Microporous filter for efficient concentrated fluosilicic acid deiodination

By using the combined technology of microporous filters and activated carbon in the fluorine chemical industry, impurities such as iodine and arsenic in fluorosilicic acid are efficiently removed, solving the problem that hydrogen fluoride products in the existing technology do not meet electronic grade requirements, and achieving high efficiency and environmental protection. production of hydrogen fluoride products.

CN222368559UActive Publication Date: 2025-01-21FUJIAN WENGFU LANTIAN FLUORINE CHEM IND CO LTD
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Patent Information

Application Number
CN202323324593.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2023-12-07
Publication Date
2025-01-21
Estimated Expiration
2033-12-07

AI Technical Summary

Technical Problem

In the prior art, when the wet phosphoric acid by-product fluorosiliic acid is used to produce anhydrous hydrogen fluoride, it is difficult to effectively remove impurities such as arsenic, iodine, chlorine and metal ions, resulting in the production of hydrogen fluoride that cannot meet the electronic grade usage requirements.

Method used

A microporous filter is used to intercept solid particles and colloids in the solution through the microporous filter, and then react with the hydrogen peroxide solution, and are sent to the microporous filter through the delivery pump to fully contact the activated carbon. Carry out removal to achieve efficient removal of iodine and arsenic.

Benefits of technology

The iodine removal rate in the solution is over 95%, and a certain arsenic removal effect is achieved, ensuring that the hydrogen fluoride product produced from concentrated fluorosilicic acid after removal can meet the requirements for the production of electronic-grade hydrofluoric acid.

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Abstract

The utility model relates to the technical field of fluorine chemical industry, in particular to a microporous filter for high-efficiency concentrated fluosilicic acid deiodination, which comprises a slurry tank connected with a microporous filter I, the microporous filter I is connected with a feeding pipe and a filtrate buffer tank, the filtrate buffer tank is connected with a motor and a rotating shaft, and the rotating shaft is connected with the motor. A filtrate delivery pump and a microporous filter II are arranged on one side of the filtrate buffer tank; the iodine removal device has the beneficial effects that solid particles and jelly in a solution are intercepted by the microporous filter I, the intercepted filtrate reacts with a hydrogen peroxide solution and then is fed into the microporous filter II through the conveying pump, and the filtrate is in full contact with activated carbon at the position so as to be removed, and the removal rate of iodine in the solution is more than 95% through laboratory and pilot tests, so that the iodine removal rate is more than 95%. Meanwhile, a certain arsenic removal effect is achieved, and removed and separated iodine can be recycled, so that a hydrogen fluoride product produced by concentrated fluosilicic acid after removal can meet the requirement for producing electronic-grade hydrofluoric acid.
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Description

Technical Field

[0001] The utility model relates to the technical field of fluorine chemical industry, in particular to a microporous filter used for high-efficiency deiodination of concentrated fluorosilicic acid. Background Art

[0002] Many application areas of fluorine chemical industry are based on the production of hydrofluoric acid. At present, more than half of the world's fluorite production is used to produce hydrofluoric acid. According to statistics from the National Bureau of Statistics and the Ministry of Land and Resources, the basic reserves of fluorite resources identified in my country in 2018 were about 45.543 million tons, mainly concentrated in Zhejiang, Fujian, Jiangxi, Hunan, Inner Mongolia and other regions, and several representative fluorine chemical industry parks have been formed around the above-mentioned regions. With the deepening of the national industrial structure adjustment and the improvement of the technical level of downstream industries, the demand for anhydrous hydrogen fluoride for electronic-grade fluorides, fluorine-containing refrigerants, fluorine-containing polymer materials, fluorine-containing fine chemicals and other products has grown rapidly. However, as a national strategic resource, there are plans and restrictions on the mining of fluorite.

[0003] Some domestic companies have developed technology to utilize fluorosilicic acid, a by-product of wet-process phosphoric acid, to produce anhydrous hydrogen fluoride, which has greatly alleviated the mining and dependence on fluorite and played a positive protective role for fluorite.

[0004] However, due to the influence of phosphate rock, the production of hydrogen fluoride from fluorosilicic acid, a by-product of wet phosphoric acid, will bring in a lot of impurities, mainly arsenic, iodine, chlorine and metal ions. The current method is not convenient for effectively removing impurities, resulting in the production of hydrogen fluoride that cannot meet electronic grade requirements. Utility Model Content

[0005] The utility model aims to provide a microporous filter for high-efficiency concentrated fluorosilicic acid deiodination to solve the problems raised in the above-mentioned background technology.

