CN113929120A - Preparation method of magnesium hydroxide material - Google Patents
Preparation method of magnesium hydroxide material Download PDFInfo
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- CN113929120A CN113929120A CN202111296843.7A CN202111296843A CN113929120A CN 113929120 A CN113929120 A CN 113929120A CN 202111296843 A CN202111296843 A CN 202111296843A CN 113929120 A CN113929120 A CN 113929120A
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- magnesium hydroxide
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 170
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 170
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 170
- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000011268 mixed slurry Substances 0.000 claims abstract description 102
- 239000002994 raw material Substances 0.000 claims abstract description 48
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 46
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 33
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 235000002639 sodium chloride Nutrition 0.000 claims abstract description 25
- 239000011780 sodium chloride Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 23
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 239000001103 potassium chloride Substances 0.000 claims abstract description 15
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 15
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 11
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 8
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims description 35
- 239000000047 product Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 22
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 22
- 229920000058 polyacrylate Polymers 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 239000007858 starting material Substances 0.000 claims 2
- 238000011085 pressure filtration Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 19
- 230000008569 process Effects 0.000 abstract description 8
- 238000006011 modification reaction Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 45
- 239000000243 solution Substances 0.000 description 27
- 239000013078 crystal Substances 0.000 description 20
- 239000000126 substance Substances 0.000 description 17
- 230000002776 aggregation Effects 0.000 description 15
- 238000005054 agglomeration Methods 0.000 description 14
- 230000000694 effects Effects 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 12
- 230000004048 modification Effects 0.000 description 12
- 238000012986 modification Methods 0.000 description 12
- 239000002002 slurry Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000010335 hydrothermal treatment Methods 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 8
- 238000012216 screening Methods 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- -1 wastewater treatment Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 229920002319 Poly(methyl acrylate) Polymers 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000051 modifying effect Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005614 potassium polyacrylate Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of a magnesium hydroxide material, which comprises the following steps: preparing mixed slurry containing a magnesium hydroxide raw material and a viscosity regulator; carrying out hydrothermal reaction treatment on the mixed slurry, and carrying out filtering treatment, washing treatment and drying treatment after the reaction is finished to prepare a magnesium hydroxide product; wherein the viscosity regulator is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate. The viscosity regulator added in the invention can reduce the viscosity of the mixed slurry formed in the hydrothermal modification reaction process of the magnesium hydroxide, thereby increasing the concentration of the magnesium hydroxide raw material in the mixed slurry and improving the production efficiency of the unit volume of equipment.
Description
Technical Field
The invention relates to the technical field of magnesium hydroxide materials, in particular to a preparation method of a magnesium hydroxide material.
Background
Magnesium hydroxide is an important multifunctional material and is widely applied to fire retardants, wastewater treatment, flue gas desulfurization, heavy metal removal, preservatives, medicaments and the like. As a novel high-efficiency, superior and environment-friendly additive inorganic flame retardant, magnesium hydroxide is greatly developed in the field of inorganic flame retardants and is widely applied to the polymer material industry. The preparation method of magnesium hydroxide can be divided into a physical method and a chemical synthesis method according to the state: physical methods represent brucite processing; the chemical synthesis method is to react raw materials containing magnesium ions with alkali substances in different reaction systems to generate magnesium hydroxide, and mainly comprises a lime milk method, a sodium hydroxide method, an ammonia method, a reverse precipitation method, a hydration method and the like. The magnesium hydroxide prepared by the existing method has poor crystal form and serious agglomeration, and the application of the magnesium hydroxide is seriously influenced.
