CN113929120B - Preparation method of magnesium hydroxide material - Google Patents
Preparation method of magnesium hydroxide material Download PDFInfo
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- CN113929120B CN113929120B CN202111296843.7A CN202111296843A CN113929120B CN 113929120 B CN113929120 B CN 113929120B CN 202111296843 A CN202111296843 A CN 202111296843A CN 113929120 B CN113929120 B CN 113929120B
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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 175
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 175
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 175
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011268 mixed slurry Substances 0.000 claims abstract description 101
- 239000002994 raw material Substances 0.000 claims abstract description 50
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 46
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 44
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000004034 viscosity adjusting agent Substances 0.000 claims abstract description 32
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims abstract description 24
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000011780 sodium chloride Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 18
- 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
- 235000002639 sodium chloride 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
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 22
- 229920000058 polyacrylate Polymers 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 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
- 235000021463 dry cake Nutrition 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 235000012970 cakes Nutrition 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 13
- 238000006011 modification reaction Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- 239000000047 product Substances 0.000 description 34
- 238000001878 scanning electron micrograph Methods 0.000 description 24
- 239000000243 solution Substances 0.000 description 23
- 239000013078 crystal Substances 0.000 description 20
- 238000005054 agglomeration Methods 0.000 description 15
- 230000002776 aggregation Effects 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000010335 hydrothermal treatment Methods 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 5
- 230000000051 modifying effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- -1 wastewater treatment Substances 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
- 238000000053 physical method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000001131 transforming effect Effects 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
- 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
- 229910052599 brucite Inorganic materials 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
- 229940079593 drug Drugs 0.000 description 1
- 230000007613 environmental effect Effects 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
- 238000009472 formulation Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 239000004571 lime 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
- 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
- 238000003825 pressing Methods 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
- 238000005303 weighing Methods 0.000 description 1
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
Abstract
The invention discloses a preparation method of a magnesium hydroxide material, which comprises the following steps: preparing mixed slurry containing magnesium hydroxide raw material and viscosity modifier; carrying out hydrothermal reaction treatment on the mixed slurry, and after the reaction is finished, carrying out filtration treatment, washing treatment and drying treatment 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 modifier 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 the 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 flame retardants, wastewater treatment, flue gas desulfurization, heavy metal removal, antistaling agents, medicines and the like. As a novel additive inorganic flame retardant with high efficiency, superior performance and environmental protection, magnesium hydroxide is developed in the field of inorganic flame retardants, and is widely applied in the polymer material industry. The preparation modes of magnesium hydroxide can be classified into a physical method and a chemical synthesis method according to the states: physical methods represent brucite processing; the chemical synthesis method is to react magnesium ion-containing material with alkali material in different reaction systems to produce magnesium hydroxide, and includes lime milk process, sodium hydroxide process, ammonia process, reverse precipitation process, hydration process, etc. The magnesium hydroxide prepared by the existing method has poor crystal form and serious agglomeration, and seriously influences the application of the magnesium hydroxide.
The current method for improving the crystal form and agglomeration of magnesium hydroxide is realized by hydrothermal treatment or roasting-hydration. The hydrothermal treatment is a relatively general method for improving the crystal form and agglomeration of magnesium hydroxide, and is generally carried out by subjecting a slurry containing magnesium hydroxide and a crystal form conversion agent (for example, an alkaline substance such as sodium hydroxide or potassium hydroxide) to the hydrothermal treatment under a certain hydrothermal temperature and stirring intensity. When the hydrothermal treatment is carried out, as 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 equipment per unit volume, i.e. to obtain more magnesium hydroxide products after the equipment carries out one hydrothermal treatment, the content of the magnesium hydroxide subjected to each hydrothermal treatment needs to be increased, i.e. the concentration of the magnesium hydroxide in the mixed slurry is increased. However, in the existing 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 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 magnesium hydroxide material to solve the problem of how to reduce the viscosity of slurry and thereby increase 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 magnesium hydroxide raw material and viscosity modifier;
carrying out hydrothermal reaction treatment on the mixed slurry, and after the reaction is finished, carrying out filtration treatment, washing treatment and drying treatment 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 formulation of the mixed slurry comprising magnesium hydroxide raw material and viscosity modifier comprises:
preparing a viscosity regulator solution with the concentration of 0.1mol/L to 5.0 mol/L;
firstly, placing a certain weight of magnesium hydroxide raw material into a reaction container, and then adding the viscosity regulator solution into the reaction container, stirring and mixing to obtain the mixed slurry; or firstly placing the viscosity regulator solution into a reaction container, and then adding a certain weight of magnesium hydroxide raw material to stir and mix to obtain the mixed slurry;
wherein the weight of the magnesium hydroxide raw material 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 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, magnesium hydroxide dry filter cake or magnesium hydroxide wet filter cake.
