CN1241977C - Method for manufacturing nanometer magnesium hydroxide fire retardant - Google Patents
Method for manufacturing nanometer magnesium hydroxide fire retardant Download PDFInfo
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- CN1241977C CN1241977C CN 200310108397 CN200310108397A CN1241977C CN 1241977 C CN1241977 C CN 1241977C CN 200310108397 CN200310108397 CN 200310108397 CN 200310108397 A CN200310108397 A CN 200310108397A CN 1241977 C CN1241977 C CN 1241977C
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 82
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 82
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 82
- 239000003063 flame retardant Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 23
- 238000004945 emulsification Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 239000000725 suspension Substances 0.000 claims description 22
- 239000012266 salt solution Substances 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 18
- 229920001223 polyethylene glycol Polymers 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 235000019359 magnesium stearate Nutrition 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003223 protective agent Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 239000003607 modifier Substances 0.000 claims description 2
- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 21
- 238000001914 filtration Methods 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000010008 shearing Methods 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000003995 emulsifying agent Substances 0.000 abstract description 2
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 238000011049 filling Methods 0.000 abstract description 2
- 229920000098 polyolefin Polymers 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract 2
- 239000002585 base Substances 0.000 abstract 1
- 238000011197 physicochemical method Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 241001131796 Botaurus stellaris Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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Abstract
The present invention relates to a method for manufacturing nanometer magnesium hydroxide fire retardant, which belongs to the technical field of manufacture of a physicochemical method of compounds. The method of the present invention is characterized in that soluble magnesium salt and soluble alkali are used as raw materials, and under the action of high-molecular protectant, magnesium hydroxide nanometer powder can be obtained by forcible emulsification and precipitation of a high-shearing homogenized emulsifier, filtration washing and dryness. A high-shearing homogenized emulsifying reactor specially used for the method of the present invention is characterized in that the reactor is composed of a motor, fixing screws, a solution inlet pore, a shell body, a stator, a material outlet pore, a rotor and a liquid flow guiding device; rotor speed is in a ranging from 3000 to 8000 rpm, and rotational speed is regulated according to grain diameters of required products. The method of the present invention has the advantages of simple process flows, little investment, low cost, homogeneous grain diameter distribution of products and high purity good intermiscibility of modified oleophilic surfaces of the products and polyolefine base materials; grain diameters of magnesium hydroxide grains are ordinarily in a scope ranging from 50 to 200 nm, and flame retardant property, filling property, etc. are greatly superior to those of products of other ordinary magnesium hydroxide; thus, the present invention has better application prospect.
Description
Technical Field
The invention relates to a method for preparing a nano magnesium hydroxide flame retardant, belonging to the technical field of physical and chemical method preparation of compounds.
Background
With the further development of science and technology, the processed products of chemical building materials plastics and organic polymer materials are more and more widely used in the fields of building, traffic, electrical appliances, communication and the like. The fire hazard caused by the inherent flammability of these materials has become a social problem of global concern, and at present, the flammability of the polymer is reduced mainly by adding a flame retardant to slow down the combustion speed of the polymer.
Among various flame retardant varieties, the halogen flame retardant is widely applied due to good flame retardant effect and no influence on the physical and chemical properties of materials. However, the polymer added with the halyard flame retardant has a large smoke amount during combustion, easily emits corrosive gases (such as HCl, HBr and the like) and harmful gases, and easily causes secondary damage. Therefore, the research on flame retardants in the world is moving toward non-halogenation. The aluminum hydroxide and magnesium hydroxide flame retardant plays a role in flame retardance by absorbing heat through chemical decomposition and releasing water during application, and has the advantages of no toxicity, no corrosion to processing machinery, and stable chemical properties of aluminum oxide and magnesium oxide generated after decomposition, so that no secondary harm is generated. Magnesium hydroxide is one of the fastest growing inorganic flame retardants in recent years. Compared with aluminum hydroxide, the decomposition temperature of magnesium hydroxide is higher (about 220 ℃ for aluminum hydroxide, and about 350 ℃ for magnesium hydroxide and 400 ℃) and is more suitable for the processing requirements of certain polymers, and the magnesium hydroxide also has the function of promoting the carbonization of the polymers. Therefore, magnesium hydroxide flame retardants have been studied more and their application fields have been expanding.
