TWI802152B - Isopropanol regeneration system and method - Google Patents

Abstract

The present invention relates to an isopropanol regeneration system and method, which utilizes the isopropanol regeneration system comprising sequentially connected units for removing high-concentration ions, units for removing water, units for removing particles and units for removing low-concentration ions to receive isopropanol The alcohol liquid is used to remove water, remove particles, and remove ions to remove most of the water, particle impurities, anion impurities, cation impurities, and organic impurities to produce semiconductor electronic grade isopropanol regeneration liquid. Especially, the isopropanol content of the isopropanol feed liquid is not more than 99.85%, the isopropanol content of the isopropanol regeneration liquid is not less than 99.99%, the water content is not more than 50 ppm, and the particle impurity content is The number of particulate impurities larger than 0.03 μm is not more than 860, while the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb.

Description

Isopropanol regeneration system and method

The invention relates to an isopropanol regeneration system and method, in particular to an isopropanol regeneration system that utilizes sequentially connected units for removing high-concentration ions, units for removing water, units for removing particles, and units for removing low-concentration ions to receive The isopropanol solution is used to remove water, remove particles and remove ions to remove most of the water, particle impurities, anion impurities, cation impurities, and organic impurities to produce semiconductor electronic grade isopropanol regeneration liquid. Especially, the isopropanol content of the isopropanol feed liquid is not more than 99.85%, the isopropanol content of the isopropanol regeneration liquid is not less than 99.99%, the water content is not more than 50 ppm, and the particle impurity content is The number of particulate impurities larger than 0.03 μm is not more than 860, while the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb.

Isopropanol is a widely used chemical, and it is one of the isomers of propanol. It is a colorless, flammable liquid with a strong odor at normal temperature and pressure. Its molecular formula is C ₃ H ₈ O. In addition, isopropanol is miscible with water, alcohols, ethers and chloroform. The vast majority of isopropanol is used as a solvent or cleaning agent for coatings or industrial production processes, such as cleaning solvents for cleaning semiconductor wafer impurities. Especially as an extractant in pharmaceutical applications, because the residual toxicity is quite low and safe. In addition, isopropanol can also be used as an additive in gasoline.

As a cleaning solvent, due to the increasingly stringent requirements for the cleanliness of wafers in high-end semiconductor manufacturing processes, a large amount of low-concentration isopropanol is produced, so the demand for low-concentration isopropanol has also increased significantly.

The general known technology is to upgrade the low-concentration isopropanol liquid to industrial grade isopropanol by means of a distillation tower with a vapor permeable membrane system, such as upgrading 10% isopropanol to electronic grade 99.9% isopropanol. On the whole, the structure of the distillation tower is quite complicated, and skilled operators are required to be competent, especially frequent maintenance is required, so the overall processing cost is quite high. Vapor permeation membrane is to use osmosis to purify the vapor state waste liquid, so as to remove impurities. However, the above-mentioned technology cannot be further improved to electronic grade isopropanol, for example, the purity is greater than 99.99%, the content of anions is 4-5 ppb, and the content of cations is 0.09-1 ppb.

Therefore, need a kind of innovative isopropanol regeneration system and method, utilize the isopropanol regeneration system of removing high-concentration ion unit, removing water unit, removing particle unit and removing low-concentration ion unit connected in sequence, in order to receive isopropanol Alcohol liquid is used to remove water, remove particles and remove ions to remove most of the water, particle impurities, anion impurities, cation impurities, and organic impurities to produce semiconductor electronic grade isopropanol regeneration liquid, especially, the isopropanol liquid The isopropanol content is not more than 99.85%, the isopropanol content of the isopropanol regeneration solution is not less than 99.99%, the water content is not more than 50 ppm, and the particulate impurity content is the number of particulate impurities greater than 0.03 μm per milliliter It is not more than 860, and the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb, so as to solve the above-mentioned problems of the prior art.

The main object of the present invention is to provide a kind of isopropanol regeneration system, comprise the removal high-concentration ion unit, remove water unit, remove cation unit, remove particle unit and remove low-concentration ion unit connected in order, in order to receive and contain isopropanol , water, particulate impurities, anionic impurities, cationic impurities, and isopropanol liquid of organic impurities, and after removing most of the water, particulate impurities, anionic impurities, cationic impurities, and organic impurities, an isopropanol regeneration solution is produced. The isopropanol content of the alcohol regeneration liquid is higher than that of the isopropanol liquid, thereby achieving the regeneration and purification of the isopropanol.

