CN103665939A - Method for integrally preparing high-dispersity ultrafine magnesium hydroxide flame retardant - Google Patents
Method for integrally preparing high-dispersity ultrafine magnesium hydroxide flame retardant Download PDFInfo
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Abstract
The invention discloses a method for integrally preparing a high-dispersity ultrafine magnesium hydroxide flame retardant, which comprises the following steps: continuously synthesizing high-purity magnesium hydroxide; and carrying out single cycle wet grinding and surface modification on magnesium hydroxide and integrally implementing particle size control and surface processing of the magnesium hydroxide flame retardant. According to the invention, the technical difficulties of control on purity, slurry viscosity, particle size, particle size distribution and specific surface area of the magnesium hydroxide flame retardant, the existence of the phenomena of secondary coagulation and bonding during the drying process and the like; a hydrophilic surface of magnesium hydroxide flame retardant powder is modified into a lipophilic surface, so that the intermiscibility and dispersity of the powder in a macromolecule polymeric material are improved, the influence of the high-dispersity ultrafine magnesium hydroxide flame retardant on the processing performance and the mechanical performance of a polymer product is reduced, and the comprehensive properties of the macromolecule polymer, such as flame retardance, processing, mechanics, electrics, are optimized.
Description
Technical field
The present invention relates to flame retardant of magnesium hydroxide preparation field, relate in particular to a kind of integration system for the method for polymolecularity ultra-fine magnesium hydroxide flame retardant.
Background technology
The trend of 21 century International flame retardant development is just towards the future development of environmental protection, the low fuming of low toxicity, high efficiency, multifunction, and external many countries have limited production and the use that environment is had to the fire retardant of pollution.Europe has started to limit the sale of halogen containing flame-retardant, produces sour gas fire retardant when Japan bans use of cable fire, and the U.S. has formulated the regulation that adopts low halogen cable coating layer.Fast development along with China's economic construction, the raising that safety performance is required, people are on green, the attention of environmental protection and the impact of other various factors, the state-of-the-art facilitys such as many Highrise buildingss, subway, tunnel, Nuclear power plants, boats and ships all require to adopt low-smoke halogen-free flame-retardant electric wire and cable, increasing to the demand of low-smoke halogen-free flame-retardant electric wire and cable.Electric cable material with low smoke and halogen free industry attracts increasing enterprises pay attention, and numerous domestic producer all goes into overdrive electric cable material with low smoke and halogen free to develop.Due to the market of China own and demand in line with international standards, fire retardant is changed from the non-environment-friendly type of halogen to halogen-free environment-friendly type flame-proof agent.
Magnesium hydroxide meets current fire retardant to the needs of environment-friendly type development completely with its superior flame retardant properties, and it belongs to human health and environmentally friendly inorganic non-halogen flame retardant, and the sector is classified as novel strategic industry by country.The multiple performances such as that magnesium hydroxide has is fire-retardant, eliminate smoke, resistance is dripped, filling, have a wide range of applications at fire-retardant, environmental protection, medicine and the aspect such as ceramic, own through being deep into the every field of national economy.Along with the continuous progress of society, people improve constantly the requirement of novel material, and the quality index of magnesium hydroxide products not only rests in initial product purity, and product form and size-grade distribution are also had higher requirement.
The method of producing at present magnesium hydroxide mainly contains two kinds: the one, and the direct comminuting method of brucite; The 2nd, containing magnesium raw material reaction conversion method.Due to the direct comminuting method of brucite, affected by many defects such as brucite foreign matter content is high, whiteness is low etc., its product can only be used as low side flame retardant of magnesium hydroxide.And compositional rule can be prepared the magnesium hydroxide products of different size by controlling differential responses condition, therefore, synthesis method is to produce now the main method of high-end magnesium hydroxide.In prior art, mainly contain the large-grain magnesium hydroxide that directly synthetic median size is greater than 10 μ m, and directly synthesize small-particle or the super fine magnesium hydroxide that median size is less than 10 μ m.The former major advantage is easy filtration washing, and flow process is short and cost is low, but can not directly use as fire retardant, needs secondary processing.And the latter can directly use as flame retardant of magnesium hydroxide, but easily reunite or gelation, cause filtration washing difficulty and production cost high, it is global problem that super fine magnesium hydroxide filters.
