Production system of electronic-grade isopropanol

Abstract

The utility model provides a production system of electronic-grade isopropanol, and belongs to the technical field of purification devices. The production system of the electronic-grade isopropanol comprises an adsorption tower, a flash tank, a light component removal rectifying tower and a heavy component removal rectifying tower, an industrial-grade isopropanol raw material feeding hole and a crude product discharging hole are formed in the tower bottom of the adsorption tower, and an ionic liquid feeding hole is formed in the tower top of the adsorption tower; the crude product discharging hole is connected with a feeding hole of the flash tank through a pipeline; an ionic liquid discharge hole is formed in the bottom end of the flash tank, and an isopropanol discharge hole is formed in the top of the flash tank; the ionic liquid discharging hole is connected with an ionic liquid feeding hole in the top of the adsorption tower through a pipeline; the isopropanol discharge port is connected with a feed port of the light component removal rectifying tower through a pipeline; and a discharge port at the bottom of the light component removal rectifying tower is connected with a feed port of the heavy component removal rectifying tower through a pipeline. The electronic-grade isopropanol production system provided by the utility model not only is simple to operate, can obtain electronic-grade isopropanol above G5 grade, but also can be used for large-scale production, and is low in production cost.

Description

Technical Field

[0001] The utility model belongs to the technical field of purification devices, and particularly relates to a production system for electronic-grade isopropanol. Background Art

[0002] In recent years, with the continuous development of the semiconductor manufacturing process, the purity requirements for the chemical reagents used have become increasingly high. The metal ion purity of electronic-grade isopropanol has developed from the ppm level of single metal ion content to the current ppb and ppt levels, the water content is less than 50 ppm, and the gas-phase purity is greater than 99.99% in terms of quality requirements. According to the standards of the International Semiconductor Association SEMI, except for organic impurities, the metal ions in G4-grade isopropanol should be less than 1 ppb, the single metal ions in G5-grade isopropanol should be less than 10 ppt, and the water content should be less than 30 ppm.

[0003] Currently, for ultra-pure electronic-grade isopropanol above G4 level applied in the semiconductor electronics industry, conventional methods such as rectification, adsorption, and precision filtration are used for purification, but the effect is poor. For example, Chinese Patent CN115806472A discloses a preparation method of electronic-grade isopropanol. This method sequentially uses rectification to remove light components and heavy components; uses a molecular sieve membrane to dehydrate; uses an adsorption resin to remove metal ions, acids, and alkalis; and finally uses a membrane separation device to remove microparticles in the product. Although rectification can remove organic impurities, its ability to remove water and metal ions is limited; using a molecular sieve to adsorb water will introduce a large amount of metal ions such as sodium, calcium, and silicon, and although using a resin can adsorb metal ions, it will introduce water. Since water can form an azeotrope with isopropanol, as a result, the water content in the final product is very easy to exceed 50 ppm. Moreover, most of the current domestic production and development process technologies can only produce mid- to low-end electronic-grade isopropanol products below G4 level, and the production scale rarely reaches a production capacity of thousands of tons. Content of the Utility Model

[0004] The utility model provides a production system for electronic-grade isopropanol. The production system for electronic-grade isopropanol provided by the utility model is not only simple to operate, can obtain electronic-grade isopropanol above G5 level, but also can be produced on a large scale with low production costs.

[0005] In order to achieve the above object, the utility model provides a production system for electronic-grade isopropanol, including an adsorption tower, a flash tank, a light-component rectification tower, and a heavy-component rectification tower;

[0006] An industrial-grade isopropanol raw material inlet and a crude product outlet are arranged at the bottom of the adsorption tower, and an ionic liquid inlet is arranged at the top of the adsorption tower;

[0007] The crude product discharge port is connected to the feed port of the flash tank through a pipeline; an ionic liquid discharge port is provided at the bottom end of the flash tank, and an isopropanol discharge port is provided at the top of the tank; the ionic liquid discharge port is connected to the ionic liquid feed port at the top of the adsorption tower through a pipeline;

[0008] The isopropanol discharge port is connected to the feed port of the light component removal distillation column through a pipeline; the discharge port at the bottom of the light component removal distillation column is connected to the feed port of the heavy component removal distillation column through a pipeline.