Specifically, the unit for removing high-concentration ions is to receive the isopropanol liquid permeated by steam, and the unit for removing high-concentration ions includes ion exchange resin tower, ion exchange resin and feed pump, wherein the ion exchange resin tower has a feed inlet and The bed structure of the outlet and the ion exchange resin are filled in the ion exchange resin tower respectively, and the inlet is connected to the outlet of the vapor permeation system, and the isopropanol liquid is injected into the ion exchange by the feed pump. resin tower. In the ion exchange resin tower, the isopropanol liquid contacts the ion exchange resin to remove high concentrations of metal elements and non-metal elements (ppm reduced to ppb).

In addition, the water removal unit receives isopropanol liquid, and the water removal unit essentially includes a molecular sieve adsorption bed, a molecular sieve dehydrating agent and a vacuum regeneration system, wherein the molecular sieve adsorption bed is a hollow bed structure with an inlet and an outlet. And the molecular sieve dehydrating agent is filled in the molecular sieve adsorption bed, and the feed port is connected to the discharge port of the ion exchange resin tower, and the isopropanol liquid is injected into the molecular sieve adsorption bed. In the molecular sieve adsorption bed, the isopropanol liquid contacts the molecular sieve dehydrating agent to remove water, and then produces a water-removed recovery liquid, which is discharged through the discharge port. Molecular-scale pores, for example, are between 3 Å and 4 Å.

The above-mentioned molecular sieve dehydrating agent is granular and hydrophilic, and has multiple molecular-level holes, and the size of the molecular-level holes is larger than the size of water molecules and smaller than the size of isopropanol molecules, so that water can pass, contact, and pass through. The hydrophilic adsorption is used to absorb water, while blocking and retaining the isopropanol, thereby achieving the effect of water removal. Therefore, the water content of the water removal recovery liquid is lower than that of the isopropanol liquid.

In addition, the particle removal unit receives the dewatered recovery liquid from the water removal unit, and includes a microfiltration membrane and an ultrafiltration membrane, wherein the microfiltration membrane and the ultrafiltration membrane are arranged in a filter shell, and the filter shell has a feed inlet and a The outlet, and the inlet is connected to the outlet of the water removal unit, and the microfiltration membrane and the ultrafiltration membrane have a plurality of filtration holes, especially, the size of the filtration holes is 0.1 μm to 0.2 μm and 0.02 μm to 0.05 μm, respectively. Between μm, it is used to filter out the particulate impurities in the water recovery liquid to produce a filtered recovery liquid, which is further discharged from the outlet.

The unit for removing low-concentration ions receives the filtered recovery liquid from the particle removal unit, and includes a hollow filter housing and an ion exchange membrane, wherein the ion exchange membrane is arranged in the filter housing, and the filter housing has an inlet and an outlet. Furthermore, the feed port is connected to the discharge port of the particle removal unit, and the ion exchange membrane removes the ionic impurities in the filtered recovery liquid by means of adsorption, thereby generating isopropanol regeneration liquid, and further passes through the discharge port discharge.

For example, the isopropanol content of the above-mentioned isopropanol liquid is not more than 99.85%, the water content of the water-recovered liquid is not more than 50 ppm, and the particulate impurity content of the filtered recovered liquid is greater than 0.03 μm per milliliter The number is not more than 860 (860 pcs/ml), and the isopropanol content of the isopropanol regeneration solution is not less than 99.99%, especially, the anion content of the isopropanol regeneration solution is 4-5 ppb, while the isopropanol regeneration The cation content of the alcohol regeneration solution is 0.09-1 ppb.

In addition, another object of the present invention is to provide a method for regenerating isopropanol, which includes the steps of removing high-concentration ions, removing water, removing particles and removing low-concentration ions to receive impurities containing isopropanol, water, and particles. , anion impurities, cationic impurities, and isopropanol liquid of organic impurities, and after removing most of the water, particle impurities, anion impurities, cationic impurities, and organic impurities, an isopropanol regeneration liquid is produced, and the isopropanol regeneration liquid is The content of propanol is higher than that of isopropanol liquid, so as to achieve the effect of regeneration and purification of isopropanol.