The character on flame retardant of magnesium hydroxide surface natural presenting " hydrophilic oleophobic ", if with not surface treated magnesium hydrate powder filled polymer material, in organic polymer, be difficult to disperse equably, other performance (as mechanical property and processing characteristics etc.) severe exacerbation of polymer materials, therefore, must carry out surface modification to magnesium hydroxide, to change the surface properties of its natural " hydrophilic oleophobic ", the consistency that improves itself and polymkeric substance, reduces it and even makes them increase on the impact of polymeric articles processing characteristics and mechanical property.Existing Technology mainly adopts dry method modification, and the method is compared with wet method, and energy consumption is high, and technical process is complicated.
Summary of the invention
The object of this invention is to provide a kind of integration system for the method for polymolecularity ultra-fine magnesium hydroxide flame retardant, to synthesize magnesium hydroxide, Ultra-fine control and surface modification integrated, to solve the control of flame retardant of magnesium hydroxide purity, slurry viscosity, particle diameter, size distribution and specific surface area, the technical barriers such as the secondary aggregation occurring when dry and bonding phenomenon, and the character on flame retardant of magnesium hydroxide surface natural presenting " hydrophilic oleophobic ".
For addressing the above problem, the present invention by the following technical solutions:
Integration system is for a method for polymolecularity ultra-fine magnesium hydroxide flame retardant, will synthesize magnesium hydroxide, Ultra-fine is controlled and surface modification is integrated, comprises the steps:
Step 1, prepare inorganic magnesium salt solution and alkaline solution, Mg respectively
2+volumetric molar concentration is 0.5～5mol/l, OH
-volumetric molar concentration is 1～10mol/l, OH
-volumetric molar concentration and Mg
2+the ratio of volumetric molar concentration is 2～5;
Step 2, inorganic magnesium salt solution and alkaline solution that step 1 is prepared are heated to respectively 35～60 ℃, the flow velocity of 10～500ml/min of afterwards the inorganic magnesium salt solution of same volume and alkaline solution being take joins in the closed reaction vessel that stirring velocity is 50～1500rpm simultaneously, synthetic magnesium hydroxide slurry stops 10～30min in reaction vessel, and in stop process, temperature is that 60～100 ℃, stirring velocity are 50～1500rpm;
Step 3, the magnesium hydroxide slurry that step 2 is obtained proceed in digestion tank, ageing 20～30min at 60～100 ℃, and filtration washing repeatedly, obtains magnesium hydroxide wet cake afterwards; Described magnesium hydroxide wet cake moisture is 40wt%～50wt%, hydroxide Mg content≤99wt% in solid matter;
Step 4, the magnesium hydroxide wet cake that step 3 is obtained and silane modifier join in controlling wet-type finishing machine and grind 20～30min at 40～60 ℃, and wherein, silane modifier add-on is 0.1～10wt% of magnesium hydroxide wet cake; In controlling wet-type finishing machine, zirconium white spheroid diameter is respectively 3mm, 1mm, 0.5mm, and quality proportioning is 1～5:3～6:2～3; Filter afterwards, the dry polymolecularity ultra-fine magnesium hydroxide flame retardant that obtains.
Described in step 4, silane modifier is RSiX
3in one or more, in formula, R is amino, sulfydryl, vinyl, epoxy group(ing), cyano group or methacryloxy, X is halogen, alkoxyl group or acyloxy.
Step 4 is also included in and in controlling wet-type finishing machine, adds stearic acid or oleic acid and magnesium hydroxide wet cake and silane modifier jointly to grind, and the add-on of described stearic acid or oleic acid is 0.1～5wt% of magnesium hydroxide wet cake.
Beneficial effect of the present invention:
1, the particle diameter of synthesis phase magnesium hydroxide is controlled with the particle diameter in wet grinding stage and controlled and combine, can realize single loop grinding and just can obtain the novel process of qualified product.The combination of these two kinds of methods, the control that has mainly solved magnesium hydroxide purity and uniform particles degree at synthesis phase, owing to no longer introducing impurity, mainly solves the control of particle diameter, size distribution and the specific surface area of flame retardant of magnesium hydroxide in the grinding stage.Therefore reunion or the defect such as gelation, filtration washing difficulty and production cost height of direct synthesizing superfine magnesium hydroxide, have been avoided.
