Beryllium ore dissociation and beryllium oxide preparation method

Abstract

The invention relates to the technical field of inorganic materials, in particular to a beryllium ore dissociation and beryllium oxide preparation method which comprises the following steps: adding an aluminum-containing material or a silicon-containing material to adjust the ratio of silicon to aluminum in beryllium ore; under the alkaline and high-pressure conditions, water is used as a leaching medium to leach the beryllium ore subjected to silicon and aluminum element ratio adjustment, the beryllium-rich leachate is obtained, and the problems that in beryllium smelting preparation in the prior art, beryllium ore is not prone to dissociation, the element yield is low, pollution is large, and waste liquid treatment is difficult are solved. According to the method disclosed by the invention, dissociation of various beryllium ores can be realized, and beryllium leaching can be realized by using the method no matter easy-to-smelt beryl stone and bertrandite or low-grade chrysoberyl and the like; the purity of beryllium oxide is greater than 96%; and the beryllium element yield of the beryllium ore is greater than 96%.

Description

Technical Field

[0001] The invention relates to the technical field of beryllium industry, and in particular to a method for dissociating beryllium ore and preparing beryllium oxide. Background Art

[0002] Beryllium is an indispensable and important material in atomic energy, rockets, missiles, aviation and metallurgical industries, but it is extremely harmful to the environment. Although my country has large reserves of beryllium resources, most of them exist in the form of co-existing ores, the quality of beryllium concentrate is poor, the output is not high, and the country is highly dependent on imports. In view of the unfavorable form of excessive dependence on foreign beryllium ore resources and the bottleneck problem of independent supply of beryllium resources that needs to be solved urgently, the development and utilization of complex beryllium associated mineral resources has become an inevitable choice for the sustainable development of my country's beryllium industry.

[0003] In the prior art, acid leaching is mainly used to dissociate beryllium ore, mainly sulfuric acid method and fluoridation method. The existing process of extracting beryllium from beryllium ore has the following defects: on the one hand, during acid leaching, the associated element ions (such as trivalent iron) of beryllium in the beryllium ore will be introduced into the leachate, and the associated element ions often affect the separation effect of beryllium and cause the loss of beryllium. The decrease in the recovery rate of beryllium will cause some beryllium to flow into the nature, causing pollution; on the other hand, soluble alkaline substances (sodium hydroxide or ammonia water) need to be added during the extraction process to adjust the acidity of the solution in the extraction process, resulting in the introduction of soluble alkali cations into the leachate, greatly increasing the difficulty of subsequent wastewater treatment. Therefore, there is an urgent need for an efficient and environmentally friendly method for dissociating beryllium ore and preparing beryllium oxide in the market. Summary of the invention

[0004] In view of the above analysis, the present invention aims to provide a method for dissociating beryllium ore and preparing beryllium oxide, which solves at least one of the problems existing in the prior art of beryllium smelting and preparation, namely, low beryllium element yield, low purity of beryllium product, high pollution and difficulty in waste liquid treatment.

[0005] The purpose of the present invention is mainly achieved through the following technical solutions:

[0006] A method for dissociating beryllium ore and preparing beryllium oxide, comprising:

[0007] Add aluminum-containing materials or silicon-containing materials to adjust the ratio of silicon and aluminum elements in the beryllium ore;

[0008] Under alkaline and high-pressure conditions, water is used as a leaching medium to leach beryllium ore with adjusted silicon and aluminum element ratios to obtain a beryllium-rich leaching solution.

[0009] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide further comprises: utilizing the difference in solubility of beryllium and aluminum in solutions with different pH values ​​to separate beryllium and aluminum elements in the beryllium-rich leaching solution.

[0010] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide comprises:

[0011] Step 1, beryllium ore is refined to obtain beryllium ore powder within a target particle size range;

[0012] Step 2, adding an appropriate amount of aluminum-containing material or silicon-containing material according to the content of silicon and aluminum in the beryllium ore, and then adding an alkaline solution to perform a pressure boiling leaching reaction at a pressure greater than normal pressure, and filtering the leachate to obtain a beryllium- and aluminum-rich leachate;

[0013] Step 3: After the beryllium- and aluminum-rich leaching solution is diluted and boiled, beryllium hydroxide precipitate is obtained to achieve separation of beryllium and aluminum.

