CN117602629A - A kind of production method of potassium fluorosilicate - Google Patents

Abstract

The invention discloses a method for producing potassium fluosilicate. The production process of the potassium fluosilicate in the invention comprises the following steps: 1) Refining fluosilicic acid, and placing the fluosilicic acid in a fluosilicic acid storage tank for standby; 2) Dissolving and removing impurities from potassium chloride to prepare a potassium chloride solution; 3) The refined fluosilicic acid and potassium chloride solution react in a synthesis tank to prepare potassium fluosilicate crystal slurry, and the potassium fluosilicate crystal slurry is centrifuged by a centrifuge and washed to prepare the potassium fluosilicate. The production method of the potassium fluosilicate is simple, filtrate and filter residues generated in the production process can be reasonably utilized, and the production cost is reduced.

Description

A kind of production method of potassium fluorosilicate

Technical field

The invention belongs to the technical field of potassium fluorosilicate preparation, and specifically relates to a production method of potassium fluorosilicate.

Background technique

Potassium fluorosilicate is used as an auxiliary in the smelting of magnesium and aluminum in the metallurgical industry. It is used in the glass industry to make potassium glass, optical glass, and opaque glass. In the pesticide industry, it is used to make pesticides. In the chemical industry, it is used to make intermediates. It is used as an analytical reagent in analytical chemistry and can also be used to synthesize mica in ceramics.

The patent application number CN202211275261.5 discloses a method for preparing potassium fluorosilicate from fluorine-containing liquid. In this preparation method, silicon slag is first treated, and then the treated silicon slag is stirred and reacted with fluorine-containing liquid, and then added Potassium salt is used to prepare potassium fluorosilicate. Although this method can prepare potassium fluorosilicate, the purity of the obtained potassium fluorosilicate is not high, which limits the application of potassium fluorosilicate in some fields.

Contents of the invention

In order to solve the above technical problems, the object of the present invention is to provide a production method of potassium fluorosilicate.

The object of the present invention can be achieved through the following technical solutions:

A method for producing potassium fluorosilicate, including the following steps:

Step S1: Add the mother liquor, water and potassium chloride into the potassium chloride dissolving tank, stir and mix evenly, then add hydrochloric acid with a concentration of 6 mol/L to adjust the pH of the solution to 5.3, turn on the stirrer and stir for 1.5 hours, then take the potassium chloride The solution is analyzed and tested. After the concentration of potassium chloride reaches 220-240g/L, it is sent to the filter press for filtering. The filtrate is then sent to the potassium chloride impurity removal tank for impurity removal. The filtrate after impurity removal is then sent to the filter press. Machine is used for press filtration, and the filtrate after press filtration is stored in a potassium chloride storage tank for later use;

Further, the usage ratio of reused mother liquor, water and potassium chloride is 5-15m ³ : 10-30m ³ : 4.5-13.5t.

Step S2: Pump the potassium chloride solution and refined fluorosilicic acid to the potassium chloride metering tank and the fluorosilicic acid metering tank respectively for measurement, and then send the measured potassium chloride solution and refined fluorosilicic acid simultaneously to the synthesis via pipelines. In the tank, react for 1 hour at normal temperature and pressure. After the reaction is completed, potassium fluorosilicate slurry will be obtained. The chemical equations involved are:

H ₂ S iF ₆ +2KC l→K ₂ S iF ₆ ↓+2HCl

Further, the dosage of potassium chloride solution and refined fluosilicic acid is 3-9m ³ :2.5-7.5m ³ .

Step S3: Centrifuge the potassium fluorosilicate crystal slurry in a centrifuge to separate the product and mother liquor. The mother liquor is sent to the mother liquor storage tank for reuse to dissolve potassium chloride. The product is washed with clean water, centrifuged, and then sent to a single cylinder for drying and rotation. Drying is carried out in the kiln, and the dried products are screened through a single-layer vibrating screen to distinguish qualified products from unqualified products. Unqualified products are centrifuged and washed and then added to a potassium chloride dissolving tank. Qualified products are processed by an automatic packaging machine. After packaging and molding, potassium fluorosilicate is obtained.

The refined fluorosilicic acid is prepared by the following steps:

The raw material fluosilicic acid with a concentration of 30-40% is pumped from the raw material storage tank to the fluosilicic acid blending tank, and then water is added to blend to a concentration of 12%, and then sent to the filter press for filtration, and the silicon-containing filter residue is returned to the blending tank. The filtrate is sent to the fluosilicic acid storage tank for later use.

Beneficial effects of the present invention:

The invention is a production method of potassium fluorosilicate. First, the fluorosilicic acid is refined and placed in a fluorosilicic acid storage tank for later use; then the potassium chloride is dissolved and impurities are removed to prepare a potassium chloride solution; finally, the potassium chloride is dissolved and impurities are removed. Refined fluosilicate and potassium chloride solutions are reacted in a synthesis tank to prepare potassium fluosilicate crystal slurry, which is then centrifuged and washed with a centrifuge to prepare potassium fluosilicate.

