CN109574049B - Hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate - Google Patents
Hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate Download PDFInfo
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Abstract
The invention relates to a hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, belonging to the technical field of inorganic chemical material preparation. The method comprises the following steps: crushing magnesite, calcining at the temperature of 600 ℃ and 900 ℃ for 1-5h to obtain light-burned magnesia powder; adding the light-burned magnesia powder into a hydrating agent solution at the calcining temperature, wherein the solid-liquid weight ratio is 1: 5-20, and the anions in the hydrating agent solution are: at least one of chloride ion, nitrate ion, sulfate ion, acetate ion and oxalate ion, and the cation in the hydrating agent solution is: at least one of hydrogen ion, sodium ion, magnesium ion, calcium ion, iron ion, ferrous ion, aluminum ion and ammonium ion, the concentration of the hydrator solution is 0.5-5%, and the solution is stirred homogeneously at the speed of 800-2000 rpm. The invention realizes the regulation and control of the dissolution rate of the synthesized magnesium hydroxide slurry by organically combining three technologies of heat treatment, chemical treatment and mechanical activation.
Description
Technical Field
The invention relates to a hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, belonging to the technical field of inorganic chemical material preparation.
Background
The magnesium hydroxide is called as 'third alkali', is a green and safe environment treatment agent, has good application prospect in the fields of acid waste gas and wastewater treatment and the like, and particularly has huge environment-friendly requirement on slurry-shaped magnesium hydroxide.
The low dissolution rate of magnesium hydroxide has its safety advantages, but also has the disadvantage of low efficiency. For example, in the nitrogen and phosphorus recovery process of wastewater struvite method using magnesium hydroxide as magnesium source, OH-And Mg2+The slow release process can control the crystallization reaction on the surface of the magnesium hydroxide particles, thereby relieving the pipeline scaling caused by the random crystallization of struvite in the system; however, the recovery efficiency is directly affected by too slow dissolution speed, and the magnesium hydroxide is covered by a product layer before dissolution, so that the reaction is stopped. Therefore, the magnesium hydroxide is regulated and controlled according to a specific application systemThe dissolving speed of the slurry can greatly improve the application efficiency and expand the application range.
The synthesis method of magnesium hydroxide is various, mainly comprises a magnesium salt precipitation method and a hydration method, and magnesium salt precipitation consumes a large amount of acid and alkali, so that the subsequent treatment is complicated, the cost is high, and the method is not suitable for synthesizing environment-friendly magnesium hydroxide slurry. The hydration method mainly uses light-burned magnesium oxide as a precursor to react with water at different temperatures to generate magnesium hydroxide, and has simple process and low cost. CN102502726A and CN105256405A are hydrated into hexagonal flaky and fibrous magnesium hydroxide by magnesite calcine, a modifier, a dispersant, an active agent and a crystal seed, and are used as flame-retardant fillers. CN104609449A discloses a method for roasting agglomerated magnesium hydroxide with the aid of an inorganic flux, and then hydrating the roasted product and adding a dispersant and a morphology controlling agent, in order to obtain highly dispersed magnesium hydroxide powder. CN106495268A discloses a method for removing pollutants in water by using a magnesium oxide adsorbent, wherein magnesium oxide subjected to heat treatment at 100-700 ℃ is directly reacted with wastewater to generate magnesium hydroxide slurry in situ for adsorbing and treating heavy metal pollutants in water. CN103864121A discloses a method for synthesizing magnesium hydroxide by gas-phase hydration of magnesium oxide, which is mainly technically characterized by high liquid-solid ratio and low energy consumption in subsequent drying. The research on the hydration of magnesium oxide into magnesium hydroxide is also reported in this subject group, for example: CN102120126A discloses a method for synthesizing slurry for ship exhaust gas desulfurization by hydration of magnesium oxide in a seawater system, CN103303947A provides a gas-liquid-solid three-phase magnesium oxide high-efficiency hydration mode, and CN106365185A provides an ultrasonic-assisted magnesium oxide high-efficiency hydration technology.
At present, related researches mainly focus on the aspects of dispersibility, crystal shape, synthesis efficiency and the like, and do not relate to the regulation of the dissolution rate of the magnesium hydroxide slurry.
