CN1314778C - Process for preparing nano inorganic compound flame retardant by transfer method - Google Patents
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- CN1314778C CN1314778C CNB2005100086959A CN200510008695A CN1314778C CN 1314778 C CN1314778 C CN 1314778C CN B2005100086959 A CNB2005100086959 A CN B2005100086959A CN 200510008695 A CN200510008695 A CN 200510008695A CN 1314778 C CN1314778 C CN 1314778C
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Abstract
The present invention relates to a method for preparing a nanometer inorganic composite flame retardant by a transfer method, which is a method for modifying the surface of a nanometer compound flame retardant by using micron-order large magnesium hydroxide particles in a composite flame retardant raw material as carriers. The nanometer inorganic composite flame retardant is composed of a nanometer-order inorganic flame retardant, micron-order magnesium hydroxide and an auxiliary flame retardant. The nanometer-order inorganic flame retardant is nanometer aluminum hydroxide or nanometer magnesium hydroxide, and the average particle diameter of the nanometer-order inorganic flame retardant is less than or equal to 100 nanometers; the average particle diameter of the micron-order magnesium hydroxide is between 1 and 10 micrometers. Firstly, a surface modifier and the micron-order magnesium hydroxide are stirred and mixed at high speed; then, the nanometer-order inorganic flame retardant is added to the mixture to be continuously stirred and mixed; subsequently, the auxiliary flame retardant is added, and stirred and mixed at high speed; finally, the nanometer inorganic composite flame retardant coated with the surface modifier on the surface is obtained. The nanometer inorganic composite flame retardant prepared by the present invention can obviously improve the tensile strength of flame retardation composite materials when used for the flame retardation composite materials.
Description
Technical field
The present invention relates to the composite nanometer flame retardant particle is carried out the method for surface modification treatment, is that a kind of micron order magnesium hydroxide macrobead that utilizes in the composite flame-retardant agent raw material is made carrier carries out surface modification treatment to composite nanometer flame retardant method.
Background technology
The principal item of inorganic combustion inhibitor is aluminium hydroxide and magnesium hydroxide, has function fire-retardant, that eliminate smoke, is the main flame-retardant composition of bittern-free flame-proof material.The principal item of inorganic nano fire retardant is nano-aluminum hydroxide, nano-sized magnesium hydroxide, and flame retardant effect is that nano level is better than micron order.
Aluminium hydroxide and magnesium hydroxide are as inorganic combustion inhibitor, and the addition in flame-proof composite material is bigger.When aluminium hydroxide used separately, addition must just have flame retardant effect preferably more than 60%.Yet high addition can influence the mechanical property of flame-proof composite material.Adopt nano level aluminium hydroxide or magnesium hydroxide, the mechanical property of flame-proof composite material can be better than micron-sized aluminium hydroxide or magnesium hydroxide.But, must carry out surface modification to nano level aluminium hydroxide or magnesium hydroxide, just can make flame-proof composite material reach higher mechanical property.
The surface modification of nano level aluminium hydroxide or magnesium hydroxide is suitable for " wet-process modified ".Wet-process modified be with inorganic fire-retarded powder suspended dispersed in liquid medium, surface-modifying agent added and be scattered in the liquid medium, make inorganic fire-retarded powder under the state of " hygrometric state ", carry out the method for surface modification.Liquid medium can be a water, also can be organic solvent.But, adopt organic solvent to relate to problems such as cost, recovery, environment, thereby the medium of normal employing is a water.When being medium, requiring surface-modifying agent in water, to dissolve maybe and can be emulsified into emulsion state with water.
Wet-process modified is the method that the fire-retardant particle surface modification of present nano grade inorganic generally adopts.Its advantage is that properties-correcting agent coats evenly, and modified effect is good, goes for the fire-retardant particulate surface modification of nano grade inorganic.The shortcoming of this method is to need drying process, and technology is comparatively complicated, the also corresponding raising of cost.And wet-process modified have special requirement to properties-correcting agent, therefore limited the range of choice of properties-correcting agent.Have only minority kind properties-correcting agent can be used for water and do the wet-process modified of medium.
The method more easier than wet method modification is " dry method modification ".The dry method modification method is that surface-modifying agent and inorganic particle are stirred in homogenizer, modification is carried out on the inorganic particle surface handled.Directly be added to surface-modifying agent in the homogenizer, or surface-modifying agent is added in the homogenizer after with the small diluted amount dilution agent, make inorganic particle under the state of " dry state ", by means of the high shear force and the high-speed mixing effect of high-speed stirring, properties-correcting agent is coated on the inorganic particle surface and forms surface-treated layer.
