CN214361604U

CN214361604U - Organic silicon waste catalyst extraction-back extraction system

Info

Publication number: CN214361604U
Application number: CN202023168521.8U
Authority: CN
Inventors: 黄明刚; 李军; 唐裕霞; 徐淳; 陈兵
Original assignee: Sichuan Vocational College of Chemical Technology
Current assignee: Sichuan Vocational College of Chemical Technology
Priority date: 2020-12-24
Filing date: 2020-12-24
Publication date: 2021-10-08
Anticipated expiration: 2030-12-24

Abstract

The utility model relates to the technical field of catalyst recovery systems, and provides an organic silicon waste catalyst extraction-back extraction system, which comprises a sulfonation device, an extraction device, a back extraction device and a reduction device which are sequentially communicated; the sulfonation device comprises a kerosene liquid storage tank, a concentrated sulfuric acid liquid storage tank, a sulfonation reaction tank and a water-oil separator; the extraction device comprises an extraction tower; the stripping device comprises a stripping tower; the reduction device comprises a reduction reaction tank and a solid-liquid separation device; the oil phase discharge hole of the back extraction tower is communicated with the feed inlet of the extraction tower. Can carry out high-efficient recovery to the copper ion in the organosilicon abandonment catalyst.

Description

Organic silicon waste catalyst extraction-back extraction system

Technical Field

The utility model relates to a catalyst recovery system technical field particularly, relates to an organic silicon waste catalyst extraction-reextraction system.

Background

Copper-catalyzed reactions such as the Sandmeyer reaction, the Meerwein reaction and the like have important applications in the field of organic synthesis, for example, for synthesizing organosilane compounds, but the reactions can cause the reaction waste catalyst to contain a large amount of copper ions. As a heavy metal ion, copper ions can permeate into water and soil to cause great harm to the water and the soil, and as solid waste, the copper ions can cause great harm to the environment, so that strict copper ion discharge standards are set by many countries, and high requirements are provided for copper pollution treatment technologies. Meanwhile, copper is a precious metal, and the recovery of the copper from the waste catalyst has high economic value.

For this reason, the prior art has tried to recover copper ions by different methods to limit the discharge of copper ions and increase the recovery of copper ions, but none of them is ideal.

For example, sodium hydroxide is used to convert copper ions into copper hydroxide, but since a large amount of other cations in the waste residue of the copper-containing catalyst also react with sodium hydroxide, the amount of sodium hydroxide is large, and the recovery cost is increased.

And if an iron powder replacement method is adopted to convert copper ions into copper, the method not only has incomplete reaction, but also can lead waste liquid to introduce a large amount of iron ions to cause environmental pollution.

Metallic copper can also be obtained by electroplating, but a large amount of electric energy is consumed, making the method difficult to implement in large-scale industrial production.

Therefore, those skilled in the art need to search a new copper ion recovery system which can avoid the emission of copper ions, reduce the recovery cost, and can be implemented in large-scale industrial production.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide an organosilicon abandonment catalyst extraction-reextraction system, it can carry out high-efficient the recovery to the copper ion in the organosilicon abandonment catalyst.

The embodiment of the utility model discloses a realize through following technical scheme:

an organic silicon waste catalyst extraction-back extraction system comprises a sulfonation device, an extraction device, a back extraction device and a reduction device which are communicated in sequence; the sulfonation device comprises a kerosene liquid storage tank, a concentrated sulfuric acid liquid storage tank, a sulfonation reaction tank and a water-oil separator; the extraction device comprises an extraction tower; the stripping device comprises a stripping tower; the reduction device comprises a reduction reaction tank and a solid-liquid separation device; the oil phase discharge hole of the back extraction tower is communicated with the feed inlet of the extraction tower.

Further, a kerosene liquid storage tank is communicated with a feeding hole of the sulfonation reaction tank through a first feeding pipe, and a concentrated sulfuric acid liquid storage tank is communicated with the feeding hole of the sulfonation reaction tank through a second feeding pipe; the first feeding pipe is provided with a first feeding valve, and the second feeding pipe is provided with a second feeding valve.

Furthermore, the extraction device also comprises a liquid mixing pool, a discharge hole of the water-oil separator is communicated with a feed inlet of the liquid mixing pool, and a discharge hole of the liquid mixing pool is communicated with a feed inlet of the extraction tower; the oil phase discharge hole of the back extraction tower is communicated with the feed inlet of the liquid mixing pool through a circulating pipeline.

Further, a flow monitor is arranged at a feed inlet of the liquid mixing tank.

Further, a stirrer is arranged in the liquid mixing pool.

