CN116651212A - Ultra-clean high-purity isopropanol production device and method - Google Patents
Ultra-clean high-purity isopropanol production device and method Download PDFInfo
- Publication number
- CN116651212A CN116651212A CN202310580591.3A CN202310580591A CN116651212A CN 116651212 A CN116651212 A CN 116651212A CN 202310580591 A CN202310580591 A CN 202310580591A CN 116651212 A CN116651212 A CN 116651212A
- Authority
- CN
- China
- Prior art keywords
- membrane
- inlet
- permeate
- storage tank
- filtering membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title description 9
- 239000012528 membrane Substances 0.000 claims abstract description 259
- 238000001914 filtration Methods 0.000 claims abstract description 154
- 239000002994 raw material Substances 0.000 claims abstract description 58
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000012466 permeate Substances 0.000 claims description 133
- 238000003860 storage Methods 0.000 claims description 113
- 239000007788 liquid Substances 0.000 claims description 46
- 239000012465 retentate Substances 0.000 claims description 39
- 239000002131 composite material Substances 0.000 claims description 34
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 18
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 18
- 239000002033 PVDF binder Substances 0.000 claims description 14
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 14
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 14
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 14
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 14
- 239000004952 Polyamide Substances 0.000 claims description 13
- 229920002647 polyamide Polymers 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- 229920001661 Chitosan Polymers 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- -1 polydimethylsiloxane Polymers 0.000 claims 1
- 238000005325 percolation Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000009776 industrial production Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000012824 chemical production Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/02—Monohydroxylic acyclic alcohols
- C07C31/10—Monohydroxylic acyclic alcohols containing three carbon atoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses an ultra-clean high-purity isopropyl alcohol production device, which comprises a raw material tank, a first filtering membrane, a second filtering membrane, a first filtering membrane and a second filtering membrane, wherein a first inlet of the first filtering membrane is connected with an output port of the raw material tank, and a first percolation side of the first filtering membrane is connected with an input port of the raw material tank; the second inlet of the second filtering membrane is connected with the first permeation side of the first filtering membrane, and the second residual permeation side of the second filtering membrane is connected with the first inlet of the first filtering membrane; the third filter membrane is provided with a third inlet connected with the second permeation side of the second filter membrane, the third residual permeation side of the third filter membrane is connected with the second inlet of the second filter membrane, and the third permeation side of the third filter membrane is used for obtaining a target product; the heating assembly is used for heating the isopropanol to be processed at the first inlet, the second inlet and the third inlet; and the condensing assembly is used for condensing the isopropanol to be processed at the first permeation side, the second permeation side and the third permeation side. The invention can improve the purity of the ultra-clean high-purity isopropanol product, has small equipment occupation, and is suitable for large-scale industrialized production.
Description
Technical Field
The invention relates to the technical field of microelectronic chemical reagents, in particular to an ultra-clean high-purity isopropanol production device and method.
Background
As one of the important cleaning agents for the electronics industry, the demand for ultra-clean high-purity isopropyl alcohol will become increasingly greater in the future, and the demand for isopropyl alcohol is expected to increase rapidly at a rate of more than 10% of the annual average. Electronic grade isopropanol has the excellent performance of being capable of being gasified rapidly and free of residues, and ultra-clean high-purity isopropanol has been widely applied to cleaning and corrosion in the industries of semiconductors, metal degreasing, ultra-large scale integrated circuits and the like.
At present, ultra-clean high-purity isopropanol is generally prepared by taking industrial grade isopropanol as a raw material for purification and refining, and rectification is a main method for industrially purifying isopropanol, and comprises azeotropic rectification, extractive distillation and the like. However, ultra-clean high-purity isopropanol used in the microelectronics chemical industry has very strict requirements on the size and content of metal impurities and particles, the rectification process cannot meet the requirements, and equipment occupation area required by the rectification process is large, so that the ultra-clean high-purity isopropanol is not suitable for large-scale industrial production.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an ultra-clean high-purity isopropanol production device and method, which can improve the purity of the ultra-clean high-purity isopropanol product, occupy less equipment space and are suitable for large-scale industrial production.