2, magnesium hydrate powder is in process of lapping, and its surface atom is in height active state, the dispersion energy that surface energy is very large and lower, and easy conglomerate between powder, not only filtration difficulty, causes subsequent technique very complicated.The inventive method adopts single loop wet grinding and surface modification magnesium hydroxide to combine, and a step has completed particle diameter, the size distribution of flame retardant of magnesium hydroxide, control and the surface modification of specific surface area.Not only suppress the rising of magnesium hydroxide slurry viscosity in process of lapping and increased substantially the filtering rate of magnesium hydroxide, make the water ratio of wet cake be down to and be less than 30% from 50% left and right.And, make magnesium hydroxide there is good hydrophobicity and dispersiveness, broken through the secondary aggregation and the bonding technology difficult problem that occur when dry, after product drying, do not need to pulverize and screening, significantly the energy consumption of production cost and drying products, shortened technical process, improved productivity effect.
3, adopt single or multiple surperficial modified magnesium hydroxide, make to grind and modified product not reunion completely, surface coating rate reaches more than 99.9%, and powder reaches 100% to the coupling activity of polymer base material.Consistency in solution system between organic polymer/magnesium hydroxide mineral filler component interface, guarantees that flame retardant of magnesium hydroxide, in macromolecular material, can not only reach fire-retardant and smoke suppressing effect, and less on the performance index impact of macromolecular material.Improve rheological and dispersiveness that product adds man-hour, improve flame retardant properties and the mechanical strength of material, optimizing product quality and performance.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is done further and explained.Specific embodiment is intended to describe in more detail the present invention below.The object of these embodiment is to explain the present invention, and should not be construed as limiting the scope of the invention.
Integration system is for a method for polymolecularity ultra-fine magnesium hydroxide flame retardant, as shown in Figure 1, will synthesize magnesium hydroxide, Ultra-fine is controlled and surface modification is integrated, comprises the steps:
Step 1, prepare inorganic magnesium salt solution and alkaline solution, Mg respectively
2+volumetric molar concentration is 0.5～5mol/l, OH
-volumetric molar concentration is 1～10mol/l, OH
-volumetric molar concentration and Mg
2+the ratio of volumetric molar concentration is 2～5.
Step 2, inorganic magnesium salt solution and alkaline solution that step 1 is prepared are heated to respectively 35～60 ℃, the flow velocity of 10～500ml/min of afterwards the inorganic magnesium salt solution of same volume and alkaline solution being take joins in the closed reaction vessel that stirring velocity is 50～1500rpm simultaneously, synthetic magnesium hydroxide slurry stops 10～30min in reaction vessel, and in stop process, temperature is that 60～100 ℃, stirring velocity are 50～1500rpm.According to the size of synthetic magnesium hydroxide (D50=5～50 μ m), change the stirring velocity of its reinforced flow velocity and reaction vessel, control crystal nucleation and growth conditions; Synthetic magnesium hydroxide slurry stays Shi Jian≤10min at the Ting of reaction vessel, play the effect that adds crystal seed, accelerate the agglomeration of magnesium hydroxide crystal and grow up, having overcome in prior art particle inhomogeneous, the unmanageable defect of the overall dimensions of crystal grain and particle size.
Step 3, the magnesium hydroxide slurry that step 2 is obtained proceed in digestion tank, ageing 20～30min at 60～100 ℃, and filtration washing repeatedly, obtains magnesium hydroxide wet cake afterwards; Described magnesium hydroxide wet cake moisture is 40wt%～50wt%, hydroxide Mg content≤99wt% in solid matter.The magnesium hydroxide slurry particle diameter that step 1 to three successive reaction generates is at D50=5～50 μ m, uniform particles, and its technical process is simple, and processing parameter is easily controlled, and magnesium hydroxide purity and the magnesium rate of recovery of acquisition are all high.