[0006] To achieve the above object, the utility model provides the following technical solution: a microporous filter for high-efficiency concentrated fluorosilicic acid deiodination, the microporous filter for high-efficiency concentrated fluorosilicic acid deiodination comprising:

[0007] A slurry tank, wherein the slurry tank is connected to a microporous filter 1, the microporous filter 1 is connected to a feed pipe and a connecting pipe 2, the connecting pipe 2 is connected to a filtrate buffer tank, the filtrate buffer tank is connected to a motor and a rotating shaft, one end of the rotating shaft is provided with a stirring blade, one side of the filtrate buffer tank is provided with a delivery pipe 2, a filtrate delivery pump and a delivery pipe 1, the delivery pipe 1 is connected to a microporous filter 2, and the microporous filter 2 is connected to a discharge pipe.

[0008] Preferably, a connecting pipe 1 is provided on the middle side wall of the upper end of the slurry trough, and a connecting pipe 4 is provided on one side of the connecting pipe 1 of the slurry trough, and the slurry trough is fixedly connected to a microporous filter 1 through the connecting pipe 1.

[0009] Preferably, the microporous filter has fixed frame plates fixedly connected to both symmetrical outer walls thereof, a lower end of the microporous filter is funnel-shaped, and a lower end of the microporous filter is fixedly connected to a feed pipe.

[0010] Preferably, the two ends of the connecting pipe 2 are fixedly connected to the microporous filter 1 and the upper end of the filtrate buffer tank respectively, and the upper end of the filtrate buffer tank is provided with a connecting pipe 3, and the outer wall of the connecting pipe 3 is fixedly connected to the end of the connecting pipe 4 away from the slurry tank.

[0011] Preferably, the middle side wall at the upper end of the filtrate buffer tank is fixedly connected to the motor, the output end of the motor passes through the side wall of the filtrate buffer tank and is fixedly connected to the rotating shaft, and stirring blades are fixedly connected to both sides of the outer wall at the other end of the rotating shaft symmetrically.

[0012] Preferably, one side of the outer wall of the filtrate buffer tank is fixedly connected to delivery pipe 2, the other end of delivery pipe 2 is fixedly connected to the input end of the filtrate delivery pump, the output end of the filtrate delivery pump is fixedly connected to delivery pipe 1, and delivery pipe 1 is fixedly connected to the upper end of microporous filter 2.

[0013] Preferably, two symmetrical sides of the outer wall of the second microporous filter are fixedly connected with a second fixing frame plate, and the outer wall of the lower end of the second microporous filter is fixedly connected to the discharge pipe.

[0014] Compared with the prior art, the beneficial effects of the utility model are:

[0015] The solid particles and colloids in the solution are intercepted by the microporous filter 1, and the intercepted filtrate reacts with the hydrogen peroxide solution and is sent to the microporous filter 2 by the delivery pump, where it is fully contacted with the activated carbon for removal. According to laboratory and pilot tests, the iodine removal rate in the solution is more than 95%, and there is also a certain arsenic removal effect. The iodine separated by the removal can be recycled, so that the hydrogen fluoride product produced from the concentrated fluorosilicic acid after the removal can meet the requirements for the production of electronic grade hydrofluoric acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0017] Figure 2 This is a schematic diagram of the internal structure of the filtrate buffer tank of the utility model;

[0018] Figure 3 For this utility model Figure 2 A schematic diagram of the enlarged structure in the middle.

[0019] In the figure: 1. slurry tank; 2. connecting pipe 1; 3. feed pipe; 4. fixed frame plate 1; 5. microporous filter 1; 6. connecting pipe 2; 7. connecting pipe 3; 8. motor; 9. conveying pipe 1; 10. fixed frame plate 2; 11. microporous filter 2; 12. discharge pipe; 13. filtrate conveying pump; 14. conveying pipe 2; 15. filtrate buffer tank; 16. connecting pipe 4; 17. rotating shaft; 18. stirring blade. DETAILED DESCRIPTION

[0020] In order to make the purpose and technical solution of the utility model clearly and completely described, and the advantages more clearly understood, the embodiments of the utility model are further described in detail in conjunction with the accompanying drawings. It should be understood that the specific embodiments described here are part of the embodiments of the utility model, not all of the embodiments, and are only used to explain the embodiments of the utility model, and are not used to limit the embodiments of the utility model. All other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0021] Embodiment 1:

[0022] See also Figure 1-Figure 3 The utility model provides a technical solution: a microporous filter for high-efficiency concentrated fluorosilicic acid deiodination, the microporous filter for high-efficiency concentrated fluorosilicic acid deiodination comprises:

[0023] A slurry tank 1, the slurry tank 1 is connected with a microporous filter 5, the microporous filter 5 is connected with a feed pipe 3 and a connecting pipe 2 6, the connecting pipe 2 6 is connected with a filtrate buffer tank 15, the filtrate buffer tank 15 is connected with a motor 8 and a rotating shaft 17, one end of the rotating shaft 17 is provided with a stirring blade 18, one side of the filtrate buffer tank 15 is provided with a delivery pipe 2 14, a filtrate delivery pump 13 and a delivery pipe 9, the delivery pipe 9 is connected with a microporous filter 2 11, and the microporous filter 2 11 is connected with a discharge pipe 12; a connecting pipe 2 is provided on the middle side wall of the upper end of the slurry tank 1, and a connecting pipe 4 16 is provided on one side of the connecting pipe 2, and the slurry tank 1 is fixedly connected to the microporous filter 5 through the connecting pipe 2; the microporous filter 5 has a fixed frame plate 4 fixedly connected to the outer walls on both symmetrical sides, the lower end of the microporous filter 5 is funnel-shaped, and the lower end of the microporous filter 5 is fixedly connected to the feed pipe 3;

[0024] In order to ensure the absorption effect and reduce equipment operation failures, fluorine-containing materials or polytetrafluoroethylene linings should be selected for the filtrate buffer tank 15 and the inside of the microporous filter to reduce the corrosion of the medium to the equipment. When used in the fluorine chemical industry or in an acidic environment, carbon steel pipes should not be used directly for the conveying pipeline to prevent corrosion and leakage of the medium. Appropriate lining materials should be selected according to the characteristics of the medium used; the microporous filter 15 should be fed from the bottom. The acid at the bottom can use the weight of the solid particles to sink, which is conducive to the removal of the intercepted solid particles.

[0025] Embodiment 2:

[0026] On the basis of Example 1, in order to accelerate the reaction of the filtrate, the two ends of the connecting pipe 2 6 are fixedly connected to the microporous filter 1 5 and the upper end of the filtrate buffer tank 15, respectively. The upper end of the filtrate buffer tank 15 is provided with a connecting pipe 3 7, and the outer wall of the connecting pipe 3 7 is fixedly connected to the end of the connecting pipe 4 16 away from the slurry tank 1; the middle side wall of the upper end of the filtrate buffer tank 15 is fixedly connected to the motor 8, and the output end of the motor 8 passes through the side wall of the filtrate buffer tank 15 and is fixedly connected to the rotating shaft 17, and the outer wall of the other end of the rotating shaft 17 is symmetrically fixedly connected with stirring blades 18 on both sides;

[0027] A hydrogen peroxide solution is added to the filtrate buffer tank 15 through the connecting pipe 3 7. After the filtrate buffer tank 15 contacts the hydrogen peroxide solution, the motor 8 is started to drive the rotating shaft 17 to rotate, thereby accelerating the reaction under the action of the stirring blades 18. When used in the fluorine chemical industry or other places where toxic gases are easily generated, the filtrate buffer tank 15 should be equipped with a negative pressure system to keep the storage tank in a slightly negative pressure environment, effectively avoiding the overflow of toxic gases and causing unnecessary safety and environmental protection incidents.

[0028] Embodiment three:

[0029] On the basis of the first embodiment, in order to further ensure the filtering effect, one side of the outer wall of the filtrate buffer tank 15 is fixedly connected to the second delivery pipe 14, the other end of the second delivery pipe 14 is fixedly connected to the input end of the filtrate delivery pump 13, the output end of the filtrate delivery pump 13 is fixedly connected to the delivery pipe 19, and the delivery pipe 19 is fixedly connected to the upper end of the second microporous filter 11; the outer wall of the second microporous filter 11 is fixedly connected with a fixed frame plate 10 on both symmetrical sides, and the outer wall of the lower end of the second microporous filter 11 is fixedly connected to the discharge pipe 12;

[0030] The microporous filter 211 should choose to inlet acid from the top, which can effectively prevent the activated carbon from flowing out with the liquid, and at the same time reduce the possibility of the activated carbon being impacted, protect the activated carbon to the greatest extent, and prevent the activated carbon skeleton from being destroyed; add an activated carbon blowing program at the bottom of the microporous filter 211. When the activated carbon is gradually compacted, it can be switched to the blowing step for blowing, which effectively avoids the need to stop and refill after the activated carbon is compacted.

