An ultra-clean high-purity isopropanol production device and method

Abstract

The application discloses an ultra-clean high-purity isopropanol production device, which comprises a raw material tank, a first filter membrane, a second filter membrane and a third filter membrane, wherein the first inlet of the first filter membrane is connected with the output port of the raw material tank, the first permeation side of the first filter membrane is connected with the input port of the raw material tank; the second inlet of the second filter membrane is connected with the first permeation side of the first filter membrane, and the second permeation side of the second filter membrane is connected with the first inlet of the first filter membrane; the third inlet of the third filter membrane is connected with the second permeation side of the second filter membrane, the third permeation side of the third filter membrane is connected with the second inlet of the second filter membrane, and the third permeated side obtains a target product; a heating assembly is arranged for heating isopropanol to be processed at the first inlet, the second inlet and the third inlet; and a condensing assembly is arranged for condensing isopropanol to be processed at the first permeation side, the second permeation side and the third permeation side. The application can improve the purity of the ultra-clean high-purity isopropanol product, occupies less land, and is suitable for large-scale industrial production.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of microelectronic chemicals, in particular to a production device and method of super-clean high-purity isopropyl alcohol. BACKGROUND

[0002] As one of important cleaning agents in electronic industry, the demand for super-clean high-purity isopropyl alcohol will be more and more large in the future, and the demand for isopropyl alcohol is expected to grow at a rate of more than 10% per year. Electronic-grade isopropyl alcohol has excellent performance of fast gasification and no residue, and super-clean high-purity isopropyl alcohol has been widely used in cleaning and corrosion in the industries of semiconductor, metal degreasing, and ultra-large-scale integrated circuit.

[0003] At present, super-clean high-purity isopropyl alcohol is usually purified and refined from industrial-grade isopropyl alcohol, and distillation is the main method for industrial purification of isopropyl alcohol, including azeotropic distillation, extraction distillation, etc. However, the super-clean high-purity isopropyl alcohol used in the microelectronic chemical industry has very strict requirements on the content of metal impurities and particle size, and the distillation process cannot meet the requirements, and the equipment required by the distillation process occupies a large area, which is not suitable for large-scale industrial production. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides a production device and method of super-clean high-purity isopropyl alcohol, which can improve the purity of super-clean high-purity isopropyl alcohol products, and has a small equipment area and is suitable for large-scale industrial production.

[0005] The present application is realized by the following technical solutions:

[0006] A production device of super-clean high-purity isopropyl alcohol comprises:

[0007] A raw material tank for storing isopropyl alcohol to be processed;

[0008] A first filter membrane, a first inlet of which is connected with an outlet of the raw material tank, and a first retentate side of which is connected with an inlet of the raw material tank;

[0009] A second filter membrane, a second inlet of which is connected with a first permeate side of the first filter membrane, and a second retentate side of which is connected with a first inlet of the first filter membrane;

[0010] A third filter membrane, a third inlet of which is connected with a second permeate side of the second filter membrane, a third retentate side of which is connected with a second inlet of the second filter membrane, and a third permeate side of which obtains a target product;

[0011] A heating assembly for heating isopropyl alcohol to be processed located at the first inlet, the second inlet, and the third inlet;

[0012] condensing components for condensing the isopropyl alcohol to be processed located at the first, second and third permeation sides.

[0013] Further, the first, second and third filter membranes are composite membranes.

[0014] Further, the first filter membrane has a three-layer structure, the first layer is a PP membrane, the second layer is a PTFE membrane, and the third layer is a polydimethylsiloxane composite membrane modified by polyammoniated chitosan.

[0015] Further, the second filter membrane has a three-layer structure, the first layer is a PVDF membrane, the second layer is a PTFE membrane, and the third layer is a polydimethylsiloxane composite membrane modified by polyammoniated chitosan.

[0016] Further, the third filter membrane has a three-layer structure, the first layer is a PFA membrane, the second layer is a PTFE membrane, and the third layer is a polydimethylsiloxane composite membrane modified by polyammoniated chitosan.

