CN115947347A - Periclase and preparation method thereof - Google Patents
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- CN115947347A CN115947347A CN202310070403.2A CN202310070403A CN115947347A CN 115947347 A CN115947347 A CN 115947347A CN 202310070403 A CN202310070403 A CN 202310070403A CN 115947347 A CN115947347 A CN 115947347A
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Abstract
The invention provides a periclase and a preparation method thereof, which is prepared by adding bischofite or old brine in a salt lake into a sodium borate solution for reaction. The method for preparing the periclase trigonotidis from the bischofite or the old brine which is a byproduct of the salt lake solves the technical problems of low purity, high cost, high energy consumption and the like of the periclase trigonotidis, improves the utilization efficiency of the boron-magnesium and boron resources of the salt lake, and widens the high-value utilization approach of the magnesium-boron resources of the salt lake.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of salt lake resources magnesium and boron, in particular to a trigonellite and a preparation method thereof, and specifically relates to a method for preparing the trigonellite by using salt lake brine or salt lake abundant bischofite.
Background
Boron is a typical non-metallic element, located in the third main group of the second period in the periodic table of elements, and has unique electron-deficient characteristics, and mainly exists in nature in the form of inorganic boric acid and boric acid salts. In borates, boron in the form of a polymeric boroxine complex anion can produce a wide variety of borate compounds with complex structures. The borate has the properties of wear resistance, high strength, flame retardance, heat resistance, corrosion resistance, nonlinear optics and the like, and is widely applied to the fields of metallurgy, machinery, building materials, medicines, pesticides and the like. Magnesium borate is a novel reinforced, antifriction, antiwear and luminescent matrix material. The hydrated magnesium borate is an important chemical raw material, can be used as an additive in the industries of high-grade glass, ceramics, rubber, plastic polymers and the like, has a superior enhancement modification effect, and can also be used as a metal protective agent and a fireproof agent.
Various forms of magnesium borate salts exist in nature, and abundant boron magnesium minerals are stored in salt lake regions of Qinghai-Tibet plateau in China, for example, the number of magnesium borate salts in 9 types of borate minerals found in the great Chadan lake region is 5: bordetella columna (MgO.3) 2 O 3 ·3H 2 O), polyboromagnesite (2 MgO.3B) 2 O 3 ·15H 2 O), cokeite (2 MgO.3B) 2 O 3 ·15H 2 O), octo-boron magnesium stone (MgO.2B) 2 O 3 ·9H 2 O) and periclase (MgO.3B) 2 O 3 ·7.5H 2 O). In order to explore the forming conditions of different magnesium borate salts, high-rise academicians in China carry out a great deal of basic research on the formation and the conversion of the magnesium borate salts under the conditions of low temperature and high temperature, provide experimental basis for the geochemical cause of the boresite of the Qinghai-Tibet plateau, and provide a new way for the preparation, the property, the development and the utilization of the magnesium borate.
Currently, common hydrated magnesium hexaborate is MgO.3b 2 O 3 ·7.5H 2 O (periclase), mgO.3b 2 O 3 ·7H 2 O and MgO 3b 2 O 3 6H2O, etc. The research on the evaporation, salting-out, concentration, freezing and dilution with water of magnesium sulfate subtype bittern and MgO & nB 2 O 3 -MgCl 2 -H 2 When the O concentrated salt solution is crystallized, the periclase, mainly a mixture of magnesium hexaborate, can be prepared, and the salting-out time is relatively long. Kipcaket et al in The Synthesis and physical properties of magnesium salts of ammonium synthesized from sodium salts [ J]Advances in Materials Science and engineering,2014, 2014:1-9 proposed the chemical formula of MgO and B 2 O 3 And H 3 bO 3 The products of the method for synthesizing magnesium hexaborate in different proportions are mostly mixtures of magnesium borate. Meral Yildirim et al in Sonochemical-assisted magnesium borate synthesis from different boron sources[J]Polish Journal of Chemical Technology,2017, 19 (1): in 81-88, magnesium chloride hexahydrate (MgCl) was studied respectively by using ultrasonic-assisted conditions 2 ·6H 2 O) and borax (Na) 2 b 4 O 7 ·10H 2 O), boric acid (H) 3 bO 3 ) And boron oxide (B) 2 O 3 ) The method synthesizes the periclase with different boron sources, the reaction temperature is 60-100 ℃, the ultrasonic time is 5-20 min, the research improves the synthesis rate, shortens the reaction time, but the product purity is lower. The Chinese patent application CN101696017A uses basic magnesium carbonate or magnesium oxide as a raw material to prepare activated magnesium oxide, and then uses the activated magnesium oxide, boric acid and water as raw materials to prepare magnesium hexaborate through mixing reaction, crystallization, filtration, washing and drying according to a certain mass ratio. The Chinese patent CN101746770A mixes boric acid and magnesium compound with organic solvent, and carries out the processes of azeotropic distillation, solvent removal, drying treatment and the like to prepare hydrated magnesium borate. The Chinese patent CN101177274A takes industrial boric acid and light-burned magnesium as raw materials, the hydrothermal reaction is carried out for 6 to 16 hours at 100 to 250 ℃ and 0.1 to 3.5MP, then the product is aged and crystallized for 0.5 to 6 hours at 60 to 95 ℃, and the product is obtained by filtering, washing and drying. The magnesium borate prepared by the technical scheme adopted by the prior art has the defects of low product purity, long process flow and the like, and the adopted raw materials are mostly chemical raw materials, so that the cost and energy consumption for preparing the product are higher, and the large-scale application and popularization of the product are limited.