The invention is realized by the following technical scheme:
an ultra-clean high-purity isopropyl alcohol production device, comprising:
a raw material tank for storing isopropyl alcohol to be processed;
the first filter membrane is connected with the output port of the raw material tank at a first inlet, and the first percolation side of the first filter membrane is connected with the input port of the raw material tank;
the second inlet of the second filtering membrane is connected with the first permeation side of the first filtering membrane, and the second residual permeation side of the second filtering membrane is connected with the first inlet of the first filtering membrane;
the third filter membrane is provided with a third inlet connected with the second permeation side of the second filter membrane, the third residual permeation side of the third filter membrane is connected with the second inlet of the second filter membrane, and the third permeation side of the third filter membrane is used for obtaining a target product;
the heating assembly is used for heating the isopropanol to be processed at the first inlet, the second inlet and the third inlet;
and the condensing assembly is used for condensing the isopropanol to be processed at the first permeation side, the second permeation side and the third permeation side.
Further, the first filtering membrane, the second filtering membrane and the third filtering membrane are all composite membranes.
Further, the first filtering 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 polydimethyl siloxane composite membrane modified by polyamide chitosan.
Further, the second filtering 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 polydimethyl siloxane composite membrane modified by polyamide chitosan.
Further, the third filtering 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 polydimethyl siloxane composite membrane modified by polyamide chitosan.
Further, the heating assembly includes:
the inlet of the first heater is connected with the output port of the raw material tank, and the outlet of the first heater is connected with the first inlet of the first filtering membrane;
a second heater, the inlet of which is connected with the first permeation side of the first filtering membrane, and the outlet of which is connected with the second inlet of the second filtering membrane;
and the inlet of the third heater is connected with the second permeation side of the second filtering membrane, and the outlet of the third heater is connected with the third inlet of the third filtering membrane.
Further, the condensing assembly includes:
a first condenser having an inlet connected to the first permeate side of the first filtration membrane and an outlet connected to the inlet of the second heater;
a second condenser having an inlet connected to the second permeate side of the second filtration membrane and an outlet connected to the inlet of the third heater;
a third condenser having an inlet connected to a third permeate side of the third filtration membrane;
and the vacuum pump is connected with the first condenser, the second condenser and the third condenser at the same time.
Further, the production device further comprises:
the inlet of the second storage tank is connected with the outlet of the first condenser, and the outlet of the second storage tank is connected with the inlet of the second heater;
the inlet of the fourth storage tank is connected with the outlet of the second condenser, and the outlet of the fourth storage tank is connected with the inlet of the third heater;
and the inlet of the sixth storage tank is connected with the outlet of the third condenser, and the outlet of the sixth storage tank outputs a product.
Further, the production device further comprises:
the inlet of the first storage tank is connected with the outlet of the first condenser, and the outlet of the first storage tank is connected with the input port of the raw material tank;
the inlet of the third storage tank is connected with the outlet of the second condenser, and the outlet of the third storage tank is connected with the input port of the raw material tank;
and the inlet of the fifth storage tank is connected with the outlet of the third condenser, and the outlet of the fifth storage tank is connected with the input port of the raw material tank.
The production method of the ultra-clean high-purity isopropanol comprises the following steps:
the isopropanol to be processed enters a first filtering membrane after being heated from a storage tank, permeate liquid coming out of a first permeation side of the first filtering membrane is collected in two parts, part of the permeate liquid enters the first storage tank, the other part of the permeate liquid enters a second storage tank, permeate liquid collected by the first storage tank and retentate liquid positioned on a first permeation residual side of the first filtering membrane are returned to a raw material tank, and residual liquid in the raw material tank is used as raffinate;
heating the permeate collected by the second storage tank, then, entering the second filtering membrane, collecting the permeate coming out of the second permeate side of the second filtering membrane in two parts, wherein part of the permeate enters the third storage tank, the other part of the permeate enters the fourth storage tank, the permeate collected by the third storage tank returns to the raw material tank, and the retentate at the second retentate side of the second filtering membrane returns to the first filtering membrane;
and heating the permeate collected by the fourth storage tank, then, enabling the permeate to enter a third filtering membrane, collecting the permeate from the third permeate side of the third filtering membrane in two parts, partially entering a fifth storage tank, partially entering a sixth storage tank, returning the permeate collected by the fifth storage tank to a raw material tank, returning the retentate positioned on the third retentate side of the third filtering membrane to the second filtering membrane, and taking the permeate collected in the sixth storage tank as a target product.
Compared with the prior art, the invention has the advantages that:
1. the invention adopts the three-stage membrane system to remove metal ions and particles at the same time, and compared with the traditional multi-effect rectification and ultrafiltration membrane to remove the particles, the invention simplifies the process, reduces the equipment occupation area and the equipment height, and is suitable for large-scale industrial production.