Step 4, the magnesium hydroxide wet cake that step 3 is obtained and silane modifier join in controlling wet-type finishing machine and grind 20～30min at 40～60 ℃, wherein, silane modifier add-on is the 0.1-10wt% of magnesium hydroxide wet cake, in controlling wet-type finishing machine, zirconium white spheroid diameter is respectively 3mm, 1mm, 0.5mm, and quality proportioning is 1～5:3～6:2～3; Filter afterwards, the dry polymolecularity ultra-fine magnesium hydroxide flame retardant that obtains.This step adopts single loop wet grinding and surface modification magnesium hydroxide, and the particle diameter of flame retardant of magnesium hydroxide is controlled and surface treatment total implementation.By adjusting, grind the proportioning of packing medium different diameter zirconium white spheroid, control particle diameter, size distribution and the specific surface area of flame retardant of magnesium hydroxide.By changing the proportioning of zirconium white spheroid, single loop realizes D50=0.1～6.0 μ m and specific surface area at 4～10m
2the magnesium hydroxide of/g different size.
Described silane modifier is RSiX
3in one or more, in formula, R represents the groups such as amino, sulfydryl, vinyl, epoxy group(ing), cyano group or methacryloxy, these groups and different matrix resins all have stronger response capacity; X is the group that representative can be hydrolyzed, as halogen, alkoxyl group or acyloxy etc.By adding one or more different silane modifiers, modified superfine magnesium hydroxide, can obtain the flame retardant of magnesium hydroxide of difference in functionality, for the preparation of different flame-retardant high-molecular polymkeric substance; The add-on of silane modifier is 0.1～10%(wt% of magnesium hydroxide); Through wet grinding prepare median size in D50=0.1～6.0 μ m and specific surface area at 4～10m
2the ultra-fine slurries of magnesium hydroxide of/g, after filtration and dry, make qualified polymolecularity ultra-fine magnesium hydroxide flame retardant finished product.The method combines single loop wet grinding with surface modification magnesium hydroxide, when completing the control of magnesium hydroxide particle diameter, size distribution and specific surface area, the particle surface of magnesium hydroxide is carried out to hydrophobic treatment.Due to adding of silane modifier, not only suppress the rising of magnesium hydroxide slurry viscosity in process of lapping and increased substantially the filtering rate of magnesium hydroxide, and, make magnesium hydroxide there is good hydrophobicity and dispersiveness, control the secondary aggregation and the bonding phenomenon that while being dried, occur, after product drying, do not need to pulverize, effectively improved dispersiveness and the consistency of its powder in polymeric material.
For meeting the demand of different high molecular polymer base materials, step 4 is also included in controlling wet-type finishing machine and adds stearic acid or oleic acid etc. jointly to grind with magnesium hydroxide wet cake and silane modifier, and the add-on of described stearic acid or oleic acid is 0.1～5wt% of magnesium hydroxide wet cake.Adopt multiple properties-correcting agent composite, meet the requirement that high molecular polymer base material adds mechanical property after magnesium hydroxide, flame retardant properties, electric property, processing characteristics simultaneously.Synthetic high purity magnesium hydroxide wet cake
Embodiment 1
The MgCl of preparation 4.5mol/L
2the NH of solution 1000L and 9.0mol/L
3h
2o solution 1000L, be heated to respectively 35 ℃ of left and right, by volume pump, take the feed rate of 500ml/min joins these two kinds of solution in the airtight reaction vessel that stirring velocity is 1500rpm simultaneously, synthetic slurries residence time in reaction vessel of magnesium hydroxide is 10min left and right, in stop process, temperature is 100 ℃, and stirring velocity is 1500rpm.The synthetic slurries of magnesium hydroxide are proceeded in digestion tank, and at 100 ℃, after ageing 20mim, by the synthetic slurries filtration washing of magnesium hydroxide, making moisture is 50wt% left and right, impurity Cl in solid matter
-≤ 0.05wt%, Fe
3+≤ 0.05wt%, obtains D50=5 μ m high purity magnesium hydroxide wet cake.