On the other hand, salt lake old brine is rich in a large amount of magnesium ions, and is mostly discharged back to the salt lake in a remote discharge mode at present to form bischofite through solarization and evaporation; with the continuous expansion of the production scale of potassium chloride, the salt lake old brine generated along with the potassium chloride and the bischofite which is a byproduct obtained by adopting the treatment mode are increased year by year, so that not only is the waste of magnesium resources caused, but also the natural ecological balance of the salt lake is seriously influenced. Therefore, how to improve the utilization rate of the old brine in the salt lake or the bischofite in the salt lake and relieve the environmental problems brought by the magnesium resource in the salt lake also becomes a technical problem to be solved urgently.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a method for preparing the trigonal boron magnesium stone, which is used for preparing the trigonal boron magnesium stone by taking bischofite or old brine which is a byproduct of a salt lake as a raw material, solves the technical problems of low purity, high cost, high energy consumption and the like of the trigonal boron magnesium stone, improves the utilization efficiency of the boron and magnesium resources of the salt lake, and widens the high-valued utilization approach of the boron and magnesium resources of the salt lake.
In order to achieve the purpose, the invention provides the following technical scheme that the preparation method of the periclase trigonotide is prepared by adding bischofite in a salt lake or old brine in the salt lake into a sodium borate solution for reaction. Wherein the content of magnesium ions and boron (as B) 2 O 3 Calculated) is 2.5-24: 1.
Preferably, the sodium borate solution is in the form of H 3 BO 3 Adding deionized water into the raw materials and then heating and stirring the mixture to react to obtain the aqueous solution; the heating temperature is 25-80 ℃.
Preferably, H 3 BO 3 The molar ratio of the NaOH to the NaOH is 2-7: 1; mass of deionized water is H 3 BO 3 5 to 15 times of the mass.
Preferably, the salt lake old brine is diluted and then added into a sodium borate solution, the dilution ratio is that the volume ratio of water to the salt lake old brine is 1-4, and the pH value is adjusted to be 4-7.
Preferably, the volume of the salt lake old brine is 1-4 times of the volume of the sodium borate solution.
Preferably, the bischofite of the salt lake or the diluted old brine of the salt lake is added into the sodium borate solution, wherein the old brine of the salt lake is added at one time or in equal amount-in batches.
Preferably, the content of magnesium ions in the salt lake old brine is 100-120g/L, and the content of boron is B 2 O 3 The weight is 5-40g/L.
Preferably, the purity of the bischofite in the salt lake is 90-98%.
Preferably, the periclase in the salt lake or the product obtained after the reaction of the old brine in the salt lake and the sodium borate solution is crystallized and separated out, and the periclase is obtained after the treatment of the processes of solid-liquid separation, solid-phase washing and drying.
Preferably, the washing liquid in the solid phase washing process is one or two of deionized water and ethanol, and the mass ratio of the washing liquid to the solid phase is 6: 1-15: 1; in the drying process, the drying temperature is 25-70 ℃, and the drying time is 0.5-10 h.
The periclase prepared by the preparation method is hexagonal flaky fine crystals with the crystal granularity of 5-10 mu m.