However, the flame retardant efficiency of magnesium hydroxide is low, and the requirement for higher addition amount is high, and when the common magnesium hydroxide reaches the flame retardant share, the particle size is large, the interface binding force is small, and the magnesium hydroxide is difficult to uniformly disperse in a polymer, so that the mechanical property of the polymer material is greatly reduced; the nano magnesium hydroxide has small particle size and large specific surface area, enhances the interaction with the matrix material, can be more uniformly dispersed in the matrix material, and can effectively improve the mechanical property of the matrix material while exerting the flame retardant effect. Therefore, the ultrafine grinding of the magnesium hydroxide powder is a future development direction.
Currently, there are two main ways for the industrial production of magnesium hydroxide: one way is by grinding natural mineral brucite to the desired particle size; the other method is a chemical synthesis method, namely, raw materials such as bittern containing magnesium chloride, halogen ore and the like are reacted with caustic alkali in an aqueous medium, and the generated magnesium hydroxide is obtained by filtering, washing and drying. In the former method, the components of natural minerals cannot be controlled, so that the product has high impurity content and poor service performance; the traditional chemical synthesis method also has a plurality of defects: the particle size distribution is not uniform and is not easy to control, the particle size is not refined enough, strong cohesiveness exists among particles, agglomeration is easy to disperse by secondary particles of 10-100 mu m, the production process flow is long, the energy consumption is high, and the like.
In recent years, several methods for preparing nano magnesium hydroxide have been developed. Liyadona and the like take high-purity magnesium powder and distilled water as raw materials, 1, 2-ethylenediamine as a solvent, and a hydrothermal method is adopted to prepare the rod-shaped nano magnesium hydroxide under the conditions of high temperature and high pressure. The method has high raw material cost, harsh reaction conditions and low reaction yield, and is difficult for industrial production (Advanced Materials, 12(1), 2000P 818-821). Chinese patent CN1389521A proposes that the ultrasonic oscillation method is used to disperse the magnesium hydroxide colloid prepared in advance, and then the magnesium hydroxide nanometer powder is obtained by dehydration and sintering. Chinese patent CN1341694A reports that a rotary packed bed (supergravity) is used as a reactor to prepare nano magnesium hydroxide, a soluble magnesium salt solution of a reaction material reacts with ammonia water (ammonia gas) on the surface of a filler, so that the microscopic reaction area is increased, but magnesium hydroxide generated by the reaction is easy to precipitate in the gaps between the filler, blocks the packed bed, and causes adverse consequences such as tower blockage, flooding and the like.
Disclosure of Invention
The invention aims to provide an advanced preparation method of a nano-scale magnesium hydroxide flame retardant capable of improving a microscopic reaction and a microscopic mixing state, namely a high-shear homogeneous emulsification method.
Another object of the present invention is to provide a high shear homogeneous emulsification reactor for forced precipitation of reactants.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing nano magnesium hydroxide fire retardant is characterized in that the method adopts a high-shear homogeneous emulsification reactor to realize liquid-liquid two-phase mixing precipitation reaction, and the preparation process comprises the following steps:
a. preparing a magnesium salt solution added with a macromolecular protective agent polyethylene glycol and an alkali solution;
b. adding the magnesium salt solution into a high-shear homogenizing emulsification reactor, heating and raising the temperature, wherein the magnesium salt solution is controlled at 20-80 ℃;
c. starting the reactor, adjusting the rotating speed, adding the prepared alkali liquor into the reactor for reaction at the reaction temperature of 25-45 ℃ to obtain a magnesium hydroxide suspension;
d. then aging the magnesium hydroxide suspension at 20 ℃ for 12 hours;
e. carrying out suction filtration on the aged magnesium hydroxide product, washing with deionized water, and drying a filter cake at 130 ℃ for 8 hours to obtain nano magnesium hydroxide powder;
f. carrying out surface modification on the magnesium hydroxide powder to obtain lipophilic modified nano magnesium hydroxide powder; the surface modifier is any one of stearic acid, magnesium stearate, a silane coupling agent and a titanate coupling agent.
The magnesium salt solution is any one of magnesium chloride, magnesium nitrate and magnesium sulfate aqueous solutions, and the concentration of the magnesium salt solution is 0.05-4.0 mol/l; the alkali solution is any one of sodium hydroxide, ammonia water and potassium hydroxide water solution, and the concentration of the alkali solution is 0.1-6 mol/l; the rotor speed of the high-shear homogeneous emulsification reactor is 3000-8000rpm, and the rotation speed is adjusted according to the particle size of the required product.