Preferably, the hydrothermal reaction treatment includes: 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 a vacuum filtration treatment or a press filtration treatment; and/or washing by deionized water and then 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 addition amount of the dispersing agent is 0.1% -5.0% of the weight of the magnesium hydroxide raw material.
More preferably, the dispersant is added in an amount of 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, wherein the viscosity regulator is one or more than two of sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate, and the 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, we also find that the viscosity regulator has the effect of reducing the viscosity of the mixed slurry and 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 image of magnesium hydroxide powder No. 1 of example 1 of the present invention;
FIG. 2 is an SEM image of the magnesium hydroxide product A of example 1 of the invention;
FIG. 3 is an SEM image of magnesium hydroxide product B of example 1 of the invention;
fig. 4 is an SEM image of magnesium hydroxide powder No. 1 in example 2 of the present invention;
fig. 5 is an SEM image of magnesium hydroxide product C in example 2 of the present invention;
fig. 6 is an SEM image of magnesium hydroxide powder No. 2 in example 3 of the present invention;
fig. 7 is an SEM image of the magnesium hydroxide product of example 3 of the present invention;
FIG. 8 is an SEM image of the powder after grinding and sieving of the No. 3 magnesium hydroxide dry cake in example 4 of the present invention;
fig. 9 is an SEM image of the magnesium hydroxide product in example 4 of the present invention;
fig. 10 is an SEM image of magnesium hydroxide No. 4 powder in example 5 of the present invention;
fig. 11 is an SEM image of the magnesium hydroxide product in example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of the embodiments of the present invention will be given 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 merely exemplary and the invention is not limited to these embodiments.
It should be noted here that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to the solution according to the present invention are shown in the drawings, while other details not greatly related 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:
and step S10, preparing mixed slurry containing magnesium hydroxide raw material and viscosity modifier.
And step S20, carrying out hydrothermal reaction treatment on the mixed slurry, and after the reaction is finished, carrying out filtration treatment, washing treatment and drying treatment 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, before the hydrothermal modification treatment, a viscosity modifier is added, wherein the viscosity modifier is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate, and the added viscosity modifier can reduce the viscosity of the mixed slurry during the hydrothermal reaction, so that the concentration of the magnesium hydroxide raw material in the mixed slurry can be increased, and the production efficiency per unit volume of the apparatus can be improved.
In the process of further research, we also find that the viscosity modifier has the effect of reducing the viscosity of the mixed slurry, has good effect of improving the morphology and agglomeration of the magnesium hydroxide material, can improve the crystal form of the magnesium hydroxide product, ensures that the finally obtained magnesium hydroxide product has good morphology, can also reduce the agglomeration of the product, and improves the dispersibility. Therefore, 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 (such as sodium hydroxide, potassium hydroxide and other alkaline conversion agents commonly used in the prior art).
Further, the viscosity modifier also has a good effect of improving the morphology and agglomeration of the magnesium hydroxide material, and the technical scheme provided by the embodiment of the invention has the following advantages:
in some existing technical schemes, in order to make the magnesium hydroxide product obtained by preparation have better morphology, alkaline substances (such as sodium hydroxide and potassium hydroxide) are added as crystal form conversion agents before hydrothermal treatment, and then the hydrothermal treatment is carried out, however, the alkaline substances such as sodium hydroxide and potassium hydroxide are added to have strong corrosiveness on equipment, and the alkaline substances are usually very expensive, so that the method is limited in large-scale industrial use. The viscosity modifier (specifically sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate or potassium sulfate) used in the invention is neutral substance, has low corrosiveness and low price, so that the preparation method of the magnesium hydroxide material provided by the invention is more suitable for large-scale industrialized production.
In a specific scheme, the step S10 may be: firstly, preparing a viscosity regulator solution with the concentration of 0.1mol/L to 5.0 mol/L; firstly placing a certain weight of magnesium hydroxide raw material into a reaction container, and then adding the viscosity modifier solution into the reaction container, stirring and mixing to obtain 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 for stirring and mixing, so as to obtain the mixed slurry. Wherein the weight of the magnesium hydroxide raw material is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 8.0% -50%.