[0009] Preferably, a vacuum drying device is further provided; the feed port of the vacuum drying device is connected to the ionic liquid discharge port at the bottom end of the flash tank through a pipeline; the discharge port of the vacuum drying device is connected to the ionic liquid feed port at the top of the adsorption tower through a pipeline.

[0010] Preferably, a light component collection tank is further provided; the light component collection tank is connected to the discharge port at the top of the light component removal distillation column through a pipeline.

[0011] Preferably, an electronic grade isopropanol storage tank is further provided; the electronic grade isopropanol storage tank is connected to the discharge port at the top of the heavy component removal distillation column through a pipeline.

[0012] Preferably, a heavy component collection tank is further provided; the heavy component collection tank is connected to the discharge port at the bottom of the heavy component removal distillation column through a pipeline.

[0013] Preferably, liquid pumps are provided on the pipeline connected to the feed port of the heavy component removal distillation column and on the pipeline connected to the heavy component collection tank.

[0014] Preferably, a circulating feed port is further provided at the bottom of the light component removal distillation column, so that the heavy components discharged from the light component removal distillation column can be returned to the light component removal distillation column.

[0015] Preferably, a circulating feed port is further provided at the bottom of the heavy component removal distillation column, so that the heavy components removed from the heavy component removal distillation column can be returned to the heavy component removal distillation column.

[0016] Compared with the prior art, the advantages and positive effects of the present utility model are as follows:

[0017] The production system of electronic grade isopropanol provided by the present utility model first sets an adsorption tower, and adsorbs through the ionic liquid adsorbent in the adsorption tower, while removing water and metal ions in the isopropanol, thereby greatly reducing the water and metal element content in the electronic grade isopropanol. Then, a flash tank is used for flash evaporation to separate the ionic liquid adsorbed with water and metal ions from the isopropanol. Then, the isopropanol is sequentially transferred into the light component removal distillation column and the heavy component removal distillation column for light component removal and heavy component removal to obtain electronic grade isopropanol. This production system can not only obtain G5 grade electronic isopropanol, but also has simple operation, continuous production, low production cost, and can also have a production capacity of thousands of tons, making it suitable for industrial production.

[0018] By setting up a vacuum drying device, the ionic liquid that adsorbs moisture and metal ions in the flash evaporation tank is dried, so that the ionic liquid can be reused, which not only enables continuous production but also further reduces costs. Brief Description of the Drawings

[0019] Figure 1 It is a schematic structural diagram of the production system of electronic-grade isopropyl alcohol of the present utility model;

[0020] Wherein: 1 - adsorption tower, 2 - flash evaporation tank, 3 - light component distillation column, 4 - heavy component distillation column, 5 - vacuum drying device, 6 - light component collection tank, 7 - electronic-grade isopropyl alcohol storage tank, 8 - heavy component collection tank, 9 - liquid pump. Detailed Embodiments

[0021] Next, the technical solutions in the embodiments of the present utility model will be described clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present utility model without creative efforts shall fall within the protection scope of the present utility model.

[0022] As Figure 1 shown, the present utility model provides a production system of electronic-grade isopropyl alcohol, including an adsorption tower 1, a flash evaporation tank 2, a light component distillation column 3, and a heavy component distillation column 4;

[0023] An industrial-grade isopropyl alcohol raw material inlet and a crude product outlet are provided at the bottom of the adsorption tower 1, and an ionic liquid inlet is provided at the top of the tower;

[0024] The crude product outlet is connected to the inlet of the flash evaporation tank 2 through a pipeline; an ionic liquid outlet is provided at the bottom end of the flash evaporation tank 2, and an isopropyl alcohol outlet is provided at the top of the tank; the ionic liquid outlet is connected to the ionic liquid inlet at the top of the adsorption tower 1 through a pipeline;

[0025] The isopropyl alcohol outlet is connected to the inlet of the light component distillation column 3 through a pipeline; the outlet at the bottom of the light component distillation column 3 is connected to the inlet of the heavy component distillation column 4 through a pipeline.