2. The invention adopts the polydimethyl siloxane composite membrane modified by the polyamide, the adopted operation condition does not reach the boiling point of feed liquid, the permeation side is in a gaseous state, and the invention has good removing property for metal ions; meanwhile, the three filtering membranes are compact membranes, and have good removal effect on particulate matters.
3. The systems of different layers of membranes respectively adopt high-purity PP, PVDF, PFA materials, so that not only is the investment cost reduced, but also the requirement that the contact materials do not produce dissolved matters in the wet electronic chemical production is met.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing ultra-clean high purity isopropyl alcohol according to an embodiment of the present invention;
FIG. 2 is a flow chart of an apparatus for producing ultra-clean high purity isopropyl alcohol according to an embodiment of the present invention.
1. A raw material tank; 10. an input port; 11. an output port; 12. a discharge port; 2. a first filtration membrane; 20. a first inlet; 21. a first retentate side; 22. a first permeate side; 23. a first storage tank; 24. a second storage tank; 3. a second filtration membrane; 30. a second inlet; 31. a second retentate side; 32. a second permeate side; 33. a third tank; 34. a fourth tank; 4. a third filtration membrane; 40. a third inlet; 41. a third retentate side; 42. a third permeate side; 43. a fifth storage tank; 44. a sixth storage tank; 5. a heating assembly; 50. a first heater; 51. a second heater; 52. a third heater; 6. a condensing assembly; 60. a first condenser; 61. a second condenser; 62. a third condenser; 63. and a vacuum pump.
Detailed Description
The technical scheme of the invention is further described in non-limiting detail below with reference to the preferred embodiments and the accompanying drawings. In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. refer to the azimuth or positional relationship based on the azimuth or positional relationship shown in the drawings. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
As shown in fig. 1, an ultra-clean high-purity isopropyl alcohol production device according to an embodiment of the present invention includes a raw material tank 1, a first filtering membrane 2, a second filtering membrane 3, a third filtering membrane 4, a heating component 5, and a condensing component 6, where the raw material tank 1 is used for storing isopropyl alcohol to be processed; the first inlet 20 of the first filtering membrane 2 is connected with the output port 11 of the raw material tank 1, the first residual osmosis side 21 of the first filtering membrane 2 is connected with the input port 10 of the raw material tank 1, the second inlet 30 of the second filtering membrane 3 is connected with the first osmosis side 22 of the first filtering membrane 2, the second residual osmosis side 31 of the second filtering membrane 3 is connected with the first inlet 20 of the first filtering membrane 2, the third inlet 40 of the third filtering membrane 4 is connected with the second osmosis side 32 of the second filtering membrane 3, the third residual osmosis side 41 of the third filtering membrane 4 is connected with the second inlet 30 of the second filtering membrane 3, the third osmosis side 42 of the third filtering membrane 4 is used for obtaining a target product, and the heating component 5 is used for heating isopropanol to be processed at the first inlet 20, the second inlet 30 and the third inlet 40; the condensing assembly 6 is used to condense the isopropyl alcohol to be processed 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 to 8000Pa.
The heating assembly 5 comprises a first heater 50, a second heater 51 and a third heater 52, wherein the inlet of the first heater 50 is connected with the output port 11 of the feed tank 1, the outlet of the first heater 50 is connected with the first inlet 20 of the first filtration membrane 2, the inlet of the second heater 51 is connected with the first permeate side 22 of the first filtration membrane 2, the outlet of the second heater 51 is connected with the second inlet 30 of the second filtration membrane 3, the inlet of the third heater 52 is connected with the second permeate side 32 of the second filtration membrane 3, and the outlet of the third heater 52 is connected with the third inlet 40 of the third filtration 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 to 60 ℃.
The condensation module 6 comprises a first condenser 60, a second condenser 61, a third condenser 62 and a vacuum pump 63, wherein the inlet of the first condenser 60 is connected with the first permeate side 22 of the first filtration 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 permeate side 32 of the second filtration membrane 3, the outlet of the second condenser 61 is connected with the inlet of the third heater 52, and the inlet of the third condenser 62 is connected with the third permeate side 42 of the third filtration 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, and the vacuum pump 63 pumps air in the condensers to avoid the pressure rise of the condensers caused by other non-condensable gases such as nitrogen, oxygen and the like in the air.