The existing method for improving the crystal form and the agglomeration of the magnesium hydroxide is realized by hydrothermal treatment or roasting-hydration. The hydrothermal treatment is a common method for improving the crystal form and agglomeration of magnesium hydroxide, and is generally performed by subjecting a slurry containing magnesium hydroxide and a crystal form converting agent (e.g., an alkaline substance such as sodium hydroxide or potassium hydroxide) to hydrothermal treatment under conditions of a certain hydrothermal temperature and stirring strength. When hydrothermal treatment is carried out, because the volume of the equipment and the maximum hydrothermal treatment volume of the equipment are fixed, in order to improve the production efficiency of the unit volume of the equipment, namely, more magnesium hydroxide products can be obtained after the equipment carries out hydrothermal treatment once, the content of magnesium hydroxide which is subjected to hydrothermal treatment each time needs to be increased, namely, the concentration of the magnesium hydroxide in the mixed slurry is increased. However, in the conventional hydrothermal reaction process, since the reaction slurry becomes thick after the magnesium hydroxide raw material reaches a certain concentration in the mixed slurry, the viscosity of the slurry is too high, and the production efficiency per unit volume of the equipment cannot be improved by continuously increasing the concentration of the magnesium hydroxide raw material in the mixed slurry.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a magnesium hydroxide material, so as to solve the problem of how to reduce the viscosity of slurry and thereby improve the production efficiency per unit volume of equipment.
In order to solve the problems, the invention adopts the following technical scheme:
a method of preparing a magnesium hydroxide material, comprising:
preparing mixed slurry containing a magnesium hydroxide raw material and a viscosity regulator;
carrying out hydrothermal reaction treatment on the mixed slurry, and carrying out filtering treatment, washing treatment and drying treatment after the reaction is finished to prepare a magnesium hydroxide product;
wherein the viscosity regulator is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate.
Preferably, the formulating a mixed slurry containing a magnesium hydroxide raw material and a viscosity modifier comprises:
preparing a viscosity regulator solution with the concentration of 0.1-5.0 mol/L;
firstly, putting a certain weight of magnesium hydroxide raw material into a reaction vessel, adding the viscosity regulator solution into the reaction vessel, and stirring and mixing to obtain the mixed slurry; or, the viscosity regulator solution is firstly placed in a reaction vessel, and then a certain weight of magnesium hydroxide raw material is added to be stirred and mixed, so as to obtain the mixed slurry;
wherein the magnesium hydroxide raw material with a certain weight is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 8.0% -50%.
More preferably, the concentration of the viscosity modifier solution is 0.5mol/L to 2.0mol/L, and the certain weight of the magnesium hydroxide raw material is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 15% to 25%.
Preferably, the magnesium hydroxide raw material is magnesium hydroxide powder, a magnesium hydroxide dry filter cake or a magnesium hydroxide wet filter cake.
Preferably, the hydrothermal reaction treatment comprises: and transferring the mixed slurry to a high-pressure reaction kettle, and carrying out hydrothermal reaction for 0.1-8 h under the conditions that the temperature is 100-220 ℃ and the stirring strength is 10-800 r/min.
Preferably, the filtration treatment is vacuum filtration treatment or filter pressing treatment; and/or the washing treatment is specifically washing with deionized water and then washing with ethanol; and/or in the drying treatment, the drying temperature is 100-140 ℃ and the drying time is 5-20 h.
Preferably, a dispersant is further added to the mixed slurry.
Preferably, the dispersant is a polyacrylate or polyacrylate.
Preferably, the amount of the dispersant added is 0.1 to 5.0% by weight of the magnesium hydroxide raw material.
More preferably, the amount of the dispersant added is 0.5 to 2.0% by weight of the magnesium hydroxide raw material.
According to the preparation method of the magnesium hydroxide material provided by the embodiment of the invention, the viscosity regulator is added before the hydrothermal modification treatment, the viscosity regulator is selected from one or more of sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate, and the added viscosity regulator can reduce the viscosity of the mixed slurry in the hydrothermal reaction process, so that the concentration of the magnesium hydroxide raw material in the mixed slurry can be increased, and the production efficiency of the unit volume of equipment is improved; in the process of further research, the viscosity regulator not only has the effect of reducing the viscosity of the mixed slurry, but also has a good effect of improving the morphology and the agglomeration of the magnesium hydroxide material, so that the preparation method of the magnesium hydroxide material provided by the embodiment of the invention does not need to additionally add other crystal form conversion agents.