First, in the step of removing high-concentration ions, the high-concentration ion removal unit is mainly used to receive isopropanol liquid to remove high-concentration ions to generate deionization recovery liquid, wherein the isopropanol liquid contains isopropanol, water, particulate impurities, and anion impurities , cationic impurities and organic impurities. Further, the unit for removing high-concentration ions includes an ion exchange resin tower, an ion exchange resin, and a feed pump, and the ion exchange resin tower is a hollow bed structure with an inlet and an outlet. The ion exchange resin is filled in the ion exchange resin tower, and the feed port is connected to the outlet of the steam permeation system, and the isopropanol liquid is injected into the ion exchange resin tower by the feed pump. In the ion exchange resin tower, the isopropanol liquid contacts the ion exchange resin to remove high-concentration metal elements and non-metal elements, and then discharges the deionized recovery liquid through the outlet.

In the water removal step, the water removal unit is mainly used to receive the isopropanol liquid to remove water to generate a water removal recovery liquid. Further, the water removal unit includes a molecular sieve adsorption bed, a molecular sieve dehydrating agent and a vacuum regeneration system, and the molecular sieve adsorption bed is a hollow tubular structure with an inlet and an outlet. The molecular sieve dehydrating agent is filled in the molecular sieve adsorption bed, the feed port is connected to the outlet of the ion exchange resin tower, and isopropanol liquid is injected into the molecular sieve adsorption bed, and the dehydration occurs after contacting the molecular sieve dehydrating agent to remove water. The recovery liquid is then discharged through the discharge port to remove the water recovery liquid.

The above-mentioned molecular sieve dehydrating agent is granular and hydrophilic, and has multiple molecular-level pores. In particular, the size of the molecular-level pores is larger than the size of water molecules and smaller than the size of isopropanol molecules, which are used to allow water to pass through, contact, By means of hydrophilic adsorption, water can be adsorbed, and at the same time, the isopropanol can be blocked and retained, wherein the water content of the water removal recovery liquid is lower than that of the isopropanol liquid.

Then enter the particle removal step, use the particle removal unit to receive the water-recovery liquid from the water-removal step and filter out the particulate impurities in the water-recovery liquid to produce a filtered recovery liquid. Further, the particle removal unit includes a microfiltration membrane and an ultrafiltration membrane, wherein the microfiltration membrane and the ultrafiltration membrane are arranged in a filter housing, wherein the feed port is connected to the discharge port of the water removal unit, and the microfiltration and ultrafiltration membrane There are a plurality of filtering holes, especially, the sizes of the filtering holes are respectively between 0.1 μm to 0.2 μm and 0.02 μm to 0.05 μm. In addition, the dewatering recovery liquid enters the filter shell from the feed port and then contacts the microfiltration membrane and ultrafiltration membrane, and filters out particulate impurities through the microfiltration membrane and ultrafiltration membrane to produce a filtered recovery liquid, which is then discharged from the discharge port for filtration Recovery fluid.

Finally, in the step of removing low-concentration ions, the unit for removing low-concentration ions is used to receive the filtered recovery liquid from the step of removing particles, and the unit for removing low-concentration ions includes a hollow filter shell and an ion exchange membrane. In addition, the ion exchange membrane is placed in the filter housing, and the filter housing has a feed port and a discharge port, wherein the feed port is connected to the discharge port of the particle removal unit, and the filtered recovery liquid enters the filter case from the feed port , and contact the ion-exchange membrane, and remove the ionic impurities in the filtered recovered liquid through the ion-exchange membrane by adsorption to generate isopropanol regeneration liquid, which is discharged from the discharge port.

The particle impurity content of the filtered recovery liquid is not more than 860 pcs/ml, the isopropanol content of the isopropanol regeneration liquid is not less than 99.99%, the anion content of the isopropanol regeneration liquid is 4-5 ppb, and the isopropanol regeneration liquid The cationic content of 0.09-1 ppb.