The ultra-clean high-purity isopropyl alcohol production device 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, wherein 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 tank 34 is connected to the outlet of the second condenser 61, the outlet of the fourth tank 34 is connected to the inlet of the third heater 52, the inlet of the sixth tank 44 is connected to the outlet of the third condenser 62, and the outlet of the sixth tank 44 outputs the product. The inlet of the first tank 23 is connected to the outlet of the first condenser 60, the outlet of the first tank 23 is connected to the inlet 10 of the raw material tank 1, the inlet of the third tank 33 is connected to the outlet of the second condenser 61, the outlet of the third tank 33 is connected to the inlet 10 of the raw material tank 1, the inlet of the fifth tank 43 is connected to the outlet of the third condenser 62, and the outlet of the fifth tank 43 is connected to the inlet 10 of the raw material tank 1. The residual part of liquid in the raw material tank 1 is residual liquid with high content of trapped metal ions and particles, and 5-20% of the total residual amount in the raw material tank 1 is used as residual liquid. Wherein, the amount of the permeate entering the first storage tank 23 is 2-10% of the total amount entering the first filtering membrane 2, the amount of the permeate entering the third storage tank 33 is 2-10% of the total amount entering the second filtering membrane 3, and the amount of the permeate entering the fifth storage tank 43 is 2-10% of the total amount entering the third filtering membrane 4.
In the embodiment, the isopropyl alcohol to be processed is industrial grade isopropyl alcohol, and the isopropyl alcohol content is more than or equal to 99.7%.
In this embodiment, the first filtering membrane 2, the second filtering membrane 3 and the third filtering membrane 4 are all dense membranes, and are simultaneously composite membranes, which may be organic composite folded membranes or organic tubular composite membranes.
The first filtering membrane 2 has a three-layer structure, the first layer is a PP membrane, and the average pore diameter is 500-1000 nm; the second layer is PTFE film with average pore diameter of 20-100 nm; the third layer is an effective separation layer and takes a polydimethyl siloxane composite membrane modified by polyamide as an active layer. If an organic composite folding membrane is adopted, the framework (not shown in the figure) and the component filter shell (not shown in the figure) of the folding membrane are high-temperature-resistant high-purity PP; if the organic tubular composite membrane is adopted, the filter shell of the organic tubular membrane is high-purity PP, and the material of the raw material tank 1, the first storage tank 23 and the second storage tank 24 is high-purity PP.
The second filtering membrane 3 has a three-layer structure, the first layer is a PVDF membrane, and the average pore diameter is 500-1000 nm; the second layer is PTFE film with average pore diameter of 20-100 nm; the third layer is an effective separation layer and takes a polydimethyl siloxane composite membrane modified by polyamide as an active layer. If an organic composite folding membrane is adopted, the framework and the component filter shell of the folding membrane are high-temperature-resistant high-purity PVDF; if an organic tubular composite membrane is adopted, the filter shell of the organic tubular membrane is made of high-purity PVDF, and the materials of the third storage tank 33 and the fourth storage tank 34 are made of high-purity PVDF.
The third filtering membrane 4 has a three-layer structure, the first layer is a PFA membrane, and the average pore diameter is 500-1000 nm; the second layer is PTFE film with average pore diameter of 20-100 nm; the third layer is an effective separation layer and takes a polydimethyl siloxane composite membrane modified by polyamide as an active layer. If an organic composite folding membrane is adopted, the framework and the component filter shell of the folding membrane are high-temperature-resistant high-purity PFA; if an organic tube type composite membrane is adopted, the filter shell of the organic tube type membrane is high-purity PFA or stainless steel lining PFA, and the materials of the third storage tank 33 and the fourth storage tank 34 are high-purity PFA or stainless steel lining PFA.
