CN112723994A - Purification method of semiconductor grade isopropanol - Google Patents
Purification method of semiconductor grade isopropanol Download PDFInfo
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- CN112723994A CN112723994A CN202011614988.2A CN202011614988A CN112723994A CN 112723994 A CN112723994 A CN 112723994A CN 202011614988 A CN202011614988 A CN 202011614988A CN 112723994 A CN112723994 A CN 112723994A
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- isopropanol
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- raw material
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000000746 purification Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000004065 semiconductor Substances 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 239000012528 membrane Substances 0.000 claims abstract description 15
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- 208000005156 Dehydration Diseases 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000001728 nano-filtration Methods 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 239000008139 complexing agent Substances 0.000 claims description 9
- 239000012024 dehydrating agents Substances 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010533 azeotropic distillation Methods 0.000 claims description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 claims description 6
- 239000012629 purifying agent Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- RXTCWPTWYYNTOA-UHFFFAOYSA-N O=P1OCCCCCO1 Chemical compound O=P1OCCCCCO1 RXTCWPTWYYNTOA-UHFFFAOYSA-N 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 3
- -1 amine trimethyl phosphate Chemical class 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001223 reverse osmosis Methods 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 7
- 238000004140 cleaning Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 150000001450 anions Chemical class 0.000 abstract description 3
- 150000001768 cations Chemical class 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- UXYAJXBVMZFRMS-UHFFFAOYSA-N 2-hydroxy-1,3,2$l^{5}-dioxaphosphepane 2-oxide Chemical compound OP1(=O)OCCCCO1 UXYAJXBVMZFRMS-UHFFFAOYSA-N 0.000 description 1
- 241001550224 Apha Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000013527 degreasing agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
-
- 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
- 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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
-
- 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
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a purification method of semiconductor grade isopropanol, which comprises the steps of carrying out ion purification and dehydration treatment on an industrial grade isopropanol raw material, finely controlling the rectification temperature, strictly controlling the azeotropic point and stripping the water in the isopropanol raw material. And the water and the plasma in the fraction are further intercepted through the extraction tower, and the concentration of the isopropanol is increased. In addition, a nanofiltration membrane is arranged at the inlet of the final purification collector, so that the cooled isopropanol is further purified of particle impurities, and the purity and quality of the isopropanol are further improved. The isopropanol obtained by the method has the main body content of 99.99 percent, the water content of less than 50ppm, the cation content of less than 0.1ppb and the anion content of less than 50ppb, meets the 12-grade standard of chemical materials established by international semiconductor equipment and material organizations, and can be used for cleaning, drying and the like in the assembling and processing processes of semiconductors and large-scale integrated circuits.
Description
Technical Field
The invention relates to the technical field of semiconductor-grade isopropanol, in particular to a purification method of semiconductor-grade isopropanol.
Background
Since the first discovery by the father faraday of electronics of british scientists in 1833 that the resistance of silver sulfide decreases with increasing temperature, a semiconductor phenomenon, research and applications on semiconductors have been developed. Generally, a semiconductor (semiconductor) refers to a material having a conductive property between a conductor (semiconductor) and an insulator (insulator) at normal temperature. The production of semiconductors typically goes through three major processes, tape-out, packaging and testing, wherein the tape-out process includes the manufacturing processes of dicing, lapping, polishing, epitaxy, oxidation, etc. In these semiconductor manufacturing processes, since the machine table, the operation panel, and the like are kept clean and free of contamination, it is necessary to use an appropriate cleaning agent. Isopropyl alcohol, which is freely miscible with water, has a stronger solubility for lipophilic substances than ethanol, and is a preferred cleaning degreaser in the electronics industry.
With the development of the information industry, the demand for semiconductor production and manufacturing is higher and higher, and the purity of isopropyl alcohol used is also higher and higher. The existing isopropanol is mainly obtained from the azeotrope with high purity by a distillation method. Because the water content of the isopropanol obtained by the method is too high to meet the requirement, the document proposes that industrial isopropanol is used as a raw material, carbonate is used for adjusting the pH value, a dehydrating agent is added for reflux reaction, and then the isopropanol meeting the requirement is obtained through the working procedures of distillation, rectification, filtration and the like. However, the quality of the product prepared by the preparation method is not stable, and the product contains metal ions and various particle impurities which are not suitable for the production requirement of semiconductors. Therefore, how to obtain isopropanol which meets the production requirements of semiconductors becomes one of the important problems in the production of conductors at present.
