Preparation method of plate-shaped barium sulfate

Abstract

The invention discloses a preparation method of plate-shaped barium sulfate, which comprises the following steps: preparing a barium sulfate reaction raw material and an auxiliary agent which is pentaerythritol, adding the barium sulfate reaction raw material and the auxiliary agent into an enamel reactor for reaction, controlling the reaction temperature and the reaction pressure, carrying out filter pressing and washing on the reaction liquid of the enamel reactor to prepare a filter cake, and drying the filter cake to obtain the plate-shaped barium sulfate. The concentration of pulpified barium sulfide O4 is 12%-15%, the pH value is adjusted through potassium hydroxide in the process, filter pressing and washing are conducted again to remove impurity ions, the filter cake obtained through secondary filter pressing and washing is dewatered, and the high-purity plate-shaped barium sulfate is obtained. The preparation method has the beneficial effects that the barium sulfate with larger thickness-length ratio and particle size can be prepared, the barium sulfate is in a plate shape, other impurity ions are not introduced in the reaction, the obtained product is higher in purity, the product is not easy to break, the original particle size and shape can be well kept, the purity is higher, the whiteness is higher, the preparation method is simpler, and the application scene is wider.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of barium sulfate preparation, in particular to a preparation method of plate-shaped barium sulfate. BACKGROUND

[0002] Barium sulfate is widely used, and it plays an important role in paper, paint, paint, textiles, plastics and lithographic printing ink fields. The existing barium sulfate is mostly barium sulfate precipitate after production, and its shape is mostly granular. Plate-shaped barium sulfate has larger thick long wall and particle size, and can effectively absorb X-ray, gamma-ray and other radioactive substances, so it has more advantages in medical or cosmetic industry applications. However, the current barium sulfate preparation method and process mostly produce granular precipitate, the particles are not dense enough, and the thickness-length ratio and particle size are relatively small. Therefore, a method for preparing plate-shaped barium sulfate is needed to meet market demand. SUMMARY

[0003] The purpose of the present application is to provide a preparation method of plate-shaped barium sulfate.

[0004] The present application achieves the above-mentioned purpose by the following technical solutions:

[0005] A preparation method of plate-shaped barium sulfate, comprising the following steps:

[0006] S1, preparing barium sulfate reaction raw materials and additives, the additive is pentaerythritol;

[0007] S2, adding the barium sulfate reaction raw materials and additives into the porcelain reactor for reaction, and controlling the reaction temperature and reaction pressure;

[0008] S3, filtering and washing the reaction liquid of the porcelain reactor to prepare filter cake, slurry and heat preservation of the filter cake, the concentration of slurry barium sulfate O4 is 12% to 15%, and the pH value is adjusted by potassium hydroxide in this process;

[0009] S4, removing impurity ions by filtering and washing again;

[0010] S5, dehydrating the filter cake obtained by the secondary filtering and washing to obtain high-purity plate-shaped barium sulfate.

[0011] Further, at least one of drying or calcining is selected for dehydrating the filter cake in step S5, the drying temperature is 200 DEG C, and the calcining temperature is 700 DEG C.

[0012] Further, in step S1, the barium sulfate reaction raw materials are 1000L of barium sulfide solution (barium sulfide content is 150-160g / L), 230g of citric acid, 1000L of sodium sulfate solution (sodium sulfate content is 210-225g / L), and sufficient deionized water, and the pentaerythritol is 1100g.

[0013] Further, the barium sulfate reaction raw material in step S1 is 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), 230g of citric acid, and sufficient amount of deionized water, and the pentaerythritol is 1100g.

[0014] Further, the barium sulfate reaction raw material in step S1 is 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), 10L of lithium hydroxide solution (lithium hydroxide content is 50-55g / L), 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), and sufficient amount of deionized water, and the pentaerythritol is 1100g.

[0015] Further, the barium sulfate reaction raw material in step S1 is 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), 10L of lithium hydroxide solution (lithium hydroxide content is 50-55g / L), 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), and sufficient amount of deionized water, and the pentaerythritol is 1100g.