Therefore, the present invention utilizes the isopropanol regeneration system connected in sequence to remove high-concentration ion units, water-removal units, particle-removal units, and low-concentration ion units to receive isopropanol liquid to remove water, remove particles, and The ion removal step removes most of the water, particle impurities, anion impurities, cation impurities, and organic impurities to produce semiconductor electronic grade isopropanol regeneration solution. In particular, the isopropanol content of the isopropanol liquid is not more than 99.85%, the isopropanol content of the isopropanol regeneration solution is not less than 99.99%, the water content is not more than 50 ppm, and the particle impurity content is greater than 0.03 per milliliter The number of micron particulate impurities is not more than 860, the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb.

The implementation of the present invention will be described in more detail below in conjunction with the diagrams and component symbols, so that those skilled in the art can implement it after studying this specification.

Please refer to FIG. 1 , which is a schematic diagram of an isopropanol regeneration system according to an embodiment of the present invention. As shown in Figure 1, the isopropanol regeneration system of the embodiment of the present invention comprises removing high-concentration ion unit 1, removing water unit 10, removing particle unit 20 and removing low-concentration ion unit 30, and removing high-concentration ion unit 1, removing The water unit 10, the particle removal unit 20 and the low-concentration ion removal unit 30 are sequentially connected to receive the isopropanol liquid LW, wherein the isopropanol liquid LW contains isopropanol, water, particulate impurities, anion impurities, and cation impurities , organic impurities, and most of the water, particulate impurities, anion impurities, cationic impurities, and organic impurities of the isopropanol liquid LW are removed by the isopropanol regeneration system of the present invention to produce the isopropanol regeneration liquid LR, especially, the isopropanol regeneration liquid The isopropanol content of LR is higher than the isopropanol content of isopropanol liquid LW, and then achieve the effect of regeneration and purification of isopropanol.

Specifically, removal of high-concentration ion unit 1 is as shown in Figure 2, receives isopropanol liquid LW, and comprises ion-exchange resin tower 1A, ion-exchange resin 1B and feed pump 1C, wherein ion-exchange resin tower 1A is It has a bed structure with an inlet 1D and an outlet 1E, and the ion exchange resin 1B is filled in the ion exchange resin tower 1A. Feed port 1D is connected to the discharge port of vapor permeation system, and injects isopropanol liquid LW to ion exchange resin tower 1A by feed pump 1C, and in ion exchange resin tower 1A, isopropanol liquid LW is High-concentration metal elements and non-metal elements are removed by contacting the ion exchange resin 1B, so as to form the deionization recovery liquid LA, which is discharged from the discharge port 1E.

In addition, the water removal unit 10 is as shown in Figure 3, in order to receive deionization recovery liquid LA, and the water removal unit 10 is to comprise molecular sieve adsorption bed 11, molecular sieve dehydrating agent 12 and vacuum regeneration system 13, wherein molecular sieve adsorption bed 11 is A hollow bed structure with an inlet 11A and an outlet 11B. The molecular sieve dehydrating agent 12 is filled in the molecular sieve adsorption bed 11 , and the feed port 11A is connected to the discharge port 1E of the ion exchange resin tower 1A, and injects the deionization recovery liquid LA into the molecular sieve adsorption bed 11 . In the molecular sieve adsorption bed 11 , the deionized recovered liquid LA is contacted with the molecular sieve dehydrating agent 12 to remove water, thereby generating the dehydrated recovered liquid LC, which is discharged through the outlet 11B.

In essence, the molecular sieve dehydrating agent 12 is granular, for example, it is composed of aluminum silicate, and is hydrophilic. In particular, the partially enlarged area A of the molecular sieve dehydrating agent 12 in the figure shows that it has a size larger than a water molecule and smaller than an isopropanol molecule. Multiple molecular-level pores H of different sizes, for example, the size of the molecular-level pores H is between 3 Å and 4 Å, which can be used to allow water W to pass, contact, and pass through, thereby absorbing water W through hydrophilic adsorption, while blocking and retaining water W. Propanol P, and then achieve the effect of water removal. Therefore, the water content of the water-recovered liquid LC is lower than that of the isopropanol liquid LW.

In addition, the particulate removal unit 20 receives the dewatering recovery liquid LC, and as shown in FIG. 4 , includes a microfiltration membrane 21 and an ultrafiltration membrane 22, wherein the microfiltration membrane 21 and the ultrafiltration membrane 22 are arranged in a filter housing 23, The filter shell 23 has a material inlet 23A and a material outlet 23B, and the material inlet 23A is connected to the material outlet 11B of the water removal unit 10 . The microfiltration membrane 21 and the ultrafiltration membrane 22 have a plurality of filtration holes (not shown in the figure) for filtering particulate impurities in the water recovery liquid LC to produce a filtered recovery liquid LP, which is further discharged from the outlet 23B.