[0017] Further, the heating components include:

[0018] a first heater, the inlet of which is connected to the outlet of the raw material tank, and the outlet of which is connected to the first inlet of the first filter membrane;

[0019] a second heater, the inlet of which is connected to the first permeation side of the first filter membrane, and the outlet of which is connected to the second inlet of the second filter membrane;

[0020] a third heater, the inlet of which is connected to the second permeation side of the second filter membrane, and the outlet of which is connected to the third inlet of the third filter membrane.

[0021] Further, the condensing components include:

[0022] a first condenser, the inlet of which is connected to the first permeation side of the first filter membrane, and the outlet of which is connected to the inlet of the second heater;

[0023] a second condenser, the inlet of which is connected to the second permeation side of the second filter membrane, and the outlet of which is connected to the inlet of the third heater;

[0024] a third condenser, the inlet of which is connected to the third permeation side of the third filter membrane;

[0025] a vacuum pump, which is connected to the first, second and third condensers simultaneously.

[0026] Further, the production device further includes:

[0027] a second storage tank, the inlet of which is connected to the outlet of the first condenser, and the outlet of which is connected to the inlet of the second heater;

[0028] a fourth storage tank, the inlet of which is connected with the outlet of the second condenser, and the outlet of which is connected with the inlet of the third heater;

[0029] a sixth storage tank, the inlet of which is connected with the outlet of the third condenser, and the outlet of which outputs the product.

[0030] Further, the production device further comprises:

[0031] a first storage tank, the inlet of which is connected with the outlet of the first condenser, and the outlet of which is connected with the input of the raw material tank;

[0032] a third storage tank, the inlet of which is connected with the outlet of the second condenser, and the outlet of which is connected with the input of the raw material tank;

[0033] a fifth storage tank, the inlet of which is connected with the outlet of the third condenser, and the outlet of which is connected with the input of the raw material tank.

[0034] A production method of ultra-clean high-purity isopropyl alcohol, comprising the following steps:

[0035] The isopropyl alcohol to be processed is heated and then enters the first filter membrane, the permeate liquid from the first permeation side of the first filter membrane is collected in two parts, one part enters the first storage tank, and the other part enters the second storage tank, the permeate liquid collected by the first storage tank and the retentate liquid located at the first retentate side of the first filter membrane are returned to the raw material tank, and the residual liquid in the raw material tank is used as a residual liquid;

[0036] The permeate liquid collected by the second storage tank is heated and then enters the second filter membrane, the permeate liquid from the second permeation side of the second filter membrane is collected in two parts, one part enters the third storage tank, and the other part enters the fourth storage tank, the permeate liquid collected by the third storage tank is returned to the raw material tank, and the retentate liquid located at the second retentate side of the second filter membrane is returned to the first filter membrane;

[0037] The permeate liquid collected by the fourth storage tank is heated and then enters the third filter membrane, the permeate liquid from the third permeation side of the third filter membrane is collected in two parts, one part enters the fifth storage tank, and the other part enters the sixth storage tank, the permeate liquid collected by the fifth storage tank is returned to the raw material tank, the retentate liquid located at the third retentate side of the third filter membrane is returned to the second filter membrane, and the permeate liquid collected in the sixth storage tank is the target product.

[0038] Compared with the prior art, the advantages of the present application are that:

[0039] 1. The three-stage membrane system is adopted to remove metal ions and particulate matter, compared with the traditional multi-effect rectification and ultrafiltration membrane for removing particulate matter, the process is simplified, the equipment occupation area is reduced, the equipment height is reduced, and large-scale industrial production is suitable.

[0040] 2、The polyammoniated chitosan modified polydimethylsiloxane composite membrane is adopted, the operating condition is not reached the boiling point of the material liquid, the permeation side is gaseous, and the metal ions are well removed; meanwhile, the three filter membranes are dense membranes, and the particulate matters are well removed.