Wherein 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, preferably controlled within a range of 0.5mol/L to 2.0 mol/L.
Wherein 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 is preferably controlled in the range of 15% to 25%.
Wherein the magnesium hydroxide raw material is magnesium hydroxide raw material with any properties such as magnesium hydroxide powder, magnesium hydroxide dry filter cake or magnesium hydroxide wet filter cake.
In a further preferred embodiment, a dispersant is further added to the mixed slurry prepared in step S10. The dispersant is preferably polyacrylate or polyacrylate, for example, polyacrylate such as sodium polyacrylate, potassium polyacrylate, aluminum polyacrylate, ammonium polyacrylate, etc., or polyacrylate such as polymethyl acrylate, polyethyl acrylate, etc. By adding the dispersing agent, the viscosity of the mixed slurry can be further reduced, so that the concentration of the magnesium hydroxide raw material in the mixed slurry can be further increased, and the production efficiency per unit volume of the equipment can be improved.
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 the step S20:
the hydrothermal reaction treatment includes: 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 filtering treatment is vacuum filtering 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 is used, and ethanol 1 to 2 times the dry weight of magnesium hydroxide is used for 0 to 1 time.
In the drying treatment, the drying temperature is 100-140 ℃ and the drying time is 5-20 h. Further, the magnesium hydroxide product with the predetermined size range is obtained by sieving after drying.
Wherein, when preparing the mixed slurry in the step S10, the solvent is water; in a more preferred embodiment, the mixed slurry is prepared using the filtrate obtained by the filtration treatment in step S20 and the washing solution obtained by the washing treatment as a solvent.
Example 1
Preparing a sodium chloride solution with the concentration of 1.0mol/L, namely taking neutral sodium chloride as a viscosity regulator; 340g of No. 1 magnesium hydroxide powder is added into a reactor, 1660g of sodium chloride solution is weighed and poured into the reactor, and mixed slurry A is obtained by stirring and mixing. Wherein the mass concentration of magnesium hydroxide in the mixed slurry A is 17%.
Transferring the mixed slurry A in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ and stirring intensity of 300r/min for 3h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 428 mPas.
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 sodium hydroxide solution with the concentration of 0.75mol/L, namely taking alkaline substance sodium hydroxide as a crystal form transforming agent according to the prior technical scheme for preparing the magnesium hydroxide material; 320g of No. 1 magnesium hydroxide powder is added into a reactor, 1680g of sodium hydroxide solution is weighed and poured into the reactor to be stirred and mixed to obtain mixed slurry B. Wherein the mass concentration of magnesium hydroxide in the mixed slurry B is 16%.
Transferring the mixed slurry B in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ and stirring intensity of 300r/min for 3h. 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 viscosity parameter data of the mixed slurry obtained according to the mass concentration of magnesium hydroxide in the above examples and the test are collated in the following table 1.
TABLE 1
| Mixed slurry A | Mixed slurry B | |
| Magnesium hydroxide mass concentration (%) | 17 | 16 |
| Viscosity of the slurry mixture after the reaction (mPa. S) | 428 | 690 |
As is clear from comparison of the data in table 1, in the prior art scheme (comparison experiment 1), when sodium hydroxide is added as a crystal form conversion agent, the viscosity of the mixed slurry is higher at the completion of the hydrothermal reaction in the case that 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 and is reduced by about 38% when the hydrothermal reaction is completed under the condition that the mass concentration of magnesium hydroxide is higher (17%). It can be understood that 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 the unit volume of the equipment is improved, and the production cost is reduced.
The morphology of the magnesium hydroxide raw material used in this example and the magnesium hydroxide product obtained by preparation was observed using a Scanning Electron Microscope (SEM): fig. 1 is an SEM image of magnesium hydroxide powder raw material No. 1 used in the present example, fig. 2 is an SEM image of magnesium hydroxide product a prepared in the present example, and fig. 3 is an SEM image of magnesium hydroxide product B prepared in the present example.
