CN104803400A - Ammonium magnesium sulfate preparation method - Google Patents
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- CN104803400A CN104803400A CN201410033795.6A CN201410033795A CN104803400A CN 104803400 A CN104803400 A CN 104803400A CN 201410033795 A CN201410033795 A CN 201410033795A CN 104803400 A CN104803400 A CN 104803400A
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Abstract
The present invention relates to an ammonium magnesium sulfate preparation method, which comprises: mixing a magnesium-containing raw material and ammonium sulfate, heating, carrying out thermal insulation, and reacting to obtain the ammonium magnesium sulfate, optionally, carrying out impurity removing, crystallization and other steps after completing the reaction to obtain the ammonium magnesium sulfate. The present invention provides a solid-phase ammonium magnesium sulfate preparation method, wherein the reaction process is performed without water, such that the water consumption is saved, the water removing step is eliminated, and the new way for preparing the ammonium magnesium sulfate is provided.
Description
Technical field
The invention belongs to technical field of chemical material preparation, be specifically related to a kind of preparation method of ammonium magnesium sulfate, particularly relate to a kind of method being prepared ammonium magnesium sulfate by ammonium sulfate and the raw material containing magnesium elements.
Background technology
Six water magnesium sulfate ammonium molecular formula are (NH
4)
2mg (SO
4)
26 (H
2o), belong to monoclinic sulfuric acid double salt, molecular weight is 360.6, is commonly used for industrial chemicals and compound manure.Conventional magnesium sulfate and ammonium sulfate solution crystallization process obtain (Physica Status Solidi (A) Applied Research, 1988,109(2) at present: 635-640).Chinese patent 101497453 discloses one by after roasting magnesite vitriolization ammonium solution, and continue to add ammonium sulfate, obtain the method for six water magnesium sulfate ammoniums through liquid phase crystallization, technique is comparatively complicated, and a certain amount of crystal water of content in product.Therefore, moisture removal is absolutely necessary a step, and this step theoretical energy consumption is higher.
Therefore, a kind of preparation method of ammonium magnesium sulfate is urgently developed in this area, and described method technique is simple, and treatment capacity is large, and reaction process is without the need to the participation of water, and energy consumption is lower.
Summary of the invention
The step complexity existed in the technique of ammonium magnesium sulfate is prepared for existing, treatment capacity is little, and there are the remnants of a large amount of water, not only cause the waste of water resources, also create the too high consumption of energy in removal process, the object of the present invention is to provide a kind of preparation method of ammonium magnesium sulfate, described reaction is without the need to the participation of water, decrease the waste of water, save the energy, reduce investment.
The present invention is achieved through the following technical solutions:
A preparation method for ammonium magnesium sulfate, described method is mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, heat temperature raising, and insulation, after reaction terminates, obtains ammonium magnesium sulfate;
Alternatively, after reaction terminates, through removal of impurities, crystallization, obtains ammonium magnesium sulfate.
The raw material of the method for the invention is be the raw material containing magnesium elements of solid form and ammonium sulfate under room temperature, and both mixing also, after homogenizing, are reacted at a certain temperature, obtained ammonium magnesium sulfate.Reaction only adds solid material, without the need to carrying out in aqueous, decreasing the use of water, eliminating the step dewatered.
Of the present inventionly prepare in the method for ammonium magnesium sulfate, removal of impurities and crystallization are optional step, specifically can select according to containing the raw material type of magnesium elements and the quality of ammonium magnesium sulfate to be prepared, such as: when with containing the compound of magnesium elements be containing the raw material of magnesium elements and ammonium sulfate react prepare anhydrous magnesium sulfate ammonium time, due to less containing impurity in the compound of magnesium elements, then do not need removal of impurities, the example of the typical but non-limiting compound containing magnesium elements has magnesium halide, magnesiumcarbonate, Magnesium hydrogen carbonate, hydroxyhalide magnesium, hydroxy carbonate magnesium, organic magnesium-containing compound, magnesium hydroxide or magnesium oxide etc.
When reacting using the raw mineral materials containing the compound containing magnesium elements as the raw material and ammonium sulfate containing magnesium elements, when preparing ammonium magnesium sulfate, in order to remove the impurity in raw mineral materials, can select removal of impurities and crystallisation step, the example of the typical but non-limiting raw mineral materials containing the compound containing magnesium elements has magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern.