[0041] 3、The system of different levels of membranes of the present application respectively adopts high-purity PP, PVDF and PFA materials, not only reduces the investment cost, but also meets the requirement that the contact materials do not produce elution in the production of wet electronic chemicals. BRIEF DESCRIPTION OF DRAWINGS

[0042] Figure 1 The working principle diagram of the super-clean high-purity isopropyl alcohol production device of an embodiment of the present application;

[0043] Figure 2 The flow chart of the super-clean high-purity isopropyl alcohol production device of an embodiment of the present application.

[0044] 1, raw material tank; 10, input port; 11, output port; 12, discharge port; 2, first filter membrane; 20, first inlet; 21, first retentate side; 22, first permeate side; 23, first storage tank; 24, second storage tank; 3, second filter membrane; 30, second inlet; 31, second retentate side; 32, second permeate side; 33, third storage tank; 34, fourth storage tank; 4, third filter membrane; 40, third inlet; 41, third retentate side; 42, third permeate side; 43, fifth storage tank; 44, sixth storage tank; 5, heating assembly; 50, first heater; 51, second heater; 52, third heater; 6, condensing assembly; 60, first condenser; 61, second condenser; 62, third condenser; 63, vacuum pump. DETAILED DESCRIPTION

[0045] The following detailed, non-limiting description of the invention's technical solutions, in conjunction with preferred embodiments and accompanying drawings, is provided. In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the invention, and should not be construed as limiting the invention.

[0046] like Figure 1 As shown, an embodiment of the present invention provides an ultra-clean high-purity isopropanol production apparatus, comprising a raw material tank 1, a first filter membrane 2, a second filter membrane 3, a third filter membrane 4, a heating assembly 5, and a condensing assembly 6. The raw material tank 1 is used to store isopropanol to be processed. The first inlet 20 of the first filter membrane 2 is connected to the outlet 11 of the raw material tank 1, and the first permeate side 21 of the first filter membrane 2 is connected to the inlet 10 of the raw material tank 1. The second inlet 30 of the second filter membrane 3 is connected to the first permeate side 22 of the first filter membrane 2, and the second permeate side 31 of the second filter membrane 3 is connected to the first permeate side 22 of the first filter membrane 2. The first inlet 20 of filter membrane 2 is connected, the third inlet 40 of the third filter membrane 4 is connected to the second permeate side 32 of the second filter membrane 3, the third residual side 41 of the third filter membrane 4 is connected to the second inlet 30 of the second filter membrane 3, and the target product is obtained from the third permeate side 42 of the third filter membrane 4. Heating assembly 5 is used to heat the isopropanol to be processed located at the first inlet 20, the second inlet 30, and the third inlet 40. Condensation assembly 6 is used to condense the isopropanol to be processed located at the first permeate side 22, the second permeate side 32, and the third permeate side 42. The absolute pressure at the first permeate side 22, the second permeate side 32, and the third permeate side 42 is 3000–8000 Pa.

[0047] The heating assembly 5 comprises a first heater 50, a second heater 51 and a third heater 52, the inlet of the first heater 50 is connected with the outlet 11 of the raw material tank 1, the outlet of the first heater 50 is connected with the first inlet 20 of the first filter membrane 2, the inlet of the second heater 51 is connected with the first permeation side 22 of the first filter membrane 2, the outlet of the second heater 51 is connected with the second inlet 30 of the second filter membrane 3, the inlet of the third heater 52 is connected with the second permeation side 32 of the second filter membrane 3, the outlet of the third heater 52 is connected with the third inlet 40 of the third filter membrane 4. When the isopropyl alcohol to be processed passes through the first heater 50, the second heater 51 and the third heater 52, the isopropyl alcohol to be processed is heated to 40-60℃.