Disclosure of Invention
The invention controls the defect formation and microstructure change of magnesium hydroxide by adjusting the synthesis environment and process parameters, thereby regulating and controlling the dissolution rate of the magnesium hydroxide.
The invention provides a hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, which comprises the following steps: crushing magnesite, calcining at the temperature of 600 ℃ and 900 ℃ for 1-5h to obtain light-burned magnesia powder; adding the light-burned magnesia powder into the hydration agent solution at the calcining temperature, and uniformly stirring to obtain magnesium hydroxide slurry; the solid-liquid weight ratio is 1: 5-20 parts of; the anions in the hydrating agent solution are: at least one of chloride ion, nitrate ion, sulfate ion, acetate ion and oxalate ion, and the cation in the hydrating agent solution is: at least one of hydrogen ions, sodium ions, magnesium ions, calcium ions, iron ions, ferrous ions, aluminum ions, and ammonium ions; the concentration of the hydrating agent solution is 0.5-5%; the homogenizing and stirring speed is 800-2000 rpm; the time of the hydration reaction is 0.2-2 h.
The magnesite is preferably crushed to 200-1500 meshes.
The invention preferably has the calcination conditions that: calcining at 700 ℃ and 800 ℃ for 2-3 h.
The invention preferably has the solid-liquid weight ratio of 1: 10-15.
Preferably, the anions in the hydrating agent solution are: sulfate ions or acetate, and the cation in the hydrating agent solution is: magnesium ions or ammonium ions.
The invention preferably provides a concentration of the hydrating agent solution of 1 to 3%.
The invention preferably has the homogeneous stirring speed of 1000-1500 rpm.
The time of the hydration reaction is 0.5-1.5 h.
The invention has the beneficial effects that:
according to the invention, the high temperature contained in the magnesite calcination product is utilized, the heat is directly used in the hydration synthesis process, the powder or solution does not need to be heated again, the energy is saved, the Gibbs free energy on the surface of the product is increased, and the dissolution rate is improved;
the invention constructs a plurality of hydration agent systems, and controls the formation of crystal defects through the doping, substitution, coordination and directional adsorption of ions, thereby realizing the regulation and control of the dissolution rate;
based on a mechanical activation technology, agglomeration is reduced through homogeneous stirring, the defect exposure degree is controlled, and the dissolution rate regulation and control are realized;
the invention organically combines three technologies of heat treatment, chemical treatment and mechanical activation to realize the regulation and control of the dissolution rate of the synthesized magnesium hydroxide slurry, and similar processes are not reported at home and abroad.
Drawings
In the figure 3 of the attached drawings of the invention,
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a graph showing a comparison of the dissolution rates of the synthetic products of the hydration agent system constructed with acetate ions and different cations according to examples 1-6;
FIG. 3 is a graph showing a comparison of the dissolution rates of the resultant hydration agent system constructed with magnesium ions and different anions of examples 7-9.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate comprises the following steps:
4000g of magnesite raw stone is crushed to 1250 meshes and calcined for 3 hours at 650 ℃ to obtain light-burned magnesia powder;
adding 20g of light-burned magnesia powder into 200mL of hydrating agent solution at the calcining temperature, and uniformly stirring to obtain magnesium hydroxide slurry;
the hydrating agent solution is sodium acetate with the concentration of 1 percent;
the homogenizing stirring speed is 1300 rpm;
the time of the hydration reaction is 0.5 h;
the dissolution rate of the magnesium hydroxide slurry is measured by a constant pH titration method, and a hydration agent is not added in a control group.
Example 2
The hydration synthesis method of the magnesium hydroxide slurry with controllable dissolution rate is different from the hydration synthesis method of the magnesium hydroxide slurry in the embodiment 1 in that: the hydrating agent solution is ammonium acetate.
Example 3
The hydration synthesis method of the magnesium hydroxide slurry with controllable dissolution rate is different from the hydration synthesis method of the magnesium hydroxide slurry in the embodiment 1 in that: the hydrating agent solution is acetic acid.
Example 4
The hydration synthesis method of the magnesium hydroxide slurry with controllable dissolution rate is different from the hydration synthesis method of the magnesium hydroxide slurry in the embodiment 1 in that: the hydrating agent solution is aluminum acetate.