In particular, the size of the filter pores of the microfiltration membrane 21 is 0.2 μm to 0.1 μm, while the size of the filter pores of the ultrafiltration membrane 22 is between 0.02 μm and 0.05 μm.

Furthermore, the unit 30 for removing low-concentration ions receives the filtered recovery liquid LP, and as shown in FIG. The filter housing 31 has a material inlet 31A and a material outlet 31B. The feed port 31A is connected to the discharge port 23B of the particle removal unit 20, and the ion exchange membrane 32 is used to remove the ionic impurities in the filtered recovery liquid LP by means of adsorption, and then generate the isopropanol regeneration liquid LR, which is produced by the outlet The feed port 31B is discharged.

Specifically, the ion exchange membrane 32 is made of polytetrafluoroethylene (PTFE), and has a positively charged surface or a negatively charged surface, wherein the positively charged surface removes anions among ion impurities by adsorption Impurities, while the negatively charged surface removes cationic impurities from ionic impurities by adsorption. The ion exchange membrane 32 whose surface is positively charged serves as an anion exchange membrane, and the ion exchange membrane 32 whose surface has a negative charge serves as a cation exchange membrane. For example, the filter housing 31 can be equipped with an anion exchange membrane alone, a cation exchange membrane can be installed separately, or an anion exchange membrane and a cation exchange membrane can be placed at the same time, but the anion exchange membrane and the cation exchange membrane are separated from each other without interfering with each other. .

For example, the above-mentioned ion exchange membrane 32 can have a plurality of pores with a size of 0.05-0.2 μm, and can be operated at a maximum pressure difference of 2.4-2.7 bar, especially, the overall feed flow can be 60 L/H , the number of cycles can reach 1-20, and the maximum operating temperature is 60°C. Furthermore, the unit 30 for removing low-concentration ions can also be configured with a plurality of ion exchange membranes 32 connected in series, wherein each ion exchange membrane 32 has a plurality of pores of different sizes. The membrane 32 is connected with an ion exchange membrane 32 with a pore size of 0.05 μm, so as to remove ions more effectively.

Overall, the isopropanol content of the isopropanol liquid LW is not more than 99.85%, the water content of the dewatering recovery liquid LC is not more than 50 ppm, and the particulate impurity content of the filtered recovery liquid LP is greater than 0.03 μm per milliliter The number of particulate impurities is not more than 860, and it is expressed as 860 pcs/ml. In addition, the isopropanol content of the isopropanol regeneration liquid LR is not less than 99.99%, while the anion content of the isopropanol regeneration liquid LR is 4 -5 ppb, and the cationic content of isopropanol regeneration solution LR is 0.09-1 ppb.

For example, the microfiltration membrane 21 and ultrafiltration membrane 22 connected in series can be arranged in the particle removal unit 20, and the size of the filtration pores of the microfiltration membrane is 0.1 μm, and the size of the filtration pores of the ultrafiltration membrane 22 is 0.02 μm. μm, moreover, the particle removal unit 20 can be equipped with a microfiltration membrane with a filter hole size of 0.1 μm to match a microfiltration membrane with a filter hole size of 0.02 μm, and a microfiltration membrane with a filter hole size of 0.2 μm The microfiltration membrane is matched with an ultrafiltration membrane with a filter hole size of 0.05 μm, and is connected to the water removal unit 10 in parallel, that is, two sets of independent pipelines are formed, which can effectively filter out particles according to actual needs and increase treatment quantity, increase production capacity.

For example, when using a microfiltration membrane with a filter hole size of 0.1 μm, its efficacy can include that the number of particulate impurities not greater than 0.1 μm is not greater than 143, and the number of particulate impurities not greater than 0.2 μm is not greater than 1003, The number of particulate impurities not greater than 0.3 μm is not greater than 50, and the number of particulate impurities not greater than 0.5 μm is not greater than 10. In addition, when using an ultra-filtration membrane with a filter hole size of 0.02 μm, its efficacy can include The number of particulate impurities not greater than 0.03 μm is not greater than 860, and the number of particulate impurities not greater than 0.05 μm is not greater than 428.