The old brine of the salt lake is also called bitter brine, halogen alkali and old brine, and is prepared by evaporating and cooling mother liquor remained in a salt pond after salt is prepared from seawater or salt lake water, separating out magnesium chloride crystals, and generating solid, namely bischofite. Specifically, the main components of the old brine of the salt lake comprise: magnesium ion, sodium ion, potassium ion, sulfate ion, chloride ion and B 2 O 3 And the like. The chemical formula of the bischofite in the salt lake is MgCl 2 ·6H 2 O, pure substance, no other component.
In the invention, salt lake old brine or salt lake bischofite is used as a raw material and reacts with sodium borate, and the specific reaction mechanism comprises the following steps:
by the above mechanism, it can be seen that boric acid reacts with sodium hydroxide to produce a sodium pentaborate solution, producing polyborate ions such as B 3 O 3 (OH) 4 - 、B 5 O 6 (OH) 4 - And B (OH) 4 - Ions, addition of bischofite promoting B 3 O 3 (OH) 4 - The ions are subjected to polycondensation reaction to generate B 6 O 7 (OH) 7 2- And ions are combined with magnesium ions to generate periclase, and crystallization is carried out.
The technical effect of the technical scheme of the invention is as follows:
1. by adopting the technical scheme of the invention, the salt lake old brine or the salt lake bischofite serving as a byproduct of the salt lake is used as a raw material to react with sodium borate, so that the technical problems of complex technological process, high cost, high energy consumption and the like of the trigonellite are solved, the utilization efficiency of the salt lake magnesium boron resource is improved, the utilization value of the salt lake magnesium boron resource is improved, and the high-value utilization way of the salt lake magnesium boron resource is widened.
2. By adopting the technical scheme of the invention, the salt lake byproduct is used as the raw material, the production cost is reduced, the energy consumption in the production process is low, the preparation process is simple, and the preparation method is suitable for large-scale application and popularization.
3. By adopting the technical scheme of the invention, the salt lake by-products are fully utilized, the serious damage to the natural ecological balance of the salt lake caused by discharging the salt lake old brine back to the salt lake is relieved, and the magnesium resource can be fully utilized to promote the conversion of the salt lake old brine in a high-value direction.
4. The components of the product of the periclase prepared by the technical scheme of the invention are close to theoretical values, and the method has the advantages of high purity and low cost.
Drawings
Fig. 1 is an XRD pattern of the solid periclase phase prepared in examples 1 and 2 of the present invention.
Fig. 2 is an SEM image of periclase prepared in example 3 of the present invention.
Fig. 3 is a thermogravimetric analysis diagram of the periclase prepared in example 4 of the present invention.
Detailed Description
The purpose, technical solutions and advantages of the embodiments of the present invention are made clearer, and the technical solutions in the embodiments of the present invention are clearly and completely described. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of periclase, which is prepared by adding bischofite in a salt lake or old brine in the salt lake into a sodium borate solution for reaction; wherein, the salt lake old brine contains magnesium ion content and boron content (as B) 2 O 3 Calculated) is 2.5-24: 1; preferably 20-24: 1.
In a preferred embodiment, the sodium borate solution is in the form of H 3 BO 3 Adding deionized water into the raw materials and then heating and stirring the mixture to react to obtain the aqueous solution; the heating temperature is 25-80 ℃.
In a preferred embodiment, H 3 BO 3 The molar ratio of the NaOH to the NaOH is 2-7: 1; mass of deionized water is H 3 BO 3 5 to 15 times of the mass.
In a preferred embodiment, the salt lake old brine is diluted and then added into the sodium borate solution, the dilution ratio is that the volume ratio of water to the salt lake old brine is 1-4, and the pH value is adjusted to be 4-7.
In a preferred embodiment, the volume of the salt lake old brine is 1 to 4 times of the volume of the sodium borate solution.
In a preferred embodiment, equal amounts of bischofite from a salt lake or diluted old brine from a salt lake are added in portions to the sodium borate solution.
In a preferred embodiment, the content of magnesium ions in the salt lake old brine is 100-120g/L, and the content of boron is B 2 O 3 The weight is 5-40g/L.
In a preferred embodiment, the periclase in the salt lake or the product obtained after the reaction of the old brine in the salt lake and the sodium borate solution is crystallized and separated out, and the periclase is obtained after the treatment of solid-liquid separation, solid-phase washing and drying processes.