Drawings
FIG. 1 is an SEM photograph of magnesium hydroxide powder No. 1 in example 1 of the present invention;
FIG. 2 is an SEM photograph of a magnesium hydroxide product A in example 1 of the present invention;
FIG. 3 is an SEM photograph of a magnesium hydroxide product B in example 1 of the present invention;
FIG. 4 is an SEM photograph of magnesium hydroxide powder No. 1 in example 2 of the present invention;
FIG. 5 is an SEM photograph of a magnesium hydroxide product C in example 2 of the present invention;
FIG. 6 is an SEM photograph of magnesium hydroxide powder No. 2 in example 3 of the present invention;
FIG. 7 is an SEM photograph of a magnesium hydroxide product in example 3 of the present invention;
FIG. 8 is an SEM image of the powder after grinding and sieving of the magnesium hydroxide No. 3 dry filter cake in example 4 of the invention;
FIG. 9 is an SEM photograph of a magnesium hydroxide product in example 4 of the present invention;
FIG. 10 is an SEM photograph of magnesium hydroxide powder No. 4 in example 5 of the present invention;
FIG. 11 is an SEM photograph of a magnesium hydroxide product of example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The embodiment of the invention provides a preparation method of a magnesium hydroxide material, which comprises the following steps:
step S10, preparing a mixed slurry containing a magnesium hydroxide raw material and a viscosity modifier.
And step S20, carrying out hydrothermal reaction treatment on the mixed slurry, and carrying out filtering treatment, washing treatment and drying treatment after the reaction is finished to prepare the magnesium hydroxide product.
In step S10, the viscosity modifier is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate, and potassium sulfate.
The applicant of the present invention has found through research that by adding a viscosity modifier selected from one or more of sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate before hydrothermal modification treatment, the viscosity of the mixed slurry can be reduced during hydrothermal reaction, and thus the concentration of the magnesium hydroxide raw material in the mixed slurry can be increased, thereby improving the production efficiency per unit volume of the equipment.
In the process of further research, the viscosity regulator not only has the effect of reducing the viscosity of the mixed slurry, but also has a good effect of improving the appearance and the agglomeration of the magnesium hydroxide material, can improve the crystal form of the magnesium hydroxide product, enables the finally obtained magnesium hydroxide product to have good appearance, and can also reduce the agglomeration of the product and improve the dispersibility. Therefore, the preparation method of the magnesium hydroxide material provided in the embodiment of the invention does not need to additionally add other crystal form converting agents (for example, alkaline converting agents such as sodium hydroxide and potassium hydroxide commonly used in the prior art).
Further, based on the viscosity regulator having a good effect of improving the morphology and the agglomeration of the magnesium hydroxide material, the technical solution provided in the embodiment of the present invention has the following advantages:
in some existing technical schemes, in order to enable the prepared magnesium hydroxide product to have a better appearance, an alkaline substance (such as sodium hydroxide and potassium hydroxide) is added as a crystal transformation agent before hydrothermal treatment, and then hydrothermal treatment is performed, however, the alkaline substance added with sodium hydroxide or potassium hydroxide has strong corrosivity on equipment, and the alkaline substance is usually very high in price, so that the method is limited to be used in large scale in industry. The viscosity regulator (specifically sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate or potassium sulfate) used in the invention is a neutral substance, and has low corrosivity and low price, so that the preparation method of the magnesium hydroxide material provided by the invention is more suitable for large-scale industrial production.
In a specific embodiment, the step S10 may be: firstly, preparing a viscosity regulator solution with the concentration of 0.1-5.0 mol/L; then putting a certain weight of magnesium hydroxide raw material into a reaction vessel, adding the viscosity regulator solution into the reaction vessel, and stirring and mixing to obtain the mixed slurry; or the viscosity regulator solution is firstly placed in a reaction vessel, and then a certain weight of magnesium hydroxide raw material is added to be stirred and mixed, so as to obtain the mixed slurry. Wherein the magnesium hydroxide raw material with a certain weight is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 8.0% -50%.