Further, a third feeding valve is arranged at the feeding hole of the extraction tower.

Further, the feed inlet of the stripping tower is provided with a fourth feed valve.

Further, the solid-liquid separation device is a filter or a centrifugal separator.

The utility model discloses technical scheme has following advantage and beneficial effect at least:

the utility model provides an organosilicon abandonment catalyst extraction-reextraction system, concentrated sulfuric acid and kerosene carry out the sulfonation processing in the sulfonation unit, and sulfonated kerosene is again extracted the copper ion in the organosilicon abandonment catalyst in the extraction unit, and the back extraction of reuse dilute sulfuric acid obtains copper sulfate solution in the reextraction unit, and copper sulfate solution is reduced into metallic copper by the iron powder in the reduction plant; by using the system, copper ions can be effectively extracted from the organic silicon waste catalyst, the recovery rate is high, and the content of heavy metals in solid waste is reduced; moreover, the oil phase after the back extraction comprises sulfonated kerosene and an extractant, and the back extraction effect is good, so that the extraction can be directly recycled, the waste liquid is reduced, and the environment is benefited; the system reduces the production cost and can be used in large-scale industrial production.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

Fig. 1 is a schematic structural diagram of an organosilicon waste catalyst extraction-back extraction system provided in embodiment 1 of the present invention.

Icon:

the device comprises a 1-kerosene storage tank, a 2-concentrated sulfuric acid storage tank, a 3-sulfonation reaction tank, a 4-water-oil separator, a 5-liquid mixing tank, a 6-extraction tower, a 7-stripping tower, an 8-reduction reaction tank, a 9-solid-liquid separation device, a 10-first feed valve, a 11-second feed valve, a 12-flow monitor, a 13-third feed valve, a 14-fourth feed valve and a 15-circulating pipeline.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention, as generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations.

Thus, the following detailed description of the embodiments of the present invention, presented in the accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.

In the description of the present invention, it should be noted that if the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate an orientation or positional relationship based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship which is usually placed when the product of this application is used, the description is merely for convenience and simplicity of description, and it is not intended to indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.

In the description of the present invention, it should be further noted that unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" should be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

Example 1

As shown in fig. 1, this embodiment provides an organic silicon waste catalyst extraction-back extraction system, which includes a sulfonation device, an extraction device, a back extraction device, and a reduction device, which are sequentially connected; the sulfonation device comprises a kerosene liquid storage tank 1, a concentrated sulfuric acid liquid storage tank 2, a sulfonation reaction tank 3 and a water-oil separator 4; the extraction device comprises an extraction tower 6; the stripping apparatus comprises a stripping column 7; the reduction device comprises a reduction reaction tank 8 and a solid-liquid separation device 9; the oil phase discharge hole of the back extraction tower 7 is communicated with the feed inlet of the extraction tower 6.

The method comprises the following steps of (1) sulfonating concentrated sulfuric acid and kerosene in a sulfonating device, extracting copper ions in the organic silicon waste catalyst in an extracting device by the sulfonated kerosene, back-extracting the copper ions in a back-extracting device by dilute sulfuric acid to obtain a copper sulfate solution, and reducing the copper sulfate solution into metal copper by iron powder in a reducing device; by using the system, copper ions can be effectively extracted from the organic silicon waste catalyst, the recovery rate is high, and the content of heavy metals in solid waste is reduced; moreover, the oil phase after the back extraction comprises sulfonated kerosene and an extractant, and the back extraction effect is good, so that the extraction can be directly recycled, the waste liquid is reduced, and the environment is benefited; the system reduces the production cost and can be used in large-scale industrial production.

In the embodiment, a kerosene liquid storage tank 1 is communicated with a feeding hole of a sulfonation reaction tank 3 through a first feeding pipe, and a concentrated sulfuric acid liquid storage tank 2 is communicated with a feeding hole of the sulfonation reaction tank 3 through a second feeding pipe; the first feeding pipe is provided with a first feeding valve 10, and the second feeding pipe is provided with a second feeding valve 11.

Can control the input speed of concentrated sulfuric acid and kerosene through first feed valve 10 and second feed valve 11 for the concentrated sulfuric acid is fixed with the feeding proportion of kerosene, and the sulfonated kerosene steady quality of producing guarantees the extraction effect. Specifically, the volume ratio of kerosene to concentrated sulfuric acid is 8: 2.

in this embodiment, the extraction apparatus further includes a liquid mixing tank 5, a discharge port of the water-oil separator 4 is communicated with a feed port of the liquid mixing tank 5, and a discharge port of the liquid mixing tank 5 is communicated with a feed port of the extraction tower 6; the oil phase discharge port of the back extraction tower 7 is communicated with the feed port of the liquid mixing tank 5 through a circulating pipeline 15.