As shown in fig. 2, the method for producing ultra-clean high-purity isopropyl alcohol is characterized by comprising the following steps:
s1: the isopropanol to be processed enters the first filtering membrane 2 after being heated from the storage tank, the permeate liquid coming out of the first permeation side 22 of the first filtering membrane 2 is collected in two parts, part of the permeate liquid enters the first storage tank 23, the other part of the permeate liquid enters the second storage tank 24, the permeate liquid collected by the first storage tank 23 and the retentate liquid positioned on the first retentate side 21 of the first filtering membrane 2 are returned to the raw material tank 1, and part of the liquid remained in the raw material tank 1 is used as the raffinate liquid;
s2: heating the permeate collected by the second storage tank 24, then, entering the second filtering membrane 3, collecting the permeate coming out of the second permeate side 32 of the second filtering membrane 3 in two parts, wherein part of the permeate enters the third storage tank 33, the other part of the permeate enters the fourth storage tank 34, the permeate collected by the third storage tank 33 returns to the raw material tank 1, and the retentate at the second retentate side 31 of the second filtering membrane 3 returns to the first filtering membrane 2;
and S3, heating the permeate collected by the fourth storage tank 34, then, enabling the permeate to enter the third filtering membrane 4, collecting the permeate from the third permeate side 42 of the third filtering membrane 4 in two parts, wherein part of the permeate enters the fifth storage tank 43, the other part of the permeate 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 positioned on the third retentate side 41 of the third filtering membrane 4 is returned to the second filtering membrane 3, and the permeate collected in the sixth storage tank 44 is a target product.
Example 1:
1000kg of raw materials are heated to 40 ℃ from a raw material tank 1 and enter a first filtering membrane 2, permeate liquid from a first permeation side 22 of the first filtering membrane 2 is collected in two parts, 20kg of permeate liquid is collected in one part and enters a first storage tank 23, the other part of permeate liquid enters a second storage tank 24, permeate liquid collected in the first storage tank 23 and retentate liquid positioned on a first retentate side 21 of the first filtering membrane 2 are returned to the raw material tank 1, and 50kg of permeate liquid remains in the raw material tank 1 as raffinate liquid; continuing to heat the permeate in the second storage tank 24 to 40 ℃ and then entering the second filtering membrane 3, collecting the permeate coming out of the second permeate side 32 of the second filtering membrane 3 in two parts, collecting 20kg of permeate and then entering the third storage tank 33, and the other part of permeate entering the fourth storage tank 34, returning the permeate collected by the third storage tank 33 to the raw material tank 1, and returning the retentate located on the second retentate side 31 of the second filtering membrane 3 to the first filtering membrane 2; the permeate collected in the fourth storage tank 34 is heated to 40 ℃ and enters the third filtering membrane 4, the permeate coming out of the third permeate side 42 of the third filtering membrane 4 is collected in two parts, 20kg of permeate is collected and enters the fifth storage tank 43, the other part of permeate 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 on the third retentate side 41 of the third filtering membrane 4 is returned to the second filtering membrane 3, and the permeate collected in the sixth storage tank 44 is the target product.
The first filtering membrane 2 adopts an organic tubular composite membrane, the first layer is PP with the aperture of 500nm, and the second layer is PTFE with the average aperture of 20 nm; the filter shell and the storage tank of the first filter membrane 2 are made of high-purity PP.
The second filtering membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with the aperture of 500nm, and the second layer is PTFE with the average aperture of 20 nm; the filter shell and the storage tank of the second filter membrane 3 are made of high-purity PVDF.
The third filtering membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with the aperture of 500nm, and the second layer is PTFE with the average aperture of 20 nm; the filter shell and the storage tank of the secondary membrane are made of high-purity PFA.
The first filtering membrane 2, the second filtering membrane 3 and the third filtering membrane 4 all adopt a polydimethyl siloxane composite membrane modified by polyamide as an effective separating layer, the pressure of the permeation side of the membrane is 3000Pa, the content of isopropanol is 99.95%, and the experimental results are shown in table 1.
Example 2:
1000kg of raw materials are heated to 60 ℃ from a raw material tank 1 and enter a first filtering membrane 2, permeate liquid from a first permeation side 22 of the first filtering membrane 2 is collected in two parts, 50kg of permeate liquid is collected in one part and enters a first storage tank 23, the other part of permeate liquid enters a second storage tank 24, permeate liquid collected in the first storage tank 23 and retentate liquid positioned on a first retentate side 21 of the first filtering membrane 2 are returned to the raw material tank 1, and 200kg of permeate liquid remains in the raw material tank 1 as raffinate liquid; continuing to heat the permeate in the second storage tank 24 to 60 ℃ and then entering the second filtering membrane 3, collecting the permeate from the second permeate side 32 of the second filtering membrane 3 in two parts, collecting 50kg of permeate, entering the third storage tank 33, and the other part of permeate entering the fourth storage tank 34, returning the permeate collected by the third storage tank 33 to the raw material tank 1, and returning the retentate located on the second retentate side 31 of the second filtering membrane 3 to the first filtering membrane 2; the permeate collected in the fourth tank 34 is heated to 60 ℃ and enters the third filtering membrane 4, the permeate coming out of the third permeate side 42 of the third filtering membrane 4 is collected in two parts, 50kg of permeate is collected and enters the fifth tank 43, the other part of permeate enters the sixth tank 44, the permeate collected in the fifth tank 43 is returned to the raw material tank 1, the retentate located on the third retentate side 41 of the third filtering membrane 4 is returned to the second filtering membrane 3, and the permeate collected in the sixth tank 44 is the target product.
