Preparation method of barite ultrafine powder

Abstract

The invention provides a barite ultrafine powder preparation method which comprises the following steps: S1, cleaning the surface of a barite block, and coarsely crushing the barite block until the particle size of the coarsely crushed material is less than 4mm; s2, finely crushing the coarsely crushed material to obtain a fine material, wherein the particle size of the fine material is 500-150 [mu] m; s3, mixing and stirring the fine material and water, and freezing after stirring; and S4, crushing after freezing, crushing the crushed material again, drying the crushed material to volatilize moisture, and keeping the particle size of the residual dry material in a range of 80-150 [mu] m. The water molecules and the barite are integrated and then are subsequently crushed to form powder, and a fine powder structure is left after the water is gradually volatilized; the purpose of preparing the material with the particle size of 80-150 microns can be achieved through a common sample grinding machine capable of achieving mass production, so that industrial mass production is achieved, the problem of using a high-precision ball grinding machine is avoided, cost is saved, and efficiency is improved.

Description

Technical Field

[0001] The invention relates to a process for preparing fine ore powder, and in particular to a preparation technology for realizing industrial mass production of ultrafine barite powder. Background Art

[0002] Baryte, with the chemical formula BaSO4, is an important mineral; barite is widely used as a mud filler in oil and gas drilling to increase the density of the mud, thereby helping to control downhole pressure. In addition, it is also used in the manufacture of paints, plastics, rubber and pharmaceuticals.

[0003] After barite is mined, it generally needs to be crushed and screened multiple times, and different particle sizes require different crushing machines, so that the required particle size of barite can be finally obtained. In the prior art, in order to obtain ultrafine barite powder, it is generally less than 200μm, and such ultrafine powder has a wider range of uses.

[0004] However, the process of preparing ultrafine powder barite less than 200μm is usually cumbersome. After coarse and fine grinding to obtain a particle size of 1mm to 150μm, ultrafine grinding equipment is usually required. This ultrafine grinding equipment is expensive and has low production efficiency, making it impossible to achieve industrial mass production. In addition, this equipment is prone to damage and requires maintenance.

[0005] Therefore, it is necessary to make improvements to avoid the use of ultrafine grinding equipment and still achieve the purpose of industrial mass production of ultrafine barite powder. Summary of the invention

[0006] In order to solve the problems existing in the above-mentioned technologies, the present invention provides a technology for realizing industrial mass production of ultrafine barite powder and reducing production costs.

[0007] The present invention provides a method for preparing ultrafine barite powder, characterized in that it comprises the following steps:

[0008] S1: After cleaning the surface of the barite block, it is coarsely crushed, and the particle size of the coarsely crushed material is less than 4mm;

[0009] S2: finely crushing the coarsely crushed material to obtain a fine material, wherein the particle size of the fine material is 500 μm to 150 μm;

[0010] S3: mixing the fine material with water, and freezing after mixing;

[0011] S4: After freezing, the material is crushed, and the crushed material is crushed again. The crushed material is dried to evaporate the water, and the particle size of the remaining dry material is 80μm to 150μm.

[0012] Preferably, a small jaw crusher is used for coarse crushing;

[0013] The crushing equipment used for fine crushing is hydraulic compression vibration mill ZM-1XY type.

[0014] Preferably, the required particle size is obtained by screening through a screen in the steps of coarse pulverization and fine material pulverization.

[0015] Preferably, after the fine material is mixed and stirred with water, the solid matter is obtained by filtering or centrifugation, and impurities are removed by water.

[0016] Preferably, the dry material is refined to remove impurities, and the refining process includes the following steps:

[0017] Add dry materials to water and stir;

[0018] A silane coupling agent is added, and the silane coupling agent reacts with the surface hydroxyl groups of impure silicon dioxide in the dry material to form modified silicon dioxide;

[0019] The introduction of silane coupling agent promotes the dissolution of silica in the water phase;

[0020] The liquid is filtered out to leave the refined solid barite fine powder material, which is then dried to obtain the product.

[0021] Preferably, the silane coupling agent is KH560 silane coupling agent, and the weight of KH560 silane coupling agent added is 0.001% to 0.01% of the dry material.

[0022] Preferably, ethanol is added to the modified silica aqueous solution, and the volume of the ethanol added is 5% to 15% of the volume ratio of the aqueous solution. After stirring, silica microspheres are formed, and other impurities are encapsulated and / or adsorbed during the formation process.

[0023] The beneficial effects of the present invention are as follows: the present invention forms a block structure of the material by freezing, and then subsequently crushes the water molecules and barite into a whole to form a powder, and the ice crystal structure is used to accelerate and promote the grinding process of the powder during crushing, that is, the ice crystal plays the role of a grinding accelerator; and after the water evaporates gradually, a fine powder structure is left, thereby achieving the purpose of obtaining ultrafine powder barite that meets the particle size; that is, the purpose of preparing materials with a particle size of 80μm to 150μm can be achieved through an ordinary mass-producible grinding machine, which not only realizes industrial mass production, but also avoids the problem of using a high-precision ball mill, saves costs, and improves efficiency.