[0014] Preferably, in step 2, the molar amount of aluminum is 1 to 1.5 times the molar amount of silicon.

[0015] Preferably, during leaching in step 2, the liquid-solid volume ratio of the leaching medium to the beryllium ore satisfies: 4:1 to 10:1.

[0016] Preferably, the heating temperature during leaching in step 2 is between 150°C and 300°C.

[0017] Preferably, during leaching in step 2, the amount of alkali in the leaching medium satisfies: 150 g / L to 300 g / L.

[0018] Preferably, the alkali used for leaching in step 2 is one or more of sodium hydroxide and potassium hydroxide.

[0019] Preferably, in step 2, the aluminum-containing material is aluminum oxide or aluminum salt, and the silicon-containing material is silicon dioxide or silicate.

[0020] A beryllium oxide is prepared by the above-mentioned beryllium ore dissociation and beryllium oxide preparation method, and the purity of the beryllium oxide is ≥96%.

[0021] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects:

[0022] (1) The present invention adjusts the ratio of silicon and aluminum in the beryllium ore and leaches the beryllium ore under alkaline conditions by pressure cooking, so that silicon, iron, calcium and magnesium are retained in the leached slag, thereby achieving separation of impurity elements from beryllium and obtaining a beryllium-rich leachate. The above operation, on the one hand, retains silicon in the leached slag, avoiding silicon from entering the leachate in the form of silicate under an alkaline environment; on the other hand, compared with the acid leaching beryllium process in the prior art, avoids the introduction of associated element ions of beryllium in the beryllium ore (such as trivalent iron) into the leachate, reducing the loss of beryllium and the flow of beryllium into the natural world to cause pollution; at the same time, it avoids the introduction of cations of soluble alkali during the extraction process, reducing the difficulty of subsequent wastewater treatment. The method of the invention can realize the dissociation of various beryllium ores, and can be used to leach beryllium from beryl, beryllite, or chrysoberyl with low grade, which are easy to smelt. The purity of beryllium oxide is greater than 96%; and the beryllium element yield of beryllium ore is greater than 96%.

[0023] (2) The present invention reduces the alkalinity of the leachate by diluting the beryllium-rich leachate, and obtains beryllium hydroxide precipitate and aluminum solution by heating or even boiling, thereby achieving the separation of aluminum and beryllium without adding a pH adjusting reagent and without introducing new anionic and cationic impurities. Compared with the traditional method, the separation process can effectively reduce the reagent consumption and the treatment amount of aluminum-containing waste liquid, thereby reducing the cost and environmental damage.

[0024] (3) Compared with the traditional extraction method of beryllium, the solution of the present invention does not have an extraction phase and impure cations introduced. The aluminum-rich leachate obtained after filtration can be directly reused as an aluminum-containing raw material. At the same time, the alkali in the aluminum-rich leachate is recycled, which reduces the waste liquid recovery and the discharge treatment cost, and effectively solves the discharge problem of beryllium-containing wastewater; at the same time, the alkali, aluminum, and a small amount of unprecipitated beryllium are recycled, which improves the recovery rate of beryllium, reduces the treatment cost of beryllium ore, and reduces pollution to the environment.

[0025] Other features and advantages of the present invention will be described in the following description, and some advantages may become apparent from the description, or may be understood by practicing the present invention. The purpose and other advantages of the present invention may be realized and obtained through the contents particularly pointed out in the embodiments of the description and the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 : A process flow chart of a beryllium ore smelting method of the present invention. DETAILED DESCRIPTION

[0027] The preferred embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings, wherein the accompanying drawings constitute a part of the present invention and are used together with the embodiments of the present invention to illustrate the principles of the present invention, but are not used to limit the scope of the present invention.

[0028] In one aspect, the present invention discloses a method for dissociating beryllium ore and preparing beryllium oxide, the method comprising:

[0029] Add aluminum-containing materials or silicon-containing materials to adjust the ratio of silicon and aluminum elements in the beryllium ore;

[0030] Under alkaline and high-pressure conditions, water is used as a leaching medium to leach beryllium ore with adjusted silicon and aluminum element ratios to obtain a beryllium-rich leaching solution.