The first filtering membrane 2 adopts an organic tubular composite membrane, the first layer is PP with the aperture of 1000nm, and the second layer is PTFE with the average aperture of 100nm; the filter shell and the storage tank of the first filter membrane 2 are made of high-purity PP.
The second filtering membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with the aperture of 1000nm, and the second layer is PTFE with the average aperture of 100nm; the filter shell and the storage tank of the second filter membrane 3 are made of high-purity PVDF.
The third filtering membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with the aperture of 1000nm, and the second layer is PTFE with the average aperture of 100nm; the filter shell and the storage tank of the secondary membrane are made of high-purity PFA.
The first filtering membrane 2, the second filtering membrane 3 and the third filtering membrane 4 all adopt a polydimethyl siloxane composite membrane modified by polyamide as an effective separating layer, the pressure of the permeation side of the membrane is 8000Pa, the content of isopropanol is 99.98%, and the experimental results are shown in table 1.
Example 3:
1000kg of raw materials are heated to 50 ℃ from a raw material tank 1 and enter a first filtering membrane 2, permeate liquid from a first permeation side 22 of the first filtering membrane 2 is collected in two parts, 30kg of permeate liquid is collected in one part and enters a first storage tank 23, the other part of permeate liquid enters a second storage tank 24, permeate liquid collected in the first storage tank 23 and retentate liquid positioned on a first retentate side 21 of the first filtering membrane 2 are returned to the raw material tank 1, and 100kg of permeate liquid remains in the raw material tank 1 as raffinate liquid; continuing to heat the permeate in the second storage tank 24 to 50 ℃ and then entering the second filtering membrane 3, collecting the permeate from the second permeate side 32 of the second filtering membrane 3 in two parts, collecting 30kg of permeate, entering the third storage tank 33, and the other part of permeate entering the fourth storage tank 34, returning the permeate collected by the third storage tank 33 to the raw material tank 1, and returning the retentate located on the second retentate side 31 of the second filtering membrane 3 to the first filtering membrane 2; the permeate collected in the fourth tank 34 is heated to 50 ℃ and enters the third filtering membrane 4, the permeate coming out of the third permeate side 42 of the third filtering membrane 4 is collected in two parts, 30kg of permeate is collected and enters the fifth tank 43, the other part of permeate enters the sixth tank 44, the permeate collected in the fifth tank 43 is returned to the raw material tank 1, the retentate located on the third retentate side 41 of the third filtering membrane 4 is returned to the second filtering membrane 3, and the permeate collected in the sixth tank 44 is the target product.
The first filtering membrane 2 adopts an organic tubular composite membrane, the first layer is PP with the aperture of 800nm, and the second layer is PTFE with the average aperture of 50 nm; the filter shell and the storage tank of the first filter membrane 2 are made of high-purity PP.
The second filtering membrane 3 adopts an organic tubular composite membrane, the first layer is PVDF with the aperture of 800nm, and the second layer is PTFE with the average aperture of 50 nm; the filter shell and the storage tank of the second filter membrane 3 are made of high-purity PVDF.
The third filtering membrane 4 adopts an organic tubular composite membrane, the first layer is PFA with the aperture of 800nm, and the second layer is PTFE with the average aperture of 50 nm; the filter shell and the storage tank of the secondary membrane are made of high-purity PFA.
The first filtering membrane 2, the second filtering membrane 3 and the third filtering membrane 4 all adopt a polydimethyl siloxane composite membrane modified by polyamide as an effective separating layer, the pressure of the permeation side of the membrane is 5000Pa, the content of isopropanol is 99.96%, and the experimental results are shown in table 1.
Table 1 example experiment results comparison table
From the above table it follows: compared with the conventional rectification scheme, the technical scheme of the invention greatly improves the effect of removing metal ions in isopropanol.