[0016] The preparation method of the plate-shaped barium sulfate has the beneficial effects that: through the method, barium carbonate and barium sulfide can be used to prepare barium sulfate with a larger thickness-length ratio and particle size, the barium sulfate is in a plate shape, no other impurity ions are introduced in the reaction, the obtained product has higher purity, after high-temperature calcination, the product is not easy to break, can well maintain the original particle size and shape, has higher purity, higher whiteness, simpler preparation method, and wider use scenarios. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 The plate-shaped barium sulfate of Example One provided by the embodiment of the present application is prepared into a plate-shaped barium sulfate structure distribution diagram.

[0018] Figure 2 The plate-shaped barium sulfate of Example Two provided by the embodiment of the present application is prepared into a plate-shaped barium sulfate structure distribution diagram.

[0019] Figure 3 The plate-shaped barium sulfate of Example Three provided by the embodiment of the present application is prepared into a plate-shaped barium sulfate structure distribution diagram.

[0020] Figure 4 The plate-shaped barium sulfate of Example Four provided by the embodiment of the present application is prepared into a plate-shaped barium sulfate structure distribution diagram.

[0021] Figure 5 The plate-shaped barium sulfate of the comparative example provided by the embodiment of the present application is prepared into a barium sulfate structure distribution diagram. DETAILED DESCRIPTION

[0022] With reference to the drawings of the embodiments of the present application, the technical solutions in the embodiments of the present application will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those of ordinary skill in the art without creative effort belong to the scope of the present application.

[0023] A preparation method of plate-shaped barium sulfate, comprising the following steps:

[0024] S1, preparing barium sulfate reaction raw materials and an auxiliary agent, the auxiliary agent being pentaerythritol;

[0025] S2, adding the barium sulfate reaction raw materials and the auxiliary agent into a porcelain reaction vessel to perform a reaction, and controlling a reaction temperature and a reaction pressure;

[0026] S3, pressure-filtering and washing the reaction liquid of the porcelain reaction vessel to prepare filter cakes, slurryzing the filter cakes and keeping warm, the concentration of barium sulfate O4 after slurryzing being 12% to 15%, and the temperature being raised to 60°C to 65°C to keep warm for 1 hour, and the process needing to adjust the pH value by potassium hydroxide;

[0027] S4, removing impurity ions by pressure-filtering and washing again;

[0028] S5, dehydrating the filter cakes obtained by the secondary pressure-filtering and washing to obtain plate-shaped barium sulfate with high purity, wherein the dehydrating of the filter cakes is realized by drying and calcining.

[0029] Next, the implementation process of the method of the present application will be described in combination with specific embodiments.

[0030] Embodiment 1

[0031] S1, adding 1000L of barium sulfate solution (the content of barium sulfate being 150 to 160g / L) into a 2m 3 long plastic PP reaction kettle, then adding 230g of citric acid and 1100g of pentaerythritol into the barium sulfate solution to mix uniformly, adding 1000L of sodium sulfate solution (the content of sodium sulfate being 210 to 225g / L) into another plastic PP reaction kettle, and preparing enough deionized water for standby;

[0032] S2, simultaneously adding the solutions in the two plastic PP reaction kettles into a sealed porcelain reaction vessel, the temperature in the porcelain reaction vessel being 90 to 100°C, and the pressure being 0.02 to 0.05MPa;

[0033] S3, after the reaction is completed, keeping warm at 70°C for 2 hours, then pressure-filtering and washing to obtain filter cakes, slurryzing the filter cakes, slurryzing the barium sulfate O4 to a concentration of 12% to 15% by deionized water, then adding potassium hydroxide to adjust the pH value to 10 and raising the temperature to 60°C to 65°C to keep warm for 1 hour;

[0034] S4, washing and removing impurity ions again by pressure filtration;

[0035] S5, drying the filter cake after secondary washing at 200℃ for 6h to obtain high-purity flaky barium sulfate.