In a preferred embodiment, the washing liquid in the solid phase washing process is one or two of deionized water and ethanol, and the mass ratio of the washing liquid to the solid phase is 6: 1-15: 1; in the drying process, the drying temperature is 25-70 ℃, and the drying time is 0.5-10 h.
The technical means of the present invention will be described in further detail with reference to specific examples.
Example 1
The embodiment provides a method for preparing periclase, which comprises the following specific steps:
1. weigh 7.80g of H 3 BO 3 And 1.02g of NaOH, adding 40.0g of deionized water, heating and stirring to fully dissolve the sodium borate, and reacting to obtain a sodium borate solution.
2. Adding 120mL of diluted 1-time old salt lake brine into the sodium borate solution in the step 1 at one time, wherein the magnesium ions in the old salt lake brine are 100g/L, and B 2 O 3 5g/L and the pH value is 5.0, so that after the salt lake old brine is completely dissolved, the salt lake old brine reacts for 2 hours in a thermostatic water bath under the temperature condition of 25 ℃ by magnetic stirring, and a solid is crystallized and separated out.
3. And (3) carrying out solid-liquid separation on the product obtained in the step (2), washing the solid phase for 2 times by using water slurry, wherein the liquid-solid ratio is 6: 1, and drying the washed product for about 4 hours at 40 ℃ to obtain the periclase trilateral product.
Example 2
This example differs from example 1 in that the magnesium ion content in the old brine of salt lake is 120g/L, B 2 O 3 Is 5g/L.
Example 3
This example differs from example 1 in that the magnesium ion content in the salt lake old brine is 100g/L, B 2 O 3 The concentration was 40g/L.
Example 4
This example differs from example 1 in that magnesium is present in the old brine of the salt lakeIon 120g/L, B 2 O 3 The concentration was 40g/L.
Example 5
The difference between this example and example 1 is that in step 2, salt lake old brine is completely dissolved in sodium borate solution, and the reaction is magnetically stirred for 2 hours in a thermostatic water bath at the temperature of 40 ℃, so as to crystallize and separate out solid.
Example 6
The difference between this example and example 1 is that in step 2, salt lake old brine is completely dissolved in sodium borate solution, and the reaction is magnetically stirred for 2 hours in a thermostatic water bath at the temperature of 60 ℃, so as to crystallize and separate out solid.
Example 7
The difference between this example and example 1 is that in step 2, salt lake old brine is completely dissolved in sodium borate solution, and the reaction is magnetically stirred for 2 hours in a thermostatic water bath at the temperature of 80 ℃, so as to crystallize and separate out solid.
Example 8
This example differs from example 3 in that 120mL of 4-fold diluted old salt lake brine is added in 4 times in equal amount in the sodium borate solution prepared in step 1, each batch is added for 2 minutes, wherein the magnesium ion content in the old salt lake brine is 100g/L, and B is 2 O 3 The concentration was 40g/L.
Example 9
The embodiment provides a preparation method of periclase, which comprises the following specific steps:
1. weigh 7.80g of H 3 bO 3 And 1.02g of NaOH, adding 100.0g of deionized water, heating and stirring to fully dissolve the NaOH solution to obtain a sodium borate solution.
2. Adding 200mL of diluted 4-time old salt lake brine into the sodium borate solution in the step 1 in 4 times in equal amount, wherein the adding time interval of each batch is 2 minutes, the magnesium ions in the old salt lake brine are 120g/L, B 2 O 3 40g/L and pH 7.0, and after both are completely dissolved, the mixture is magnetically stirred in a thermostatic water bath at the temperature of 40 ℃ for reaction for 15 hours, and then a solid is crystallized and precipitated.
3. And (3) performing solid-liquid separation on the product in the step (2), washing the solid phase for 2 times by using water and ethanol slurry, wherein the liquid-solid ratio is 15: 1, and drying the washed product at 40 ℃ for 6 hours to obtain a periclase product.
Example 10
The embodiment provides a method for preparing periclase, which comprises the following specific steps:
1. weigh 7.80g of H 3 bO 3 And 1.02g of NaOH, adding 78.0g of deionized water, heating and stirring to fully dissolve the NaOH solution to obtain a sodium borate solution.
2. And (2) adding 150.0g of 90% pure chloromagnesite into the sodium borate solution in the step 1 in 10 batches in equal amount, wherein each batch is separated by 2 minutes, and after the two are completely dissolved, carrying out magnetic stirring reaction in a constant-temperature water bath at the temperature of 80 ℃ for 20 hours, and crystallizing to separate out a solid.