The advantage of dry method modification method is simple and easy to do, and it is wet-process modified that shortcoming is that cladding uniformity is not so good as.When being used for the inorganic fire-retarded particulate surface modification of micron order, though the effect of dry method modification still can be used not as wet method.Particle grain size is littler, adopts the effect of dry method modification just poorer.Surface modification for nano level aluminium hydroxide or magnesium hydroxide, because nano-scale particle particle diameter and quality are small, the kinetic energy that nano particle obtains when moving along with high-speed stirring is also very little, be not enough to drive the dispersion of surface-modifying agent between nano particle, also just be difficult to realize the even coating of surface-modifying agent at nano grain surface.
(publication number: patent application CN1536000A) discloses the nano inorganic compound flame retardant of being made up of nano grade inorganic fire retardant and micron order magnesium hydroxide and auxiliary flame retardant to the inventor at " nano inorganic compound flame retardant that is used for macromolecular material ".This fire retardant can reach fire-retardant and press down the purpose of cigarette, and it is fire-retardant to be used for engineering plastics, is a kind of new and effective environmentally friendly composite flame-retardant agent.The nano grade inorganic fire retardant is the nano-aluminum hydroxide or the nano-sized magnesium hydroxide of median size≤100 nanometers in this fire retardant; The median size of micron order magnesium hydroxide is 1～10 micron; Auxiliary flame retardant: zinc borate, zinc oxide, ferric oxide, red phosphorus, phosphoric acid salt, carbonate or organosilicon.The mass ratio of nano grade inorganic fire retardant and micron order magnesium hydroxide is 80: 20 to 10: 90; The mass fraction sum of nano grade inorganic fire retardant and micron order magnesium hydroxide is 100 parts, and the mass fraction of auxiliary flame retardant is 10 to 30 parts.Adopt nano-aluminum hydroxide or nano-sized magnesium hydroxide and micron magnesium hydroxide and auxiliary flame retardant blend, be prepared into composite flame-retardant agent.This composite flame-retardant agent can be applicable to flame-proof composite materials such as polyethylene, polypropylene, ABS, nylon, polycarbonate, polyvinyl chloride, EVA, polyester.The method of known dry method modification is adopted in the preparation of composite flame-retardant agent, mixes with homogenizer, adds general organic modifiers simultaneously and carries out surface modification, and general organic modifiers is as titanic acid ester, aluminic acid ester, silane or lipid acid etc.In preparation nano inorganic compound flame retardant process, find that through contrast the working method of dry method modification also will influence the mechanical property of flame-proof composite material.Respectively each component in the composite flame-retardant agent is adopted after the common dry method surface treatment remix or each component mixed after add surface-modifying agent again and carry out surface treatment, though the fire retardant that these two kinds of dry method modification methods obtain does not have big influence to the flame retardant effect of flame-proof composite material, the mechanical property of flame-proof composite material there is bigger influence.
Summary of the invention
The objective of the invention is to propose a kind of method, to improve the mechanical property of flame-proof composite material to the nano inorganic compound flame retardant surface modification.Promptly (publication number: CN 1536000A) disclosed nano inorganic compound flame retardant carries out the method for transfer method surface modification to " nano inorganic compound flame retardant that is used for macromolecular material ".
The present invention prepares the method for nano inorganic compound flame retardant with transfer method, nano inorganic compound flame retardant is made up of nano grade inorganic fire retardant and micron order magnesium hydroxide and auxiliary flame retardant, the nano grade inorganic fire retardant is nano-aluminum hydroxide or nano-sized magnesium hydroxide, the median size of nano grade inorganic fire retardant≤100 nanometers, the median size of micron order magnesium hydroxide is at 1～10 micron, adopt dry method that nano inorganic compound flame retardant is carried out surface modification treatment, it is characterized in that: earlier surface-modifying agent is mixed with micron order magnesium hydroxide high-speed stirring, add the nano grade inorganic fire retardant then and continue the high-speed stirring mixing, adding the auxiliary flame retardant high-speed stirring at last again mixes, finally obtain the nano inorganic compound flame retardant that the surface is coated with surface-modifying agent, auxiliary flame retardant is a zinc borate, zinc oxide, ferric oxide, red phosphorus, phosphoric acid salt, carbonate or organosilicon.
Method of the present invention, the mass fraction sum of nano grade inorganic fire retardant and micron order magnesium hydroxide is 100 parts, the mass ratio of nano grade inorganic fire retardant and micron order magnesium hydroxide is 80: 20 to 10: 90, the mass fraction of auxiliary flame retardant is 10 to 30 parts, and the addition of surface-modifying agent is pressed 0.5%～3% of nano grade inorganic fire retardant and micron order magnesium hydroxide consumption sum.