[0026] During operation, the industrial-grade isopropyl alcohol raw material and the ionic liquid enter the adsorption tower 1 from the industrial-grade isopropyl alcohol raw material inlet at the bottom of the adsorption tower 1 and the ionic liquid inlet at the top of the tower respectively. In the adsorption tower 1, the ionic liquid adsorbs water and metal ions, and then enters the flash tank 2. Since the boiling point of the ionic liquid is high, the ionic liquid rich in water and metal ions is distilled out from the bottom of the flash tank 2 as the heavy component, while the dehydrated and de-metallized isopropyl alcohol is discharged from the top of the flash tank 2 as the light component. The isopropyl alcohol from which water and metal ions have been removed flows into the de-light rectification tower 3 through a pipeline from the feed inlet and is de-lighted. The de-lighted isopropyl alcohol flows out from the discharge port at the bottom of the de-light rectification tower 3 and flows into the de-heavy rectification tower 4 through a pipeline from the feed inlet for de-heavy. The de-heavy isopropyl alcohol flows out from the discharge port at the top of the de-heavy rectification tower 4 to obtain electronic-grade isopropyl alcohol.

[0027] In the present utility model, the ionic liquid is preferably 1-methyl-3-(3-propylsulfonic acid) imidazole chloride, 1-butyl-3-(3-propylsulfonic acid) imidazole chloride, 1-hexyl-3-(3-propylsulfonic acid) imidazole chloride, 1-methyl-3-(6-propylsulfonic acid) imidazole chloride, 1-methyl-3-(4-propylsulfonic acid) imidazole chloride, 1-butyl-3-(4-propylsulfonic acid) imidazole chloride, 2-(3-propylsulfonic acid)-N-methyl-pyridine chloride, 1-butyl-2-phenylthiourea pyridine bromide, 1-methyl-3-(2-thioureido) imidazole dibromide, and 1-methyl-2-methyl-3-(2-thioureido) imidazole dibromide.

[0028] In the present utility model, a vacuum drying device 5 is preferably further provided; the feed inlet of the vacuum drying device 5 is connected to the ionic liquid discharge port at the bottom end of the flash tank 2 through a pipeline; the discharge port of the vacuum drying device 5 is connected to the ionic liquid inlet at the top of the adsorption tower 1 through a pipeline. In the present utility model, by providing the vacuum drying device 5, the ionic liquid rich in water and metal ions flowing out of the distillation tank can be adsorbed, so that the ionic liquid can be recycled.

[0029] In the present utility model, in order to facilitate the collection of the light component, a light component collection tank 6 is preferably further provided; the light component collection tank 6 is connected to the discharge port at the top of the de-light rectification tower 3 through a pipeline.

[0030] In the present utility model, in order to facilitate the storage of the end product electronic-grade isopropyl alcohol, an electronic-grade isopropyl alcohol storage tank 7 is preferably further provided; the electronic-grade isopropyl alcohol storage tank 7 is connected to the discharge port at the top of the de-heavy rectification tower 4 through a pipeline.

[0031] In the present utility model, in order to facilitate the collection of the heavy component, a heavy component collection tank 8 is preferably further provided; the heavy component collection tank 8 is connected to the discharge port at the bottom of the de-heavy rectification tower 4 through a pipeline.

[0032] In the present utility model, for the convenience of transportation, it is preferred to provide a liquid pump 9 on the pipeline connected to the feed inlet of the deweight rectification column 4 and on the pipeline connected to the heavy component collection tank 8.

[0033] In the present utility model, it is preferred to further provide a circulating feed inlet at the bottom of the light component removal rectification column 3. In the present utility model, providing a circulating feed inlet at the bottom of the light component removal rectification column 3 can function as a storage tank. When the material in the deweight rectification column 4 is full, the heavy components discharged from the light component removal rectification column 3 can be returned to the light component removal rectification column 3 for temporary storage.

[0034] In the present utility model, it is preferred to further provide a circulating feed inlet at the bottom of the deweight rectification column 4. In the present utility model, providing a circulating feed inlet at the bottom of the deweight rectification column 4 can function as a storage tank. When the material in the heavy component collection tank 8 is full, the heavy components removed from the deweight rectification column 4 can be returned to the deweight rectification column 4 for temporary storage.

[0035] To further illustrate the present utility model, the technical solutions provided by the present utility model will be described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present utility model.