[0031] During implementation, aluminum-containing materials or silicon-containing materials are introduced according to the silicon and aluminum contents in the beryllium ore, and a suitable aluminum-silicon ratio is maintained during the autoclave process, so that the silicon and aluminum in the ore can enter the slag in the form of water and sodium aluminosilicate. After filtration, the separation of beryllium and impurity element silicon can be effectively achieved.

[0032] It should be noted that the impurities of iron oxide, calcium oxide and magnesium oxide in the ore are difficult to be dissolved by the reaction and will also enter the slag together; after filtering, beryllium can be effectively separated from the impurity elements of iron, calcium and magnesium, and beryllium and part of the aluminum enter the leachate, effectively solving the problem of the introduction of associated elements.

[0033] It should be noted that the high pressure referred to in the present invention is a pressure far greater than one atmospheric pressure, for example, it can be 8MPa to 15MPa.

[0034] Compared with the prior art, the present invention adjusts the ratio of silicon and aluminum in the beryllium ore, and leaches the beryllium ore under alkaline conditions by pressure cooking, so that silicon, iron, calcium and magnesium are retained in the leached slag, thereby achieving the separation of impurity elements and beryllium, and obtaining a beryllium-rich leachate. The above operation, on the one hand, retains silicon in the leached slag, avoiding silicon from entering the leachate in the form of silicate under an alkaline environment; on the other hand, compared with the acid leaching beryllium process in the prior art, avoids the introduction of associated element ions of beryllium in the beryllium ore (such as trivalent iron) into the leachate, reducing the loss of beryllium and the flow of beryllium into the natural world to cause pollution; at the same time, it avoids the introduction of cations of soluble alkali during the extraction process, reducing the difficulty of subsequent wastewater treatment.

[0035] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide further comprises: utilizing the difference in solubility of beryllium and aluminum in solutions with different pH values ​​to separate beryllium and aluminum elements in the beryllium-rich leaching solution.

[0036] Specifically, the method of separating beryllium and aluminum elements in a beryllium-rich leaching solution by utilizing the difference in solubility of beryllium and aluminum in solutions of different pH values ​​includes: reducing the alkalinity of the beryllium-rich leaching solution by diluting the beryllium-rich leaching solution; and heating the low-alkalinity beryllium-rich leaching solution to obtain beryllium hydroxide precipitate.

[0037] During implementation, the alkalinity of the leachate is reduced by dilution based on the difference in solubility between beryllium and aluminum in the precipitation range and at different pH values; heating or even boiling can cause beryllium to form beryllium hydroxide precipitate, while aluminum remains in the solution in ionic form, thereby achieving the separation of aluminum and beryllium elements.

[0038] Compared with the prior art, the present invention reduces the alkalinity of the leachate by diluting the beryllium-rich leachate, and obtains beryllium hydroxide precipitate and aluminum solution by heating or even boiling, thereby realizing the separation of aluminum and beryllium without adding a pH adjusting reagent and without introducing new anionic and cationic impurities. Compared with the traditional method, the separation process can effectively reduce the reagent consumption and the treatment amount of aluminum-containing waste liquid, thereby reducing the cost and environmental harm.

[0039] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide comprises:

[0040] Step 1, beryllium ore is refined to obtain beryllium ore powder within a target particle size range;

[0041] Step 2, adding an appropriate amount of aluminum-containing material or silicon-containing material according to the content of silicon and aluminum in the beryllium ore, and then adding an alkaline solution to perform a pressure boiling leaching reaction at a pressure greater than normal pressure, and filtering the leachate to obtain a beryllium- and aluminum-rich leachate;

[0042] Step 3: After the beryllium- and aluminum-rich leaching solution is diluted and boiled, beryllium hydroxide precipitate is obtained to achieve separation of beryllium and aluminum.

[0043] Preferably, the particle size of the mineral powder described in step 1 is above 30 mesh, preferably 100-200 mesh, and can be 100 mesh, 110 mesh, 120 mesh, 130 mesh, 140 mesh, 150 mesh, 160 mesh, 170 mesh, 180 mesh, 190 mesh or 200 mesh.