The concentration of the viscosity modifier solution is, for example, 0.1mol/L, 0.2mol/L, 0.5mol/L, 0.8mol/L, 1.0mol/L, 1.2mol/L, 1.5mol/L, 1.8mol/L, 2.0mol/L, 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L, 4.5mol/L or 5.0mol/L, and is preferably controlled within a range of 0.5mol/L to 2.0 mol/L.
The mass concentration of the magnesium hydroxide raw material in the mixed slurry is, for example, 8.0%, 10%, 12%, 15%, 18%, 20%, 25%, 30%, 35%, 40%, 45%, or 50%, and preferably, is controlled to be in the range of 15% to 25%.
Wherein the magnesium hydroxide raw material is magnesium hydroxide powder, a magnesium hydroxide dry filter cake or a magnesium hydroxide wet filter cake and other magnesium hydroxide raw materials with any properties.
In a further preferred embodiment, a dispersant is further added to the mixed slurry obtained by the preparation in step S10. The dispersant is preferably a polyacrylate salt or polyacrylate, for example, polyacrylate salts such as sodium polyacrylate, potassium polyacrylate, aluminum polyacrylate, and ammonium polyacrylate, or polyacrylate esters such as polymethyl acrylate and polyethyl acrylate. By adding the dispersant, the viscosity of the mixed slurry can be further reduced, and the concentration of the magnesium hydroxide raw material in the mixed slurry can be further increased, thereby improving the production efficiency per unit volume of the equipment.
In a preferred embodiment, the amount of the dispersant added is 0.1% to 5% by mass of the magnesium hydroxide raw material, for example, 0.1%, 0.2%, 0.5%, 0.8%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, or 5.0%, and preferably, is controlled within a range of 0.5% to 2.0%.
In a specific embodiment, in step S20:
the hydrothermal reaction treatment comprises the following steps: and transferring the mixed slurry to a high-pressure reaction kettle, and carrying out hydrothermal reaction for 0.1-8 h under the conditions that the temperature is 100-220 ℃ and the stirring strength is 10-800 r/min.
The filtration treatment is vacuum filtration treatment or filter pressing treatment.
The washing treatment is specifically washing with deionized water and/or washing with ethanol. For example, deionized water 3 to 7 times the dry weight of magnesium hydroxide and ethanol 1 to 2 times the dry weight of magnesium hydroxide are used for washing 3 to 7 times and 0 to 1 time.
In the drying treatment, the drying temperature is 100-140 ℃ and the drying time is 5-20 h. Further, after drying, the magnesium hydroxide product with a predetermined size range is obtained by screening.
When preparing the mixed slurry in step S10, the solvent is selected to be water; more preferably, the mixed slurry is prepared by using the filtrate obtained by the filtration treatment in step S20 and the washing liquid obtained by the washing treatment as solvents.
Example 1
Preparing a sodium chloride solution with the concentration of 1.0mol/L, namely, taking a neutral substance sodium chloride as a viscosity regulator; adding 340g of No. 1 magnesium hydroxide powder into a reactor, weighing 1660g of the sodium chloride solution, pouring into the reactor, and stirring and mixing to obtain mixed slurry A. Wherein the mass concentration of magnesium hydroxide in the mixed slurry A is 17%.
And transferring the mixed slurry A in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 160 ℃ and the stirring strength of 300r/min for 3 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 428mPa · s.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product A.
The following comparative experiments were also performed in this example:
comparative experiment 1: preparing a sodium hydroxide solution with the concentration of 0.75mol/L, namely, according to the existing technical scheme for preparing the magnesium hydroxide material, taking an alkaline substance sodium hydroxide as a crystal transformation agent; adding 320g of No. 1 magnesium hydroxide powder into a reactor, weighing 1680g of the sodium hydroxide solution, pouring the sodium hydroxide solution into the reactor, and stirring and mixing to obtain mixed slurry B. Wherein the mass concentration of the magnesium hydroxide in the mixed slurry B is 16%.