As can be seen from comparison between fig. 2 and fig. 1, sodium chloride as a viscosity modifier in the present example can also modify magnesium hydroxide raw material, has good modifying effect on crystal form and agglomeration of magnesium hydroxide, can modify and obtain hexagonal flaky magnesium hydroxide product, and has good dispersibility. As shown in fig. 3, when sodium hydroxide, an alkaline substance, is used as a crystal form conversion agent in the prior art, the crystal form and agglomeration of magnesium hydroxide are well modified.
Example 2
Preparing sodium chloride solution with the concentration of 2.0mol/L, namely taking neutral sodium chloride as a viscosity regulator; 340g of No. 1 magnesium hydroxide powder is added into a reactor, 1654.9g of sodium chloride solution is weighed and poured into the reactor for stirring and mixing, then 5.1g of ammonium polyacrylate is added as a dispersing agent, and stirring and mixing are continued 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 serving as a dispersing agent is 1.5% of the mass of magnesium hydroxide powder.
Transferring the mixed slurry C in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ and stirring intensity of 500r/min for 3h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 35 mPas.
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 described in example 2 above to verify the effect of the dispersant on the slurry concentration. The method comprises the following steps:
preparing sodium hydroxide solution with the concentration of 0.75mol/L, namely taking alkaline substance sodium hydroxide as a crystal form transforming agent according to the prior technical scheme for preparing the magnesium hydroxide material; adding 320g of No. 1 magnesium hydroxide powder into a reactor, weighing 1675.2g of sodium hydroxide solution, pouring into the reactor, stirring and mixing, adding 4.8g of ammonium polyacrylate 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 serving as a dispersing agent is 1.5% of the mass of magnesium hydroxide powder.
Transferring the mixed slurry D in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ and stirring intensity of 300r/min for 3h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 508 mPas.
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 differs from example 1 mainly in that: the mixed slurry was further added with 1.5% of a dispersant, and 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. Comparative experiment 2 is mainly different from comparative experiment 1 in that: the mixed slurry was further added with 1.5% of a dispersant, and 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.
The viscosity data of the mixed slurry obtained based on the above test can be summarized as follows:
(1) The viscosity of the mixed slurry after the completion of the hydrothermal reaction can be reduced by adding a certain amount of dispersing agent to the mixed slurry in either the technical scheme provided by the invention or the technical scheme existing in the prior art.
(2) The mixed slurry a of example 1 was smaller in viscosity after completion of the reaction than the mixed slurry D of comparative experiment 2. From this, it is apparent that when the viscosity modifier is used in the technical scheme of the present invention, the viscosity of the mixed slurry at the completion of the hydrothermal reaction is lower than that of the scheme of further adding the dispersant in the prior art even if the dispersant is not added.
(3) The mixed slurry C of example 2 was reduced in viscosity from 428mpa·s to 35mpa·s after the completion of the reaction, as compared with the mixed slurry a of example 1, and the viscosity reduction was 90% or more; the mixed slurry D of comparative experiment 2 was reduced in viscosity from 690mpa·s to 508mpa·s after completion of the reaction, compared with the mixed slurry B of comparative experiment 1, and the range of the reduction in viscosity was about 26%.
Therefore, although the viscosity of the mixed slurry after the completion of the hydrothermal reaction can be reduced after a certain amount of dispersing agent is added based on the prior art, in the technical scheme of the invention, after a certain amount of dispersing agent is added into the mixed slurry, the viscosity regulator and the dispersing agent have a synergistic viscosity reduction effect, so that the viscosity of the mixed slurry after the completion of the hydrothermal reaction can be greatly reduced, and the production efficiency of the unit volume of the equipment is further improved.
The morphology of the magnesium hydroxide raw material used in example 2 and the magnesium hydroxide product C obtained by the preparation thereof was observed using a scanning electron microscope: fig. 4 is an SEM image of magnesium hydroxide powder raw material No. 1 used in the present example, and fig. 5 is an SEM image of magnesium hydroxide product C prepared in the present example.
As can be seen from comparison of fig. 5 and fig. 4, the addition of sodium chloride as a neutral substance of the viscosity modifier and the addition of the dispersing agent in this example has a good modifying effect on the crystal form and agglomeration 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; 200g of No. 2 magnesium hydroxide powder is added into a reactor, 1800g of the mixed solution is weighed and poured into the reactor, and the mixed solution is stirred and mixed to obtain mixed slurry. Wherein the mass concentration of magnesium hydroxide in the mixed slurry is 10%.