In the preparation method of ammonium magnesium sulfate of the present invention, the speed of heat temperature raising is 0.2 ~ 30 DEG C/min, such as 0.3 DEG C/min, 0.8 DEG C/min, 4 DEG C/min, 9 DEG C/min, 13 DEG C/min, 15 DEG C/min, 17 DEG C/min, 19 DEG C/min, 22 DEG C/min, 26 DEG C/min, 28 DEG C/min etc.
Preferably, the temperature of described insulation is 200 ~ 600 DEG C, such as 230 DEG C, 260 DEG C, 290 DEG C, 350 DEG C, 380 DEG C, 450 DEG C, 500 DEG C, 540 DEG C, 590 DEG C, 600 DEG C etc.
Temperature is too high or intensification is too fast easily causes the sulfate radical in ammonium sulfate to decompose or by ammonium radical ion reduction decomposition, generates SO
3or SO
2, do not reach and decompose generation bisulfate ion, ensure that bisulfate ion participates in, containing magnesium material reaction, generating the object of ammonium magnesium sulfate.Further, along with sulfate radical is reduced, ammonium root is also oxidized, generates nitrogen, causes the waste of ammonium radical ion.
Preferably, soaking time≤20h of the present invention, such as 0.6h, 1.2h, 2h, 4h, 5h, 7h, 9h, 12h, 15.8h, 18h, 19.5h etc.
Preferably, in the mixture be mixed to get containing the raw material of magnesium elements and ammonium sulfate in the method for the invention, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:(1.6 ~ 3.0), such as 1:1.62,1:1.68,1:1.75,1:1.99,1:2.05,1:2.2,1:2.8,1:2.9,1:2.96 etc.
The concrete ratio that raw material containing magnesium elements of the present invention mixes with ammonium sulfate, those skilled in the art can as requested: in mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:(1.6 ~ 3.0), carry out proportioning.
Raw material containing magnesium elements of the present invention is containing the compound of magnesium elements and/or the raw mineral materials containing described compound (i.e. the described compound containing magnesium elements).
Preferably, the described compound containing magnesium elements is selected from inorganic magnesium compound and/or organo-magnesium compound, the combination of any a kind or at least 2 kinds preferably in magnesium halide, magnesiumcarbonate, Magnesium hydrogen carbonate, hydroxyhalide magnesium, hydroxy carbonate magnesium, magnesium hydroxide, magnesium oxide.Described magnesium halide, comprises the combination of any a kind or at least 2 kinds in magnesium fluoride, magnesium chloride, magnesium bromide or magnesium iodide.
Combination containing magnesium elements compound of the present invention is typical but non-limiting to be had: the combination of magnesiumcarbonate and Magnesium hydrogen carbonate, the combination of magnesium chloride and hydroxy chloride magnesium, hydroxy carbonate magnesium and magnesian combination, magnesium chloride and magnesian combination, the combination of magnesium hydroxide and magnesiumcarbonate, magnesiumcarbonate, hydroxy chloride magnesium and magnesian combination etc.
Preferably, described raw mineral materials is selected from the combination of any a kind or at least 2 kinds in the dehydration of magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern and described raw mineral materials and/or product of roasting; Described dehydration and/or maturing temperature are 100 ~ 900 DEG C, such as 102 DEG C, 108 DEG C, 134 DEG C, 168 DEG C, 250 DEG C, 289 DEG C, 360 DEG C, 400 DEG C, 485 DEG C, 689 DEG C, 823 DEG C, 885 DEG C etc.
Combination containing magnesium elements compound of the present invention is typical but non-limiting to be had: the combination of described combination such as magnesite and rhombspar, the combination of brucite and magnesite, the combination of rhombspar and roasting magnesite, the combination etc. of rhombspar, roasting rhombspar and ammonium carnallite.
Further preferably, described magnesium halide is selected from the combination of any a kind or at least 2 kinds in magnesium fluoride, magnesium chloride, magnesium bromide or magnesium iodide.Described magnesium oxide is selected from the combination of any a kind or at least 2 kinds in light calcined magnesia, activated magnesia or light magnesium oxide.Described magnesium halide is anhydrous and/or moisture magnesium halide.Described hydroxyhalide magnesium is anhydrous and/or moisture hydroxyhalide magnesium.Described hydroxy carbonate magnesium is anhydrous and/or moisture hydroxy carbonate magnesium.