[0044] It should be noted that the smaller the particle size of the mineral powder, the more conducive it is to increasing the subsequent reaction speed and reaction degree, which helps to increase the beryllium yield; but if the particle size of the mineral powder is too small, the cost of refining processing will increase, and the beryllium yield will not be further improved.

[0045] Preferably, in step 2, the molar amount of aluminum is 1 to 1.5 times the molar amount of silicon.

[0046] It should be noted that, under this aluminum-silicon molar ratio, the silicon in the beryllium ore can form a precipitated co-salt with aluminum that is insoluble in alkali, thereby reducing the aluminum content in the leaching solution.

[0047] Specifically, during leaching in step 2, the liquid-solid volume ratio of the leaching medium to the beryllium ore satisfies: 4:1 to 10:1.

[0048] It should be noted that, under this liquid-to-solid ratio, the leaching reaction can be ensured without causing excessive reagent consumption.

[0049] Specifically, during leaching in step 2, the amount of alkali in the leaching medium meets the requirement of: 150 g / L to 300 g / L.

[0050] It should be noted that this alkali concentration can not only ensure the effective leaching of beryllium, but also enable beryllium to enter the solution in the form of ions. Too much alkali will cause unnecessary waste.

[0051] Preferably, the alkali used for leaching in step 2 is one or more of sodium hydroxide and potassium hydroxide.

[0052] Preferably, the aluminum-containing material in step 2 is aluminum oxide or aluminum salt.

[0053] Preferably, the aluminum-containing material in step 2 is one or more of aluminum oxide monohydrate, aluminum oxide trihydrate, aluminum hydroxide, aluminum sulfate, and aluminum chloride.

[0054] Preferably, the heating temperature during leaching in step 2 is between 150°C and 300°C, for example, it can be 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C or 300°C.

[0055] It should be noted that the heating temperature during leaching is 150°C to 300°C: this temperature can accelerate the reaction rate, which is conducive to the destruction of the structure of the beryllium ore by the alkaline solution, and realizes the dissociation of beryllium and aluminum in the beryllium ore; at the same time, this temperature range can reduce the amount of alkali used.

[0056] Preferably, the leaching pressure during leaching in step 2 is 8MPa to 15MPa, for example, 8MPa, 8.5MPa, 8.8MPa, 9.2MPa, 9.6MPa, 9.8MPa, 10.0MPa, 10.4MPa, 10.5MPa, 10.6MPa, 10.8MPa, 11.0MPa, 11.6MPa,

[0057] 11.8MPa, 12.0MPa, 12.6MPa, 12.8MPa, 13.2MPa, 13.4MPa,

[0058] 13.8MPa, 14.0MPa, 14.2MPa, 14.6MPa, 14.8MPa or 15MPa.

[0059] It should be noted that the heating temperature of 8MPa to 15MPa during leaching can increase the boiling point of water, which is beneficial for controlling the reaction temperature and utilizing the leaching and dissolution characteristics of the liquid to ensure the controllability and safety of the chemical reaction.

[0060] The dilution in step 3 should satisfy the following requirement: the mass concentration of alkali in the beryllium-rich and aluminum-rich leaching solution after dilution is less than 50 g / L.

[0061] It should be noted that the present invention uses direct dilution and boiling of the leachate to achieve the separation of beryllium and aluminum, and does not introduce acidic reagents to adjust the pH of the solution. According to the difference in the precipitation range of beryllium and aluminum and their solubility under different pH values, the alkalinity of the leachate is reduced by dilution, and beryllium can be formed into beryllium hydroxide precipitation under boiling conditions, while aluminum remains in the solution in the form of ions; the separation process can effectively reduce reagent consumption compared to traditional methods.

[0062] Specifically, when the alkali concentration is between 150 g / L and 300 g / L, the solution is diluted 3 to 6 times.

[0063] It should be further explained that heating will widen the pH range of beryllium precipitation. In this pH range, aluminum is still in ionic form, which is beneficial to improving the yield of beryllium.