The beneficial effects are that:
1. the invention adopts the three-stage membrane system to remove metal ions and particles at the same time, and compared with the traditional multi-effect rectification and ultrafiltration membrane to remove the particles, the invention simplifies the process, reduces the equipment occupation area and the equipment height, and is suitable for large-scale industrial production.
2. The invention adopts the polydimethyl siloxane composite membrane modified by the polyamide, the adopted operation condition does not reach the boiling point of feed liquid, the permeation side is in a gaseous state, and the invention has good removing property for metal ions; meanwhile, the three filtering membranes are compact membranes, and have good removal effect on particulate matters.
3. The systems of different layers of membranes respectively adopt high-purity PP, PVDF, PFA materials, so that not only is the investment cost reduced, but also the requirement that the contact materials do not produce dissolved matters in the wet electronic chemical production is met.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. An ultra-clean high-purity isopropyl alcohol production device, which is characterized by comprising:
a raw material tank (1) for storing isopropyl alcohol to be processed;
a first filter membrane (2), the first inlet (20) of which is connected to the outlet (11) of the raw material tank (1), and the first retentate side (21) of which is connected to the inlet (10) of the raw material tank (1);
a second filter membrane (3), the second inlet (30) of which is connected to the first permeate side (22) of the first filter membrane (2), and the second retentate side (31) of which is connected to the first inlet (20) of the first filter membrane (2);
a third filter membrane (4), wherein a third inlet (40) of the third filter membrane is connected with a second permeation side (32) of the second filter membrane (3), a third residual permeation side (41) of the third filter membrane is connected with a second inlet (30) of the second filter membrane (3), and a target product is obtained from a third permeation side (42);
a heating assembly (5) for heating the isopropanol to be processed at the first inlet (20), the second inlet (30) and the third inlet (40);
and a condensing assembly (6) for condensing isopropyl alcohol to be processed at the first permeate side (22), the second permeate side (32) and the third permeate side (42).
2. The ultra-clean high-purity isopropyl alcohol production device according to claim 1, wherein the first filtering membrane (2), the second filtering membrane (3) and the third filtering membrane (4) are all composite membranes.
3. The ultra-clean high-purity isopropyl alcohol production device according to claim 1 or 2, wherein the first filtering membrane (2) 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 polydimethyl siloxane composite membrane modified with polyamide.
4. The ultra-clean high-purity isopropyl alcohol production apparatus according to claim 1 or 2, wherein the second filtering membrane (3) 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 with a polyammonified chitosan.
5. The ultra-clean high-purity isopropyl alcohol production apparatus according to claim 1 or 2, wherein the third filtering membrane (4) 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 polydimethyl siloxane composite membrane modified with a polyamide.
6. Ultra-clean high purity isopropyl alcohol production device according to claim 1, characterized in that the heating assembly (5) comprises:
a first heater (50) having an inlet connected to the output (11) of the feed tank (1) and an outlet connected to the first inlet (20) of the first filter membrane (2);
a second heater (51) with its inlet connected to the first permeate side (22) of the first filter membrane (2) and its outlet connected to the second inlet (30) of the second filter membrane (3);
-a third heater (52) with its inlet connected to the second permeate side (32) of the second filter membrane (3) and its outlet connected to the third inlet (40) of the third filter membrane (4).
7. The ultra-clean high purity isopropyl alcohol production apparatus according to claim 6, characterized in that the condensation assembly (6) comprises:
a first condenser (60) with its inlet connected to the first permeate side (22) of the first filter membrane (2) and its outlet connected to the inlet of the second heater (51);
a second condenser (61) with its inlet connected to the second permeate side (32) of the second filter membrane (3) and its outlet connected to the inlet of the third heater (52);
a third condenser (62) with an inlet connected to a third permeate side (42) of the third filter membrane (4);
and a vacuum pump (63) connected to the first condenser (60), the second condenser (61), and the third condenser (62) at the same time.
8. The ultra-clean high purity isopropyl alcohol production apparatus according to claim 7, further comprising:
a second 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 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);
and a sixth tank (44) having an inlet connected to the outlet of the third condenser (62) and an outlet outputting the product.
9. The ultra-clean high purity isopropyl alcohol production apparatus according to claim 7, further comprising:
the inlet of the first storage tank (23) is connected with the outlet of the first condenser (60), and the outlet of the first storage tank 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), and the outlet of the third storage tank is connected with the input port (10) of the raw material tank (1);
and 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 is connected with the input port (10) of the raw material tank (1).