Further preferably, the dehydration of described raw mineral materials and/or product of roasting refer to the mixture of any a kind or at least 2 kinds in described raw mineral materials (such as magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern), the product of dehydration and/or roasting at 100 ~ 900 DEG C.Which kind of dehydration and/or maturing temperature of concrete selection, those skilled in the art can select according to practical situation.
The temperature of heat-up rate of the present invention and insulation has certain influence for reaction, and therefore for the raw material containing magnesium elements being easier to react, heat-up rate can suitably be accelerated, and holding temperature can suitably reduce, and soaking time can suitably shorten; And for more difficult reaction containing the raw material of magnesium elements, should heat up with slower speed, holding temperature also should suitably improve, and soaking time suitably increases.For be easier to and more difficult reaction multistage heating and heat preservation method all can be adopted to realize containing the raw material of magnesium elements.As for certain concrete raw material, those skilled in the art can select according to practical situation (complexity etc. as reaction).
Preferably, when containing the raw material of magnesium elements being the combination of any a kind or at least 2 kinds in magnesium halide, hydroxyhalide magnesium, Magnesium hydrogen carbonate, moisture magnesium halide, magnesium oxide or magnesium hydroxide, reaction is easier to occur, the heat-up rate of reaction is 0.5 ~ 30 DEG C/min, insulation temperature be 200 ~ 600 DEG C, insulation time≤18h.
Preferably, when containing the raw material of magnesium elements being the combination of any a kind or at least 2 kinds in magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern, react more difficult generation, the heat-up rate of reaction is 0.2 ~ 25 DEG C/min, insulation temperature be 230 ~ 600 DEG C, insulation time≤20h.
Those skilled in the art should understand, for the ore containing the described compound containing magnesium elements, the selection of heat-up rate and soaking time also can follow above-mentioned rule, such as, containing magnesiumcarbonate in rhombspar or magnesite, then belong to the ore containing magnesium elements of more difficult reaction, when therefore selecting rhombspar or magnesite to be raw material, the time of the insulation of reaction is slightly long, and the temperature of insulation is slightly high.
Dedoping step of the present invention is: the material after reaction being terminated is dissolved in water, and adjust ph, afterwards solids removed by filtration impurity, obtain the ammonium magnesium sulfate aqueous solution.
After reaction terminates, the impurity effect introduced by the raw material purity of ammonium magnesium sulfate, needs to be removed.The impurity of removal of the present invention comprises the impurity of non-metallic minerals impurity, containing metal element.Non-metallic minerals impurity, as silicon oxide, kaolinite etc., directly water insoluble, filter removal after product of roasting can being dissolved; And containing elementary metal impurities, by regulating the pH value of dissolving rear solution, make non-targeted metal ion form precipitation of hydroxide, remove after filtration in the lump.
The impurity of typical but non-limiting containing metal element is the impurity of the combination of any a kind or at least 2 kinds of elements comprised in iron, aluminium, calcium, lead, mercury, arsenic, manganese, copper, zinc, boron.
The concrete regulation range of described pH value should be selected according to practical situation.
Preferably, pH value of the present invention is 4.5 ~ 10.5, such as 4.6 ~ 4.8,5.0 ~ 5.3,5.5 ~ 5.7,5.8 ~ 6.1,6.5 ~ 7.0,7.2 ~ 7.4,7.8 ~ 8.0,8.3 ~ 8.5,8.6 ~ 8.8,8.9 ~ 9.2,9.2 ~ 9.7,10.2 ~ 10.3 etc., preferably 5.0 ~ 10.0, further preferably 5.0 ~ 9.5, particularly preferably 6.0 ~ 9.0.
Crystallisation process of the present invention is that ammonium magnesium sulfate solution removal of impurities obtained carries out decrease temperature crystalline or evaporative crystallization.
The present invention is not specifically limited for the mode of homogenizing process, comprises various method or the means that can increase mixture homogeneity.Preferably, described homogenizing process be selected from stirring, grind, dry grind, smash, the combination of any a kind or at least 2 kinds in airflow crash.
The reaction of ammonium magnesium sulfate provided by the invention is the little reaction of solid phase or liquid content, therefore, increases the effect that homogenization degree effectively can increase reaction, promotes the quality of product.