[0064] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide further comprises:

[0065] Step 4: filtering and separating the beryllium hydroxide precipitate and the aluminum-rich leachate, and reusing the aluminum-rich leachate as an aluminum-containing material after evaporation and concentration.

[0066] It should be noted that there is still a certain amount of aluminum and a high concentration of alkali in the aluminum-rich leaching solution. After evaporation and concentration, the solution can be returned to the pressure cooking stage for repeated utilization, thereby reducing wastewater discharge.

[0067] Preferably, the alkali concentration in the aluminum-rich leaching solution is concentrated to 180 g / L to 280 g / L.

[0068] It should be noted that the alkali is concentrated to this concentration, which can meet the alkali concentration required for pressure cooking and leaching, and is convenient for recycling.

[0069] Compared with the prior art, the present invention does not adopt the traditional extraction method for beryllium, and no extraction phase and impure cations are introduced into the solution. The aluminum-rich leachate obtained after filtration can be directly reused as an aluminum-containing raw material. At the same time, the alkali in the aluminum-rich leachate is recycled, which reduces waste liquid recovery and reduces emission treatment costs.

[0070] Preferably, the method for dissociating beryllium ore and preparing beryllium oxide further comprises:

[0071] Step 5: Dry and calcine the beryllium hydroxide to obtain beryllium oxide.

[0072] On the other hand, the present invention also discloses beryllium oxide, which is prepared by the above-mentioned beryllium ore dissociation and beryllium oxide preparation method, and the purity of beryllium oxide is ≥96%.

[0073] To further illustrate the present invention, the following examples and comparative examples are provided:

[0074] Example 1a

[0075] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0076] Step 1: After chrysoberyl (silicon: 29.1%, aluminum: 11.4%) is crushed and ground to obtain beryllium ore powder;

[0077] Step 2: according to the content of silicon and aluminum in the beryllium ore, a proper amount of aluminum-containing material alumina is added, and then alkali is added to perform pressure cooking and leaching reaction; the pressure cooking temperature in step 2 is 150° C. and the pressure is 8 MPa; the aluminum molar amount in the solid mixture after adjustment is 1 times the silicon molar amount, the alkali concentration is 180 g / L, and the liquid-solid ratio is 4:1;

[0078] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 5 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0079] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0080] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0081] The purity of beryllium oxide detected by the prior art method is 96.8%, and the beryllium element yield of beryllium ore is 96.9%.

[0082] Example 1b

[0083] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0084] Step 1: After chrysoberyl (silicon: 9.1%, aluminum: 41.4%) is crushed and ground to obtain beryllium ore powder;

[0085] Step 2: according to the content of silicon and aluminum in the beryllium ore, an appropriate amount of silicon-containing material silicon dioxide is added, and then alkali is added to perform pressure cooking and leaching reaction; the pressure cooking temperature in step 2 is 150° C. and the pressure is 8 MPa; the aluminum molar amount in the solid mixture after adjustment is 1 times the silicon molar amount, the alkali concentration is 180 g / L, and the liquid-solid ratio is 4:1;

[0086] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 5 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0087] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0088] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0089] The purity of beryllium oxide detected by the prior art method is 96.5%, and the beryllium element yield of beryllium ore is 97.1%.

[0090] Example 2a

[0091] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0092] Step 1: Beryllium ore powder is obtained by crushing and grinding beryllium ore (silicon: 40.6%, aluminum: 8.5%);

[0093] Step 2: adding an appropriate amount of aluminum-containing material aluminum chloride according to the content of silicon and aluminum in the beryllium ore, and then adding alkali to perform pressure cooking and leaching reaction; the pressure cooking temperature in step 2 is 300° C. and the pressure is 13 MPa; so that the aluminum molar amount in the solid mixture after adjustment is 1.5 times the silicon molar amount, the alkali concentration is 250 g / L, and the liquid-solid ratio is 6:1;

[0094] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 6 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0095] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0096] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0097] The purity of beryllium oxide detected by the prior art method is 96.4%, and the beryllium element yield of beryllium ore is 97.5%.