Method of the present invention, the surface-modifying agent of employing are at least a in titante coupling agent, aluminium esters of gallic acid coupling agent, Borate Ester as Coupling, silane coupling agent, organic class tensio-active agent or the high molecular polymer.
Organic class tensio-active agent in the surface-modifying agent that method of the present invention adopts is lipid acid, soap, fatty acid ester, aromatic esters or polyol ester.
High molecular polymer in the surface-modifying agent that method of the present invention adopts is polyethylene wax, oxidized polyethlene wax or polyethers.
Method of the present invention adopts the high-speed stirring velocity range at 500～1000r/min.
The present invention prepares the method for nano inorganic compound flame retardant with transfer method, is a kind of special dry method modification method to nano inorganic compound flame retardant.The present invention has utilized " larger particles " micron order magnesium hydroxide in the composite flame-retardant agent as the carrier of surface-modifying agent in modifying process, in homogenizer, earlier surface-modifying agent is coated on the bigger magnesium hydroxide particle of particle diameter, and then pass through high-speed stirring, make collision and friction mutually between micron particles and the nano-scale particle, drive the dispersion of surface-modifying agent between nano-scale particle effectively, surface-modifying agent is transferred to (we are referred to as " transfer method ") on the nanometer particle, realize the coating of surface-modifying agent the nano-scale particle surface.
When solids moved with certain speed, its kinetic energy was directly proportional with the quality of particle.And cube being directly proportional of the quality of particle and particle diameter.For example, the nano particle of particle diameter 100 nanometers is compared with the micron particle of 100 microns of particle diameters, supposes that both proportion is identical, and particle diameter differs 1000 times, and quality then will differ 1,000,000,000 times.If adopt the dry method modification method directly inorganic nanoparticles to be carried out modification, because the inorganic nanoparticles quality is small, the kinetic energy that obtains when moving under high-speed stirring is also very little.Small like this kinetic energy is not enough to drive the dispersion of surface-modifying agent between nano particle, also just is difficult to further realize the even coating of surface-modifying agent at nano grain surface.Here it is, and inorganic nanoparticles is directly used the bad reason of dry method modification effect.
Method of the present invention is earlier surface-modifying agent to be coated on oarse-grained surface, has utilized the kinetic energy of the bigger particle of particle diameter in high-speed motion, makes macrobead under the effect of high-speed stirring, bumps and rubs with inorganic nanoparticles.Surface-modifying agent is transferred to the surface of inorganic nanoparticles.Because the kinetic energy that macrobead obtains in homogenizer is big, can be tens thousand of to several hundred million times kinetic energy that are higher than inorganic nanoparticles, just make when macrobead is far longer than inorganic nanoparticles and is stirred separately the collision of inorganic nanoparticles and rubbing effect each other collision and rubbing effect.Thereby, can make surface-modifying agent transfer to the inorganic nanoparticles surface from large particle surface, between nano particle, disperse effectively, and then realize the coating of surface-modifying agent nano grain surface.
The surface-modifying agent that the present invention adopts all is that addition is pressed the known usual amounts of inorganic combustion inhibitor surface modification at existing dry method surface treatment surface-modifying agent commonly used.The addition of properties-correcting agent presses nano particle and the required properties-correcting agent sum of micron particle surface modification is calculated.For example: the addition of properties-correcting agent is pressed 0.5%～3% of nano grade inorganic fire retardant and micron order magnesium hydroxide consumption sum.
Embodiment
Employing " nano inorganic compound flame retardant that is used for macromolecular material " when the preparation nano inorganic compound flame retardant (publication number: disclosed prescription CN 1536000A), carry out the surface modification operation according to transfer method provided by the invention.
Embodiment 1
The inorganic nano fire retardant is the aluminium hydroxide of median size 100 nanometers, and inorganic micron fire retardant is the magnesium hydroxide of 5 microns of median sizes, and the surface-modifying agent of selecting for use is an isostearoyl ylmethyl acryl oxo ethanoyl titanic acid ester (titanate coupling agent).Nano-aluminum hydroxide is 2: 1 with the mass ratio of micron magnesium hydroxide, and the addition of titanate coupling agent is nano-aluminum hydroxide and 0.5% of micron magnesium hydroxide consumption sum.