[0048] The condensing assembly 6 comprises a first condenser 60, a second condenser 61, a third condenser 62 and a vacuum pump 63, the inlet of the first condenser 60 is connected with the first permeation side 22 of the first filter membrane 2, the outlet of the first condenser 60 is connected with the inlet of the second heater 51, the inlet of the second condenser 61 is connected with the second permeation side 32 of the second filter membrane 3, the outlet of the second condenser 61 is connected with the inlet of the third heater 52, the inlet of the third condenser 62 is connected with the third permeation side 42 of the third filter membrane 4; the vacuum pump 63 is connected with the first condenser 60, the second condenser 61 and the third condenser 62 at the same time, the vacuum pump 63 extracts the air in the condensers, so as to avoid the nitrogen, oxygen and other non-condensable gases in the air to cause the pressure of the condensers to rise.

[0049] The production device of the super-clean high-purity isopropyl alcohol further comprises a first storage tank 23, a second storage tank 24, a third storage tank 33, a fourth storage tank 34, a fifth storage tank 43 and a sixth storage tank 44. The inlet of the second storage tank 24 is connected with the outlet of the first condenser 60, and the outlet of the second storage tank 24 is connected with the inlet of the second heater 51. The inlet of the fourth storage tank 34 is connected with the outlet of the second condenser 61, the outlet of the fourth storage tank 34 is connected with the inlet of the third heater 52, the inlet of the sixth storage tank 44 is connected with the outlet of the third condenser 62, and the outlet of the sixth storage tank 44 outputs the product. The inlet of the first storage tank 23 is connected with the outlet of the first condenser 60, the outlet of the first storage tank 23 is connected with the input port 10 of the raw material tank 1, the inlet of the third storage tank 33 is connected with the outlet of the second condenser 61, the outlet of the third storage tank 33 is connected with the input port 10 of the raw material tank 1, the inlet of the fifth storage tank 43 is connected with the outlet of the third condenser 62, and the outlet of the fifth storage tank 43 is connected with the input port 10 of the raw material tank 1. The residual liquid in the raw material tank 1 is the residual liquid containing high content of metal ions and particles, and the total amount of the residual liquid in the raw material tank 1 is 5-20%. The amount of the permeate entering the first storage tank 23 is 2-10% of the total amount of the permeate entering the first filter membrane 2, the amount of the permeate entering the third storage tank 33 is 2-10% of the total amount of the permeate entering the second filter membrane 3, and the amount of the permeate entering the fifth storage tank 43 is 2-10% of the total amount of the permeate entering the third filter membrane 4.

[0050] In the embodiment, the isopropyl alcohol to be processed is industrial-grade isopropyl alcohol, and the content of isopropyl alcohol is ≥99.7%.

[0051] In the embodiment, the first filter membrane 2, the second filter membrane 3 and the third filter membrane 4 are dense membranes, and are composite membranes at the same time, which can be organic composite folded membranes or organic tubular composite membranes.

[0052] The first filter membrane 2 has a three-layer structure. The first layer is a PP membrane with an average pore size of 500-1000 nm. The second layer is a PTFE membrane with an average pore size of 20-100 nm. The third layer is an effective separation layer, and the active layer is a polydimethylsiloxane composite membrane modified by polyamino chitosan. If the organic composite folded membrane is used, the skeleton (not shown in the figure) and the assembly filter shell (not shown in the figure) of the folded membrane are high-purity PP resistant to high temperature. If the organic tubular composite membrane is used, the filter shell of the organic tubular membrane is high-purity PP, and the materials of the raw material tank 1, the first storage tank 23 and the second storage tank 24 are all high-purity PP.

[0053] The second filter membrane 3 has a three-layer structure, the first layer is a PVDF membrane with an average pore size of 500-1000 nm; the second layer is a PTFE membrane with an average pore size of 20-100 nm; and the third layer is an effective separation layer with a polyamino-modified chitosan modified polydimethylsiloxane composite membrane as the active layer. If an organic composite folding membrane is used, the skeleton and component filter shell of the folding membrane are high-purity PVDF resistant to high temperature; if an organic tubular composite membrane is used, the filter shell of the organic tubular membrane is high-purity PVDF, and the materials of the third storage tank 33 and the fourth storage tank 34 are both high-purity PVDF.

