Electronic-grade isopropanol purification system

Abstract

The utility model belongs to the field of chemical equipment, and particularly relates to an electronic-grade isopropanol purification system, which comprises a light component removal tower and a heavy component removal tower, a discharge port at the bottom of the light component removal tower is connected with a light component removal tower reboiler, the light component removal tower reboiler is communicated with a feed port at the lower part of a light component removal tower efficient demister through a light component removal tower kettle liquid pipeline, and the light component removal tower efficient demister is communicated with the heavy component removal tower. A discharge hole in the upper part of the efficient demister of the light component removal tower is communicated with a feed hole in the middle of the heavy component removal tower through a heavy component removal tower kettle liquid pipeline, a discharge hole in the top of the heavy component removal tower is respectively communicated with a heavy component removal tower top reflux gas pipeline and a heavy component removal tower top produced gas pipeline through a heavy component removal tower top gas pipeline, and an outlet of the heavy component removal tower top reflux gas pipeline is connected to a heavy component removal tower reflux device; a gas extraction pipeline at the top of the heavy component removal tower is communicated with a feed port at the lower part of the high-efficiency demister of the heavy component removal tower; and a discharge port at the upper part of the high-efficiency demister of the heavy component removal tower is communicated to a product collecting device. According to the utility model, the light component removal tower top gas phase is used as a heat source of the heavy component removal tower kettle reboiler to form thermal coupling, so that the steam consumption is greatly reduced, the production cost is reduced, and the product stability is high.

Description

Technical Field

[0001] The utility model belongs to the field of chemical equipment, in particular to an electronic-grade isopropyl alcohol purification system. Background Art

[0002] High-purity isopropyl alcohol (IPA) is an important electronic chemical, primarily used for cleaning and drying in the production of integrated circuits (ICs). As IC manufacturing processes become more sophisticated, requirements for the purity, metal ion concentration, and particulate matter content of IPA are becoming increasingly stringent, as is the demand for quality stability.

[0003] Currently, the production of high-purity isopropyl alcohol typically uses industrial-grade isopropyl alcohol as a raw material, which contains trace light components, heavy components, and water. After light and heavy components are removed and purified by dehydration, metal ions are removed by adsorption and other methods, and high-purity electronic-grade isopropyl alcohol is obtained after nanofiltration. Common methods for light and heavy components removal and dehydration purification include: Patent CN 117919747 A discloses a method for preparing electronic-grade isopropyl alcohol by combining membrane dehydration and entrainer dehydration in series. While this method can increase the yield of isopropyl alcohol and reduce tower height, it introduces a large amount of additional solvent, which affects the quality and stability of the high-purity isopropyl alcohol product. Patent CN 216934754 U discloses a method for preparing anhydrous isopropyl alcohol by combining a molecular sieve and a pervaporation membrane in series. This method overcomes the poor dehydration stability of molecular sieves and improves dehydration reliability. However, the pervaporation membrane requires negative pressure operation, requires a large membrane area, is susceptible to contamination, and is difficult to clean after membrane replacement. Utility Model Content

[0004] In view of the problems and shortcomings in the prior art, the purpose of the present invention is to provide an electronic-grade isopropyl alcohol purification system with high product stability, low energy consumption and low production cost.

[0005] Based on the above purpose, the present invention adopts the following technical solutions:

[0006] The utility model provides an electronic grade isopropyl alcohol purification system, comprising a lightness removal tower and a heavyness removal tower, wherein the bottom discharge port of the lightness removal tower is connected to the lightness removal tower reboiler, the lightness removal tower reboiler is connected to the lower feed port of the lightness removal tower high-efficiency demister through the lightness removal tower kettle liquid pipeline, the upper discharge port of the lightness removal tower high-efficiency demister is connected to the middle feed port of the heavyness removal tower through the heavyness removal tower kettle liquid pipeline, the top discharge port of the heavyness removal tower is connected to the heavyness removal tower top reflux gas pipeline and the heavyness removal tower top gas pipeline respectively through the heavyness removal tower top gas pipeline. The produced gas pipeline at the top of the deweighting tower is connected, the outlet of the reflux gas pipeline at the top of the deweighting tower is connected to the reflux device of the deweighting tower, the produced gas pipeline at the top of the deweighting tower is connected to the lower feed port of the high-efficiency demister of the deweighting tower, the upper discharge port of the high-efficiency demister of the deweighting tower is connected to the demisting high-purity isopropyl alcohol pipeline, a product condenser is connected between the demisting high-purity isopropyl alcohol pipeline and the liquid-phase high-purity isopropyl alcohol pipeline, and the product condenser outlet is connected to the product collecting device through the liquid-phase high-purity isopropyl alcohol pipeline.