Further referring to FIG. 6 , it is a schematic flow diagram of the operation flow of the isopropanol regeneration method according to another embodiment of the present invention. As shown in Figure 6, the isopropanol regeneration method of the present invention is to comprise removing high-concentration ion step S1, removing water step S10, removing particle step S20 and removing low-concentration ion step S30, in order to receive and contain isopropanol, water, Isopropanol solution of particulate impurities, anionic impurities, cationic impurities, and organic impurities, and isopropanol regeneration solution is produced after removing most of the water, particulate impurities, anion impurities, cationic impurities, and organic impurities, among which isopropanol regeneration fluid The isopropanol content of the isopropanol is higher than that of the isopropanol liquid, so as to realize the regeneration and purification of isopropanol.

First of all, the isopropanol regeneration method of the present invention begins with the step S1 of removing high-concentration ions, and uses the unit for removing high-concentration ions to receive the isopropanol liquid, so as to receive the isopropanol liquid and remove high-concentration ions in the isopropanol liquid, and then A deionization recovery liquid is produced, wherein the isopropanol liquid contains isopropanol, water, particulate impurities, anion impurities, cation impurities and organic impurities. Since the technical features of the unit for removing high-concentration ions are as shown in FIG. 2 , details will not be described below.

Afterwards, the water removal step S10 is performed, which is to use the water removal unit to receive the deionized recovered liquid to remove the water in the deionized recovered liquid to generate the deionized recovered liquid. Since the technical features of the dewatering unit are as shown in FIG. 3 , they will not be described in detail below.

Then carry out the particle removal step S20, which is to use the particle removal unit to receive the dewatering recovery liquid from the water removal step, so as to filter out the particulate impurities in the water removal recovery liquid to generate a filtered recovery liquid. Similarly, the technical characteristics of the particle removal unit It is as shown in FIG. 4 , so it will not be described in detail below.

Finally, enter the step S30 of removing low-concentration ions, and use the unit for removing low-concentration ions to receive the filtered recovery liquid from the particle removal step S20 to remove ion impurities in the filtered recovery liquid by adsorption, and then generate isopropanol regeneration liquid. Likewise, the technical features of the unit for removing low-concentration ions are as shown in FIG. 5 , so details will not be repeated below.

On the whole, the isopropanol content of the isopropanol liquid in this method is not more than 99.85%, the water content of the water-recovery liquid LC is not more than 50 ppm, and the particle impurity content of the filtered recovery liquid LP is per milliliter The number of particulate impurities larger than 0.03 μm is not more than 860 (860 pcs/ml). In addition, the isopropanol content of the isopropanol regeneration solution LR is not less than 99.99%, while the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution LR is 0.09-1 ppb.

In summary, the feature of the present invention is to utilize the isopropanol regeneration system connected in sequence to remove high-concentration ion units, water-removal units, particulate units and low-concentration ion units to receive isopropanol liquid and thereby Water removal, particle removal, and ion removal steps are used to remove most of the water, particle impurities, anion impurities, cation impurities, and organic impurities to produce semiconductor electronic grade isopropanol regeneration fluid. In particular, the isopropanol content of the isopropanol liquid is not more than 99.85%, the isopropanol content of the isopropanol regeneration solution is not less than 99.99%, the water content is not more than 50 ppm, and the particle impurity content is greater than 0.03 per milliliter The number of micron particulate impurities is not more than 860, the anion content is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb.

The above are only preferred embodiments for explaining the present invention, and are not intended to limit the present invention in any form. Therefore, any modification or change of the present invention made under the same spirit of the invention , should still be included in the scope of protection intended by the present invention.