[0036] Example 2

[0037] S1, adding 1000L of barium hydroxide monohydrate solution (50-60g / L of barium hydroxide) into a 2m 3 plastic PP reactor and adding 1000L of sulfuric acid solution (87-105g / L of sulfuric acid) into another plastic PP reactor, preparing 230g of citric acid, 1100g of pentaerythritol, and sufficient deionized water;

[0038] S2, adding 100L of deionized water into the enamel reactor, then adding 230g of citric acid and 1100g of pentaerythritol into the enamel reactor and stirring to mix uniformly, while adding the solutions in the two plastic PP reactors dropwise into the enamel reactor, controlling the excess of sulfuric acid to be 10-20g / L, the temperature to be 60-70℃, and the pH value to be 4-5;

[0039] S3, after the reaction is completed, adding potassium hydroxide to adjust the pH value to 7.0, and washing and removing the filter cake by pressure filtration, then slurring the barium sulfide O4 with deionized water to a concentration of 12%-15%, and heating to 60-65℃ for 1h;

[0040] S4, washing and removing impurity ions again by pressure filtration;

[0041] S5, drying the filter cake after secondary washing at 200℃ for 6h, and calcining the flaky barium sulfate after drying at 700℃ for 30min to obtain high-purity plate-like barium sulfate.

[0042] Example 3

[0043] S1, adding 1000L of barium hydroxide monohydrate solution (50-60g / L of barium hydroxide) and 10L of lithium hydroxide solution (50-55g / L of lithium hydroxide) into a 2m 3 plastic PP reactor, controlling the pH value and the excess of sulfate ions at the same time, which is more conducive to the formation of plate-like shape and is not easy to carry barium ion salt, causing a large amount of residual barium ions, adding 1000L of sulfuric acid solution (87-105g / L of sulfuric acid) into another plastic PP reactor, and preparing 1100g of pentaerythritol and sufficient deionized water;

[0044] S2, first add 100L deionized water into the enamel reactor, then add 1100g pentaerythritol into the enamel reactor and stir to mix evenly, while drop the solution in the two plastic PP reactors into the enamel reactor, control the excess of sulfuric acid to be 10-20g / L, the temperature to be 60-70℃, and the pH value to be between 4-5 during the reaction process;

[0045] S3, after the reaction is completed, add potassium hydroxide to adjust the pH value to 7.0, filter and wash the obtained solution to obtain filter cake, slurry the filter cake, and slurry the barium sulfate O4 to a concentration of 12%-15% with deionized water, then heat to 60-65℃ and keep for 1h;

[0046] S4, filter and wash again to remove impurity ions;

[0047] S5, dry the filter cake after washing at 200℃ for 6h to obtain high-purity plate-shaped barium sulfate.

[0048] Example 4

[0049] S1, add 1000L barium hydroxide monohydrate solution (the barium hydroxide content is 50-60g / L) into a 2m 3 plastic PP reactor, add 1000L lithium hydroxide into another plastic PP reactor, and prepare 1100g pentaerythritol and sufficient deionized water for standby;

[0050] S2, first add 100L deionized water into the enamel reactor, then add 1100g pentaerythritol into the enamel reactor and stir to mix evenly, while drop the solution in the two plastic PP reactors into the enamel reactor heated to 60-70℃, control the excess of sulfuric acid to be 10-20g / L, and the pH value to be between 4-5 during the reaction process;

[0051] S3, after the reaction is completed, add potassium hydroxide to adjust the pH value to 7.0, filter and wash the obtained solution to obtain filter cake, slurry the filter cake, and slurry the barium sulfate O4 to a concentration of 12%-15% with deionized water, then heat to 60-65℃ and keep for 1h;

[0052] S4, filter and wash again to remove impurity ions;

[0053] S5, dry the filter cake after washing at 200℃ for 6h, and calcine the plate-shaped barium sulfate after drying at 700℃ for 30min to obtain high-purity plate-shaped barium sulfate.

[0054] Comparative Example

[0055] S1, add 1000L barium hydroxide monohydrate solution (the barium hydroxide content is 50-60g / L) into a 2m 3S1, in one plastic PP reactor, add 1000L of barium hydroxide monohydrate solution (the content of barium hydroxide is 50-60g / L) and 1000L of lithium hydroxide solution; in another plastic PP reactor, add 1000L of sulfuric acid solution (the content of sulfuric acid is 87-105g / L);

[0056] S2, in the enamel reactor, first add 100L of deionized water, and then simultaneously drop the solutions in the two plastic PP reactors into the enamel reactor, and control the excess of barium hydroxide to be 10-20g / L, the temperature to be 60-70℃, and the pH value to be 9-10;

[0057] S3, after the reaction is completed, add potassium hydroxide to adjust the pH value to 7.0, filter and wash the obtained solution, and then slurry the filter cake to obtain a 12%-15% concentration barium sulfate solution, and control the temperature to be 30-45℃ for 1h;

[0058] S4, filter and wash again to remove impurity ions;

[0059] S5, dry the filter cake after the second washing at 200℃ for 6h to obtain precipitated barium sulfate.