[0007] Furthermore, the top discharge port of the light-removing tower is connected to the reboiler of the heavy-removing tower through the top gas pipeline of the light-removing tower, the reboiler of the heavy-removing tower is connected to the inlet of the reflux tank of the light-removing tower through the top condensate pipeline of the light-removing tower, the outlet of the reflux tank of the light-removing tower is connected to the inlet of the reflux pump of the light-removing tower, the outlet of the reflux pump of the light-removing tower is respectively connected to the reflux pipeline of the light-removing tower and the light component pipeline of the top of the light-removing tower, the reflux pipeline of the light-removing tower is connected to the reflux port of the upper part of the light-removing tower, and the light component pipeline of the top of the light-removing tower and the extraction pipeline (117) of the kettle of the heavy-removing tower are both connected to the outside of the system.

[0008] Furthermore, the deweighting tower reflux device includes a deweighting tower condenser, a deweighting tower reflux tank, and a deweighting tower reflux pump connected in sequence, and the deweighting tower reflux pump is connected to the upper reflux port of the deweighting tower through a deweighting tower reflux liquid pipeline.

[0009] Furthermore, the high-efficiency demister of the light-removal tower and the high-efficiency demister of the heavy-removal tower are any one of a cyclone separator, a packing separator and a filter-type gas-liquid separator.

[0010] Furthermore, the light removal tower reboiler and the heavy removal tower reboiler are both kettle reboilers.

[0011] Furthermore, the middle feed port of the lightness removal tower is connected to the industrial isopropyl alcohol raw material pipeline, and the inlet of the industrial isopropyl alcohol raw material pipeline is connected to a pump.

[0012] Furthermore, the bottom discharge port of the high-efficiency demister of the deweighting tower is connected to the middle feed port of the deweighting tower through the demister condensate pipeline.

[0013] Furthermore, the lower reflux port of the lightness removal tower is connected to the lightness removal tower reboiler.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] (1) The top gas phase of the degassing tower is used as the heat source for the reboiler of the degassing tower kettle, forming a thermal coupling, which greatly reduces steam consumption and production costs. The distillation method is used for refining, and the equipment is reliable and the product is highly stable.

[0016] (2) The reboilers of the light-tower and heavy-tower degassing towers adopt kettle-type reboilers to improve the gas-liquid separation efficiency, reduce the amount of liquid entrained in the gas phase of the tower bottom, reduce the amount of metal impurities entrained in the tower bottom, and improve the efficiency of metal impurity removal.

[0017] (3) The gas phase material produced from the bottom of the light-removal tower passes through a high-efficiency demister to remove tiny droplets before entering the heavy-removal tower to improve the removal efficiency of metal impurities.

[0018] (4) The gas phase product produced from the top of the degassing tower is condensed into the product after passing through a high-efficiency demister to remove tiny droplets, thereby improving the efficiency of removing metal impurities. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the electronic-grade isopropyl alcohol purification system of the utility model.

[0020] In the figure: 1- lightness removal tower, 2- lightness removal tower reboiler, 3- lightness removal tower high-efficiency demister, 4- lightness removal tower reflux tank, 5- lightness removal tower reflux pump, 6- heavyness removal tower reboiler, 7- heavyness removal tower, 8- heavyness removal tower condenser, 9- heavyness removal tower reflux tank, 10- heavyness removal tower reflux pump, 11- heavyness removal tower high-efficiency demister, 12- product condenser, 101- industrial isopropyl alcohol raw material pipeline, 102- lightness removal tower kettle liquid pipeline, 103- lightness removal tower top gas pipeline, 104- lightness removal tower top condensate pipeline, 105- Light tower reflux pipeline, 106-light component pipeline at the top of light-removal tower, 107-heavy-removal tower kettle liquid pipeline, 108-heavy-removal tower top gas pipeline, 109-heavy-removal tower top reflux gas pipeline, 110-heavy-removal tower reflux liquid pipeline, 111-heavy-removal tower top produced gas pipeline, 112-demist high-purity isopropyl alcohol pipeline, 113-liquid phase high-purity isopropyl alcohol pipeline, 114-demister condensate pipeline, 115-demister liquid phase return liquid pipeline, 116-light-removal tower kettle produced pipeline, 117-heavy-removal tower kettle produced pipeline. DETAILED DESCRIPTION

[0021] The following is a detailed description of the present invention, clearly and completely describing the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0022] Example 1