[0036] Embodiment 1

[0037] As shown in the attached Figure 1 The ionic liquid (1-methyl-3-(3-propylsulfonic acid) imidazole chloride) is introduced from the ionic liquid feed inlet at the top of the adsorption column 1, and the industrial-grade isopropanol raw material is introduced from the industrial-grade isopropanol raw material feed inlet at the bottom of the adsorption column 1. The ionic liquid accounts for 0.05% of the mass of the isopropanol raw material feed, the adsorption temperature is 27°C, and the pressure is 1 atm. Subsequently, the adsorbed solution enters the flash tank 2, with a distillation temperature of 84°C and a pressure of 1 atm. The isopropanol after removing water and metal ions is taken out from the top of the flash tank 2 (the mass fraction of isopropanol in the isopropanol after removing water and metal ions is 99.95%, the water content is 55.1 ppm, and the concentration of single metal ions is less than 1 ppb), and the ionic liquid is taken out from the bottom of the flash tank 2 and recycled after vacuum drying. The isopropanol after removing water and metal ions enters the light component removal rectification column 3 (the operating temperature is set at 86°C and the reflux ratio is 6.5). Light components are taken out from the top of the light component removal rectification column 3, and the isopropanol mixed solution taken out from the bottom enters the deweight rectification column 4 for deweighting (the operating temperature is set at 92°C and the reflux ratio is 3). Electronic-grade isopropanol products are taken out from the top of the deweight rectification column 4, with a mass fraction of 99.995%, a water content of 22.1 ppm, a concentration of single metal ions less than 8.5 ppt, and a total metal content of 41.7 ppt.

[0038] The above are only the preferred embodiments of the present utility model. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present utility model, several improvements and refinements can still be made, and these improvements and refinements should also be regarded as the protection scope of the present utility model.

Claims

1. A production system for electronic grade isopropyl alcohol, characterized in that: It includes an adsorption tower, a flash tank, a light removal distillation tower and a heavy removal distillation tower; The adsorption tower is provided with an industrial-grade isopropanol raw material feed port and a crude product discharge port at the bottom, and an ionic liquid feed port at the top; The crude product discharge port is connected to the feed port of the flash tank through a pipeline; the bottom of the flash tank is provided with an ionic liquid discharge port, and the top of the tank is provided with an isopropanol discharge port; the ionic liquid discharge port is connected to the ionic liquid feed port at the top of the adsorption tower through a pipeline; The isopropanol discharge port is connected to the feed port of the light removal distillation tower through a pipeline; the discharge port at the bottom of the light removal distillation tower is connected to the feed port of the heavy removal distillation tower through a pipeline.

2. The production system according to claim 1, characterized in that: A vacuum drying device is also provided; the feed port of the vacuum drying device is connected to the ionic liquid discharge port at the bottom of the flash tank through a pipeline; the discharge port of the vacuum drying device is connected to the ionic liquid feed port at the top of the adsorption tower through a pipeline.

3. The production system according to claim 1, characterized in that: A light component collecting tank is also provided; the light component collecting tank is connected to the discharge port at the top of the light component removal distillation tower through a pipeline.

4. The production system according to claim 1, characterized in that: An electronic grade isopropanol storage tank is also provided; the electronic grade isopropanol storage tank is connected to the discharge port at the top of the de-weighting distillation tower through a pipeline.

5. The production system according to claim 1, characterized in that: A heavy component collecting tank is also provided; the heavy component collecting tank is connected to the discharge port at the bottom of the heavy-removal distillation tower through a pipeline.

6. The production system according to claim 1, characterized in that: Liquid pumps are provided on the pipeline connected to the feed inlet of the de-heavy distillation tower and the pipeline connected to the heavy component collecting tank.

7. The production system according to claim 1, characterized in that: A circulating feed port is also provided at the bottom of the de-lightening distillation tower so that the heavy components discharged from the de-lightening distillation tower can be returned to the de-lightening distillation tower.

8. The production system according to claim 1, characterized in that: A circulating feed port is also provided at the bottom of the heavy-removal distillation tower, so that the heavy components removed in the heavy-removal distillation tower can be returned to the heavy-removal distillation tower.

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