Working method: earlier the micron magnesium hydroxide is added in the homogenizer, press a micron magnesium hydroxide: 100: 1.5 mass ratio of titanate coupling agent adds phthalate ester coupling agent, start homogenizer then, under rotating speed 1000r/min, high-speed stirring 10 minutes makes titanate coupling agent be coated on the surface of micron magnesium hydroxide particle.The micron magnesium hydroxide that nano-aluminum hydroxide and surface has been coated coupling agent adds homogenizer by 2.000: 1.015 mass ratio, under rotating speed 1000r/min, high-speed stirring 10 minutes, make coupling agent transfer to the surface of nano-aluminum hydroxide particle from the surface of micron magnesium hydroxide, in this process, the surface of micron magnesium hydroxide also can keep a part of coupling agent, add again at last the auxiliary flame retardant zinc borate (consumption be nano-aluminum hydroxide with micron magnesium hydroxide consumption sum 10%), discharging obtains the nano inorganic compound flame retardant of surface modification.With 100 parts of nano inorganic compound flame retardants and 165 parts of ethylene-vinyl acetate copolymers (EVA) blend, through the twin screw extruder granulation, single screw extrusion machine prepares batten, the flame-proof composite material that obtains, its tensile strength 8.9Mpa.
Embodiment 2
100 parts of nano inorganic compound flame retardants and 100 parts of EVA of embodiment 1 preparation are prepared flame-proof composite material, and its tensile strength is 8.4MPa.
Embodiment 3
The magnesium hydroxide of median size 100 nanometers is replaced nano-aluminum hydroxide among the embodiment 1, all the other conditions all with embodiment 1 identical preparation nano inorganic compound flame retardant.
Embodiment 4
In embodiment 1, the mass ratio of micron magnesium hydroxide and titanate coupling agent changes 100: 3 into, all the other conditions all with embodiment 1 identical preparation nano inorganic compound flame retardant.
Embodiment 5
In embodiment 1, the mass ratio of micron magnesium hydroxide and titanate coupling agent changes 100: 9 into, all the other conditions all with embodiment 1 identical preparation nano inorganic compound flame retardant.
Embodiment 6
In embodiment 4; isostearoyl ylmethyl acryl oxo ethanoyl titanic acid ester (titanate coupling agent) changes two (two Tegin ISO bases) aluminic acid isopropyl ester (aluminate coupling agent) into, all the other conditions all with embodiment 4 identical preparation nano inorganic compound flame retardants.
Embodiment 7
In embodiment 1, isostearoyl ylmethyl acryl oxo ethanoyl titanic acid ester (titanate coupling agent) changes sulfonyl azide silane (silane coupling agent) into, all the other conditions all with embodiment 1 identical preparation nano inorganic compound flame retardant.
Comparative Examples 1
Each component and the consumption of nano inorganic compound flame retardant are identical with embodiment 1, and nano-aluminum hydroxide and micron magnesium hydroxide is independent respectively with common dry method modification.Modification time also is 10 minutes.Carry out respectively mixing with auxiliary flame retardant again behind the dry method modification, obtain nano inorganic compound flame retardant, 100 parts of composite flame-retardant agents and 165 parts of EVA are prepared flame-proof composite material, its tensile strength 8.0MPa.
Comparative Examples 2
100 parts of nano inorganic compound flame retardants and 100 parts of EVA with Comparative Examples 1 preparation prepare flame-proof composite material, its tensile strength 6.9MPa.
Comparative Examples 3
Each component and the consumption of nano inorganic compound flame retardant are identical with embodiment 1, what adopt is to mix the dry method modification method: after soon nano-aluminum hydroxide mixes with a micron magnesium hydroxide, carry out dry method modification with titanate coupling agent, modification time also is 10 minutes, mix with auxiliary flame retardant again, obtain the nano inorganic compound flame retardant of surface modification.100 parts of composite flame-retardant agents and 165 parts of EVA are prepared flame-proof composite material, its tensile strength 8.2MPa.
Comparative Examples 4
100 parts of nano inorganic compound flame retardants and 100 parts of EVA with Comparative Examples 3 preparations prepare flame-proof composite material, its tensile strength 7.4MPa.