[0023] An electronic grade isopropyl alcohol purification system, such as Figure 1As shown, it includes a light removal tower 1 and a weight removal tower 7, the bottom discharge port of the light removal tower 1 is connected to the light removal tower reboiler 2, the light removal tower reboiler 2 is connected to the lower feed port of the light removal tower high-efficiency demister 3 through the light removal tower kettle liquid pipeline 102, the upper discharge port of the light removal tower high-efficiency demister 3 is connected to the middle feed port of the weight removal tower 7 through the weight removal tower kettle liquid pipeline 107, the top discharge port of the weight removal tower 7 is connected to the weight removal tower top reflux gas pipeline 109 and the weight removal tower top production gas pipeline 111 respectively through the weight removal tower top gas pipeline 108, the weight removal tower top reflux gas pipeline 109 outlet is connected in sequence to the weight removal tower condenser 8, the weight removal tower reflux tank 9, the weight removal tower reflux pump 1 0, the de-weighting tower reflux pump 10 is connected to the upper reflux port of the de-weighting tower 7 through the de-weighting tower reflux liquid pipeline 110; the de-weighting tower top produced gas pipeline 111 is connected to the lower feed port of the de-weighting tower high-efficiency demister 11, and the upper discharge port of the de-weighting tower high-efficiency demister 11 is connected to the de-misting high-purity isopropyl alcohol pipeline 112, and the de-misting high-purity isopropyl alcohol pipeline 112 and the liquid-phase high-purity isopropyl alcohol pipeline 113 are connected with the product condenser 12, and the outlet of the product condenser 12 is connected to the product collecting device through the liquid-phase high-purity isopropyl alcohol pipeline 113; the bottom of the de-lighting tower high-efficiency demister 3 is connected to the de-lighting tower reboiler 2 through the demister liquid-phase return liquid pipeline 115.

[0024] The top discharge port of the light-removing tower 1 is connected to the deheavy-removing tower reboiler 6 through the light-removing tower top gas pipeline 103, the deheavy-removing tower reboiler 6 is connected to the inlet of the light-removing tower reflux tank 4 through the light-removing tower top condensate pipeline 104, the light-removing tower reflux tank 4 outlet is connected to the inlet of the light-removing tower reflux pump 5, the light-removing tower reflux pump outlet is respectively connected to the light-removing tower reflux pipeline 105 and the light component pipeline 106 at the top of the light-removing tower, the light-removing tower reflux pipeline 105 is connected to the upper reflux port of the light-removing tower 1, the light component pipeline 106 at the top of the light-removing tower, the deheavy-removing tower kettle extraction pipeline 117, and the light-removing tower kettle extraction pipeline 116 at the bottom of the light-removing tower reboiler 2 are all connected to the outside of the system.

[0025] The light removal tower high-efficiency demister 3 and the heavy removal tower high-efficiency demister 11 are cyclone separators, packing separators and filter-type gas-liquid separators, and the internal parts are made of PFA or PTFE non-metallic materials; the light removal tower reboiler 2 and the heavy removal tower reboiler 6 are both kettle reboilers.

[0026] The middle feed port of the de-light tower 1 is connected to the industrial isopropyl alcohol raw material pipeline 101, and the inlet of the industrial isopropyl alcohol raw material pipeline 101 is connected to a pump; the bottom discharge port of the high-efficiency demister 11 of the de-light tower is connected to the middle feed port of the de-light tower 7 through the demister condensate pipeline 114.

[0027] During production, a batch of industrial-grade isopropyl alcohol has a composition of 99.9%, a water content of ≤1000 ppm, an acetone content of ≤100 ppm, a heavy component content of 100 ppm or less, and a metal ion content of ≤5 ppm. The industrial-grade isopropyl alcohol is pressurized by a pump and fed into the lightness removal tower 1. The operating pressure of the lightness removal tower 1 is 0.25-0.4 MPaG, the top reflux to feed ratio is 1.0-1.5, and the top temperature is 115-126°C. The bottom of the tower is taken out as anhydrous isopropyl alcohol in the vapor phase, with a water content of <50 ppm and an acetone content of <0.1 ppm. The gaseous anhydrous isopropyl alcohol is defogged by the high-efficiency demister 3 of the light removal tower and then enters the de-weighting tower 7. The operating pressure of the de-weighting tower is 5-70 kPaG, the tower top temperature is 84-97°C, the tower bottom temperature is 87-100°C, and the tower top reflux extraction ratio is 1.0-1.5. The gaseous electronic-grade isopropyl alcohol extracted from the top of the de-weighting tower has an electronic-grade isopropyl alcohol content of >99.995%, a water content of <50 ppm, an acetone content of <0.1 ppm, and a heavy component content of <1 ppm. After exiting the high-efficiency demister of the de-weighting tower, the electronic-grade isopropyl alcohol with a metal ion content of <1 ppb (G3) is condensed and further removed from the metal ions through a polishing resin adsorption column. The particulate matter is removed through circulating filtration to finally obtain the isopropyl alcohol product. The obtained isopropyl alcohol meets the requirements of electronic grade products, with a purity of >99.995%, a water content of <50ppm, an acetone content of <0.1ppm, an acidity of <0.2ppm, an alkalinity of <0.1ppm, a metal ion content of <0.01ppb, a total amount of 0.2 micron particles of <100 / mL, and an isopropyl alcohol yield of ≥98.5%.