And transferring the mixed slurry B in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 160 ℃ and the stirring strength of 300r/min for 3 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 690 mPas.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product B.
The following table 1 is collated according to the mass concentration of magnesium hydroxide in the above examples and the data of viscosity parameters of the mixed slurry obtained by the test.
TABLE 1
| Mixed slurry A | Mixed slurry B | |
| Magnesium hydroxide mass concentration (%) | 17 | 16 |
| Viscosity (mPa. s) of mixed slurry after reaction | 428 | 690 |
As can be seen from comparison of the data in table 1, in the case where the basic substance sodium hydroxide is added as the crystal form conversion agent in the prior art scheme (comparative experiment 1), the viscosity of the mixed slurry at the completion of the hydrothermal reaction is higher in the case where the mass concentration of magnesium hydroxide is relatively lower (16%). In the scheme provided by the invention, sodium chloride is added as a viscosity regulator, so that the viscosity of the mixed slurry is lower when the hydrothermal reaction is finished under the condition that the mass concentration of magnesium hydroxide is higher (17%), and the viscosity is reduced by about 38%. It can also be understood that the sodium chloride is added as a viscosity regulator in the scheme provided by the invention, and the mass concentration of the magnesium hydroxide raw material in the mixed slurry can reach a higher level under the condition that the viscosity of the mixed slurry is the same, so that the production efficiency of unit volume of equipment is improved, and the production cost is reduced.
The shapes of the magnesium hydroxide raw material used in this example and the magnesium hydroxide product obtained by the preparation were observed using a Scanning Electron Microscope (SEM): FIG. 1 is an SEM photograph of raw material No. 1 magnesium hydroxide powder used in this example, FIG. 2 is an SEM photograph of a magnesium hydroxide product A obtained in this example, and FIG. 3 is an SEM photograph of a magnesium hydroxide product B obtained in this example.
As can be seen from comparison between fig. 2 and fig. 1, in this example, sodium chloride as a viscosity modifier can also modify the magnesium hydroxide raw material, has a good modification effect on the crystal form and the agglomeration property of magnesium hydroxide, can be modified to obtain a hexagonal flaky magnesium hydroxide product, and has good dispersibility. As shown in fig. 3, when the alkaline substance sodium hydroxide is used as the crystal transformation agent in the prior art, the modification effect on the crystal form and the agglomeration of magnesium hydroxide is good.
Example 2
Preparing a sodium chloride solution with the concentration of 2.0mol/L, namely, taking a neutral substance sodium chloride as a viscosity regulator; adding 340g of No. 1 magnesium hydroxide powder into a reactor, weighing 1654.9g of the sodium chloride solution, pouring the sodium chloride solution into the reactor, stirring and mixing, adding 5.1g of ammonium polyacrylate serving as a dispersing agent, and continuously stirring and mixing to obtain mixed slurry C. Wherein the mass concentration of magnesium hydroxide in the mixed slurry C is 17%, and the addition amount of ammonium polyacrylate as a dispersant is 1.5% of the mass of the magnesium hydroxide powder.
And transferring the mixed slurry C in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 160 ℃ and the stirring strength of 500r/min for 3 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 35mPa · s.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product C.
The following comparative experiments were also performed in this example:
comparative experiment 2: on the basis of comparative experiment 1, the same proportion of dispersant was added in the manner referred to above in example 2 to verify the effect of the dispersant on the slurry concentration. The method comprises the following specific steps:
preparing a sodium hydroxide solution with the concentration of 0.75mol/L, namely, according to the existing technical scheme for preparing the magnesium hydroxide material, taking an alkaline substance sodium hydroxide as a crystal transformation agent; adding 320g of No. 1 magnesium hydroxide powder into a reactor, weighing 1675.2g of the sodium hydroxide solution, pouring the sodium hydroxide solution into the reactor, stirring and mixing, adding 4.8g of ammonium polyacrylate serving as a dispersing agent, and continuously stirring and mixing to obtain mixed slurry D. Wherein the mass concentration of magnesium hydroxide in the mixed slurry D is 16%, and the addition amount of ammonium polyacrylate as a dispersant is 1.5% of the mass of the magnesium hydroxide powder.
