a large number, and the development trend of fire retardant is non-halogen at present.Hypo-aluminum orthophosphate is a kind of novel halogen-free flame retardants, and its phosphorus content height has advantages such as Heat stability is good, water-soluble little, fire-retardant effectiveness be big, and work in-process do not cause the decomposition of polymkeric substance, does not also influence the plastics moulding compound.But the smoke suppressing of hypo-aluminum orthophosphate remains further to be improved, therefore by compounded technology make hypo-aluminum orthophosphate have concurrently fire-retardant, press down hood, impact polymer mechanical property not meets environmental protection requirement again and then can have better industrial application prospect simultaneously.
Summary of the invention
The objective of the invention is at existing performance deficiency, a kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant with good fire-retardant and smoke suppressing and preparation method thereof is provided.
To achieve these goals, the present invention has adopted following technical scheme:
A kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant, this fire retardant are to be made after mixing, sieving by the coupling agent of the magnesium oxide 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, 5-10 part and 1-3 part.
As preferably, fire retardant is through mixing, making after the screening by the coupling agent of the magnesium oxide 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, 6-8 part and 1-2 part.
Further, described coupling agent is tetrabutyl titanate coupling agent or aluminate coupling agent.
A kind of preparation method of low cigarette type hypo-aluminum orthophosphate compound flame retardant may further comprise the steps successively:
S1. the parts by weight according to each component of fire retardant take by weighing hypo-aluminum orthophosphate, hydrotalcite, zinc borate, diatomite, magnesium oxide and coupling agent;
S2. ready each component is put in the high-speed mixer with water-cooled function and mixed, mixing time is 40-80min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process.
S3. the mass transport after will mixing is tentatively sieved to vibratory screening apparatus, and the mass transport that will tentatively sieve to centrifugal screen further sieves then;
S4. will pack from the material that centrifugal screen sieves out, namely get the fire retardant finished product.
The vibratory screening apparatus that uses among the preparation method of the present invention adopts the vibratory screening apparatus of ZS series, is the vibratory screening apparatus of ZS-650 type as model, its motor 1.5kw, rotating speed 1370rpm; The model that centrifugal screen adopts is the LXS-300 type.
In the 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 effectiveness are big, are applicable to PA, PS, HIPS, ABS, PC-ABS, PC etc., but the smoke suppressing deficiency, composite back smoke suppressing effect obviously 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 break away from laminate in different temperature, thereby can (200-800 ℃) discharge fire retardant matter in lower scope.In fire-retardant process, caloric receptivity is big, and the high temperature that produces when being conducive to reduce burning can be used as the high smoke-inhibiting flame retardant agent of Halogen, is widely used in fields such as plastics, rubber, coating.Zinc borate is one of fire retardant that uses the earliest, also is important inorganic combustion inhibitor, and its characteristics are low, the smoke elimination of Heat stability is good, toxicity, and are composite respond well with other fire retardant, can reduce the material combustion smoke density after the interpolation.The diatomite light weight is and soft, and easily grinding powder has very strong adsorptive power and gas barrier property, uses as filler and can reduce material cost.Magnesium oxide can be used as fire retardant and uses, and itself and hypo-aluminum orthophosphate have synergy, can suppress the generation of smog.
Advantage of the present invention is as follows:
1. it is composite that the present invention's employing has the hydrotalcite, zinc borate and the hypo-aluminum orthophosphate that press down hood.Hydrotalcite in the composite product, zinc borate have good fire-retardant and smoke suppressing.
2. it is composite that the present invention adopts the diatomite participation, and its adsorptive power and gas barrier property have improved the fire-retardant and smoke suppressing of hypo-aluminum orthophosphate.
3. it is composite that the present invention adopts magnesium oxide and hypo-aluminum orthophosphate with synergistic effect.The collaborative smog that suppresses of magnesium oxide in the composite product and hypo-aluminum orthophosphate produces.
4. add coupling agent in all material mixing processes and carry out organic modification, improve the consistency of composite product and organic polymer, can reduce the reduction of the polymkeric substance mechanical property that causes because of the blend process.
Embodiment
Be further described below in conjunction with the present invention of embodiment:
Embodiment 1:
A kind of low cigarette type hypo-aluminum orthophosphate compound flame retardant comprises following raw material:
Hypo-aluminum orthophosphate 25kg (main content is more than 99%), hydrotalcite 10kg, zinc borate 10kg, diatomite 4kg, magnesium oxide 3kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method may further comprise the steps:
S1. take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material:
S2. above-mentioned ready each component is put in the high-speed mixer with water-cooled function and mixed, mixing time is 40min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
S3. the mass transport after will mixing is tentatively sieved to vibratory screening apparatus, removes the material of macrobead or caking, and the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
S4. will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 2:
Difference from Example 1 is: take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 50kg (main content is more than 99%), hydrotalcite 30kg, zinc borate 30kg, diatomite 8kg, magnesium oxide 8kg, tetrabutyl titanate coupling agent 3kg;
Its preparation method:
At first above-mentioned ready each component is put in the high-speed mixer with water-cooled function and mixed, mixing time is 50min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
Secondly, the mass transport after mixing is tentatively sieved to vibratory screening apparatus, remove the material of macrobead or caking, the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
At last, will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 3:
Difference from Example 1 is: take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 40kg (main content is more than 99%), hydrotalcite 15kg, zinc borate 15kg, diatomite 6kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method is as follows:
At first above-mentioned ready each component is put in the high-speed mixer with water-cooled function and mixed, mixing time is 60min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
Secondly, the mass transport after mixing is tentatively sieved to vibratory screening apparatus, remove the material of macrobead or caking, the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
At last, will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 4:
Difference from Example 1 is: take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 45kg (main content is more than 99%), hydrotalcite 30kg, zinc borate 30kg, diatomite 6kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 2kg;
Its preparation method is as follows:
At first, above-mentioned ready each component put in the high-speed mixer with water-cooled function mix, mixing time is 45min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
Secondly, the mass transport after mixing is tentatively sieved to vibratory screening apparatus, remove the material of macrobead or caking, the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
At last, will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 5:
Difference from Example 1 is: take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 60kg (main content is more than 99%), hydrotalcite 20kg, zinc borate 20kg, diatomite 8kg, magnesium oxide 6kg, tetrabutyl titanate coupling agent 3kg;
Its preparation method is as follows:
At first, above-mentioned ready each component put in the high-speed mixer with water-cooled function mix, mixing time is 60min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
Secondly, the mass transport after mixing is tentatively sieved to vibratory screening apparatus, remove the material of macrobead or caking, the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
At last, will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
Embodiment 6:
Difference from Example 1 is: take by weighing low cigarette type hypo-aluminum orthophosphate compound flame retardant raw material: hypo-aluminum orthophosphate 30kg (main content is more than 99%), hydrotalcite 15kg, zinc borate 15kg, diatomite 45kg, magnesium oxide 4kg, tetrabutyl titanate coupling agent 1kg;
Its preparation method is as follows:
At first, above-mentioned ready each component put in the high-speed mixer with water-cooled function mix, mixing time is 50min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process;
Secondly, the mass transport after mixing is tentatively sieved to vibratory screening apparatus, remove the material of macrobead or caking, the mass transport that will tentatively sieve to centrifugal screen carries out regrading then; The vibratory screening apparatus model is ZS-650, motor 1.5kw, rotating speed 1370rpm; The centrifugal screen model is LXS-300.
At last, will pack from mass transport to the pack-thread that centrifugal screen sieves out, namely get low cigarette type hypo-aluminum orthophosphate compound flame retardant finished product.
The prepared product of above example 1-3 is applied to respectively in HIPS, the ABS material, and according to the performance of national standard test material, prescription composition and The performance test results are as follows:
Table 1:HIPS prescription is formed and The performance test results
Figure BSA0000090998790000071
Table 2:ABS prescription is formed and The performance test results
Figure BSA0000090998790000072
Figure BSA0000090998790000081
More than shown only be preferred embodiment of the present invention, can not limit interest field of the present invention with this, therefore the equivalent variations of doing according to the present patent application claim still belongs to the scope that the present invention is contained.