Embodiment 2
The MgCl of preparation 4.5mol/L
2the NH of solution 1000L and 9.0mol/L
3h
2o solution 1000L, be heated to respectively 35 ℃ of left and right, by volume pump, take the feed rate of 100ml/min joins these two kinds of solution in the airtight reaction vessel that stirring velocity is 500rpm simultaneously, synthetic slurries residence time in reaction vessel of magnesium hydroxide is 20min left and right, in stop process, temperature is 80 ℃, and stirring velocity is 500rpm.The synthetic slurries of magnesium hydroxide are proceeded in digestion tank, and at 80 ℃, after ageing 20mim, by the synthetic slurries filtration washing of magnesium hydroxide, making moisture is 40wt% left and right, impurity Cl in solid matter
-≤ 0.05wt%, Fe
3+≤ 0.05wt%, obtains D50=10 μ m high purity magnesium hydroxide wet cake.
Embodiment 3
The MgCl of preparation 0.5mol/L
2the NH of solution 1000L and 2.5mol/L
3h
2o solution 1000L, be heated to respectively 60 ℃ of left and right, by volume pump, take the feed rate of 10ml/min joins these two kinds of solution in the airtight reaction vessel that stirring velocity is 50rpm simultaneously, synthetic slurries residence time in reaction vessel of magnesium hydroxide is 30min left and right, in stop process, temperature is 60 ℃, and stirring velocity is 50rmp.The synthetic slurries of magnesium hydroxide are proceeded in digestion tank, and at 60 ℃, after ageing 30mim, by the synthetic slurries filtration washing of magnesium hydroxide, making moisture is 40wt% left and right, impurity Cl in solid matter
-≤ 0.05wt%, Fe
3+≤ 0.05wt%, obtains D50=50 μ m high purity magnesium hydroxide wet cake.
Grind and surface modification magnesium hydroxide
Embodiment 4
By D50=5 μ m and the H of embodiment 1 preparation
2o=50% high purity magnesium hydroxide wet cake 100kg and 0.1kg3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (C
9h
20o
5si) join in controlling wet-type finishing machine, the proportioning of grinding packing medium zirconium white spheroid diameter is: 3mm/1mm/0.5mm=1:6:3 simultaneously.The heat that grinding and modification temperature produce by magnesium hydroxide self-friction is controlled temperature 50 ℃ of left and right, after milling time 30min, and magnesium hydroxide D50=0.8 μ m and specific surface area 9m
2/ g, is filtered with dry, obtains high purity high dispersiveness ultra-fine magnesium hydroxide flame retardant.This product is not reunited completely, surface coating rate reaches more than 99.9%, its product is filled in EVA+PE base material, powder reaches 100% to the coupling activity of base material, substantially improve dispersiveness, bounding force, the consumption factor and the inductance capacitive reactance of magnesium hydroxide in EVA+PE, and strengthened the interface bonding of magnesium hydrate powder and EVA+PE base material, and improved its reinforcement ability to EVA+PE base material, realize the maximization of processing, flame retardant properties, mechanics and electric property.
Embodiment 5
By D50=5 μ m and the H of embodiment 1 preparation
2o=50% high purity magnesium hydroxide wet cake 100kg and 0.5kg3-aminopropyl methyldiethoxysilane (C
8h
21nO
2si) join in controlling wet-type finishing machine, the proportioning of grinding packing medium zirconium white spheroid diameter is: 3mm/1mm/0.5mm=2:5:3 simultaneously.The heat that grinding and modification temperature produce by magnesium hydroxide self-friction is controlled temperature 50 ℃ of left and right, after milling time 25min, and magnesium hydroxide D50=1.5 μ m and specific surface area 7m
2/ g, is filtered with dry, obtains high purity high dispersiveness ultra-fine magnesium hydroxide flame retardant.This product is not reunited completely, surface coating rate reaches more than 99.9%, its product is filled in polyurethane base material, powder reaches 100% to the coupling activity of base material, substantially improve dispersiveness, bounding force, the electric and light transmission of magnesium hydroxide in urethane, the interface bonding that has strengthened magnesium hydrate powder and polyurethane base material, has improved its reinforcement ability to polyurethane base material, realizes the maximization of electric, weathering resistance and corrosion resistance nature.