[0054] The third filter membrane 4 has a three-layer structure, the first layer is a PFA membrane with an average pore size of 500-1000 nm; the second layer is a PTFE membrane with an average pore size of 20-100 nm; and the third layer is an effective separation layer with a polyamino-modified chitosan modified polydimethylsiloxane composite membrane as the active layer. If an organic composite folding membrane is used, the skeleton and component filter shell of the folding membrane are high-purity PFA resistant to high temperature; if an organic tubular composite membrane is used, the filter shell of the organic tubular membrane is high-purity PFA or stainless steel lined with PFA, and the materials of the third storage tank 33 and the fourth storage tank 34 are both high-purity PFA or stainless steel lined with PFA.

[0055] As shown in Figure 2 A method for producing ultra-clean high-purity isopropyl alcohol, characterized by comprising the following steps:

[0056] S1: The isopropyl alcohol to be processed is heated and then enters the first filter membrane 2. The permeate from the first permeation side 22 of the first filter membrane 2 is collected in two parts, one part enters the first storage tank 23, and the other part enters the second storage tank 24. The permeate collected in the first storage tank 23 and the retentate located at the first retentate side 21 of the first filter membrane 2 are both returned to the raw material tank 1, and the residual liquid in the raw material tank 1 is used as a residual liquid;

[0057] S2: The permeate collected in the second storage tank 24 is heated and then enters the second filter membrane 3. The permeate from the second permeation side 32 of the second filter membrane 3 is collected in two parts, one part enters the third storage tank 33, and the other part enters the fourth storage tank 34. The permeate collected in the third storage tank 33 is returned to the raw material tank 1, and the retentate located at the second retentate side 31 of the second filter membrane 3 is returned to the first filter membrane 2;

[0058] S3: The permeate collected in the fourth storage tank 34 is heated and then enters the third filter membrane 4. The permeate from the third permeation side 42 of the third filter membrane 4 is collected in two parts, one part enters the fifth storage tank 43, and the other part enters the sixth storage tank 44. The permeate collected in the fifth storage tank 43 is returned to the raw material tank 1, the retentate located at the third retentate side 41 of the third filter membrane 4 is returned to the second filter membrane 3, and the permeate collected in the sixth storage tank 44 is the target product.

[0059] Example 1

[0060] 1000 kg of raw material from the raw material tank 1 is heated to 40℃ and enters the first filtration membrane 2. The permeate from the first permeation side 22 of the first filtration membrane 2 is collected in two parts, one part of 20 kg of permeate is collected into the first storage tank 23, and the other part of permeate enters the second storage tank 24. The permeate collected in the first storage tank 23 and the retentate located at the first retentate side 21 of the first filtration membrane 2 are both returned to the raw material tank 1, and 50 kg of residue remains in the raw material tank 1. The permeate in the second storage tank 24 is continuously heated to 40℃ and enters the second filtration membrane 3. The permeate from the second permeation side 32 of the second filtration membrane 3 is collected in two parts, 20 kg of permeate is collected into the third storage tank 33, and the other part enters the fourth storage tank 34. The permeate collected in the third storage tank 33 is returned to the raw material tank 1, and the retentate located at the second retentate side 31 of the second filtration membrane 3 is returned to the first filtration membrane 2. The permeate collected in the fourth storage tank 34 is continuously heated to 40℃ and enters the third filtration membrane 4. The permeate from the third permeation side 42 of the third filtration membrane 4 is collected in two parts, 20 kg of permeate is collected into the fifth storage tank 43, and the other part enters the sixth storage tank 44. The permeate collected in the fifth storage tank 43 is returned to the raw material tank 1, and the retentate located at the third retentate side 41 of the third filtration membrane 4 is returned to the second filtration membrane 3. The permeate collected in the sixth storage tank 44 is the target product.