Claims (5)

1. one kind low cigarette type hypo-aluminum orthophosphate compound flame retardant is characterized in that: this fire retardant is through mixing, making after the screening by the coupling agent of the magnesium oxide 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, 5-10 part and 1-3 part.
2. low cigarette type hypo-aluminum orthophosphate compound flame retardant according to claim 1 is characterized in that: this fire retardant is through mixing, making after the screening by the coupling agent of the magnesium oxide 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, 6-8 part and 1-2 part.
3. low cigarette type hypo-aluminum orthophosphate compound flame retardant according to claim 1 and 2, it is characterized in that: described coupling agent is tetrabutyl titanate coupling agent or aluminate coupling agent.
4. the preparation method of one kind low cigarette type hypo-aluminum orthophosphate compound flame retardant is characterized in that: may further comprise the steps successively:
S1. the parts by weight according to each component of fire retardant take by weighing hypo-aluminum orthophosphate, hydrotalcite, zinc borate, diatomite, magnesium oxide and coupling agent;
S2. ready each component is put in the high-speed mixer with water-cooled function and mixed, mixing time is 40-80min, and the temperature of charge in the control mixing machine is lower than 100 ℃ in mixing process.
S3. the mass transport after will mixing is tentatively sieved to vibratory screening apparatus, and the mass transport that will tentatively sieve to centrifugal screen further sieves then;
S4. will pack from the material that centrifugal screen sieves out, namely get the fire retardant finished product.
5. preparation method according to claim 4 is characterized in that: among the step S3, vibratory screening apparatus adopts the vibratory screening apparatus of ZS series, is the vibratory screening apparatus of ZS-650 type as model, its motor 1.5kw, rotating speed 1370rpm; The model that centrifugal screen adopts is the 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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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865260A (en) * 2014-03-19 2014-06-18 广州琪原新材料有限公司 Composition for improving ignition temperature of plastic glowing filament as well as preparation method and application thereof
CN103980544A (en) * 2014-04-15 2014-08-13 芜湖同达新材料科技有限公司 Fire retardation non-metal 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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007536402A (en) * 2004-05-04 2007-12-13 ゼネラル・エレクトリック・カンパニイ Halogen-free flame retardant polyamide composition with improved electrical properties

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007536402A (en) * 2004-05-04 2007-12-13 ゼネラル・エレクトリック・カンパニイ Halogen-free flame retardant polyamide composition with improved electrical properties

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103865260A (en) * 2014-03-19 2014-06-18 广州琪原新材料有限公司 Composition for improving ignition temperature of plastic glowing filament as well as preparation method and application thereof
CN103865260B (en) * 2014-03-19 2016-06-01 广州琪原新材料有限公司 Improve the composition of plastics glow wire ignition temperature and its preparation method and application
CN103980544A (en) * 2014-04-15 2014-08-13 芜湖同达新材料科技有限公司 Fire retardation non-metal powder
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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