[0098] Example 2b

[0099] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0100] Step 1: Beryllium ore powder is obtained by crushing and grinding beryllium ore (silicon: 18.6%, aluminum: 28.5%);

[0101] Step 2: according to the content of silicon and aluminum in the beryllium ore, an appropriate amount of silicon-containing material sodium silicate is added, and then alkali is added to perform pressure cooking and leaching reaction; in step 2, the pressure cooking temperature is 300°C and the pressure is 13MPa; so that the aluminum molar amount in the solid mixture after adjustment is 1.5 times the silicon molar amount, the alkali concentration is 250 g / L, and the liquid-solid ratio is 6:1;

[0102] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 6 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0103] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0104] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0105] The purity of beryllium oxide detected by the prior art method is 96.3%; the beryllium element yield of beryllium ore is 97.6%.

[0106] Example 3a

[0107] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0108] Step 1: Beryl (aluminum: 10.6%, silicon: 36.5%) is crushed and ground to obtain beryllium ore powder;

[0109] Step 2: according to the silicon content in the beryllium ore, a proper amount of aluminum-containing material alumina is added, and then alkali is added to perform pressure cooking and leaching reaction; in step 2, the pressure cooking temperature is 250°C and the pressure is 10MPa; the aluminum molar amount in the solid mixture after adjustment is twice the silicon molar amount, the alkali concentration is 300 g / L, and the liquid-solid ratio is 10:1;

[0110] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 7 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0111] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0112] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0113] The purity of beryllium oxide detected by the prior art method is 96.3%; the beryllium element yield of beryllium ore is 98.2%.

[0114] Example 3b

[0115] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide. Figure 1 As shown, including:

[0116] Step 1: Beryl (aluminum: 28.6%, silicon: 10.5%) is crushed and ground to obtain beryllium ore powder;

[0117] Step 2: adding an appropriate amount of silicon-containing material silicon dioxide according to the silicon content in the beryllium ore, and then adding alkali to perform autoclave leaching reaction; the autoclave temperature in step 2 is 250° C. and the pressure is 10 MPa; the aluminum molar amount in the solid mixture after adjustment is twice the silicon molar amount, the alkali concentration is 300 g / L, and the liquid-solid ratio is 10:1;

[0118] Step 3: After the pressure cooking is completed, the beryllium and aluminum leaching solution is filtered to obtain the beryllium and aluminum leaching solution, and the silicon, iron, calcium, magnesium and other elements enter the slag; after the beryllium and aluminum leaching solution is diluted 7 times and boiled, beryllium hydroxide precipitate is obtained to achieve the separation of beryllium and aluminum;

[0119] Step 4: The aluminum-containing solution after filtration is concentrated by evaporation and returned to the pressure cooking stage for reuse;

[0120] Step 5: After beryllium hydroxide is dried and calcined, beryllium oxide is obtained.

[0121] The purity of beryllium oxide detected by the prior art method is 96.5%, and the beryllium element yield of beryllium ore is 98.1%.

[0122] Example 4

[0123] This embodiment discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from the embodiment 1 in that: the particle size of the ore powder is 40 mesh; the purity of beryllium oxide is 95.8% after testing; and the beryllium element yield of the beryllium ore is 90.2%.

[0124] Comparative Example 1

[0125] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from Example 1 in that: the particle size of the ore powder is 20 mesh; the purity of beryllium oxide is 95.6% after testing; and the beryllium element yield of the beryllium ore is 87.2%.

[0126] Comparative Example 2

[0127] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from Example 1 in that: the pressure boiling and leaching temperature in step 2 is 120° C.; the purity of beryllium oxide is 89.6% after testing; and the beryllium element yield of beryllium ore is 90%.

[0128] Comparative Example 3

[0129] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from Example 1 in that: the pressure of autoclaving in step 2 is 3 MPa; the purity of beryllium oxide is 85.2% after testing; and the beryllium element yield of beryllium ore is 83.2%.

[0130] Comparative Example 4

[0131] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from Example 1 in that: in step 2, the molar amount of aluminum is 0.5 times the molar amount of silicon, which does not meet the silicon-aluminum molar ratio range defined in the present invention; the purity of beryllium oxide is 72.3% after testing; and the beryllium element yield of beryllium ore is 93.2%.