[0061] The first filtration membrane 2 adopts an organic tubular composite membrane, the first layer is PP with a pore size of 500 nm, and the second layer is PTFE with an average pore size of 20 nm. The filter shell and storage tank of the first filtration membrane 2 are made of high-purity PP.

[0062] The second filtration membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with a pore size of 500 nm, and the second layer is PTFE with an average pore size of 20 nm. The filter shell and storage tank of the second filtration membrane 3 are made of high-purity PVDF.

[0063] The third filtration membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with a pore size of 500 nm, and the second layer is PTFE with an average pore size of 20 nm. The filter shell and storage tank of the second filtration membrane are made of high-purity PFA.

[0064] The first filtration membrane 2, the second filtration membrane 3, and the third filtration membrane 4 all use polyamino chitosan modified polydimethylsiloxane composite membrane as the effective separation layer, and the pressure on the permeation side of the membrane is 3000 Pa. The content of isopropyl alcohol is 99.95%. The experimental results are shown in Table 1.

[0065] Example 2

[0066] 1000 kg of raw material from the raw material tank 1 is heated to 60°C and enters the first filter membrane 2. The permeate from the first permeation side 22 of the first filter membrane 2 is collected in two parts, one part of 50 kg of permeate is collected into the first storage tank 23, and the other part of permeate enters the second storage tank 24. The permeate collected in the first storage tank 23 and the retentate located at the first retentate side 21 of the first filter membrane 2 are both returned to the raw material tank 1, and 200 kg of residue remains in the raw material tank 1; the permeate in the second storage tank 24 is continuously heated to 60°C and enters the second filter membrane 3. The permeate from the second permeation side 32 of the second filter membrane 3 is collected in two parts, 50 kg of permeate is collected into the third storage tank 33, and the other part enters the fourth storage tank 34. The permeate collected in the third storage tank 33 is returned to the raw material tank 1, and the retentate located at the second retentate side 31 of the second filter membrane 3 is returned to the first filter membrane 2; the permeate collected in the fourth storage tank 34 is continuously heated to 60°C and enters the third filter membrane 4. The permeate from the third permeation side 42 of the third filter membrane 4 is collected in two parts, 50 kg of permeate is collected into the fifth storage tank 43, and the other part enters the sixth storage tank 44. The permeate collected in the fifth storage tank 43 is returned to the raw material tank 1, and the retentate located at the third retentate side 41 of the third filter membrane 4 is returned to the second filter membrane 3. The permeate collected in the sixth storage tank 44 is the target product.

[0067] The first filter membrane 2 adopts an organic tubular composite membrane, the first layer is PP with a pore size of 1000 nm, and the second layer is PTFE with an average pore size of 100 nm; the filter shell and the storage tank of the first filter membrane 2 are made of high-purity PP.

[0068] The second filter membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with a pore size of 1000 nm, and the second layer is PTFE with an average pore size of 100 nm; the filter shell and the storage tank of the second filter membrane 3 are made of high-purity PVDF.

[0069] The third filter membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with a pore size of 1000 nm, and the second layer is PTFE with an average pore size of 100 nm; the filter shell and the storage tank of the second filter membrane are made of high-purity PFA.

[0070] The first filter membrane 2, the second filter membrane 3, and the third filter membrane 4 all use polyamino chitosan modified polydimethylsiloxane composite membranes as effective separation layers, and the pressure on the permeation side of the membrane is 8000 Pa. The content of isopropyl alcohol is 99.98%, and the experimental results are shown in Table 1.