1: Remove high-concentration ion units 1A: Ion exchange resin tower 1B: Ion exchange resin 1C: Feed pump 1D: feed port 1E: Outlet 10: Water removal unit 11: Molecular sieve adsorption bed 11A: Feed port 11B: Outlet 12: Molecular sieve dehydrating agent 13: Vacuum regeneration system 20:Remove particle unit 21: Microfiltration membrane 22:Ultrafiltration membrane 23: Filter housing 23A: Feed port 23B: Outlet 30: Removal of low-concentration ion units 31: filter housing 31A: feed port 31B: Outlet 32: Ion exchange membrane LW: Isopropanol LA: deionization recovery solution LC: water recovery liquid LP: Filtration recovery liquid LR: Isopropanol regeneration solution S1: Step to remove high-concentration ions S10: Water removal step S20: Particle removal step S30: step of removing low-concentration ions W: water P: Isopropanol A: zoom area H: hole

FIG. 1 shows a schematic diagram of an isopropanol regeneration system according to an embodiment of the present invention. FIG. 2 shows a schematic diagram of a unit for removing high-concentration ions in an isopropanol regeneration system according to an embodiment of the present invention. FIG. 3 shows a schematic diagram of a water removal unit in an isopropanol regeneration system according to an embodiment of the present invention. FIG. 4 shows a schematic diagram of a particle removal unit in an isopropanol regeneration system according to an embodiment of the present invention. FIG. 5 shows a schematic diagram of a unit for removing low-concentration ions in an isopropanol regeneration system according to an embodiment of the present invention. FIG. 6 shows a schematic diagram of the operation flow of the isopropanol regeneration method according to another embodiment of the present invention.

1: Remove high-concentration ion units

10: Water removal unit

20:Remove particle unit

30: Removal of low-concentration ion units

LW: Isopropanol

LA: deionization recovery solution

LC: water recovery liquid

LP: Filtration recovery liquid

LR: Isopropanol regeneration solution

Claims (6)