3. And (3) carrying out solid-liquid separation on the product obtained in the step (2), washing the solid phase for 3 times by using ethanol slurry, wherein the liquid-solid ratio is 8: 1, and drying the washed product for 0.5 hour at 70 ℃ to obtain the periclase product.
Example 11
The embodiment provides a preparation method of periclase, which comprises the following specific steps:
1. weigh 7.80g of H 3 bO 3 And 1.02g of NaOH, adding 80.0g of deionized water, heating and stirring to fully dissolve the mixture to obtain a sodium borate solution.
2. 60.0g of 98% pure chloromagnesite in a salt lake is added into the sodium borate solution in the step 1 in 7 times with equal amount, each batch is separated for 2 minutes, after the two are completely dissolved, the mixture is magnetically stirred in a thermostatic water bath at the temperature of 60 ℃ to react for 20 hours, and then solid is crystallized and precipitated.
3. And (3) carrying out solid-liquid separation on the product obtained in the step (2), washing the solid phase for 3 times by using water slurry, wherein the liquid-solid ratio is 10: 1, and airing the washed product for 10 hours at 25 ℃ to obtain the periclase trilateral product.
And (3) performance characterization:
referring to FIG. 1, XRD diffraction patterns of the respective periclase obtained from example 1 (crystalline solid phase at 25 ℃), from example 2 (crystalline solid phase at 40 ℃) and from standard periclase are shown from top to bottom. By analyzing the figure 1, the synthesized crystal has strong peaks and sub-strong peaks at 10.1 degrees, 15.3 degrees, 21.8 degrees, 27.2 degrees and 31.9 degrees, each diffraction peak corresponds to the standard spectrum of the trilobeite XRD, and the XRD diffraction patterns of the example 1 and the example 2 are consistent with the standard diffraction pattern.
Meanwhile, the solid phase components of example 1 and example 2 were analyzed. The boron content is determined by an alkaline method in the presence of mannitol and is B 2 O 3 Represents; the magnesium content was measured by the EDTA volumetric method and expressed as MgO.
Example 1 (crystalline solid phase at 25 ℃ C.), solid component MgO 10.48wt%, B 2 O 3 54.44wt%; example 2 (crystalline solid phase at 40 ℃ C.), solid phase component MgO 10.50wt%, B 2 O 3 54.42wt%; the theoretical components of the periclase are MgO 10.49wt% and B 2 O 3 54.35wt%。
SEM characterization of the periclase product prepared in example 3 was performed, see fig. 2. As shown in FIG. 2, the periclase is a hexagonal flaky fine crystal having a crystal size of 5 to 10 μm.
Thermogravimetric analysis was performed on the periclase product prepared in example 11, and the thermogravimetric analysis spectrum is shown in fig. 3.
As shown in FIG. 3, the periclase has an endothermic peak at 150-229 deg.C due to the removal of crystal water; 780 ℃ has an exothermic valley, which is an exothermic reaction caused by recrystallization of the amorphous substance after crystal water is removed. At 760-830 ℃, there is an exothermic valley for the exothermic reaction caused by recrystallization of the amorphous material after the water of crystallization is removed. With Quyihua et al, sporobolote, a new borate mineral [ J ], geological report, 1965, 45 (3), gaoyuan et al, halogenoborate chemical II, magnesium hexaborate MgO.3b precipitated from boron-containing concentrated magnesium chloride brine 2 O 3 ·7.5H 2 O [ J ], reported in the chemical bulletin, 1983, 41 (3). Further, the weight loss of periclase is 35.89%, which is close to the theoretical water content of 35.16% for the compound.
Table 1 table for analyzing solid phase composition of periclase prepared in example 1
As can be seen from the results in Table 1, examples 1 to 11 are examples of salt lake old brine having different ratios of magnesium and boron and different process conditions, and are crystallized respectively to form solid phase products of periclase, and the solid phase component contents thereof are close to theoretical values.
Further, examples 1 to 4 are examples of different ratios of magnesium and boron, and the content of magnesium ions and boron (as B) in the salt lake old brine 2 O 3 Calculated) is 2.5-24: 1; examples 1 and 2 are preferred examples, magnesium ion content and boron content (as B) 2 O 3 Calculated) is 20-24: 1.