With above three kinds of nano inorganic compound flame retardants that surface modifying method obtains, the flame-proof composite material that obtains with ethylene-vinyl acetate copolymer (EVA) blend respectively, its tensile strength is as shown in table 1.Embodiment 1 and Comparative Examples 1 contrast, embodiment 2 are contrasted as can be known with Comparative Examples 2, obtain the flame-proof composite material that nano inorganic compound flame retardant prepares with transfer method of the present invention, its tensile strength is apparently higher than adopting the method for common dry method modification to obtain the flame-proof composite material of nano inorganic compound flame retardant preparation to nano grade inorganic fire retardant and micron order magnesium hydroxide respectively.Embodiment 1,2 and Comparative Examples 3,4 are contrasted as can be known, obtain the flame-proof composite material of nano inorganic compound flame retardant preparation with transfer method of the present invention, its tensile strength apparently higher than will the nano grade inorganic fire retardant and the micron order magnesium hydroxide adopt after mixing common dry method modification (that is: mix dry method modification) method to obtain the flame-proof composite material of nano inorganic compound flame retardant preparation again.The flame retardant properties of the flame-proof composite material that transfer method modification of the present invention obtains is compared with the sample that carries out dry method modification or mixing dry method modification respectively, does not have considerable change.From the tensile strength performance contrast as can be seen, adopt transfer method modification of the present invention can obviously improve the tensile strength of flame-proof composite material.
The performance comparison of transfer method modification and common dry method modification
Table 1 (the material addition is a mass fraction)
| The transfer method modification | The difference dry method modification | Mix the back dry method modification | EVA | Tensile strength (MPa) | ||
| Nano-aluminum hydroxide/micron magnesium hydroxide | Nano-aluminum hydroxide | The micron magnesium hydroxide | Nano-aluminum hydroxide/micron magnesium hydroxide | |||
| Embodiment 1 | 66.7/33.3 | 165 | 8.9 | |||
| Embodiment 2 | 66.7/33.3 | 100 | 8.4 | |||
| Comparative Examples 1 | 66.7 | 33.3 | 165 | 8.0 | ||
| Comparative Examples 2 | 66.7 | 33.3 | 100 | 6.9 | ||
| Comparative Examples 3 | 66.7/33.3 | 165 | 8.2 | |||
| Comparative Examples 4 | 66.7/33.3 | 100 | 7.4 | |||
Claims (6)
1, a kind of method for preparing nano inorganic compound flame retardant with transfer method, nano inorganic compound flame retardant is made up of nano grade inorganic fire retardant and micron order magnesium hydroxide and auxiliary flame retardant, the nano grade inorganic fire retardant is nano-aluminum hydroxide or nano-sized magnesium hydroxide, the median size of nano grade inorganic fire retardant≤100 nanometers, the median size of micron order magnesium hydroxide is at 1～10 micron, adopt dry method that nano inorganic compound flame retardant is carried out surface modification treatment, it is characterized in that: earlier surface-modifying agent is mixed with micron order magnesium hydroxide high-speed stirring, add the nano grade inorganic fire retardant then and continue the high-speed stirring mixing, adding the auxiliary flame retardant high-speed stirring at last again mixes, finally obtain the nano inorganic compound flame retardant that the surface is coated with surface-modifying agent, auxiliary flame retardant is a zinc borate, zinc oxide, ferric oxide, red phosphorus, phosphoric acid salt, carbonate or organosilicon.
2, method according to claim 1, it is characterized in that: the mass fraction sum of nano grade inorganic fire retardant and micron order magnesium hydroxide is 100 parts, the mass ratio of nano grade inorganic fire retardant and micron order magnesium hydroxide is 80: 20 to 10: 90, the mass fraction of auxiliary flame retardant is 10 to 30 parts, and the addition of surface-modifying agent is pressed 0.5%～3% of nano grade inorganic fire retardant and micron order magnesium hydroxide consumption sum.
3, method according to claim 1 is characterized in that: surface-modifying agent is at least a in titante coupling agent, aluminium esters of gallic acid coupling agent, Borate Ester as Coupling, silane coupling agent, organic class tensio-active agent or the high molecular polymer.
4, method according to claim 3 is characterized in that: organic class tensio-active agent is lipid acid, soap, fatty acid ester, aromatic esters or polyol ester.
5, method according to claim 3 is characterized in that: high molecular polymer is polyethylene wax, oxidized polyethlene wax or polyethers.
6, method according to claim 1 is characterized in that: the high-speed stirring velocity range is at 500～1000r/min.
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| CN101186320B (en) * | 2007-12-17 | 2011-09-21 | 中国铝业股份有限公司 | Method for preparing aluminum hydroxide composite fire retardant |
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| CN106750543B (en) * | 2016-12-21 | 2018-10-19 | 普信氟硅新材料（衢州）有限公司 | A kind of preparation method of nano inorganic compound flame retardant |
| CN106957454B (en) * | 2017-04-18 | 2019-10-22 | 中国科学技术大学 | A kind of nano material coated fire retardant and preparation method thereof |
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| CN112341887A (en) * | 2020-11-26 | 2021-02-09 | 曾万祥 | Water-based flame-retardant coating and preparation method thereof |
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