[0028] The logistics in the de-light tower top gas pipeline 103 is used as the heat source of the de-heavy tower reboiler 6, and the logistics in the de-light tower top condensate pipeline 104 is pressurized by the de-light tower reflux pump 5, and part of it is returned to the tower through 105 as reflux, and part of it is extracted as light components through 106 and returned to the upstream industrial isopropyl alcohol refining unit together with the logistics of the de-heavy tower kettle extraction pipeline 117 as circulating isopropyl alcohol to recover isopropyl alcohol.

[0029] The present embodiment only needs steam for the lightness removal tower kettle reboiler, and steam consumption is 0.93t / t electronic-grade isopropyl alcohol, and circulating water consumption is 46t / t. Compared with traditional two-tower atmospheric distillation, steam consumption saves steam 0.5t / t electronic-grade isopropyl alcohol, and circulating water consumption reduces 26t / t, that is, steam consumption reduces 35.0%, and circulating water consumption reduces 36.1%, and energy consumption is significantly reduced. Both towers adopt gas phase extraction product, and remove tiny droplets through high-efficiency demister, metal ion removal efficiency is high, and product quality is more stable.

[0030] Although the present invention has been described with reference to the above specific embodiments, it is obvious that those skilled in the art will be able to make many substitutions, modifications, and variations based on the above description. Therefore, all such substitutions, modifications, and variations should fall within the scope of protection of the claims of the present invention.

Claims

1. An electronic grade isopropyl alcohol purification system, characterized in that: The invention comprises a light-removing tower (1) and a heavy-removing tower (7), wherein the bottom discharge port of the light-removing tower (1) is connected to the light-removing tower reboiler (2), the light-removing tower reboiler (2) is connected to the lower feed port of the light-removing tower high-efficiency demister (3) through the light-removing tower kettle liquid pipeline (102), the upper discharge port of the light-removing tower high-efficiency demister (3) is connected to the middle feed port of the heavy-removing tower (7) through the heavy-removing tower kettle liquid pipeline (107), and the top discharge port of the heavy-removing tower (7) is connected to the heavy-removing tower top reflux gas pipeline (109) and the heavy-removing tower top extraction gas pipeline (111) through the heavy-removing tower top gas pipeline (108). ), the outlet of the deweighting tower top reflux gas pipeline (109) is connected to the deweighting tower reflux device, the deweighting tower top production gas pipeline (111) is connected to the lower feed port of the deweighting tower high-efficiency demister (11), the upper discharge port of the deweighting tower high-efficiency demister (11) is connected to the demisting high-purity isopropyl alcohol pipeline (112), a product condenser (12) is connected between the demisting high-purity isopropyl alcohol pipeline (112) and the liquid-phase high-purity isopropyl alcohol pipeline (113), and the outlet of the product condenser (12) is connected to the product collecting device through the liquid-phase high-purity isopropyl alcohol pipeline (113).

2. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The top discharge port of the de-light tower (1) is connected to the de-heavy tower reboiler (6) through the de-light tower top gas pipeline (103), the de-heavy tower reboiler (6) is connected to the de-light tower reflux tank (4) inlet through the de-light tower top condensate pipeline (104), the de-light tower reflux tank (4) outlet is connected to the de-light tower reflux pump (5) inlet, the de-light tower reflux pump outlet is respectively connected to the de-light tower reflux pipeline (105) and the de-light tower top light component pipeline (106), the de-light tower reflux pipeline (105) is connected to the upper reflux port of the de-light tower (1), the de-light tower top light component pipeline (106) and the de-heavy tower kettle extraction pipeline (117) are both connected to the outside of the system.

3. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The deweighting tower reflux device comprises a deweighting tower condenser (8), a deweighting tower reflux tank (9), and a deweighting tower reflux pump (10) connected in sequence. The deweighting tower reflux pump (10) is connected to the upper reflux port of the deweighting tower (7) through a deweighting tower reflux liquid pipeline (110).

4. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The light removal tower high-efficiency demister (3) and the heavy removal tower high-efficiency demister (11) are any one of a cyclone separator, a packing separator, and a filter-type gas-liquid separator.

5. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The light removal tower reboiler (2) and the heavy removal tower reboiler (6) are both kettle-type reboilers.

6. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The middle feed port of the light removal tower (1) is connected to the industrial isopropyl alcohol raw material pipeline (101), and the inlet of the industrial isopropyl alcohol raw material pipeline (101) is connected to a pump.

7. The electronic grade isopropyl alcohol purification system according to claim 1, characterized in that: The bottom discharge port of the high-efficiency demister (11) of the de-weighting tower is connected to the middle feed port of the de-weighting tower (7) through the demister condensate pipeline (114).

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