[0071] Example 3:

[0072] 1000 kg of raw material from the raw material tank 1 is heated to 50°C and enters the first filter membrane 2. The permeate from the first permeation side 22 of the first filter membrane 2 is collected in two parts, one part of 30 kg of permeate is collected into the first storage tank 23, and the other part of permeate enters the second storage tank 24. The permeate collected in the first storage tank 23 and the retentate located at the first retentate side 21 of the first filter membrane 2 are both returned to the raw material tank 1, and 100 kg of residue remains in the raw material tank 1; the permeate in the second storage tank 24 is continuously heated to 50°C and enters the second filter membrane 3. The permeate from the second permeation side 32 of the second filter membrane 3 is collected in two parts, 30 kg of permeate is collected into the third storage tank 33, and the other part enters the fourth storage tank 34. The permeate collected in the third storage tank 33 is returned to the raw material tank 1, and the retentate located at the second retentate side 31 of the second filter membrane 3 is returned to the first filter membrane 2; the permeate collected in the fourth storage tank 34 is continuously heated to 50°C and enters the third filter membrane 4. The permeate from the third permeation side 42 of the third filter membrane 4 is collected in two parts, 30 kg of permeate is collected into the fifth storage tank 43, and the other part enters the sixth storage tank 44. The permeate collected in the fifth storage tank 43 is returned to the raw material tank 1, and the retentate located at the third retentate side 41 of the third filter membrane 4 is returned to the second filter membrane 3. The permeate collected in the sixth storage tank 44 is the target product.

[0073] The first filter membrane 2 adopts an organic tubular composite membrane, the first layer is PP with a pore size of 800 nm, and the second layer is PTFE with an average pore size of 50 nm; the filter shell and the storage tank of the first filter membrane 2 are made of high-purity PP.

[0074] The second filter membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with a pore size of 800 nm, and the second layer is PTFE with an average pore size of 50 nm; the filter shell and the storage tank of the second filter membrane 3 are made of high-purity PVDF.

[0075] The third filter membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with a pore size of 800 nm, and the second layer is PTFE with an average pore size of 50 nm; the filter shell and the storage tank of the second filter membrane are made of high-purity PFA.

[0076] The first filter membrane 2, the second filter membrane 3, and the third filter membrane 4 all use polyamino chitosan modified polydimethylsiloxane composite membrane as the effective separation layer, and the pressure on the permeation side of the membrane is 5000 Pa. The content of isopropyl alcohol is 99.96%, and the experimental results are shown in Table 1.

[0077] Table 1 Comparison table of experimental results

[0078]

[0079] According to the above table, compared with the conventional rectification scheme, the technical scheme of the application greatly improves the removal effect of metal ions in isopropyl alcohol.

[0080] Beneficial effects:

[0081] 1. The application adopts a three-stage membrane system to remove metal ions and particles, compared with the traditional multi-effect rectification and ultrafiltration membrane to remove particles, which simplifies the process, reduces the equipment area, reduces the equipment height, and is suitable for large-scale industrial production.

[0082] 2. The application adopts a polyammoniated chitosan modified polydimethylsiloxane composite membrane, and the operating conditions do not reach the boiling point of the feed liquid, the permeate side is gaseous, and the metal ions are well removed; at the same time, the three filter membranes are dense membranes, which have good removal effect on particles.

[0083] 3. The different stage membranes of the application respectively adopt high-purity PP, PVDF and PFA materials, which not only reduce the investment cost, but also meet the requirement that the contact materials do not produce elution in the production of wet electronic chemicals.

[0084] The above-described embodiments only express several embodiments of the application, and the description is more specific and detailed, but it cannot be understood as a limitation on the scope of the patent of the application. It should be pointed out that for ordinary skilled persons in the art, without departing from the concept of the application, a number of modifications and improvements can be made, which all belong to the protection scope of the application. Therefore, the protection scope of the patent of the application should be subject to the appended claims.