Preferably, for the raw material of granularity less (being such as less than 100 μm), stir, grind, dry grind, smash, any a kind of homogenizing that all can realize raw material in airflow crash.
Preferably, for the raw material of granularity comparatively large (being such as greater than 0.1 μm), preferably carry out after agitation grinding, dry grind, smash, the combination of in airflow crash a kind or at least 2 kinds.
After raw material containing magnesium elements of the present invention and ammonium sulfate reaction terminate, can produce by product containing the element beyond the demagging contained in the raw material of magnesium elements, as magnesium oxide and magnesium hydroxide, reaction can produce ammonia; For the magnesium salts containing halogen, reaction can produce ammonium halide; For the magnesium salts containing carbonate or bicarbonate radical, reaction can produce volatile salt or bicarbonate of ammonia; Even also at high temperature can distil for ammonium sulfate, or at high temperature redox reaction occur, generate sulfurous gas, nitrogen and water vapour etc.
And the by product produced in the preparation process of ammonium magnesium sulfate of the present invention often also all has very high chemical industry value, can be collected, for subsequent use.
Preferably, when containing the raw material of magnesium elements be magnesium oxide or magnesium hydroxide time, the by product that reaction produces is mainly ammonia, also may comprise a little water vapour;
Preferably, when the raw material containing magnesium elements is halogen-containing magnesium salts, the by product that reaction produces is mainly ammonium halide;
Preferably, when the raw material containing magnesium elements is the magnesium salts containing carbonate and/or bicarbonate radical, the by product that reaction produces is mainly volatile salt and/or bicarbonate of ammonia.
As optimal technical scheme, the method preparing ammonium magnesium sulfate of the present invention comprises the steps:
(1) mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, obtains raw mixture; Wherein, the ratio of the magnesium elements in mixture and the amount of substance of sulfate radical is in 1:(1.8 ~ 2.6) in scope;
(2) heated up with the heating rate of 0.5 ~ 20 DEG C/min by raw mixture, be warming up to 300 ~ 550 DEG C, insulation 1 ~ 10h, reaction terminates, and obtains ammonium magnesium sulfate.
This technical scheme prepares the process flow sheet of the method for ammonium magnesium sulfate as shown in Figure 1, and Fig. 1 is to be the process flow sheet preparing the method for ammonium magnesium sulfate containing the raw material of magnesium elements containing the compound of magnesium elements.
As another optimal technical scheme, the method preparing ammonium magnesium sulfate of the present invention comprises the steps:
(1) mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, obtains raw mixture; Wherein, the ratio of the magnesium elements in mixture and the amount of substance of sulfate radical is in 1:(1.8 ~ 2.6) in scope;
(2) heated up with the heating rate of 0.5 ~ 20 DEG C/min by raw mixture, be warming up to 300 ~ 550 DEG C, insulation 1 ~ 10h, reaction terminates, and obtains ammonium magnesium sulfate grog;
(3) by soluble in water for the ammonium magnesium sulfate of step (2), adjust ph is 6.0 ~ 9.0, carries out filtering and impurity removing, obtains the solution containing ammonium magnesium sulfate;
(4) moisture evaporation in ammonium magnesium sulfate solution step (3) obtained is saturated to ammonium magnesium sulfate, then carries out crystallization, obtains ammonium magnesium sulfate.
This technical scheme prepares the process flow sheet of the method for ammonium magnesium sulfate as shown in Figure 2, and Fig. 2 is the process flow sheet preparing the method for ammonium magnesium sulfate using the raw mineral materials containing the compound containing magnesium elements as the raw material containing magnesium elements.
Compared with prior art, the present invention has following beneficial effect:
(1) the invention provides a kind of method that solid phase prepares ammonium magnesium sulfate, its reaction process does not have the participation of water, eliminates the step dewatered, and economizes water environmental protection, provides one and prepare ammonium magnesium sulfate new approaches;
(2) production technique of anhydrous magnesium sulfate ammonium provided by the invention is economized and is decrystallized and dehydrating step, shortens reaction process, saves the energy, decrease manpower and equipment investment, green, energy-saving and environmental protection;
(3) production of aqueous magnesium sulfate ammonium provided by the invention, simple for process, energy consumption is less, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the method preparing ammonium magnesium sulfate described in one embodiment of the present invention;
Fig. 2 is the process flow sheet of the method preparing ammonium magnesium sulfate described in another embodiment of the present invention.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) 20kg activated magnesia (purity is 98.5wt%, and water content is less than 1.0wt%) is got and 134kg ammonium sulfate (purity is 99.0wt%) adds V-type mixer, homogenizing 2h, the raw mixture all mixed; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.04;
(2) raw mixture is warming up to 240 DEG C of insulation 18h with the speed of 0.5 DEG C/min, obtains ammonium magnesium sulfate;
(3) collect the gas that reaction produces, and passed in water, by product ammoniacal liquor can be obtained.