Embodiment 6
By D50=10 μ m and the H of embodiment 2 preparations
2o=40% high purity magnesium hydroxide wet cake 100kg and 1.0kg vinyltriethoxysilane (C
8h
18o
3si)+0.5kg stearic acid joins in controlling wet-type finishing machine simultaneously, and the proportioning of grinding packing medium zirconium white spheroid diameter is: 3mm/1mm/0.5mm=5:3:2.The heat that grinding and modification temperature produce by magnesium hydroxide self-friction is controlled temperature 40 ℃ of left and right, after milling time 20min, and magnesium hydroxide D50=3.0 μ m and specific surface area 5m
2/ g, is filtered with dry, obtains high purity high dispersiveness ultra-fine magnesium hydroxide flame retardant.This product is not reunited completely, surface coating rate reaches more than 99.9%, its product is filled in olefin polymer base material, powder reaches 100% to the coupling activity of base material, substantially improve dispersiveness and the bounding force of magnesium hydroxide in olefin polymer, the interface bonding that has strengthened magnesium hydrate powder and olefin polymer base material, has improved its reinforcement ability to olefin polymer base material, realizes processing, flame retardant properties and mechanical property maximization.
Embodiment 7
By D50=50 μ m and the H of embodiment 3 preparations
2o=40% high purity magnesium hydroxide wet cake 100kg and 10kg3-(methacryloxypropyl) propyl trimethoxy silicane (C
10h
20o
5si) join in controlling wet-type finishing machine, the proportioning of grinding packing medium zirconium white spheroid diameter is: 3mm/1mm/0.5mm=5:6:3 simultaneously.The heat that grinding and modification temperature produce by magnesium hydroxide self-friction is controlled temperature 60 ℃ of left and right, after milling time 25min, and magnesium hydroxide D50=6.0 μ m and specific surface area 4m
2/ g, is filtered with dry, obtains high purity high dispersiveness ultra-fine magnesium hydroxide flame retardant.This product is not reunited completely, surface coating rate reaches more than 99.9%, its product is filled in unsaturated polyester base material, powder reaches 100% to the coupling activity of base material, substantially improve dispersiveness and the bounding force of magnesium hydroxide in unsaturated polyester, the interface bonding that has strengthened magnesium hydrate powder and unsaturated polyester base material, has improved its reinforcement ability to unsaturated polyester base material, realizes the maximization of processing, mechanical, electric and light transmission.
These are only preferred case study on implementation of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. integration system, for a method for polymolecularity ultra-fine magnesium hydroxide flame retardant, is characterized in that, will synthesize that magnesium hydroxide, Ultra-fine are controlled and surface modification is integrated, comprises the steps:
Step 1, prepare inorganic magnesium salt solution and alkaline solution, Mg respectively
2+volumetric molar concentration is 0.5～5mol/l, OH
-volumetric molar concentration is 1～10mol/l, OH
-volumetric molar concentration and Mg
2+the ratio of volumetric molar concentration is 2～5;
Step 2, inorganic magnesium salt solution and alkaline solution that step 1 is prepared are heated to respectively 35～60 ℃, the flow velocity of 10～500ml/min of afterwards the inorganic magnesium salt solution of same volume and alkaline solution being take joins in the closed reaction vessel that stirring velocity is 50～1500rpm simultaneously, synthetic magnesium hydroxide slurry stops 10～30min in reaction vessel, and in stop process, temperature is that 60～100 ℃, stirring velocity are 50～1500rpm;
Step 3, the magnesium hydroxide slurry that step 2 is obtained proceed in digestion tank, ageing 20～30min at 60～100 ℃, and filtration washing repeatedly, obtains magnesium hydroxide wet cake afterwards; Described magnesium hydroxide wet cake moisture is 40wt%～50wt%, hydroxide Mg content≤99wt% in solid matter;
Step 4, the magnesium hydroxide wet cake that step 3 is obtained and silane modifier join in controlling wet-type finishing machine and grind 20～30min at 40～60 ℃, and wherein, silane modifier add-on is 0.1～10wt% of magnesium hydroxide wet cake; In controlling wet-type finishing machine, zirconium white spheroid diameter is respectively 3mm, 1mm, 0.5mm, and quality proportioning is 1～5:3～6:2～3; Filter afterwards, the dry polymolecularity ultra-fine magnesium hydroxide flame retardant that obtains.