Example 5
The hydration synthesis method of the magnesium hydroxide slurry with controllable dissolution rate is different from the hydration synthesis method of the magnesium hydroxide slurry in the embodiment 1 in that: the hydrating agent solution is calcium acetate.
Example 6
The hydration synthesis method of the magnesium hydroxide slurry with controllable dissolution rate is different from the hydration synthesis method of the magnesium hydroxide slurry in the embodiment 1 in that: the hydrating agent solution is zinc acetate.
Example 7
A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate comprises the following steps:
3000g of magnesite raw stone is crushed to 1000 meshes and calcined at 600 ℃ for 2.5 hours to obtain light-burned magnesia powder;
adding 10g of light-burned magnesia powder into 200mL of hydrating agent solution at the calcining temperature, and uniformly stirring to obtain magnesium hydroxide slurry;
the hydrating agent solution is magnesium chloride with the concentration of 2 percent;
the homogenizing stirring speed is 1450 rpm;
the time of the hydration reaction is 1 h;
the dissolution rate of the magnesium hydroxide slurry is measured by a constant pH titration method, and a hydration agent is not added in a control group.
Example 8
A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, which is different from the embodiment 7 in that: the hydrating agent solution is magnesium acetate.
Example 9
A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, which is different from the embodiment 7 in that: the hydrating agent solution is magnesium sulfate.
Example 10
A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate, which is different from the embodiment 7 in that: the hydrating agent solution is magnesium nitrate.
In different hydration agent systems, the dissolution rate of the magnesium oxide hydration product is inhibited or promoted, and the aim of synthesizing the magnesium hydroxide slurry with controllable dissolution rate is fulfilled.
Claims (6)
1. A hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate is characterized in that: the method comprises the following steps:
crushing magnesite, calcining at the temperature of 600 ℃ and 900 ℃ for 1-5h to obtain light-burned magnesia powder;
adding the light-burned magnesia powder into the hydration agent solution at the calcining temperature, and uniformly stirring to obtain magnesium hydroxide slurry;
the solid-liquid weight ratio is 1: 5-20 parts of;
the anions in the hydrating agent solution are: acetate ions, cations in the hydrating agent solution are: at least one of hydrogen ions, sodium ions, calcium ions, aluminum ions, and ammonium ions;
the concentration of the hydrating agent solution is 1 percent;
the homogeneous stirring speed is 800-;
the time of the hydration reaction is 0.2-2 h.
2. The hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate according to claim 1, characterized in that: the magnesite is crushed to 200-1500 meshes.
3. The hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate according to claim 1, characterized in that: the calcination conditions are as follows: calcining at 700 ℃ and 800 ℃ for 2-3 h.
4. The hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate according to claim 1, characterized in that: the solid-liquid weight ratio is 1: 10-15.
5. The hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate according to claim 1, characterized in that: the homogeneous stirring speed is 1000-.
6. The hydration synthesis method of magnesium hydroxide slurry with controllable dissolution rate according to claim 1, characterized in that: the time of the hydration reaction is 0.5-1.5 h.
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| JPH0816012B2 (en) * | 1992-12-22 | 1996-02-21 | ナストーア株式会社 | Preparation method of activated magnesium hydroxide |
| JPH1059711A (en) * | 1996-08-12 | 1998-03-03 | Daicel Amiboshi Sangyo Kk | Magnesium hydroxide and production of aqueous liquid suspension thereof |
| KR20120009069A (en) * | 2010-07-22 | 2012-02-01 | 주식회사 이에프티 | Method for preparing of polymagnesium hydroxide |
| CN103303947B (en) * | 2013-06-19 | 2014-09-03 | 大连海事大学 | Preparation method and device for efficiently preparing magnesium hydroxide |
| CN107399748B (en) * | 2017-08-01 | 2019-06-04 | 沈阳凯镁客科技有限公司 | A kind of production method for extracting magnesium hydroxide and calcium carbonate from dolomite |
| CN108314335A (en) * | 2018-04-18 | 2018-07-24 | 镇江苏博特新材料有限公司 | A kind of light-burned MgO suspension kilns coproduction Mg (OH)2Production technology and device |
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