Embodiment 2
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) by magnesite powder light-burned 18h at 750 DEG C, light-magnesite powder (content of magnesia is 96.2%) is obtained;
(2) get light calcined magnesia 200g and ammonium sulfate 1200g that step (1) obtains, add dry method ball mill, ball milling homogenizing 1h, is all mixed raw mixture; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:1.82;
(3) raw mixture is warming up to 300 DEG C with the speed of 2 DEG C/min, then is warming up to 500 DEG C of insulation 1h with 1 DEG C/min, obtain ammonium magnesium sulfate grog;
(4) slowly joined in 2000mL deionized water by anhydrous magnesium sulfate ammonium grog, constantly stir, controlling slurry temperature is 80 DEG C;
(5) regulate the pH value of slurry to 6.1-6.3, stir 1h;
(6) by the pulp centrifuged separation that step (5) obtains, obtain solution, solution is cooled to 30 DEG C, evaporation, leave standstill crystallization, gained crystal is six water magnesium sulfate ammoniums.
Embodiment 3
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) get brucite powder (magnesium hydroxide content is 95.7%) 40g, ammonium sulfate 300g to be placed in and to grind Portland and grind homogenizing 2h, all mixed raw mixture; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.35;
(2) mixture that step (1) obtains is warming up to 150 DEG C with the speed of 24 DEG C/min, then is warming up to 590 DEG C of insulation 10min with 0.2 DEG C/min, obtain ammonium magnesium sulfate grog;
(3) slowly joined in 750mL deionized water by anhydrous magnesium sulfate ammonium grog, constantly stir, controlling slurry temperature is 70 DEG C;
(4) regulate pH value to 7.0 ~ 7.2 of slurry, stir 0.5h;
(5) by the pulp centrifuged separation of step (4) gained, obtain solution, solution is cooled to 50 DEG C, evaporation, leave standstill crystallization, gained crystal is six water magnesium sulfate ammoniums.
Embodiment 4
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) get five aqueous magnesium chloride 185g, ammonium sulfate 260g, after mixing in Universalpulverizer homogenizing 1min, all mixed raw mixture; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.02;
(2) gained raw mixture is warming up to 200 DEG C with the speed of 20 DEG C/min, then is warming up to 400 DEG C with the speed of 0.5 DEG C/min, insulation 15min, obtains ammonium magnesium sulfate;
(3) gas recovery condensation, obtains byproduct---ammonium chloride.
Embodiment 5
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) get ground dolomite 184g, ammonium sulfate 380g that granularity is less than 5 μm, homogenizing 1min in Universalpulverizer, obtains mixing raw material; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.88;
(2) above-mentioned compound is warming up to 600 DEG C of insulation 2h with the speed of 1 DEG C/min, both obtains ammonium magnesium sulfate grog;
(3) gas recovery condensation, obtains byproduct---volatile salt;
(4) slowly joined in 350mL deionized water by the anhydrous magnesium sulfate ammonium grog that step (2) obtains, constantly stir, controlling slurry temperature is 70 DEG C;
(5) pH value to 5.5 ~ 6.0 of regulating step (4) gained slurry, stir 0.5h;
(6) by the pulp centrifuged separation of step (5) gained, obtain solution, by solution evaporation, gained crystal is six water magnesium sulfate ammoniums.
Embodiment 6
(1) get magnesite powder 84g, ammonium sulfate 360g that granularity is less than 2 μm, homogenizing 0.5min in Universalpulverizer, is all mixed raw mixture; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.73;
(2) raw mixture is warming up to 300 DEG C with the speed of 15 DEG C/min, then is warming up to 600 DEG C of insulation 3h with 0.2 DEG C/min, both obtain ammonium magnesium sulfate grog;
(3) gas recovery condensation, obtains byproduct---volatile salt;
(4) slowly joined in 850mL deionized water by the anhydrous magnesium sulfate ammonium grog that step (2) obtains, constantly stir, controlling slurry temperature is 80 DEG C;
(5) pH value to 6.5 ~ 7.0 of regulating step (4) gained slurry, stir 0.5h;
(6) by the pulp centrifuged separation of step (5) gained, obtain solution, solution is cooled to 50 DEG C, leave standstill crystallization, gained crystal is six water magnesium sulfate ammoniums.