And transferring the mixed slurry D in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 160 ℃ and the stirring strength of 300r/min for 3 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 508mPa · s.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product D.
Example 2 compared to example 1, the main differences are: the viscosity of the mixed slurry after completion of the hydrothermal reaction in example 2 was reduced to 35mPa · s by adjusting the process conditions as described above by adding 1.5% of a dispersant to the mixed slurry. Comparative experiment 2 compared to comparative experiment 1, the main differences are: the viscosity of the mixed slurry after completion of the hydrothermal reaction in comparative experiment 2 was reduced to 508mPa · s based on the adjustment of the process conditions by adding 1.5% of the dispersant to the mixed slurry.
The viscosity data of the mixed slurry obtained based on the above tests can be summarized as follows:
(1) in both the technical solutions proposed by the present invention and the prior art, the viscosity of the mixed slurry after completion of the hydrothermal reaction can be reduced by adding a certain amount of the dispersant to the mixed slurry.
(2) The mixed slurry a of example 1 had a lower viscosity after completion of the reaction than the mixed slurry D of comparative experiment 2. As can be seen, when the viscosity modifier is used in the embodiment of the present invention, the viscosity of the mixed slurry at the completion of the hydrothermal reaction is lower than that in the prior art in which a dispersant is further added, even if no dispersant is added.
(3) The viscosity of the mixed slurry C of example 2 was reduced from 428mPa · s to 35mPa · s after the completion of the reaction, as compared with the mixed slurry a of example 1, and the extent of the reduction in viscosity reached 90% or more; the viscosity of the mixed slurry D of comparative experiment 2 was reduced from 690mPa · s to 508mPa · s after the completion of the reaction, compared to the mixed slurry B of comparative experiment 1, and the reduction in viscosity was about 26%.
As described above, according to the conventional technique, the viscosity of the mixed slurry after completion of the hydrothermal reaction can be reduced even after a certain amount of the dispersant is added, but in the technique of the present invention, the viscosity of the mixed slurry after completion of the hydrothermal reaction can be greatly reduced by the synergistic viscosity reducing effect of the viscosity modifier and the dispersant after the certain amount of the dispersant is added to the mixed slurry, and the production efficiency per unit volume of the facility can be further improved.
The morphology of the magnesium hydroxide raw material used in example 2 and the magnesium hydroxide product C obtained by preparation was observed using a scanning electron microscope: FIG. 4 is an SEM photograph of raw material No. 1 magnesium hydroxide powder used in this example, and FIG. 5 is an SEM photograph of product C of magnesium hydroxide obtained in this example.
Comparing fig. 5 and fig. 4, it can be seen that the addition of the neutral substance sodium chloride as the viscosity modifier and the addition of the dispersant in this example has a better modification effect on the crystal form and the agglomeration property of magnesium hydroxide.
Example 3
Preparing a mixed solution of potassium chloride with the concentration of 0.5mol/L and magnesium sulfate with the concentration of 0.5mol/L, namely, taking neutral substances of potassium chloride and magnesium sulfate as viscosity regulators; adding 200g of No. 2 magnesium hydroxide powder into a reactor, weighing 1800g of the mixed solution, pouring into the reactor, and stirring and mixing to obtain mixed slurry. Wherein the mass concentration of the magnesium hydroxide in the mixed slurry is 10%.
And transferring the mixed slurry in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 140 ℃ and the stirring strength of 500r/min for 5 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 185mPa · s. The viscosity of the mixed slurry is low when the hydrothermal reaction is finished, so that the production efficiency of the unit volume of the equipment can be improved, and the production cost can be reduced.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product.