An isopropanol regeneration system is used to receive an isopropanol liquid to generate an isopropanol regeneration liquid, the isopropanol content of the isopropanol regeneration liquid is higher than that of the isopropanol liquid content, including: A unit for removing high-concentration ions is to receive isopropanol liquid, which contains isopropanol, water, particulate impurities, anion impurities, cation impurities and organic impurities. The unit for removing high-concentration ions includes an ion exchange resin tower , an ion exchange resin and a feed pump, the ion exchange resin tower is a bed structure with a feed inlet and a feed outlet, the ion exchange resin is filled in the ion exchange resin tower, the inlet The feed port is connected to the discharge port of a vapor permeation system, and the isopropanol liquid is injected into the ion exchange resin tower by the feed pump, and in the ion exchange resin tower, the isopropanol liquid is obtained by contacting The ion-exchange resin is removed of high-concentration metal elements and non-metal elements to form a deionization recovery liquid, which is discharged from the outlet; A water removal unit is connected to the high-concentration ion removal unit, the water removal unit includes a molecular sieve adsorption bed, a molecular sieve dehydrating agent and a vacuum regeneration system, the molecular sieve adsorption bed has a feed inlet and a discharge A hollow bed structure of the mouth, the molecular sieve dehydrating agent is filled in the molecular sieve adsorption bed, the feed port is connected to the outlet of the cation exchange resin tower, and the deionization recovery liquid is injected into the molecular sieve adsorption bed , in the molecular sieve adsorption bed, the deionized recovery liquid is removed by contacting the molecular sieve dehydrating agent, thereby producing a dewatered recovery liquid, which is discharged through the outlet; A particle removal unit is connected to the water removal unit to receive the water removal recovery liquid, and includes a microfiltration membrane and an ultrafiltration membrane, and the microfiltration membrane and the ultrafiltration membrane are arranged in a filter housing , the filter shell has a feed port and a discharge port, the feed port is connected to the discharge port of the water removal unit, the microfiltration membrane and the ultrafiltration membrane have a plurality of filter holes for filtering out the removing particulate impurities in the water recovery liquid to produce a filtered recovery liquid, which is further discharged from the discharge port; and A unit for removing low-concentration ions is used to receive the filtered recovery liquid, and includes a hollow filter shell and an ion exchange membrane, the ion exchange membrane is arranged in the filter shell, and the filter shell has a feed port and a discharge port, the feed port is connected to the discharge port of the particle removal unit, the ion exchange membrane system is used to remove the ionic impurities in the filtered recovery liquid by adsorption, and then generate the isopropanol regeneration liquid , and discharged from the outlet, Wherein the isopropanol content of the isopropanol liquid is not more than 99.85%, the water content of the water removal and recovery liquid is not more than 50 ppm, and the particulate impurity content of the filtered recovery liquid is more than 0.03 μm per milliliter The number is not more than 860, and expressed as 860 pcs/ml, the isopropanol content of the isopropanol regeneration liquid is not less than 99.99%, the anion content of the isopropanol regeneration liquid is 4-5 ppb, the isopropanol regeneration liquid The cation content of the alcohol regeneration solution is 0.09-1 ppb. The isopropanol regeneration system as described in Claim 1, wherein the molecular sieve dehydrating agent is granular and hydrophilic, and has a plurality of molecular-level pores, and the molecular-level pores are between 3 Å and 4 Å. The isopropanol regeneration system as described in Claim 1, wherein the size of the filter pores of the microfiltration membrane is 0.1 μm to 0.2 μm, and the size of the filter pores of the ultrafiltration membrane is between 0.02 μm and 0.05 μm. A method for regeneration of isopropanol, comprising: A high-concentration ion removal step is to use a high-concentration ion removal unit to receive the isopropanol liquid to remove high-concentration ions in the isopropanol liquid to generate a deionization recovery liquid, the isopropanol liquid contains isopropanol, Water, particulate impurities, anion impurities, cationic impurities and organic impurities, the high-concentration ion removal unit includes an ion exchange resin tower, an ion exchange resin and a feed pump, the ion exchange resin tower has a feed inlet and A bed structure of a discharge port, the ion exchange resin is filled in the ion exchange resin tower, the feed port is connected to the discharge port of a vapor permeation system, and injected into the isocyanate by the feed pump propanol liquid to the ion-exchange resin tower, in the ion-exchange resin tower, the isopropanol liquid is to remove high-concentration metal elements and non-metallic elements by contacting the ion-exchange resin to form the deionization recovery liquid, and discharged from the outlet; A water removal step is to use a water removal unit to receive the deionization recovery liquid to remove water in the deionization recovery liquid to produce a water removal recovery liquid, the water removal unit includes a molecular sieve adsorption bed, a molecular sieve dehydrating agent And a vacuum regeneration system, the molecular sieve adsorption bed is a hollow bed structure with an inlet and an outlet, the molecular sieve dehydrating agent is filled in the molecular sieve adsorption bed, the inlet is connected to the ion The discharge port of the exchange resin tower, and inject the deionization recovery liquid into the molecular sieve adsorption bed, in the molecular sieve adsorption bed, the deionization recovery liquid contacts the molecular sieve dehydrating agent to remove water, and then produces the dehydration recovery liquid , and discharged through the outlet; A particle removal step is to use a particle removal unit to receive the dewatered recovery liquid from the water removal step, and filter out the particulate impurities in the dewatered recovery liquid to produce a filtered recovery liquid, wherein the particle removal unit includes a micro filter membrane and an ultrafiltration membrane; and A step for removing low-concentration ions is to use a unit for removing low-concentration ions to receive the filtered recovery liquid from the step of removing particles, and to generate an isopropanol regeneration solution after removing low-concentration ions. The unit for removing low-concentration ions includes a hollow A filter housing and an ion exchange membrane, the ion exchange membrane is placed in the filter housing, the filter housing has a feed port and a discharge port, the feed port is connected to the discharge port of the particle removal unit , the ion exchange membrane system is used to remove the ionic impurities in the filtered recovery liquid by adsorption, and then generate the isopropanol regeneration liquid, which is discharged from the outlet, wherein the isopropanol content of the isopropanol liquid is not more than 99.85%, the water content of the water removal recovery liquid is not more than 50 ppm, the particulate impurity content of the filtered recovery liquid is not more than 860 pcs/ml, and the isopropanol content of the isopropanol regeneration liquid is not less than 99.99%, the anion content of the isopropanol regeneration solution is 4-5 ppb, and the cation content of the isopropanol regeneration solution is 0.09-1 ppb. The isopropanol regeneration method as described in Claim 4, wherein the molecular sieve dehydrating agent is granular and hydrophilic, and has a plurality of molecular-level pores, and the molecular-level pores are between 3 Å and 4 Å. The isopropanol regeneration method as described in claim 4, wherein the size of the filter pores of the microfiltration membrane is 0.1 μm to 0.2 μm, and the size of the filter pores of the ultrafiltration membrane is between 0.02 μm and 0.05 μm.

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