Embodiment 7
A preparation method for ammonium magnesium sulfate, comprises the steps:
(1) get ammonium carnallite 252.5g, bischofite 203g, ammonium sulfate 530g, mixes after mixing in Universalpulverizer, is all mixed raw mixture; In described mixture, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:2.01;
(2) gained raw mixture is warming up to 350 DEG C of insulation 18h with the speed of 1 DEG C/min, both obtains ammonium magnesium sulfate;
(3) gas recovery condensation, obtains byproduct---ammonium chloride.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a preparation method for ammonium magnesium sulfate, is characterized in that, described method is mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, heat temperature raising, and insulation, after reaction terminates, obtains ammonium magnesium sulfate;
Alternatively, after reaction terminates, through removal of impurities, crystallization, obtains ammonium magnesium sulfate.
2. the method for claim 1, is characterized in that, the speed of described heat temperature raising is 0.2 ~ 30 DEG C/min;
Preferably, the temperature of described insulation is 200 ~ 600 DEG C;
Preferably, described insulation time≤20h;
Preferably, in the mixture be mixed to get containing the raw material of magnesium elements and ammonium sulfate in described method, the ratio of the amount of substance of magnesium elements and sulfate radical is 1:(1.6 ~ 3.0).
3. method as claimed in claim 1 or 2, is characterized in that, the described raw material containing magnesium elements is the compound containing magnesium elements and/or the raw mineral materials containing described compound;
Preferably, the described compound containing magnesium elements is selected from inorganic magnesium compound and/or organo-magnesium compound, the combination of any a kind or at least 2 kinds preferably in magnesium halide, magnesiumcarbonate, Magnesium hydrogen carbonate, hydroxyhalide magnesium, hydroxy carbonate magnesium, magnesium hydroxide or magnesium oxide;
Preferably, described raw mineral materials is selected from the combination of any a kind or at least 2 kinds in the dehydration of magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern and described raw mineral materials and/or product of roasting; Described dehydration and/or maturing temperature are 100 ~ 900 DEG C;
Further preferably, described magnesium halide is selected from the combination of any a kind or at least 2 kinds in magnesium fluoride, magnesium chloride, magnesium bromide or magnesium iodide; Described magnesium oxide is selected from the combination of any a kind or at least 2 kinds in light calcined magnesia, activated magnesia or light magnesium oxide; Described magnesium halide is anhydrous and/or moisture magnesium halide; Described hydroxyhalide magnesium is anhydrous and/or moisture hydroxyhalide magnesium; Described hydroxy carbonate magnesium is anhydrous and/or moisture hydroxy carbonate magnesium.
4. the method as described in one of claims 1 to 3, it is characterized in that, when containing the raw material of magnesium elements being the combination of any a kind or at least 2 kinds in magnesium halide, hydroxyhalide magnesium, Magnesium hydrogen carbonate, magnesium oxide or magnesium hydroxide, heat-up rate is 0.5 ~ 30 DEG C/min, insulation temperature be 200 ~ 580 DEG C, insulation time≤18h;
Preferably, when containing the raw material of magnesium elements being the combination of any a kind or at least 2 kinds in magnesite, rhombspar, brucite, chloromagnesite, bischofite, ammonium carnallite, pinnoite, artinite, bittern, heat-up rate is 0.2 ~ 25 DEG C/min, insulation temperature be 230 ~ 600 DEG C, insulation time≤20h.
5. the method as described in one of Claims 1 to 4, is characterized in that, described dedoping step is: the material after reaction being terminated is dissolved in water, and adjust ph, afterwards solids removed by filtration impurity, obtain the ammonium magnesium sulfate aqueous solution;
Preferably, described pH value is 4.5 ~ 10.5, preferably 5.0 ~ 10.0, further preferably 5.0 ~ 9.5, particularly preferably 6.0 ~ 9.0.