FIG. 6 is an SEM photograph of raw material No. 2 magnesium hydroxide powder used in this example, and FIG. 7 is an SEM photograph of a magnesium hydroxide product produced in this example.
As can be seen from comparison between fig. 7 and fig. 6, the mixture of potassium chloride and magnesium sulfate as the viscosity modifier in this example can also modify the magnesium hydroxide raw material, and has a better modification effect on the crystal form and the agglomeration property of magnesium hydroxide.
Example 4
Preparing a potassium chloride solution with the concentration of 0.5mol/L, namely, taking a neutral substance potassium chloride as a viscosity regulator; adding 400g of No. 3 magnesium hydroxide dry filter cake into a reactor, weighing 1596g of potassium chloride solution, pouring into the reactor, stirring and mixing, adding 4g of ammonium polyacrylate serving as a dispersing agent, and continuously stirring and mixing to obtain mixed slurry. Wherein the mass concentration of magnesium hydroxide in the mixed slurry is 20%, and the addition amount of ammonium polyacrylate as a dispersant is 1.0% of the mass of the magnesium hydroxide powder.
And transferring the mixed slurry in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 180 ℃ and the stirring strength of 600r/min for 1 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 32mPa · s. In this example, a certain amount of the dispersant was added to greatly reduce the viscosity of the mixed slurry, thereby further improving the production efficiency per unit volume of the apparatus.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product.
FIG. 8 is an SEM picture of the powder of the dry filter cake No. 3 magnesium hydroxide used in this example after grinding and sieving, and FIG. 9 is an SEM picture of the magnesium hydroxide product prepared in this example.
Comparing fig. 9 and 8, it can be seen that the addition of potassium chloride, which is a neutral substance as a viscosity modifier, and the addition of a dispersant in this example has a better modification effect on the crystal form and the agglomeration property of magnesium hydroxide.
Example 5
Preparing a sodium chloride solution with the concentration of 2mol/L, namely, taking a neutral substance sodium chloride as a viscosity regulator; adding 280g of No. 4 magnesium hydroxide powder into a reactor, weighing 1720g of the sodium chloride solution, pouring into the reactor, and stirring and mixing to obtain mixed slurry. Wherein the mass concentration of the magnesium hydroxide in the mixed slurry is 14%.
And transferring the mixed slurry in the reactor to a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 160 ℃ and the stirring strength of 500r/min for 3 h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 133mPa · s. The viscosity of the mixed slurry is low when the hydrothermal reaction is finished, so that the production efficiency of the unit volume of the equipment can be improved, and the production cost can be reduced.
And after the hydrothermal reaction is finished, sequentially filtering, washing, drying and screening the magnesium hydroxide slurry to obtain a magnesium hydroxide product.
FIG. 10 is an SEM photograph of raw material No. 4 magnesium hydroxide powder used in this example, and FIG. 11 is an SEM photograph of a magnesium hydroxide product produced in this example.
As can be seen from a comparison of fig. 11 and 10, sodium chloride as a viscosity modifier in this example can also modify the magnesium hydroxide raw material, and has a good modifying effect on the crystal form and the aggregation property of magnesium hydroxide.
In the technical solutions of the above embodiments 1 to 5, the embodiments 1, 3 and 5 are only added with the viscosity modifier, and the embodiments 2 and 4 are added with the dispersant in addition to the viscosity modifier. Comparing the viscosity test results of example 1, example 3 and example 5 with the test results of example 2 and example 4, it can be known that: the dispersant is further added on the basis of the viscosity regulator, so that the viscosity of the mixed slurry can be better reduced when the hydrothermal reaction is finished, and the production efficiency of the unit volume of equipment can be further improved. Comparing the SEM images of the product obtained from example 1 with those of the product obtained from example 2, it can be seen that: the dispersant is further added on the basis of the viscosity regulator, and the modification effect on the crystal form and the agglomeration property of the magnesium hydroxide is not as good as that of the technical scheme only adding the viscosity regulator.