[0024] In addition, the present invention can be used to modify silicon dioxide to be soluble in water through the use of a silane coupling agent, thereby improving the separation from the barium sulfate substance after dissolution, thus playing a purification role and improving the purity. DETAILED DESCRIPTION

[0025] Embodiment 1:

[0026] The present embodiment provides a method for preparing ultrafine barite powder, comprising the following steps:

[0027] S1: After cleaning the surface of the barite block, it is coarsely crushed, and the particle size of the coarsely crushed material is less than 4mm; the coarse crushing is carried out using a small jaw crusher;

[0028] S2: finely crushing the coarsely crushed material to obtain fine material, the particle size of the fine material is 500 μm to 150 μm; the crushing equipment used for fine crushing is a hydraulic compression type vibration mill ZM-1XY type;

[0029] S3: mixing the fine material with water, and freezing after mixing;

[0030] S4: After freezing, the material is crushed, and the crushed material is crushed again, and the crushing process still uses the hydraulic compression type vibration mill ZM-1XY type; the crushed material is dried to volatilize the moisture, and the residual dry material particle size is 80μm to 150μm. Preferably, the required particle size is obtained by screening through a screen in the steps of coarse crushing and fine material crushing, and screening is an optional solution.

[0031] Preferably, after the fine material is mixed and stirred with water, the solid matter is obtained by filtering, centrifuging or layering, and impurities are removed by water.

[0032] Generally, the ice is frozen into ice cubes. Preferably, stirring is performed during the freezing process, and ice chips are formed by cooling and freezing to avoid forming large blocks. This method helps to improve efficiency and directly crush and grind, avoiding the need to crush large ice blocks before grinding.

[0033] Comparative Example 1:

[0034] Prepared using the following steps:

[0035] S1: After cleaning the surface of the barite block, it is coarsely crushed, and the particle size of the coarsely crushed material is less than 4mm; the coarse crushing is carried out using a small jaw crusher;

[0036] S2: finely crushing the coarsely crushed material to obtain fine material, the particle size of the fine material is 500 μm to 150 μm; the crushing equipment used for fine crushing is a hydraulic compression type vibration mill ZM-1XY type;

[0037] S3: The fine material is finely crushed for the second time; the obtained particle size is 260μm to 120μm.

[0038] Comparative Example 2:

[0039] Prepared using the following steps:

[0040] S1: After cleaning the surface of the barite block, it is coarsely crushed, and the particle size of the coarsely crushed material is less than 4mm; the coarse crushing is carried out using a small jaw crusher;

[0041] S2: finely crushing the coarsely crushed material to obtain fine material, the particle size of the fine material is 500 μm to 150 μm; the crushing equipment used for fine crushing is a hydraulic compression type vibration mill ZM-1XY type;

[0042] S3: Fine materials were ultrafinely ground using a high-energy planetary ball mill PLB-2L (Lesda Company); the obtained particle size was less than 120 μm.

[0043] Table 1 is a comparison of the grinding conditions of the embodiments of the present invention and the comparative examples and the comparative data of the particle sizes of the obtained materials.

[0044]

[0045]

[0046] As can be seen from Table 1 above, in Example 1 of the present invention, the introduction of ice crystals has a grinding effect, which accelerates the grinding rate and obtains a particle size less than 150 μm. In this way, a heavy crystal ultrafine powder material that meets the requirements is quickly obtained, avoiding the use of high-performance laboratory-level grinding equipment, and achieving low-cost and rapid preparation of materials that meet the particle size requirements.

[0047] In Control Example 1, the same equipment, hydraulic compression vibration mill ZM-1XY, was used for secondary grinding, but the particle size obtained was still above 150 μm. This is because the ice crystals formed after freezing were not used to promote grinding and the ultrafine powder of the required particle size could not be quickly obtained.

[0048] In Control Example 3, ultrafine powder meeting the particle size requirements was obtained by using a laboratory-grade high-energy planetary ball mill PLB-2L. However, the output of this equipment is very small, less than 0.1 tons / hour, which cannot meet the requirements of industrial mass production and is therefore not suitable for industrial production.

[0049] Embodiment 2:

[0050] On the basis of Example 1, the scheme of this embodiment is preferably as follows: the dry material is refined to remove impurities, and the refining process includes the following steps:

[0051] Add dry materials to water and stir;

[0052] A silane coupling agent is added, and the silane coupling agent reacts with the surface hydroxyl groups of impure silicon dioxide in the dry material to form modified silicon dioxide;

[0053] The introduction of silane coupling agent promotes the dissolution of silica in the water phase;

[0054] The liquid is filtered out to leave the refined solid barite fine powder material, which is then dried to obtain the product.