The special high-shearing homogenizing emulsifying reactor for the preparation method of the nano magnesium hydroxide fire retardant is characterized in that the reactor consists of a motor, a fixed screw, a solution inlet hole, a shell, a stator, a material outlet hole, a rotor and a liquid flow guiding device; a rotor connected with one end of a vertical driving shaft is arranged at the central position of the shell, the upper part of the driving shaft is connected with a motor, a stator with a plurality of micropores on the wall of thecylinder is arranged around the outer side of the rotor, and the upper bottom plate of the stator is provided with screw holes and is fixedly connected with the stator through screws; the top of the shell is provided with a solution inlet hole, and the near side of the bottom of the shell is provided with a material outlet hole; the wall of the shell is also provided with a liquid flow guiding device.
The method is characterized in that soluble magnesium salt and soluble alkali are used as raw materials, and the raw materials are forcedly emulsified and precipitated by a high-shear homogenizing emulsifier under the action of a high-molecular protective agent, filtered, washed and dried to obtain the magnesium hydroxide nano powder. The raw materials are in the high-shear homogeneous emulsification reactor. Under the high-speed drive of the motor, the materials are sucked into the rotor through the mesh of the stator, and the shearing action is carried out for dozens of thousands of times in a short time. In the shearing process, the materials are split and dispersed under the actions of centrifugal friction and high-speed impact in a precise gap between a rotor and a stator; meanwhile, due to the strong kinetic energy of the high-frequency machine, the materials form strong hydraulic shearing, liquid layer friction and tearing collision to achieve full dispersion and homogenization. After the materials fall out from the rotor-stator combination at high speed, the high-shear homogeneous emulsification reactor is provided with a guide device, and the materials form vertical three-dimensional turbulence in a specific container. Finally, the reaction is carried out to obtain magnesium hydroxide suspension, and the magnesium hydroxide suspension is cooled and aged to obtain the nanoscale flaky magnesium hydroxide.
Compared with the prior art, the invention has the following outstanding advantages and remarkable progress:
the method for preparing the nano-scale magnesium hydroxide flame retardant has the advantages of simple process flow, small investment and low cost. The particle size of magnesium hydroxide particles is generally 50-200nm, the particle size distribution of the product is uniform, the purity is high, the compatibility with polyolefin matrix materials is good after the surface oleophylic modification, the flame retardant property, the filling property and the like are far superior to other common magnesium hydroxide products, and the application prospect is good.
Drawings
FIG. 1 is a schematic structural diagram of a high shear homogeneous emulsification reactor of the special device of the present invention
FIG. 2 is a schematic view of the rotor of the example of FIG. 1
FIG. 3 is a schematic view of the stator structure of the example of FIG. 1
Detailed description of the invention
The present invention will be described in further detail with reference to specific examples.
Referring to fig. 1, fig. 2 and fig. 3, the high shear homogeneous emulsification reactor for the preparation method of the present invention comprises a motor 1, a set screw 2, a solution inlet hole 3, a housing 4, a stator 5, a material outlet hole 6, a rotor 7 and a liquid flow guiding device 8; a rotor 7 connected with one end of a vertical driving shaft is arranged at the center of the shell 4, the upper part of the driving shaft is connected with the motor 1, a stator 5 with a plurality of micropores on the wall of the cylinder is arranged around the outer side of the rotor 7, and the upper bottom plate of the stator 5 is provided with screw holes and is fixedly connected with the screw holes through screws 2; the top of the shell 4 is provided with a solution inlet hole 3, and the near side of the bottom is provided with a material outlet hole 6; a liquid flow guide 8 is also provided in the wall of the housing 4. The angle between the impellers of the rotor 7 is 70-90 degrees, and the rotating speed is 3000-8000 rpm.
The reaction of the magnesium salt solution and the alkali solution in the reactor has the following reaction formula:
the first embodiment is as follows: 102g of MgCl2·6H2Dissolving the O solid in 1000ml deionized water, adding 3g polyethylene glycol (PEG) with the concentration of 1-5% (wt%) of the magnesium salt, and stirring for 30 min; another 40g of NaOH was dissolved in 1000ml of deionized water. Firstly adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 6000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 20-25 ℃ to obtain a magnesium hydroxide suspension, and then aging the magnesium hydroxide suspension for 12 hours at 20 ℃. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 110nm, and modifying the surface with stearic acid to obtain lipophilic nano magnesium hydroxide flame retardant.
Example two: 102g of MgCl2·6H2Dissolving the O solid in 1000ml of deionized water, adding 3g of polyethylene glycol (PEG), and stirring for 30 min; another 40g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 6000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then cooling the magnesium hydroxide suspension to 20 ℃ and aging for 12 hours. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 70nm, and modifying the surface with magnesium stearate to obtain lipophilic nano magnesium hydroxide flame retardant.
Example three: 102g of MgCl2·6H2Dissolving the O solid in 1000ml of deionized water, adding 3g of polyethylene glycol (PEG), and stirring for 30 min; another 40g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 3000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then cooling the magnesium hydroxide suspension to 20 ℃ and aging for 12 hours. Filtering, washing with deionized water until no chloride ion is detected, and filtering to obtain filter cake 13Drying at 0 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 95nm, and surface modifying with silane coupling agent to obtain lipophilic nanometer magnesium hydroxide fire retardant.
Example four: 204g of MgCl2·6H2Dissolving the O solid in 1000ml of deionized water, adding 6g of polyethylene glycol (PEG), and stirring for 30 min; an additional 80g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneousemulsification reactor, starting the reactor, controlling the rotating speed to be 3000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 20-25 ℃ to obtain a magnesium hydroxide suspension, and then aging the magnesium hydroxide suspension for 12 hours at 20 ℃. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 160nm, and surface modifying with silane coupling agent to obtain lipophilic nanometer magnesium hydroxide flame retardant.
Example five: 204g of MgCl2·6H2Dissolving the O solid in 1000ml of deionized water, adding 6g of polyethylene glycol (PEG), and stirring for 30 min; an additional 80g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 3000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then aging the magnesium hydroxide suspension for 12 hours at 20 ℃. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 105nm, and surface modifying with silane coupling agent to obtain lipophilic nanometer magnesium hydroxide flame retardant.
Example six: 204g of MgCl2·6H2Dissolving the O solid in 1000ml of deionized water, adding 6g of polyethylene glycol (PEG), and stirring for 30 min; an additional 80g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 6000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then cooling the magnesium hydroxide suspension to 20 ℃ and aging for 12 hours. Filtering and removingWashing with ionized water until no chlorine ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle size of about 90nm, and surface modifying with titanate coupling agent to obtain lipophilic nano magnesium hydroxide flame retardant.
Example seven: 256g Mg (NO)3)2·6H2Dissolving the O solid in 1000ml of deionized water, adding 8g of polyethylene glycol (PEG), and stirring for 30 min; an additional 80g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling the rotating speed to be 6000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then cooling the magnesium hydroxide suspension to 20 ℃ and aging for 12 hours. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle diameter of about 85nm, and surface modifying with titanate coupling agent to obtain lipophilic nanometer magnesium hydroxide flame retardant.
Example eight: 246g MgSO4·7H2Dissolving the O solid in 1000ml of deionized water, adding 8g of polyethylene glycol (PEG), and stirring for 30 min; an additional 80g of NaOH was dissolved in 1000ml of deionized water. Adding the magnesium salt solution into a high-shear homogeneous emulsification reactor, starting the reactor, controlling therotating speed to be 6000rpm, slowly dropwise adding a sodium hydroxide aqueous solution, controlling the reaction temperature to be 40-45 ℃ to obtain a magnesium hydroxide suspension, and then cooling the magnesium hydroxide suspension to 20 ℃ and aging for 12 hours. Filtering, washing with deionized water until no chloride ion is detected, drying the filter cake at 130 deg.C for 8 hr to obtain sheet magnesium hydroxide powder with average particle size of about 240nm, and surface modifying with titanate coupling agent to obtain lipophilic nanometer magnesium hydroxide flame retardant.
Claims (2)
1. A method for preparing nano magnesium hydroxide fire retardant is characterized in that the method adopts a high-shear homogeneous emulsification reactor to realize liquid-liquid two-phase mixing precipitation reaction, and the preparation process comprises the following steps:
a. preparing a magnesium salt solution added with a macromolecular protective agent polyethylene glycol and an alkali solution;
b. adding the magnesium salt solution into a high-shear homogenizing emulsification reactor, heating and raising the temperature, wherein the magnesium salt solution is controlled at 20-80 ℃;
c. starting the reactor, adjusting the rotating speed, adding the prepared alkali liquor into the reactor for reaction at the reaction temperature of 25-45 ℃ to obtain a magnesium hydroxide suspension;
d. then aging the magnesium hydroxide suspension at 20 ℃ for 12 hours;
e. carrying out suction filtration on the aged magnesium hydroxide product, washing with deionized water, and drying a filter cake at 130 ℃ for 8 hours to obtain nano magnesium hydroxide powder;
f. carrying out surfacemodification on the magnesium hydroxide powder to obtain lipophilic modified nano magnesium hydroxide powder; the surface modifier is any one of stearic acid, magnesium stearate, a silane coupling agent and a titanate coupling agent;
the magnesium salt solution is any one of magnesium chloride, magnesium nitrate and magnesium sulfate aqueous solutions, and the concentration of the magnesium salt solution is 0.05-4.0 mol/l; the alkali solution is any one of sodium hydroxide, ammonia water and potassium hydroxide water solution, and the concentration of the alkali solution is 0.1-6 mol/l; the rotor speed of the high-shear homogeneous emulsification reactor is 3000-8000rpm, and the rotation speed is adjusted according to the particle size of the required product.
2. The special high-shear homogeneous emulsification reactor for the manufacturing method of nano magnesium hydroxide fire retardant according to claim 1 is characterized in that the reactor is composed of a motor (1), a fixing screw (2), a solution inlet hole (3), a shell (4), a stator (5), a material outlet hole (6), a rotor (7) and a liquid flow guiding device (8); a rotor (7) connected with one end of a vertical driving shaft is arranged at the center of the shell (4), the upper part of the driving shaft is connected with the motor (1), a stator (5) with a plurality of micropores on the wall of the cylinder is arranged around the outer side of the rotor (7), and the upper bottom plate of the stator (5) is provided with a screw hole and is fixedly connected with the stator through a screw (2); the top of the shell (4) is provided with a solution inlet hole (3), and the near side of the bottom is provided with a material outlet hole (6); a liquid flow guide device (8) is further arranged on the wall of the shell (4).
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| CN 200310108397 CN1241977C (en) | 2003-11-04 | 2003-11-04 | Method for manufacturing nanometer magnesium hydroxide fire retardant |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1295270C (en) * | 2005-02-23 | 2007-01-17 | 杨第伦 | Process for preparing magnesium hydroxide loose nano blocked flame retardant and products therefrom |
| CN100357394C (en) * | 2006-05-29 | 2007-12-26 | 太原理工大学 | Preparation method of hydrophobic ultrafine nanometer fire retardant magnesium hydroxide |
| CN101172628B (en) * | 2007-10-26 | 2010-11-03 | 上海大学 | Method of producing nano MgO/Mg(OH)* composite powder body |
| CN101173115B (en) * | 2007-10-27 | 2010-06-02 | 太原理工大学 | Ultra-fine magnesium hydroxide surface modifying method |
| CN101853713B (en) * | 2009-04-03 | 2012-07-04 | 上海市高桥电缆厂有限公司 | Flame-retardant filler for cable |
| CN103965655A (en) * | 2014-06-12 | 2014-08-06 | 北京化工大学 | Novel surface modification method of magnesium hydroxide fire retardant |
| CN104495883A (en) * | 2014-12-02 | 2015-04-08 | 中国科学院青海盐湖研究所 | Preparation method of magnesium hydrate with high-concentration slurry |
| CN104910997B (en) * | 2015-06-01 | 2017-03-29 | 江苏燃顺环保科技有限公司 | A kind of coal-burning boiler decoking additive and preparation method thereof |
| CN107353440A (en) * | 2017-06-09 | 2017-11-17 | 苏州市泽镁新材料科技有限公司 | A kind of fire-retardant preparation method with size tunable magnesium hydroxide |
| CN112516928A (en) * | 2020-12-11 | 2021-03-19 | 西能化工科技(上海)有限公司 | Solid sol preparation device and preparation method |
| CN114956135A (en) * | 2022-05-16 | 2022-08-30 | 安徽大学绿色产业创新研究院 | Method for preparing nano magnesium hydroxide flame retardant through high shear force |
| CN115007165B (en) * | 2022-07-06 | 2023-08-22 | 西南化工研究设计院有限公司 | Efficient catalyst for preparing formaldehyde by methanol oxidation and preparation method thereof |
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