6. the method as described in one of Claims 1 to 5, is characterized in that, described crystallisation process is that ammonium magnesium sulfate solution removal of impurities obtained carries out decrease temperature crystalline or evaporative crystallization.
7. the method as described in one of claim 1 ~ 6, is characterized in that, described homogenizing process is selected from stirring, grinds, dry grinds, smashes, the combination of any a kind or at least 2 kinds in airflow crash.
8. the method as described in one of claim 1 ~ 7, is characterized in that, when containing the raw material of magnesium elements be magnesium oxide or magnesium hydroxide time, the by product that reaction produces is mainly ammonia;
Preferably, when the raw material containing magnesium elements is halogen-containing magnesium salts, the by product that reaction produces is mainly ammonium halide;
Preferably, when the raw material containing magnesium elements is the magnesium salts containing carbonate and/or bicarbonate radical, the by product that reaction produces is mainly volatile salt and/or bicarbonate of ammonia.
9. the method as described in one of claim 1 ~ 8, is characterized in that, described method comprises the steps:
(1) mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, obtains raw mixture; Wherein, the ratio of the magnesium elements in mixture and the amount of substance of sulfate radical is in 1:(1.8 ~ 2.6) in scope;
(2) heated up with the heating rate of 0.5 ~ 20 DEG C/min by raw mixture, be warming up to 300 ~ 550 DEG C, insulation 1 ~ 10h, reaction terminates, and obtains ammonium magnesium sulfate.
10. the method as described in one of claim 1 ~ 8, is characterized in that, described method comprises the steps:
(1) mixed with ammonium sulfate by the raw material containing magnesium elements, homogenizing, obtains raw mixture; Wherein, the ratio of the magnesium elements in mixture and the amount of substance of sulfate radical is in 1:(1.8 ~ 2.6) in scope;
(2) heated up with the heating rate of 0.5 ~ 20 DEG C/min by raw mixture, be warming up to 300 ~ 550 DEG C, insulation 1 ~ 10h, reaction terminates, and obtains ammonium magnesium sulfate grog;
(3) by soluble in water for the reactant of step (2), adjust ph to 6.0 ~ 9.0, carry out filtering and impurity removing, obtain the solution containing ammonium magnesium sulfate;
(4) the ammonium magnesium sulfate solution that step (3) obtains is carried out decrease temperature crystalline or evaporative crystallization, obtain aqueous magnesium sulfate ammonium.
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| CN105271283A (en) * | 2015-11-19 | 2016-01-27 | 中国科学院青海盐湖研究所 | Preparing method for pinnoite |
| CN108164046A (en) * | 2018-01-17 | 2018-06-15 | 郑州轻工业学院 | A kind of method that high-concentration ammonia nitrogenous wastewater and recycling are handled with desulfurization wastewater |
| CN110396610A (en) * | 2019-07-29 | 2019-11-01 | 中国科学院过程工程研究所 | A kind of method of the processing of ammonium salt pressurized pyrolysis titanium mineral and metal silicate mineral |
| CN115991496A (en) * | 2023-02-22 | 2023-04-21 | 西南科技大学 | Preparation method of hydrated magnesium ammonium sulfate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105271283A (en) * | 2015-11-19 | 2016-01-27 | 中国科学院青海盐湖研究所 | Preparing method for pinnoite |
| CN105271283B (en) * | 2015-11-19 | 2017-06-20 | 中国科学院青海盐湖研究所 | The preparation method of pinnoite |
| CN108164046A (en) * | 2018-01-17 | 2018-06-15 | 郑州轻工业学院 | A kind of method that high-concentration ammonia nitrogenous wastewater and recycling are handled with desulfurization wastewater |
| CN110396610A (en) * | 2019-07-29 | 2019-11-01 | 中国科学院过程工程研究所 | A kind of method of the processing of ammonium salt pressurized pyrolysis titanium mineral and metal silicate mineral |
| CN110396610B (en) * | 2019-07-29 | 2020-12-11 | 中国科学院过程工程研究所 | Method for treating titanium minerals and metal silicate minerals through ammonium salt pressure pyrolysis |
| CN115991496A (en) * | 2023-02-22 | 2023-04-21 | 西南科技大学 | Preparation method of hydrated magnesium ammonium sulfate |
| CN115991496B (en) * | 2023-02-22 | 2024-04-30 | 西南科技大学 | Preparation method of hydrated magnesium ammonium sulfate |
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