Therefore, the preparation method of the magnesium hydroxide material provided in the embodiment of the invention comprises the following steps: if the magnesium hydroxide product with high quality and morphology is required to be obtained while the production efficiency is improved, only the viscosity regulator is added; if the modification requirement for the magnesium hydroxide product is lowered in order to require higher production efficiency, a certain amount of dispersant is further added in addition to the viscosity modifier.
In summary, in the preparation method of the magnesium hydroxide material provided in the embodiment of the present invention, the viscosity modifier is added before the hydrothermal modification treatment, and the viscosity modifier is selected from one or more of sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate, and potassium sulfate, and the added viscosity modifier can reduce the viscosity of the mixed slurry in the hydrothermal reaction process, so that the concentration of the magnesium hydroxide raw material in the mixed slurry can be increased, thereby improving the production efficiency of the unit volume of the equipment, and the used viscosity modifier has a good modification effect on the crystal form and the agglomeration property of the magnesium hydroxide.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (10)
1. A method for preparing a magnesium hydroxide material, comprising:
preparing mixed slurry containing a magnesium hydroxide raw material and a viscosity regulator;
carrying out hydrothermal reaction treatment on the mixed slurry, and carrying out filtering treatment, washing treatment and drying treatment after the reaction is finished to prepare a magnesium hydroxide product;
wherein the viscosity regulator is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate.
2. The method of claim 1, wherein the preparing a mixed slurry comprising a magnesium hydroxide raw material and a viscosity modifier comprises:
preparing a viscosity regulator solution with the concentration of 0.1-5.0 mol/L;
firstly, putting a certain weight of magnesium hydroxide raw material into a reaction vessel, adding the viscosity regulator solution into the reaction vessel, and stirring and mixing to obtain the mixed slurry; or, the viscosity regulator solution is firstly placed in a reaction vessel, and then a certain weight of magnesium hydroxide raw material is added to be stirred and mixed, so as to obtain the mixed slurry;
wherein the magnesium hydroxide raw material with a certain weight is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 8.0% -50%.
3. The method of claim 2, wherein the viscosity modifier solution has a concentration of 0.5mol/L to 2.0mol/L, and the magnesium hydroxide raw material is added in an amount such that the magnesium hydroxide raw material has a mass concentration of 15% to 25% in the mixed slurry.
4. The method for preparing a magnesium hydroxide material according to claim 1, wherein the magnesium hydroxide raw material is magnesium hydroxide powder, a magnesium hydroxide dry filter cake or a magnesium hydroxide wet filter cake.
5. The method of claim 1, wherein the hydrothermal reaction treatment comprises: and transferring the mixed slurry to a high-pressure reaction kettle, and carrying out hydrothermal reaction for 0.1-8 h under the conditions that the temperature is 100-220 ℃ and the stirring strength is 10-800 r/min.
6. The method for preparing a magnesium hydroxide material according to claim 1, wherein the filtration treatment is a vacuum filtration treatment or a pressure filtration treatment; and/or the washing treatment is specifically washing with deionized water and then washing with ethanol; and/or in the drying treatment, the drying temperature is 100-140 ℃ and the drying time is 5-20 h.
7. The method of producing a magnesium hydroxide material according to any one of claims 1 to 6, wherein a dispersant is further added to the mixed slurry.
8. The method of claim 7, wherein the dispersant is a polyacrylate or polyacrylate.
9. The method of claim 7, wherein the dispersant is added in an amount of 0.1 to 5.0% by weight based on the weight of the magnesium hydroxide starting material.
10. The method of claim 9, wherein the dispersant is added in an amount of 0.5 to 2.0% by weight based on the weight of the magnesium hydroxide starting material.
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| CN114394611B (en) * | 2022-01-21 | 2024-05-24 | 洛阳中超新材料股份有限公司 | Preparation method of high aspect ratio flaky magnesium hydroxide |
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