[0031] In actual use, foreign raw materials are delivered to the interior of the microporous filter 5 through the delivery pump and the feed pipe 3, and the solid particles and colloids in the solution are intercepted and removed by the microporous filter 5 to avoid affecting the absorption of the activated carbon inside the microporous filter 5. The intercepted solid particles are discharged from the bottom of the microporous filter 5 through the connecting pipe 2 into the slurry tank 1, and the filtered filtrate enters the filtrate buffer tank 15 through the connecting pipe 2 6 at the top of the microporous filter 5, and the hydrogen peroxide solution is added to the filtrate buffer tank 15 through the connecting pipe 3 7. After the filtrate buffer tank 15 contacts the hydrogen peroxide solution, the motor 8 is started to drive the rotating shaft 17 to rotate, thereby accelerating the reaction under the action of the stirring blade 18. After the reaction, it is transported to the microporous filter 2 11 through the delivery pipe 1 9, the filtrate delivery pump 13 and the delivery pipe 2 14. After the filtrate is adsorbed by the activated carbon inside the microporous filter 2 11, it is discharged through the discharge pipe 12 and delivered to the user for use.

[0032] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A microporous filter for efficient deiodination of concentrated fluorosilicic acid, characterized in that: The microporous filter for efficient concentrated fluorosilicic acid deiodination comprises: A slurry tank (1), wherein the slurry tank (1) is connected to a microporous filter (5), the microporous filter (5) is connected to a feed pipe (3) and a connecting pipe (6), the connecting pipe (6) is connected to a filtrate buffer tank (15), the filtrate buffer tank (15) is connected to a motor (8) and a rotating shaft (17), one end of the rotating shaft (17) is provided with a stirring blade (18), one side of the filtrate buffer tank (15) is provided with a delivery pipe (14), a filtrate delivery pump (13) and a delivery pipe (9), the delivery pipe (9) is connected to a microporous filter (11), and the microporous filter (11) is connected to a discharge pipe (12).

2. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 1, characterized in that: A connecting pipe (2) is provided on the middle side wall of the upper end of the slurry trough (1), and a connecting pipe (16) is provided on one side of the connecting pipe (2). The slurry trough (1) is fixedly connected to a microporous filter (5) via the connecting pipe (2).

3. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 1, characterized in that: The microporous filter (5) has a fixed frame plate (4) fixedly connected to both symmetrical outer walls on both sides, the lower end of the microporous filter (5) is funnel-shaped, and the lower end of the microporous filter (5) is fixedly connected to the feed pipe (3).

4. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 2, characterized in that: The two ends of the connecting pipe 2 (6) are respectively fixedly connected to the microporous filter 1 (5) and the upper end of the filtrate buffer tank (15); the upper end of the filtrate buffer tank (15) is provided with a connecting pipe 3 (7); the outer wall of the connecting pipe 3 (7) is fixedly connected to the end of the connecting pipe 4 (16) away from the slurry tank (1).

5. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 1, characterized in that: The middle side wall at the upper end of the filtrate buffer tank (15) is fixedly connected to the motor (8), the output end of the motor (8) passes through the side wall of the filtrate buffer tank (15) and is fixedly connected to the rotating shaft (17), and stirring blades (18) are fixedly connected to the outer wall of the other end of the rotating shaft (17) on both sides symmetrically.

6. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 1, characterized in that: One side of the outer wall of the filtrate buffer tank (15) is fixedly connected to the second delivery pipe (14), the other end of the second delivery pipe (14) is fixedly connected to the input end of the filtrate delivery pump (13), the output end of the filtrate delivery pump (13) is fixedly connected to the first delivery pipe (9), and the first delivery pipe (9) is fixedly connected to the upper end of the second microporous filter (11).

7. A microporous filter for high-efficiency concentrated fluorosilicic acid deiodination according to claim 1, characterized in that: The outer wall of the second microporous filter (11) is fixedly connected to a second fixed frame plate (10) on both symmetrical sides, and the outer wall of the lower end of the second microporous filter (11) is fixedly connected to a discharge pipe (12).