2. integration system according to claim 1, for the method for polymolecularity ultra-fine magnesium hydroxide flame retardant, is characterized in that, silane modifier is RSiX described in step 4
3in one or more, in formula, R is amino, sulfydryl, vinyl, epoxy group(ing), cyano group or methacryloxy, X is halogen, alkoxyl group or acyloxy.
3. integration system according to claim 1 and 2 is for the method for polymolecularity ultra-fine magnesium hydroxide flame retardant, it is characterized in that, step 4 is also included in controlling wet-type finishing machine and adds stearic acid or oleic acid and magnesium hydroxide wet cake, silane modifier jointly to grind, and the add-on of described stearic acid or oleic acid is 0.1～5wt% of magnesium hydroxide wet cake.
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| CN201410827933.8A CN104592789B (en) | 2013-12-27 | 2014-12-26 | A kind of preparation method of flame retardant of magnesium hydroxide |
| CN201410831194.XA CN104592790A (en) | 2013-12-27 | 2014-12-26 | Method for controlling and modifying grain diameter of magnesium hydrate |
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| CN201410827933.8A Active CN104592789B (en) | 2013-12-27 | 2014-12-26 | A kind of preparation method of flame retardant of magnesium hydroxide |
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| CN113583296B (en) * | 2021-07-14 | 2023-01-24 | 营口理工学院 | Modified magnesium hydroxide, flame retardant, preparation and application thereof |
| CN115744945B (en) * | 2022-11-23 | 2024-05-28 | 中南大学 | Magnesium hydroxide continuous preparation method with controllable hydrophobicity |
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| CN102491381A (en) * | 2011-12-16 | 2012-06-13 | 江苏艾特克阻燃材料有限公司 | Preparation method for flame retardant magnesium hydroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104592790A (en) * | 2013-12-27 | 2015-05-06 | 江苏艾特克阻燃材料有限公司 | Method for controlling and modifying grain diameter of magnesium hydrate |
| CN104592789B (en) * | 2013-12-27 | 2018-12-04 | 江苏艾特克阻燃材料有限公司 | A kind of preparation method of flame retardant of magnesium hydroxide |
| CN110684237A (en) * | 2019-10-28 | 2020-01-14 | 深圳市锦昊辉实业发展有限公司 | Composite modifier and preparation method thereof for modifying hydroxide flame retardant |
| CN114456620A (en) * | 2021-06-25 | 2022-05-10 | 合肥中科阻燃新材料有限公司 | Ball milling method for producing superfine magnesium hydroxide fire retardant and preparation method thereof |
| CN114456620B (en) * | 2021-06-25 | 2024-03-19 | 合肥中科阻燃新材料有限公司 | Superfine magnesium hydroxide flame retardant produced by ball milling method and preparation method thereof |
| CN113429631A (en) * | 2021-07-19 | 2021-09-24 | 山东晨旭新材料股份有限公司 | Preparation method and application of modified magnesium hydroxide flame retardant |
| CN113789185A (en) * | 2021-10-14 | 2021-12-14 | 华北理工大学 | Preparation method of coal spontaneous combustion inhibitor based on magnesium ion compound |
| CN114292532A (en) * | 2022-01-06 | 2022-04-08 | 辽宁鑫阳新材料科技有限公司 | Magnesium hydroxide ultra-fining and surface modification method and application thereof |
| CN114395274A (en) * | 2022-01-12 | 2022-04-26 | 江西广源化工有限责任公司 | Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material |
| CN114410128A (en) * | 2022-01-29 | 2022-04-29 | 辽宁鑫阳新材料科技有限公司 | Magnesium hydroxide ultra-fining and surface modification method and application thereof |
| CN114874494A (en) * | 2022-03-28 | 2022-08-09 | 洛阳中超新材料股份有限公司 | High-flow magnesium hydroxide flame retardant, preparation thereof and low-smoke halogen-free cable |
| CN114874494B (en) * | 2022-03-28 | 2023-10-17 | 洛阳中超新材料股份有限公司 | High-flow magnesium hydroxide flame retardant, preparation method thereof and low-smoke halogen-free cable |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104592789A (en) | 2015-05-06 |
| CN104592789B (en) | 2018-12-04 |
| CN104592790A (en) | 2015-05-06 |
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