The production method of potassium fluorosilicate in the present invention is simple, and can rationally utilize the filtrate and filter residue generated during the production process, thereby reducing production costs.

Description of drawings

In order to explain the technical solutions of the embodiments of the present invention more clearly, the drawings needed to describe the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without exerting creative efforts.

Figure 1 is a flow chart of the production process of potassium fluorosilicate.

Figure 2 is a flow chart of the refining process of fluorosilicic acid.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.

Example 1

A method for producing potassium fluorosilicate, including the following steps:

Step S1: Add ^5m3 mother liquor, ^10m3 water and 4.5t potassium chloride into the potassium chloride dissolving tank, stir and mix evenly, then add hydrochloric acid with a concentration of 6mol/L to adjust the pH of the solution to 5.3, turn on the stirrer and stir for 1.5h After that, take the potassium chloride solution for analysis and testing. After the potassium chloride concentration reaches 220g/L, it is sent to the filter press for filtering, and then the filtrate is sent to the potassium chloride impurity removal tank for impurity removal. The filtrate after impurity removal Then it is sent to the filter press for filtering, and the filtrate after filtering is stored in a potassium chloride storage tank for later use;

Step S2: Pump the potassium chloride solution and refined fluorosilicic acid to the potassium chloride metering tank and the fluorosilicic acid metering tank respectively for measurement, and then pass the measured 3m ³ potassium chloride solution and 2.5m ³ refined fluorosilicic acid through The pipeline is sent into the synthesis tank at the same time, and reacts at normal temperature and pressure for 1 hour. After the reaction is completed, the potassium fluorosilicate crystal slurry is obtained;

Step S3: Centrifuge the potassium fluorosilicate crystal slurry in a centrifuge to separate the product and mother liquor. The mother liquor is sent to the mother liquor storage tank for reuse to dissolve potassium chloride. The product is washed with clean water, centrifuged, and then sent to a single cylinder for drying and rotation. Drying is carried out in the kiln, and the dried products are screened through a single-layer vibrating screen to distinguish qualified products from unqualified products. Unqualified products are centrifuged and washed and then added to a potassium chloride dissolving tank. Qualified products are processed by an automatic packaging machine. After packaging and molding, potassium fluorosilicate is obtained.

Refined fluorosilicic acid is prepared by the following steps:

The raw material fluosilicic acid with a concentration of 30% is pumped from the raw material storage tank to the fluosilicic acid blending tank, and then water is added to blend to a concentration of 12%, and then sent to the filter press for filtering, and the silicon-containing filter residue is returned to the blending tank for reuse. The filtrate is sent to the fluosilicic acid storage tank for later use.

Example 2

A method for producing potassium fluorosilicate, including the following steps:

Step S1: Add ^10m3 mother liquor, ^20m3 water and 9t potassium chloride into the potassium chloride dissolving tank, stir and mix evenly, then add hydrochloric acid with a concentration of 6mol/L to adjust the pH of the solution to 5.3, turn on the stirrer and stir for 1.5h. , take the potassium chloride solution for analysis and testing. After the potassium chloride concentration reaches 230g/L, send it to the filter press for filtering, and then send the filtrate to the potassium chloride impurity removal tank for impurity removal. The filtrate after the impurity removal is sent to Enter the filter press for filtering, and the filtrate after filtering is stored in a potassium chloride storage tank for later use;

Step S2: Pump the potassium chloride solution and refined fluorosilicic acid to the potassium chloride metering tank and the fluorosilicic acid metering tank respectively for measurement, and then pass the measured 6m ³ potassium chloride solution and 5m ³ refined fluorosilicic acid through the pipeline. At the same time, it is sent into the synthesis tank and reacts at normal temperature and pressure for 1 hour. After the reaction is completed, the potassium fluorosilicate crystal slurry is obtained;

Step S3: Centrifuge the potassium fluorosilicate crystal slurry in a centrifuge to separate the product and mother liquor. The mother liquor is sent to the mother liquor storage tank for reuse to dissolve potassium chloride. The product is washed with clean water, centrifuged, and then sent to a single cylinder for drying and rotation. Drying is carried out in the kiln, and the dried products are screened through a single-layer vibrating screen to distinguish qualified products from unqualified products. Unqualified products are centrifuged and washed and then added to a potassium chloride dissolving tank. Qualified products are processed by an automatic packaging machine. After packaging and molding, potassium fluorosilicate is obtained.

Refined fluorosilicic acid is prepared by the following steps:

The raw material fluosilicic acid with a concentration of 35% is pumped from the raw material storage tank to the fluosilicic acid blending tank, and then water is added to blend to a concentration of 12%, and then sent to the filter press for filtering, and the silicon-containing filter residue is returned to the blending tank for reuse. The filtrate is sent to the fluosilicic acid storage tank for later use.