[0060] Reference Figures 1-5 The table below is obtained by comparing the parameters of the finished barium sulfate in the above four examples and the comparative example, and the electron microscope images thereof:

[0061]

[0062] As shown in the above table, the product obtained by using barium sulfide as a raw material has by-products, so the purity of the product is not high enough, and the whiteness is affected. The product obtained in Example 4 has a larger plate-shaped diameter, and after calcination, the high-speed shearing dispersion is not easy to break, the retention rate is relatively high, and the whiteness and purity are the highest. After adjusting the pH value and removing the additive in the comparative example, the plate-shaped structure cannot be formed. The plate-shaped formation mechanism is that the excess sulfate ions and pentaerythritol are adsorbed on the surface of the barium sulfate nucleus, so that the growth direction is grown in the flat direction. By washing to remove excess impurities, and by high-temperature calcination to remove crystal water, the barium sulfate shrinks more densely, and the purity is higher.

[0063] The above shows and describes the basic principles, main features and advantages of the present application. It should be understood by those skilled in the art that the present application is not limited to the above examples, and the above examples and descriptions in the specification are only to illustrate the principles of the present application. Without departing from the spirit and scope of the present application, various changes and improvements can be made to the present application, and these changes and improvements all fall within the scope of the present application. The scope of protection of the present application is defined by the appended claims and their equivalents.

Claims

1. A method for preparing plate-shaped barium sulfate, characterized in that, Includes the following steps: S1. Prepare barium sulfate reaction raw materials and auxiliaries, wherein the auxiliaries are pentaerythritol; S2. Add barium sulfate reaction raw materials and additives to an enamel reactor to carry out the reaction, and control the reaction temperature and reaction pressure. S3. Prepare filter cake by hydraulic filtration and washing of the reaction liquid in the enamel reactor. Slurry the filter cake and keep it warm. The concentration of barium sulfide O4 in the slurry is 12% to 15%. The pH value is adjusted by potassium hydroxide in this process. S4. Filter and wash again to remove impurity ions; S5. The filter cake obtained by secondary pressure filtration and washing is dehydrated to obtain high-purity plate-shaped barium sulfate.

2. The method for preparing plate-shaped barium sulfate according to claim 1, characterized in that: In step S5, the filter cake is dehydrated by at least one method, namely drying or calcination, wherein the drying temperature is 200°C and the calcination temperature is 700°C.

3. The method for preparing plate-shaped barium sulfate according to claim 1, characterized in that: The raw materials for the barium sulfate reaction in step S1 are 1000L of barium sulfide solution (barium sulfide content is 150-160g / L), 230g of citric acid, 1000L of sodium sulfate solution (sodium sulfate content is 210-225g / L), sufficient deionized water, and 1100g of pentaerythritol.

4. The method for preparing plate-shaped barium sulfate according to claim 1, characterized in that: The raw materials for the barium sulfate reaction in step S1 are 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), 230g of citric acid, sufficient deionized water, and 1100g of pentaerythritol.

5. The method for preparing plate-shaped barium sulfate according to claim 1, characterized in that: The raw materials for the barium sulfate reaction in step S1 are 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), 10L of lithium hydroxide solution (lithium hydroxide content is 50-55g / L), 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), and sufficient deionized water, and the pentaerythritol is 1100g.

6. The method for preparing plate-shaped barium sulfate according to claim 1, characterized in that: The raw materials for the barium sulfate reaction in step S1 are 1000L of barium hydroxide monohydrate solution (barium hydroxide content is 50-60g / L), lithium hydroxide, 1000L of sulfuric acid solution (sulfuric acid content is 87-105g / L), and sufficient deionized water, and the pentaerythritol is 1100g.

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