The sulfonated kerosene and the extracting agent are mixed in the liquid mixing tank 5 and then enter the extracting tower 6 after being mixed, and the extraction effect is improved by mixing the sulfonated kerosene and the extracting agent in advance; the oil phase flowing out of the stripping tower 7 returns to the liquid mixing tank 5 through a circulating pipeline 15, and reenters the extracting tower 6 together with the mixed sulfonated kerosene and the extracting agent for utilization.

In this embodiment, a flow monitor 12 is disposed at the feed inlet of the liquid mixing tank 5. The flow monitor 12 can detect the flow of the sulfonated kerosene flowing into the liquid mixing tank 5, so that the feeding speed of the extracting agent can be determined according to the feeding speed of the sulfonated kerosene, and the proportion of the sulfonated kerosene and the extracting agent is stable.

In this embodiment, a stirrer is provided in the liquid mixing tank 5. The stirrer enables the mixing effect of the sulfonated kerosene and the extracting agent in the liquid mixing pool 5 to be better, and the extracting effect to be more stable.

In this embodiment, the feed inlet of the extraction column 6 is provided with a third feed valve 13. The feeding speed of the mixed sulfonated kerosene and the extracting agent can be adjusted by adjusting the third feeding valve 13.

In this embodiment, the feed inlet of the stripping column 7 is provided with a fourth feed valve 14. The speed of the sulfonated kerosene after extraction of copper ions into the stripping column 7 can be adjusted by adjusting the fourth feed valve 14.

In this embodiment, the solid-liquid separation device 9 is a filter or a centrifugal separator. The iron powder and the copper sulfate solution in the reduction reaction tank 8 react to displace copper simple substance, the liquid in the reduction reaction tank 8 flows into a filter device, and the filter and the centrifugal separator can separate the metal copper and the salt solution after the reduction reaction to obtain the metal copper.

In conclusion, the organic silicon waste catalyst extraction-back extraction system provided by the embodiment can efficiently recover copper ions in the organic silicon waste catalyst, and the extraction liquid can be recycled, so that the production cost is reduced, and the environmental pollution is reduced.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An organic silicon waste catalyst extraction-back extraction system is characterized by comprising a sulfonation device, an extraction device, a back extraction device and a reduction device which are communicated in sequence;

the sulfonation device comprises a kerosene liquid storage tank (1), a concentrated sulfuric acid liquid storage tank (2), a sulfonation reaction tank (3) and a water-oil separator (4); the extraction device comprises an extraction column (6); the stripping unit comprises a stripping column (7); the reduction device comprises a reduction reaction tank (8) and a solid-liquid separation device (9);

and an oil phase discharge hole of the back extraction tower (7) is communicated with a feed inlet of the extraction tower (6).

2. The organosilicon spent catalyst extraction-stripping system according to claim 1, wherein the kerosene storage tank (1) is communicated with the feed inlet of the sulfonation reaction tank (3) through a first feed pipe, and the concentrated sulfuric acid storage tank (2) is communicated with the feed inlet of the sulfonation reaction tank (3) through a second feed pipe;

the first feeding pipe is provided with a first feeding valve (10), and the second feeding pipe is provided with a second feeding valve (11).

3. The organosilicon spent catalyst extraction-stripping system according to claim 1, wherein the extraction device further comprises a liquid mixing tank (5), the discharge port of the water-oil separator (4) is communicated with the feed port of the liquid mixing tank (5), and the discharge port of the liquid mixing tank (5) is communicated with the feed port of the extraction tower (6);

and an oil phase discharge hole of the back extraction tower (7) is communicated with a feed inlet of the liquid mixing pool (5) through a circulating pipeline (15).

4. The organosilicon spent catalyst extraction-stripping system according to claim 3, wherein the feed inlet of the liquid mixing tank (5) is provided with a flow monitor (12).

5. The organosilicon spent catalyst extraction-stripping system according to claim 3, wherein a stirrer is arranged in the liquid mixing tank (5).

6. The organosilicon spent catalyst extraction-stripping system according to claim 1, wherein the extractor (6) feed inlet is provided with a third feed valve (13).

7. The organosilicon spent catalyst extraction-stripping system according to claim 1, wherein the stripper (7) feed is provided with a fourth feed valve (14).

8. The organosilicon spent catalyst extraction-stripping system according to claim 1, wherein the solid-liquid separation device (9) is a filter or a centrifugal separator.