Example 3

A method for producing potassium fluorosilicate, including the following steps:

Step S1: Add ^15m3 mother liquor, ^30m3 water and 13.5t potassium chloride into the potassium chloride dissolving tank, stir and mix evenly, then add hydrochloric acid with a concentration of 6mol/L to adjust the pH of the solution to 5.3, turn on the stirrer and stir for 1.5h After that, take the potassium chloride solution for analysis and testing. After the potassium chloride concentration reaches 240g/L, it is sent to the filter press for filtering, and then the filtrate is sent to the potassium chloride impurity removal tank for impurity removal. The filtrate after impurity removal Then it is sent to the filter press for filtering, and the filtrate after filtering is stored in a potassium chloride storage tank for later use;

Step S2: Pump the potassium chloride solution and refined fluorosilicic acid to the potassium chloride metering tank and the fluorosilicic acid metering tank respectively for measurement, and then process the measured 9m ³ potassium chloride solution and 7.5m ³ refined fluorosilicic acid. The pipeline is sent into the synthesis tank at the same time, and reacts at normal temperature and pressure for 1 hour. After the reaction is completed, the potassium fluorosilicate crystal slurry is obtained;

Step S3: Centrifuge the potassium fluorosilicate crystal slurry in a centrifuge to separate the product and mother liquor. The mother liquor is sent to the mother liquor storage tank for reuse to dissolve potassium chloride. The product is washed with clean water, centrifuged, and then sent to a single cylinder for drying and rotation. Drying is carried out in the kiln, and the dried products are screened through a single-layer vibrating screen to distinguish qualified products from unqualified products. Unqualified products are centrifuged and washed and then added to a potassium chloride dissolving tank. Qualified products are processed by an automatic packaging machine. After packaging and molding, potassium fluorosilicate is obtained.

Refined fluorosilicic acid is prepared by the following steps:

The raw material fluosilicic acid with a concentration of 40% is pumped from the raw material storage tank to the fluosilicic acid blending tank, and then water is added to blend to a concentration of 12%, and then sent to the filter press for filtering, and the silicon-containing filter residue is returned to the blending tank for reuse. The filtrate is sent to the fluosilicic acid storage tank for later use.

In the description of the specification, reference to the terms "one embodiment," "example," "specific example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one aspect of the invention. in an embodiment or example. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The above contents are only examples and explanations of the concept of the invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or substitute them in similar ways, as long as they do not deviate from the concept of the invention. or beyond the scope defined by the claims, shall belong to the protection scope of the present invention.

Claims (4)

1. A method for producing potassium fluorosilicate, characterized in that it includes the following steps: Step S1: Add the mother liquor, water and potassium chloride into the potassium chloride dissolving tank, stir and mix evenly, then add hydrochloric acid with a concentration of 6 mol/L to adjust the pH of the solution to 5.3, turn on the stirrer and stir for 1.5 hours, then take the potassium chloride solution For analysis and testing, after the potassium chloride concentration reaches 220-240g/L, it is sent to the filter press for filtering, and then the filtrate is sent to the potassium chloride impurity removal tank for impurity removal. The impurity-removed filtrate is then sent to the filter press. Carry out press filtration, and store the filtrate after press filtration in a potassium chloride storage tank for later use; Step S2: Pump the potassium chloride solution and refined fluorosilicic acid to the potassium chloride metering tank and the fluorosilicic acid metering tank respectively for measurement, and then send the measured potassium chloride solution and refined fluorosilicic acid simultaneously to the synthesis via pipelines. In the tank, react for 1 hour at normal temperature and pressure. After the reaction is completed, potassium fluorosilicate crystal slurry will be obtained; Step S3: Centrifuge the potassium fluorosilicate crystal slurry in a centrifuge to separate the product and mother liquor. The mother liquor is sent to the mother liquor storage tank for reuse to dissolve potassium chloride. The product is washed with clean water, centrifuged, and then sent to a single cylinder for drying and rotation. Drying is carried out in the kiln, and the dried products are screened through a single-layer vibrating screen to distinguish qualified products from unqualified products. Unqualified products are centrifuged and washed and then added to a potassium chloride dissolving tank. Qualified products are processed by an automatic packaging machine. After packaging and molding, potassium fluorosilicate is obtained. 2. A method for producing potassium fluorosilicate according to claim 1, characterized in that in step S1, the dosage of potassium chloride solution and refined fluorosilicic acid is ^3-9m3 : ^2.5-7.5m3 . 3. A kind of potassium fluorosilicate production method according to claim 1, characterized in that the dosage ratio of reused mother liquor, water and potassium chloride in the potassium chloride solution is ^5-15m3 :10-30m ³ : 4.5-13.5t. 4. A kind of potassium fluorosilicate production method according to claim 1, characterized in that the refined fluorosilicic acid is prepared by the following steps: The raw material fluosilicic acid with a concentration of 30-40% is pumped from the raw material storage tank to the fluosilicic acid blending tank, and then water is added to blend to a concentration of 12%, and then sent to the filter press for filtration, and the silicon-containing filter residue is returned to the blending tank. The filtrate is sent to the fluosilicic acid storage tank for later use.