Claims

1. A high-purity, ultra-clean isopropanol production apparatus, characterized in that, The production device comprises: a raw material tank (1) for storing isopropyl alcohol to be processed; a first filter membrane (2) having a first inlet (20) connected to an outlet (11) of the raw material tank (1) and a first retentate side (21) connected to an inlet (10) of the raw material tank (1); a second filter membrane (3) having a second inlet (30) connected to a first permeate side (22) of the first filter membrane (2) and a second retentate side (31) connected to the first inlet (20) of the first filter membrane (2); a third filter membrane (4) having a third inlet (40) connected to a second permeate side (32) of the second filter membrane (3), a third retentate side (41) connected to the second inlet (30) of the second filter membrane (3), and a third permeate side (42) for obtaining a target product; a heating assembly (5) for heating isopropyl alcohol to be processed located at the first inlet (20), the second inlet (30), and the third inlet (40); a condensing assembly (6) for condensing isopropyl alcohol to be processed located at the first permeate side (22), the second permeate side (32), and the third permeate side (42); the first filter membrane (2), the second filter membrane (3), and the third filter membrane (4) are all composite membranes, and the three-stage membrane system simultaneously removes metal ions and particulate matter; the heating assembly (5) comprises: a first heater (50) having an inlet connected to the outlet (11) of the raw material tank (1) and an outlet connected to the first inlet (20) of the first filter membrane (2); a second heater (51) having an inlet connected to the first permeate side (22) of the first filter membrane (2) and an outlet connected to the second inlet (30) of the second filter membrane (3); a third heater (52) having an inlet connected to the second permeate side (32) of the second filter membrane (3) and an outlet connected to the third inlet (40) of the third filter membrane (4); the condensing assembly (6) comprises: a first condenser (60) having an inlet connected to the first permeate side (22) of the first filter membrane (2) and an outlet connected to the inlet of the second heater (51); a second condenser (61) having an inlet connected to the second permeate side (32) of the second filter membrane (3) and an outlet connected to the inlet of the third heater (52); a third condenser (62) having an inlet connected to the third permeate side (42) of the third filter membrane (4); a vacuum pump (63) connected to the first condenser (60), the second condenser (61), and the third condenser (62) simultaneously; the production device further comprises: a second storage tank (24) having an inlet connected to the outlet of the first condenser (60) and an outlet connected to the inlet of the second heater (51); a fourth storage tank (34) having an inlet connected to the outlet of the second condenser (61) and an outlet connected to the inlet of the third heater (52); a sixth storage tank (44) having an inlet connected to the outlet of the third condenser (62) and an outlet for outputting a product. The first storage tank (23) is connected with the outlet of the first condenser (60) and the input (10) of the raw material tank (1); The third storage tank (33) is connected with the outlet of the second condenser (61) and the input (10) of the raw material tank (1); The fifth storage tank (43) is connected with the outlet of the third condenser (62) and the input (10) of the raw material tank (1).

2. The method for producing ultra-clean high-purity isopropanol according to claim 1, wherein The method comprises the following steps: The isopropyl alcohol to be processed is heated and then enters the first filter membrane (2). The permeate from the first permeation side (22) of the first filter membrane (2) is collected in two parts, one part enters the first storage tank (23), and the other part enters the second storage tank (24). The permeate collected by the first storage tank (23) and the retentate located at the first retentate side (21) of the first filter membrane (2) are returned to the raw material tank (1), and the residual liquid in the raw material tank (1) is used as a residual liquid; The permeate collected by the second storage tank (24) is heated and then enters the second filter membrane (3). The permeate from the second permeation side (32) of the second filter membrane (3) is collected in two parts, one part enters the third storage tank (33), and the other part enters the fourth storage tank (34). The permeate collected by the third storage tank (33) is returned to the raw material tank (1), and the retentate located at the second retentate side (31) of the second filter membrane (3) is returned to the first filter membrane (2); The permeate collected by the fourth storage tank (34) is heated and then enters the third filter membrane (4). The permeate from the third permeation side (42) of the third filter membrane (4) is collected in two parts, one part enters the fifth storage tank (43), and the other part enters the sixth storage tank (44). The permeate collected by the fifth storage tank (43) is returned to the raw material tank (1), the retentate located at the third retentate side (41) of the third filter membrane (4) is returned to the second filter membrane (3), and the permeate collected in the sixth storage tank (44) is the target product. The first filter membrane (2), the second filter membrane (3), and the third filter membrane (4) are all composite membranes, and the three-stage membrane system simultaneously removes metal ions and particulate matter.

Images