10. The production method of the ultra-clean high-purity isopropanol is characterized by comprising the following steps of:
the isopropanol to be processed enters the first filtering membrane (2) after being heated from the storage tank, the permeate liquid coming out of the first permeation side (22) of the first filtering membrane (2) is collected in two parts, part of the permeate liquid enters the first storage tank (23), the other part of the permeate liquid enters the second storage tank (24), the permeate liquid collected by the first storage tank (23) and the retentate liquid positioned on the first retentate side (21) of the first filtering membrane (2) are returned to the raw material tank (1), and part of the liquid remained in the raw material tank (1) is used as the raffinate liquid;
heating the permeate collected by the second storage tank (24) and then entering the second filtering membrane (3), collecting the permeate coming out of the second permeate side (32) of the second filtering membrane (3) in two parts, wherein part of the permeate enters the third storage tank (33), the other part of the permeate enters the fourth storage tank (34), the permeate collected by the third storage tank (33) returns to the raw material tank (1), and the retentate positioned on the second retentate side (31) of the second filtering membrane (3) returns to the first filtering membrane (2);
the permeate collected by the fourth storage tank (34) enters the third filtering membrane (4) after being heated, the permeate coming out of the third permeation side (42) of the third filtering membrane (4) is collected in two parts, part of the permeate enters the fifth storage tank (43), the other part of the permeate enters the sixth storage tank (44), the permeate collected by the fifth storage tank (43) returns to the raw material tank (1), the retentate positioned on the third permeation side (41) of the third filtering membrane (4) returns to the second filtering membrane (3), and the permeate collected in the sixth storage tank (44) is a target product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310580591.3A CN116651212A (en) | 2023-05-19 | 2023-05-19 | Ultra-clean high-purity isopropanol production device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310580591.3A CN116651212A (en) | 2023-05-19 | 2023-05-19 | Ultra-clean high-purity isopropanol production device and method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116651212A true CN116651212A (en) | 2023-08-29 |
Family
ID=87716413
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310580591.3A Pending CN116651212A (en) | 2023-05-19 | 2023-05-19 | Ultra-clean high-purity isopropanol production device and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116651212A (en) |
-
2023
- 2023-05-19 CN CN202310580591.3A patent/CN116651212A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20090057128A1 (en) | Liquid separation by membrane assisted vapor stripping process | |
| JP6289852B2 (en) | Liquid organic matter and water separation system and separation method | |
| JP5793157B2 (en) | Solution processing equipment | |
| JP2011050860A (en) | Anhydrization method of hydrated organic substance | |
| JP6636111B2 (en) | Organic solvent purification system and method | |
| JPH0634898B2 (en) | Concentrator / dehydrator for organic / aqueous mixed solutions | |
| CN110938047A (en) | Tetrahydrofuran-benzene-water mixture separation process and device | |
| CN113912019A (en) | Production method of electronic grade hydrogen peroxide aqueous solution | |
| CN101559993A (en) | Method for removing trace alcohol in organic wastewater | |
| CN219942404U (en) | Ultra-clean high-purity isopropanol production device | |
| CN116651212A (en) | Ultra-clean high-purity isopropanol production device and method | |
| CN100408531C (en) | Process for producing high concentration tert-butyl alcohol by permeation vaporization method and products therefrom | |
| CN219032050U (en) | Production system of ultra-clean high-purity isopropanol | |
| CN111909120B (en) | Energy-saving separation process of water-containing ternary azeotropic system | |
| CN113233434B (en) | Production process and production device of electronic-grade nitric acid | |
| CN215667785U (en) | Octamethylcyclotetrasiloxane purification equipment | |
| CN219424122U (en) | Preparation facilities of high-purity N-ethyl pyrrolidone | |
| CN113943209B (en) | Method and device for purifying isopropanol waste liquid | |
| CN217828928U (en) | Production device of ultra-pure methanol | |
| CN106986769B (en) | Separation and integration system and separation and integration method of ethyl acetate-water system | |
| CN214361095U (en) | Energy-saving separation device of water-containing ternary azeotropic system | |
| CN216777947U (en) | Continuous purification device containing ethanolamine and dimethyl sulfoxide recovery liquid | |
| JPH0832294B2 (en) | Compressor system equipped with a device for continuously purifying hydraulic fluid | |
| CN115006864A (en) | Production device and method of ultra-pure methanol | |
| KR101256613B1 (en) | Recovery of high purity phosphoric acid from mixed waste acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |