CN110342552B - Method for preparing active micro-nano magnesium hydroxide flame retardant by chemical method - Google Patents
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Abstract
The invention relates to a method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method, belonging to the field of non-metallic mineral processing and preparation of environment-friendly flame-retardant functional materials. The method comprises the following steps: crushing magnesite tailings serving as a raw material, adding magnesium chloride hexahydrate, uniformly mixing, and calcining to obtain active light-burned magnesium; grinding the active light calcined magnesium, and then uniformly mixing the active light calcined magnesium with water to obtain magnesium hydroxide slurry; adding ethylene glycol into the magnesium hydroxide slurry, grinding, adding a modifier, and carrying out hydration reaction; and drying and cleaving the hydrated magnesium hydroxide slurry to obtain the active micro-nano magnesium hydroxide. The method utilizes the hydration reaction of light-burned magnesium to prepare the micro-nano magnesium hydroxide flame retardant, fully utilizes tailing resources, and accords with the concept of sustainable development.
Description
Technical Field
The invention relates to a method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method, belonging to the field of non-metallic mineral processing and preparation of environment-friendly flame-retardant functional materials.
Background
The halogen-free, high-efficiency, smoke-eliminating, low-toxicity and multifunctional environment-friendly inorganic flame retardant is the mainstream direction for the development of new flame-retardant materials, and can effectively improve the flame retardance of the materials and reduce the release amount of smoke and toxic gases. Research shows that in the flame-retardant process of magnesium hydroxide, a formed polymer carbonization zone can effectively inhibit combustion; the decomposed product magnesium oxide is a high-temperature-resistant substance, and the magnesium oxide covers the surface of the high polymer, so that the air isolation efficiency can be greatly improved, and the effect of further preventing combustion is achieved. The magnesium hydroxide has high decomposition temperature, soft texture and fine granularity, and is suitable for the processing requirement of polymers. When the particle size of the hydroxide flame retardant is reduced to 1um, the oxygen index of the flame retardant polymer system is obviously improved, and the inorganic compound with the micro-nano superfine particle size is achieved, so that the effect of strengthening and toughening the polymer material can be achieved. Along with the ultra-fining of the substance, the electronic structure and the crystal structure on the surface are changed, and the surface effect, the small-size effect, the volume effect, the quantum effect and the macroscopic quantum effect which are not possessed by a macroscopic object are generated, so that the ultra-fine powder has a series of excellent special properties in the aspects of light, electricity, sound, magnetism, heat, mechanics, catalysis and the like compared with the conventional particle material.
In consideration of economic benefit, resource utilization, flame-retardant smoke-eliminating effect, environmental protection and the like, the magnesium hydroxide is selected as the composite material flame retardant, and the composite material has the competitive advantages of rich resources and relatively low production cost. The preparation technology of the superfine magnesium hydroxide can be mainly divided into two categories: physical methods and chemical methods. The physical method is that natural brucite ore is ground into powder, and mutual grinding and impact between medium and material are used to obtain superfine particles. The flame retardant has the defects of simple processing, more impurities, large and irregular particle size and poor flame retardant effect when being applied to the field of flame retardance. The chemical preparation methods are various, most of the chemical preparation methods take alkaline substances as a precipitator and magnesium salts as reaction raw materials, and the magnesium oxide with different particle sizes is prepared through precipitation reaction.
Disclosure of Invention
The invention uses magnesite tailings as raw materials, the tailings are calcined at low temperature, magnesium carbonate is decomposed into solid mineral light-burned magnesium, the main component of the light-burned magnesium is active magnesium oxide, also called light-burned magnesium powder, the light-burned magnesium powder is ground and hydrated to generate sheet crystal magnesium hydroxide, and the sheet crystal magnesium hydroxide is dried and cleaved to obtain the micro-nano magnesium hydroxide flame retardant. The method develops a unique method for tailings, saves and utilizes mineral resources, improves the added value of the light-burned magnesium powder product, has simple process design and easily controlled parameters, and is suitable for large-scale production.
The invention provides a method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method, which comprises the following steps: crushing magnesite tailings serving as a raw material to 10-20mm, adding magnesium chloride hexahydrate with the weight of 1-2% of that of the magnesite tailings, uniformly mixing, and calcining at 650-750 ℃ for 0.5-1.5h to obtain active light-burned magnesium; grinding the active light-burned magnesium to 100-325 meshes, and then mixing the active light-burned magnesium and water according to the weight ratio of 1:2-4, uniformly mixing to obtain magnesium hydroxide slurry; adding ethylene glycol into the magnesium hydroxide slurry according to 0.07-0.50% of the weight of the active light-burned magnesium, grinding according to 2-3 grades, adding a modifier which is 0.2-0.4% of the weight of the active light-burned magnesium into the ground magnesium hydroxide slurry at 60-70 ℃, and hydrating for 4-8 hours; and drying and cleaving the hydrated magnesium hydroxide slurry to obtain the active micro-nano magnesium hydroxide.
It is further preferred according to the invention that the magnesite tailings are crushed to 12-18 mm.
Most preferably according to the invention the weight of the magnesium chloride hexahydrate is 1.5% of the weight of the magnesite tailings.
The calcination temperature of 680-720 ℃ is further preferred.
The calcination time is further preferably 1 hour.
Most preferably, the activated soft burned magnesium is ground to 200 mesh.
The invention most preferably adopts the following steps that the weight ratio of the active light-burned magnesium to water is 1: 3, mixing evenly.
Most preferably, the ethylene glycol is added to the magnesium hydroxide slurry at 0.30% by weight of the active light-burned magnesium.
The invention preferably selects MgCO in the magnesite tailings3The content of the magnesite tailing is more than 50 percent, and impurities are removed from the magnesite tailing through mineral separation.
The conditions of the calcination in the present invention are preferably: the temperature rising speed is 2-8 ℃/min.
The temperature rise rate is most preferably 5 ℃/min.
The active light-burned magnesium is preferably screened by 20-40 meshes.
Most preferably, the activated soft burned magnesium is sieved by 30 meshes.
The invention preferably mixes the active light-burned magnesium and water, and then stirs for 1-2h at 60-80 rpm.
Most preferably, the activated soft burned magnesium is mixed with water and then stirred at a speed of 70 rpm.
Most preferably, the activated soft-burned magnesium is mixed with water and stirred for 1.5 h.
The magnesium hydroxide slurry and ethylene glycol are preferably mixed uniformly, filtered and pumped into a grinding stripping machine, the lining of a cylinder of the grinding stripping machine is polyurethane resin or corundum, and a zirconia sphere or corundum sphere is used as a grinding stripping medium.
The grinding conditions of the grade 2 are preferably as follows: the granularity of the grade 1 grinding medium is 2-3mm, the adding amount of the grinding medium is 20-40% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation number of the grinding and stripping machine is 1300-1400 rpm; the granularity of the 2 nd-grade grinding medium is 0.1-0.5mm, the adding amount of the grinding medium is 40-60% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation speed of the grinding and stripping machine is 1600-1700 rpm; or the grinding conditions of grade 3 are: the granularity of the grade 1 grinding medium is 2-3mm, the adding amount of the grinding medium is 20-40% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation number of the grinding and stripping machine is 1300-1400 rpm; the granularity of the 2 nd-grade grinding medium is 0.6-1.5mm, the adding amount of the grinding medium is 30-50% of the weight of the magnesium hydroxide slurry in the grinding stripping machine, and the rotation number of the grinding stripping machine is 1450-1550 rpm; the grain size of the 3 rd-grade grinding medium is 0.1-0.5mm, the adding amount of the grinding medium is 40-60% of the weight of the magnesium hydroxide slurry in the grinding stripping machine, and the rotation speed of the grinding stripping machine is 1600-1700 rpm.
Most preferably, the invention is that the addition amount of the grade 1 grinding medium in the grade 2 grinding conditions is 30% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine
Most preferably according to the invention, the stage 2 grinding media is added in the stage 2 grinding conditions in an amount of 50% by weight of the magnesium hydroxide slurry in the mill stripper.
Most preferably according to the invention, the stage 1 grinding media is added to the stage 3 grinding conditions in an amount of 30% by weight of the magnesium hydroxide slurry in the mill stripper.
Most preferably according to the invention, the stage 2 grinding media is added to the stage 3 grinding conditions in an amount of 40% by weight of the magnesium hydroxide slurry in the mill stripper.
Most preferably according to the invention, the 3 rd stage grinding media is added in the 3 rd stage grinding conditions in an amount of 50% by weight of the magnesium hydroxide slurry in the mill stripper.
In the invention, the modifier is preferably a silane coupling agent or a titanate coupling agent.
The invention preferably dries and breaks up the hydrated magnesium hydroxide slurry in a cleavage machine, the atomization pressure is 4-8MPa, and the drying temperature is 260-300 ℃.
The invention has the beneficial effects that:
according to the invention, the light-burned magnesium hydration reaction is utilized to prepare the micro-nano magnesium hydroxide flame retardant, so that tailing resources are fully utilized, and the concept of sustainable development is met;
the invention adopts a multistage grinding process, the granularity is controlled to be ultra-fine, and excellent quantum effect and surface effect are generated along with the change of a crystal structure;
the invention solves the technical problems of secondary condensation, adhesion and the like during drying through surface activation, and simultaneously activates the surface of the flame retardant powder from hydrophilicity to lipophilicity, thereby improving the intermiscibility and the dispersibility of the flame retardant powder in a high polymer material.
Drawings
In the figure 2 of the attached drawings of the invention,
FIG. 1 is an SEM image of an active micro-nano magnesium hydroxide flame retardant prepared by the chemical method described in example 1;
FIG. 2 is an SEM image of an active micro-nano magnesium hydroxide flame retardant prepared by the chemical method described in example 2.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
In the following examples, the measurement of each index was as follows:
observing the crystal morphology by using a Scanning Electron Microscope (SEM) and a FEISIrion200 (Philips);
the average particle size of the sample was measured using a laser particle size analyzer (BT-9300S) from Dandong Baite instruments Ltd.
Example 1
A method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method comprises the following steps:
taking MgCO3Magnesite tailings with the content of 58 percent are used as raw materials, impurities such as gangue and the like are removed from the raw materials through primary manual mineral separation, the separated raw materials are crushed into particles with the particle size of 10-20mm, magnesium chloride hexahydrate with the weight of 2 percent of the weight of the magnesite tailings is added and mixed evenly, the mixture is heated in a kiln at the speed of 5 ℃/min and calcined at the temperature of 700 ℃ for 1h to obtain active light-burned magnesium, the active light-burned magnesium is screened by a 60-mesh sieve, and CaCO which is not chemically decomposed is removed3And impurities such as silicate, and the like, and further purifying;
grinding the active light-burned magnesium to 200 meshes, and stirring the active light-burned magnesium and water in a stirring tank according to the weight ratio of 1:2, mixing and stirring at 80rpm for 1h to obtain magnesium hydroxide slurry;
adding ethylene glycol as dispersant in 0.1 wt% of active light burned magnesium into magnesium hydroxide slurry, mixing to reduce adhesive agglomeration, filtering, purifying, grinding and stripping with polyurethane resin as the lining of the barrel to prevent pollution, grinding in three stages with zirconia ball as grinding and stripping medium, the first stage with granularity of 2-3mm, the first stage with granularity of 40 wt% of magnesium hydroxide slurry, the third stage with granularity of 0.1-0.5mm, the second stage with granularity of 0.6-1.5mm, the third stage with granularity of 50 wt% of magnesium hydroxide slurry, the rotation number of the grinding stripping machine is 1700rpm, the ground magnesium hydroxide slurry is added with a silane coupling agent with the weight of 0.3 percent of that of the active light-burned magnesium at the temperature of 60 ℃, the mixture is stirred at 120rpm, and the hydration time is 8 hours;
and (3) carrying out spray drying and cleavage on the hydrated magnesium hydroxide slurry in a cleavage machine, wherein the atomization pressure is 8MPa, and the drying temperature is 280 ℃, so as to obtain the active micro-nano magnesium hydroxide.
An SEM image of the active micro-nano magnesium hydroxide flame retardant prepared by the chemical method in example 1 is shown in figure 1, and the particle size detection D50-240 nm and D90-0.47 um are shown in the figure.
Example 2
A method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method comprises the following steps:
taking MgCO3Magnesite tailings with the content of 68% are used as raw materials, impurities such as gangue and the like are removed from the raw materials through primary manual mineral separation, the separated raw materials are crushed into particles with the particle size of 10-20mm, magnesium chloride hexahydrate with the weight of 1% of the magnesite tailings is added and mixed evenly, the mixture is heated in a kiln at the speed of 5 ℃/min and calcined at the temperature of 650 ℃ for 0.5h to obtain active light-burned magnesium, the active light-burned magnesium is screened by a 60-mesh sieve, and CaCO which is not chemically decomposed is removed3And impurities such as silicate, and the like, and further purifying;
grinding the active light-burned magnesium to 200 meshes, and stirring the active light-burned magnesium and water in a stirring tank according to the weight ratio of 1:2, mixing and stirring at 60rpm for 2 hours to obtain magnesium hydroxide slurry;
adding ethylene glycol as a dispersing agent into magnesium hydroxide slurry according to 0.3 percent of the weight of the active light burned magnesium, uniformly mixing to reduce the phenomenon of bonding agglomeration, purifying by a filter screen, pumping into a grinding stripping machine, wherein the lining of a cylinder body of the grinding stripping machine is corundum to prevent pollution, taking a corundum sphere as a grinding stripping medium, grinding according to a second stage, the granularity of a first-stage grinding stripping medium is unequal to 2-3mm, the adding amount of the first-stage grinding stripping medium is 30 percent of the weight of the magnesium hydroxide slurry in the grinding stripping machine, the revolution of the grinding stripping machine is 1400rpm, the granularity of a second-stage grinding stripping medium is unequal to 0.1-0.5mm, the adding amount of the second-stage grinding stripping medium is 50 percent of the weight of the magnesium hydroxide slurry in the grinding stripping machine, the revolution of the grinding stripping machine is 1600rpm, adding a titanate coupling agent with the weight of the active light burned magnesium at 70 ℃, stirring at 120rpm, and hydrating for 4 hours;
and (3) carrying out spray drying and cleavage on the hydrated magnesium hydroxide slurry in a cleavage machine, wherein the atomization pressure is 4MPa, and the drying temperature is 260 ℃, so as to obtain the active micro-nano magnesium hydroxide.
An SEM image of the active micro-nano magnesium hydroxide flame retardant prepared by the chemical method in example 2 is shown in figure 2, and the particle size detection D50-0.48 um and D90-97 um are shown in the figure.
Claims (7)
1. A method for preparing an active micro-nano magnesium hydroxide flame retardant by a chemical method is characterized by comprising the following steps: the method comprises the following steps:
crushing magnesite tailings serving as a raw material to 10-20mm, adding magnesium chloride hexahydrate with the weight of 1-2% of that of the magnesite tailings, uniformly mixing, and calcining at the temperature of 650-8 ℃/min and 750 ℃ for 0.5-1.5h to obtain active light-burned magnesium;
grinding the active light-burned magnesium to be 100-325 meshes, and uniformly mixing the active light-burned magnesium and water according to the weight ratio of 1:2-4 to obtain magnesium hydroxide slurry;
adding ethylene glycol into the magnesium hydroxide slurry according to 0.07-0.50 percent of the weight of the active light-burned magnesium, and grinding according to 2-3 grades, wherein the grinding conditions of the 2 grades are as follows: the granularity of the grade 1 grinding medium is 2-3mm, the adding amount of the grinding medium is 20-40% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation number of the grinding and stripping machine is 1300-1400 rpm;
the granularity of the 2 nd-grade grinding medium is 0.1-0.5mm, the adding amount of the grinding medium is 40-60% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation speed of the grinding and stripping machine is 1600-1700 rpm;
or the grinding conditions of grade 3 are:
the granularity of the grade 1 grinding medium is 2-3mm, the adding amount of the grinding medium is 20-40% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation number of the grinding and stripping machine is 1300-1400 rpm;
the granularity of the 2 nd-grade grinding medium is 0.6-1.5mm, the adding amount of the grinding medium is 30-50% of the weight of the magnesium hydroxide slurry in the grinding stripping machine, and the rotation number of the grinding stripping machine is 1450-1550 rpm;
the granularity of the 3 rd-grade grinding medium is 0.1-0.5mm, the adding amount of the grinding medium is 40-60% of the weight of the magnesium hydroxide slurry in the grinding and stripping machine, and the rotation speed of the grinding and stripping machine is 1600-1700 rpm;
adding modifier with the weight of 0.2-0.4% of that of the active light-burned magnesium into the ground magnesium hydroxide slurry at the temperature of 60-70 ℃ for hydration for 4-8 h;
and drying and cleaving the hydrated magnesium hydroxide slurry to obtain the active micro-nano magnesium hydroxide.
2. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 1, wherein the method is characterized in that: MgCO in magnesite tailings3The content of the magnesite tailing is more than 50 percent, and impurities are removed from the magnesite tailing through mineral separation.
3. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 2 is characterized in that: and screening the active light burned magnesium by 20-40 meshes.
4. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 3, which is characterized in that: mixing the active light-burned magnesium with water, and stirring at 60-80rpm for 1-2 h.
5. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 4, which is characterized in that: and uniformly mixing the magnesium hydroxide slurry with ethylene glycol, filtering, and pumping into a grinding stripping machine, wherein the lining of a cylinder of the grinding stripping machine is made of polyurethane resin or corundum, and a zirconia sphere or corundum sphere is used as a grinding stripping medium.
6. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 5, which is characterized in that: the modifier is a silane coupling agent or a titanate coupling agent.
7. The method for preparing the active micro-nano magnesium hydroxide flame retardant by the chemical method according to claim 6, which is characterized in that: drying and scattering the hydrated magnesium hydroxide slurry in a cleavage machine, wherein the atomization pressure is 4-8MPa, and the drying temperature is 260-300 ℃.
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