The examples 1 and 5 to 7 are examples at different reaction temperatures, respectively, and the solid phase component analysis results at 25 ℃ (example 1) are superior to those at other temperatures (40 ℃,60 ℃,80 ℃), and it is clear from the test results of the present invention that the preparation of periclase at 25 ℃ can reduce energy consumption, the reaction conditions are milder, and better test results are obtained.
Example 3 and example 8 are the same magnesium boron ratio condition, salt lake old brine is diluted by different times and added into boric acid solution in equal amount-batch for reaction comparison, and the purity of the periclase is improved after dilution by higher times. The purity of the periclase prepared in example 8 was superior to that of the periclase prepared in example 3.
In both examples 10 and 11, the periclase was prepared from bischofite in a salt lake as a raw material, and the preferable results were obtained.
Therefore, the analysis of the XRD diffraction pattern, the solid phase components and the test result of thermogravimetric analysis shows that the product prepared by the technical scheme of the invention is the periclase, and the purity can be close to a theoretical value.
According to the characterization results of the embodiments, the technical scheme of the invention is adopted, and biscompartite is obtained by using biscompartite in a salt lake or salt lake old brine as a raw material and reacting with a sodium borate solution, and the preparation method has the characteristics of simple preparation process and low energy consumption. The preparation process adopts the salt lake old brine or the salt lake bischofite as the raw material, has the characteristic of low cost, can improve the utilization rate of the salt lake old brine or the salt lake bischofite, and relieves the technical problem caused by the magnesium harm of the salt lake.
The above is only a preferred embodiment of the present invention, which is not intended to limit the scope of the present invention, and various modifications and variations of the present invention are possible to those skilled in the art. Variations, modifications, substitutions, integrations and parameter changes of the embodiments may be made without departing from the principle and spirit of the invention, which may be within the spirit and principle of the invention, by conventional substitution or may realize the same function.
Claims (10)
1. A preparation method of periclase is characterized in that bischofite or salt lake old brine is added into a sodium borate solution to react to prepare the periclase.
2. The method of claim 1, wherein said sodium borate solution is in the form of H 3 bO 3 Adding deionized water into the raw materials and then heating and stirring the mixture to react to obtain the aqueous solution; the heating temperature is 25-80 ℃.
3. The method of producing terse according to claim 2, wherein H is H 3 BO 3 The molar ratio of the NaOH to the NaOH is 2-7: 1; mass of deionized water is H 3 bO 3 5 to 15 times of the mass.
4. The method of claim 1, wherein the salt lake old brine is diluted and added to a sodium borate solution, the dilution ratio is such that the volume ratio of water to the salt lake old brine is 1-4, and the pH is adjusted to 4-7.
5. The method of claim 4, wherein the volume of the salt lake brine is 1-4 times of the volume of the sodium borate solution.
6. The method of claim 5, wherein said bischofite or said diluted old brine of said salt lake is added to said sodium borate solution; wherein, the salt lake old brine is added in one time or in equal batch.
7. The method of producing terludwigite according to any one of claims 1 to 6, wherein the salt lake old brine has a magnesium ion content of 100 to 120g/L and a boron content of B 2 O 3 5-40g/L; the purity of the bischofite in the salt lake is 90-98%.
8. The method for preparing terludwigite according to claim 7, wherein the terludwigite is obtained by crystallizing and separating out the product of the reaction of the bischofite in the salt lake or the old brine in the salt lake and the sodium borate solution, and performing solid-liquid separation, solid-phase washing and drying processes.
9. The method for preparing periclase according to claim 7, wherein the washing solution in the solid phase washing process is one or both of deionized water and ethanol, and the mass ratio of the washing solution to the solid phase is 6: 1-15: 1; in the drying process, the drying temperature is 25-70 ℃, and the drying time is 0.5-10 h.
10. A periclase prepared by the method of any one of claims 1 to 9; the periclase is hexagonal flaky fine crystal with the crystal granularity of 5-10 mu m.
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CN118343779A (en) * | 2024-04-25 | 2024-07-16 | 青海中信国安锂业发展有限公司 | A simple method for preparing Zhang's boraxite and boraxite |
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CN112079362A (en) * | 2019-06-14 | 2020-12-15 | 中国科学院青海盐湖研究所 | Preparation method of polyboromagnesite |
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CN101696017A (en) * | 2009-09-30 | 2010-04-21 | 河南理工大学 | A kind of preparation method of magnesium hexaborate |
CN112079362A (en) * | 2019-06-14 | 2020-12-15 | 中国科学院青海盐湖研究所 | Preparation method of polyboromagnesite |
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