[0132] Comparative Example 5

[0133] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide. The difference from Example 1 is that the alkali concentration in step 2 is 80 g / L, which does not meet the alkali concentration limit of the present invention.

[0134] Range; the purity of beryllium oxide is 60% after testing; the beryllium element yield of beryllium ore is 65%.

[0135] Comparative Example 6

[0136] This comparative example discloses a method for dissociating beryllium ore and preparing beryllium oxide, which is different from Example 1 in that: the dilution factor in step 3 is 2, which does not meet the limited range of the present invention; the dilution factor is not enough, the alkalinity is too high, and no precipitation is produced.

[0137] As can be seen from the above, the purity of beryllium oxide prepared in Example 1a-4 of the present invention is greater than 96%; the beryllium element yield of beryllium ore is greater than 96%; the present invention can achieve the dissociation of a variety of beryllium ores, whether it is easy to smelt beryl, hydroxysilicate beryllite or low-grade chrysoberyl, the method can be used to achieve beryllium leaching.

[0138] By comparison between the embodiments and the comparative examples, it can be seen that the pressure cooking leaching temperature exceeds 150°C to 300°C, the pressure cooking leaching pressure exceeds 8MPa to 15MPa, the aluminum-silicon molar ratio after the beryllium ore is added with the aluminum-containing material exceeds 1:1 to 1.5, the pressure cooking leaching alkali dosage is 150g / L to 300g / L, and the dilution multiple in step 2 exceeds the limited range of 3 times to 6 times, which will have an adverse effect on the purity of beryllium oxide and the beryllium element yield of the beryllium ore.

Claims

1. A method for dissociating beryllium ore and preparing beryllium oxide, characterized in that: The method for dissociating beryllium ore and preparing beryllium oxide comprises: Add aluminum-containing materials or silicon-containing materials to adjust the ratio of silicon and aluminum elements in the beryllium ore; Under alkaline and high-pressure conditions, water is used as a leaching medium to leach beryllium ore with adjusted silicon and aluminum element ratios to obtain a beryllium-rich leaching solution.

2. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 1, characterized in that: The method for dissociating beryllium ore and preparing beryllium oxide also includes: utilizing the difference in solubility of beryllium and aluminum in solutions with different pH values ​​to separate beryllium and aluminum elements in the beryllium-rich leaching solution.

3. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 2, characterized in that: The method for dissociating beryllium ore and preparing beryllium oxide comprises: Step 1, beryllium ore is refined to obtain beryllium ore powder within a target particle size range; Step 2, adding an appropriate amount of aluminum-containing material or silicon-containing material according to the content of silicon and aluminum in the beryllium ore, and then adding an alkaline solution to perform a pressure boiling leaching reaction at a pressure greater than normal pressure, and filtering the leachate to obtain a beryllium- and aluminum-rich leachate; Step 3: After the beryllium- and aluminum-rich leaching solution is diluted and boiled, beryllium hydroxide precipitate is obtained to achieve separation of beryllium and aluminum.

4. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 3, characterized in that: In step 2, the molar amount of aluminum is 1 to 1.5 times the molar amount of silicon.

5. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 4, characterized in that: During leaching in step 2, the liquid-solid volume ratio of the leaching medium to the beryllium ore satisfies: 4:1 to 10:

1.

6. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 5, characterized in that: The heating temperature during leaching in step 2 is between 150°C and 300°C.

7. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 6, characterized in that: During leaching in step 2, the amount of alkali in the leaching medium meets the requirement of: 150 g / L to 300 g / L.

8. The method for dissociating beryllium ore and preparing beryllium oxide according to claim 7, characterized in that: The alkali used for leaching in step 2 is one or more of sodium hydroxide and potassium hydroxide.

9. The method for dissociating beryllium ore and preparing beryllium oxide according to any one of claims 2 to 8, characterized in that: In step 2, the aluminum-containing material is aluminum oxide or aluminum salt, and the silicon-containing material is silicon dioxide or silicate.

10. A beryllium oxide, characterized in that: The beryllium oxide is prepared by the beryllium ore dissociation and beryllium oxide preparation method according to any one of claims 1 to 9, and the purity of the beryllium oxide is ≥ 96%.

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