[0055] Preferably, the silane coupling agent is KH560 silane coupling agent, and the weight of KH560 silane coupling agent added is 0.001% to 0.01% of the dry material.

[0056] Table 2, the composition comparison obtained after analyzing the dry materials in different embodiments.

[0057] Barium sulfate content Silica content Iron oxide and aluminum oxide and others Example 1 98.5％ 1.2％ 0.3％ Example 2 99.1％ 0.6％ 0.3％

[0058] As can be seen from Table 2 above, by adding a silane coupling agent, it can react with silicon dioxide to generate a molecular structure of modified silicon dioxide, which makes silicon dioxide more easily soluble in the aqueous phase. After precipitation, the lower layer of material is retained as precipitated barium sulfate material, and then the aqueous phase and barium sulfate are separated after stratification. The separation process is preferably to directly suck the upper aqueous phase through a straw, so that the aqueous phase with the modified silicon dioxide inside can be directly taken away, so that the content of barite powder is increased and the content of silicon dioxide is reduced.

[0059] Preferably, the reaction modification of the silane coupling agent and the silicon dioxide surface is carried out at 70-90° C. for 2-5 hours. For details, reference may also be made to the prior art.

[0060] Embodiment 3:

[0061] Preferably, ethanol is added to the modified silica aqueous solution, and the volume of the ethanol added is 5% to 15% of the volume ratio of the aqueous solution. After stirring, silica microspheres are formed, and other impurities are encapsulated and / or adsorbed during the formation process.

[0062] Table 3, the composition comparison of the dry materials in different embodiments after analysis.

[0063] Barium sulfate content Silica content Iron oxide and aluminum oxide and others Example 1 98.5％ 1.2％ 0.3％ Example 2 99.3％ 0.6％ 0.3％ Example 3 99.6％ 0.3％ 0.1％

[0064] In Table 3 above, after the addition of ethanol, ethanol and water form a solution. Since the modified silica solution is an amphiphilic molecule, it is easier to form a nano-microsphere structure in the aqueous solution. In the process of forming this structure, part of the iron oxide and aluminum oxide substances will be wrapped. More importantly, the nanostructure formed by the surface-modified silica has a large surface area, which makes it easier to adsorb iron oxide and aluminum oxide substances and reduce the presence of these substances. In this way, the impurity content is reduced, achieving the purpose of purification.

Claims

1. A method for preparing ultrafine barite powder, characterized in that: The following steps are included: S1: After cleaning the surface of the barite block, it is coarsely crushed, and the particle size of the coarsely crushed material is less than 4mm; S2: finely crushing the coarsely crushed material to obtain a fine material, wherein the particle size of the fine material is 500 μm to 150 μm; S3: mixing the fine material with water, and freezing after mixing; S4: After freezing, the material is crushed, and the crushed material is crushed again. The crushed material is dried to evaporate the water, and the particle size of the remaining dry material is 80μm to 150μm.

2. The method for preparing ultrafine barite powder according to claim 1, characterized in that Small jaw crusher is used for coarse crushing; The crushing equipment used for fine crushing is hydraulic compression vibration mill ZM-1XY type.

3. The method for preparing ultrafine barite powder according to claim 1, characterized in that Stirring is performed during the freezing process to cool down and freeze ice chips to avoid the formation of large blocks.

4. The method for preparing ultrafine barite powder according to claim 1, characterized in that In the steps of coarse pulverization and fine material pulverization, the required particle size is obtained by screening through a screen.

5. The method for preparing ultrafine barite powder according to claim 1, characterized in that: After the fine material is mixed with water and stirred, it is filtered or centrifuged to obtain the solid matter, and the impurities are removed by water.

6. The method for preparing ultrafine barite powder according to claim 1, characterized in that: For the dry material to be refined to remove impurities, the refining process includes the following steps: Add dry materials to water and stir; A silane coupling agent is added, and the silane coupling agent reacts with the surface hydroxyl groups of impure silicon dioxide in the dry material to form modified silicon dioxide; The introduction of silane coupling agent promotes the dissolution of silica in the water phase; The liquid is removed by filtering or layering to leave the refined solid barite fine powder material, which is then dried to obtain the product.

7. The method for preparing ultrafine barite powder according to claim 6, characterized in that: The silane coupling agent is KH560 silane coupling agent, and the weight of the added amount of KH560 silane coupling agent is 0.001% to 0.01% of the dry material.

8. The method for preparing ultrafine barite powder according to claim 7, characterized in that: Ethanol is added to the modified silica aqueous solution, the volume of the ethanol added being 5% to 15% of the volume of the aqueous solution, and the silica microspheres are formed after stirring, during which other impurities are encapsulated and / or adsorbed.

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