Transferring the mixed slurry in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at the temperature of 140 ℃ and the stirring intensity of 500r/min for 5h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 185 mPas. The viscosity of the mixed slurry is lower 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 is 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 image of magnesium hydroxide powder No. 2 raw material used in the present example, and fig. 7 is an SEM image of the magnesium hydroxide product obtained in the present example.
As can be seen from comparison between fig. 7 and 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 modifying effect on the crystal form and agglomeration of magnesium hydroxide.
Example 4
Preparing a potassium chloride solution with the concentration of 0.5mol/L, namely taking neutral substance potassium chloride as a viscosity regulator; 400g of No. 3 magnesium hydroxide dry filter cake is added into a reactor, 1596g of potassium chloride solution is weighed and poured into the reactor for stirring and mixing, and then 4g of ammonium polyacrylate is added as a dispersing agent, and stirring and mixing are continued to obtain mixed slurry. Wherein the mass concentration of magnesium hydroxide in the mixed slurry is 20%, and the addition amount of ammonium polyacrylate serving as a dispersing agent is 1.0% of the mass of magnesium hydroxide powder.
Transferring the mixed slurry in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 180 ℃ and stirring intensity of 600r/min for 1h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 32 mPas. In this embodiment, a certain amount of dispersant is added, so that the viscosity of the mixed slurry is greatly reduced, and the production efficiency of the unit volume of the equipment is further improved.
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 image of powder of the magnesium hydroxide No. 3 dry cake raw material used in the present example after grinding and sieving, and fig. 9 is an SEM image of the magnesium hydroxide product obtained in the present example.
As can be seen from comparison between fig. 9 and 8, in this example, the addition of the neutral substance potassium chloride as a viscosity modifier and the addition of the dispersing agent has a good modifying effect on the crystal form and agglomeration of magnesium hydroxide.
Example 5
Preparing sodium chloride solution with the concentration of 2mol/L, namely taking neutral sodium chloride as a viscosity regulator; 280g of No. 4 magnesium hydroxide powder is added into a reactor, 1720g of sodium chloride solution is weighed and poured into the reactor, and the mixture is stirred and mixed to obtain mixed slurry. Wherein the mass concentration of the magnesium hydroxide in the mixed slurry is 14%.
Transferring the mixed slurry in the reactor into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 160 ℃ and stirring intensity of 500r/min for 3h. The viscosity of the mixed slurry after completion of the hydrothermal reaction was measured and found to be 133 mPas. The viscosity of the mixed slurry is lower 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 is 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 image of the magnesium hydroxide powder No. 4 raw material used in the present example, and fig. 11 is an SEM image of the magnesium hydroxide product obtained in the present example.
As can be seen from comparison between fig. 11 and 10, sodium chloride as a viscosity modifier in the present example also modifies the magnesium hydroxide raw material, and has a good modifying effect on the crystal form and agglomeration of magnesium hydroxide.
In the embodiments of the present invention from example 1 to example 5, examples 1, 3 and 5 are examples in which only the viscosity modifier was added, and examples 2 and 4 are examples in which a dispersant was added in addition to the viscosity modifier. As can be seen by comparing the viscosity test results of example 1, example 3 and example 5 with the test results of example 2 and example 4: the viscosity of the mixed slurry after the hydrothermal reaction is finished can be better reduced by further adding the dispersing agent on the basis of adding the viscosity regulator, and the production efficiency of the unit volume of the equipment is further improved. Comparing the SEM image of the product obtained by example 1 with the SEM image of the product obtained by example 2, it can be known that: on the basis of adding the viscosity modifier, the dispersant is further added, so that the modification effect on the crystal form and agglomeration of the magnesium hydroxide is rather inferior to the technical scheme of adding the viscosity modifier only.
Therefore, the preparation method of the magnesium hydroxide material provided by the embodiment of the invention comprises the following steps: if the magnesium hydroxide product with high quality morphology is required to be obtained while the production efficiency is improved, only the viscosity regulator is selected to be added; if the modification requirement on the magnesium hydroxide product is reduced in order to require higher production efficiency, a certain amount of dispersant is further added on the basis of adding the viscosity regulator.
In summary, in the preparation method of the magnesium hydroxide material provided in the embodiment of the invention, the viscosity modifier is added before the hydrothermal modification treatment, wherein the viscosity modifier is one or more selected from sodium chloride, potassium chloride, sodium sulfate, magnesium sulfate and potassium sulfate, and the 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, the production efficiency of the unit volume of the equipment is improved, and the viscosity modifier has a good modification effect on the crystal form and agglomeration of the magnesium hydroxide.
The foregoing is merely exemplary of the application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the application and are intended to be comprehended within the scope of the application.
Claims (9)
1. A method for preparing a magnesium hydroxide material, comprising:
preparing mixed slurry containing magnesium hydroxide raw material and viscosity modifier;
carrying out hydrothermal reaction treatment on the mixed slurry, and after the reaction is finished, carrying out filtration treatment, washing treatment and drying treatment 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;
wherein, the preparation of the mixed slurry containing the magnesium hydroxide raw material and the viscosity modifier comprises the following steps:
preparing a viscosity regulator solution with the concentration of 0.1mol/L to 5.0 mol/L;
firstly, placing a certain weight of magnesium hydroxide raw material into a reaction container, and then adding the viscosity regulator solution into the reaction container, stirring and mixing to obtain the mixed slurry; or firstly placing the viscosity regulator solution into a reaction container, and then adding a certain weight of magnesium hydroxide raw material to stir and mix to obtain the mixed slurry;
wherein the weight of the magnesium hydroxide raw material is such that the mass concentration of the magnesium hydroxide raw material in the mixed slurry is 8.0% -50%.
2. The method for producing a magnesium hydroxide material according to claim 1, wherein the concentration of the viscosity modifier solution is 0.5mol/L to 2.0mol/L, and the 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%.
3. The method for producing a magnesium hydroxide material according to claim 1, wherein the magnesium hydroxide raw material is a magnesium hydroxide powder, a magnesium hydroxide dry cake or a magnesium hydroxide wet cake.
4. The method of preparing a magnesium hydroxide material according to claim 1, wherein said hydrothermal reaction treatment comprises: 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.
5. The method for producing a magnesium hydroxide material according to claim 1, wherein the filtration treatment is a vacuum filtration treatment or a press filtration treatment; and/or washing by deionized water and then ethanol; and/or in the drying treatment, the drying temperature is 100-140 ℃ and the drying time is 5-20 h.
6. The method for producing a magnesium hydroxide material according to any one of claims 1 to 5, wherein a dispersant is further added to the mixed slurry.
7. The method of preparing a magnesium hydroxide material according to claim 6, wherein the dispersant is polyacrylate or polyacrylate.
8. The method for preparing a magnesium hydroxide material according to claim 6, wherein the dispersant is added in an amount of 0.1% to 5.0% by weight based on the weight of the magnesium hydroxide raw material.
9. The method for preparing a magnesium hydroxide material according to claim 8, wherein the dispersant is added in an amount of 0.5% to 2.0% by weight based on the weight of the magnesium hydroxide raw material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800020A (en) * | 2005-12-23 | 2006-07-12 | 清华大学 | Water heat modification method for high dispersion magnesium hydroxide nanometer sheet |
| CN102050472A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院过程工程研究所 | Method for preparing submicron flaky magnesium hydroxide from magnesium oxide |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN109133126A (en) * | 2018-08-23 | 2019-01-04 | 中国科学院青海盐湖研究所 | A kind of magnesium hydroxide products and preparation method thereof |
| CN112403213A (en) * | 2020-11-25 | 2021-02-26 | 大连海事大学 | Magnesium hydroxide slurry and preparation method thereof |
-
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800020A (en) * | 2005-12-23 | 2006-07-12 | 清华大学 | Water heat modification method for high dispersion magnesium hydroxide nanometer sheet |
| CN102050472A (en) * | 2009-10-28 | 2011-05-11 | 中国科学院过程工程研究所 | Method for preparing submicron flaky magnesium hydroxide from magnesium oxide |
| CN102205980A (en) * | 2011-04-07 | 2011-10-05 | 中国科学院青海盐湖研究所 | Method for preparing monodisperse flaky magnesium hydroxide flame retardant |
| CN108034991A (en) * | 2017-12-08 | 2018-05-15 | 中国科学院青海盐湖研究所 | The preparation method of 311 type alkali magnesium sulfate crystal whiskers |
| CN109133126A (en) * | 2018-08-23 | 2019-01-04 | 中国科学院青海盐湖研究所 | A kind of magnesium hydroxide products and preparation method thereof |
| CN112403213A (en) * | 2020-11-25 | 2021-02-26 | 大连海事大学 | Magnesium hydroxide slurry and preparation method thereof |
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