Disclosure of Invention
In order to achieve the purpose, the invention provides the following technical scheme: a process for purifying semiconductor grade isopropanol, comprising the steps of:
s1, adjusting the pH value: adjusting the pH value of an industrial grade isopropanol raw material with the content of 98% to 5.5-7.5 by using carbonate;
s2, ion purification treatment: adding a metal ion purifying agent accounting for 0.5-5 wt% of the weight of the isopropanol raw material into a purifying processor for purification reaction for 30-120 min;
s3, dehydration treatment: adding a dehydrating agent into the purified isopropanol raw material, and then carrying out dehydration reaction for 4 hours under a reflux state;
s4, azeotropic distillation: introducing the dehydrated isopropanol raw material into a rectifying tower, strictly controlling the rectifying temperature, and finely separating isopropanol and water;
s5, extraction and filtration: introducing a product subjected to azeotropic distillation into an extraction tower, wherein an extraction filter membrane is arranged at the bottom of the extraction tower, and further stripping moisture and ions in the fraction;
s6, recovery and purification: and introducing the fraction extracted and filtered by the extraction tower into a recovery tower, cooling and condensing the fraction by a condensing system in the tower, and then introducing the fraction into a purification collector to obtain the semiconductor grade isopropanol.
The carbonate is sodium carbonate or sodium bicarbonate or a mixture of the two.
The carbonate is a mixture of sodium carbonate and sodium bicarbonate, and the mass ratio of the mixture of the sodium carbonate and the sodium bicarbonate is as follows: 1:1.5.
And adjusting the pH value of the isopropanol raw material to be 6-7.
The ion purifying agent is an organic phosphonate ion complexing agent.
The organic phosphonate ion complexing agent is one of ethylene diamine tetra methylene sodium phosphate, diethylene triamine penta methylene phosphonate or amine trimethyl phosphate.
The dehydrating agent is a mixture of silica gel and magnesium sulfate, and the mass ratio of the mixture of the silica gel and the magnesium sulfate is as follows: 1:2.
The rectification temperature is controlled as follows: under the protection of nitrogen, starting at 50 ℃ and keeping for 2 min; then heating to 82 ℃ at the speed of 5 ℃/min, and keeping for 5 min; then raising the temperature to 82.45 ℃ at the speed of 0.05 ℃/min, and rectifying and separating the water.
The extraction filter membrane at the bottom of the extraction tower is a reverse osmosis membrane which is three layers, an ion complexing agent is filled between the lowest layer and the middle layer, and calcium carbonate is filled between the middle layer and the uppermost layer.
And a nanofiltration membrane with the aperture of 0.5-1.5 nm is arranged at the inlet of the purification collector.
Compared with the prior art, the invention has the beneficial effects that: after industrial-grade isopropanol raw material is subjected to ion purification and dehydration treatment, the water in the isopropanol raw material is stripped by finely controlling the rectification temperature and strictly controlling the azeotropic point. And the water and the plasma in the fraction are further intercepted through the extraction tower, and the concentration of the isopropanol is increased. In addition, a nanofiltration membrane is arranged at the inlet of the final purification collector, so that the cooled isopropanol is further purified of particle impurities, and the purity and quality of the isopropanol are further improved. The isopropanol obtained by the method has the main body content of 99.99 percent, the water content of less than 50ppm, the cation content of less than 0.1ppb and the anion content of less than 50ppb, meets the 12-grade standard of chemical materials established by international semiconductor equipment and material organizations, and can be used for cleaning, drying and the like in the assembling and processing processes of semiconductors and large-scale integrated circuits.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a purification method of semiconductor grade isopropanol comprises the following steps: adjusting the pH value: firstly, the pH value of industrial grade isopropanol raw material with the content of 98% is adjusted to 5.5-7.5 by using carbonate, wherein the carbonate is sodium carbonate or sodium bicarbonate or a mixture of the sodium carbonate and the sodium bicarbonate. In this embodiment, the carbonate is a mixture of sodium carbonate and sodium bicarbonate, and the mass ratio of the mixture of the sodium carbonate and the sodium bicarbonate is as follows: 1:1.5, adjusting the pH value of the isopropanol raw material to 6.5, and performing ion purification treatment: adding a metal ion purifying agent accounting for 0.5-5 wt% of the weight of the isopropanol raw material into a purifying processor for purification reaction for 30-120 min; the ion purifying agent is an organic phosphonate ion complexing agent and comprises one of ethylene diamine tetra methylene sodium phosphate, diethylene triamine penta methylene phosphonate or amine trimethylene phosphate. In this embodiment, the organic phosphonate ion complexing agent is sodium ethylene diamine tetra methylene phosphate, and the dehydration treatment comprises: adding a dehydrating agent into the purified isopropanol raw material, and then carrying out dehydration reaction for 4 hours under a reflux state. In the embodiment, the dehydrating agent is a mixture of silica gel and magnesium sulfate, the mass ratio of the mixture of the silica gel and the magnesium sulfate is 1:2, and the azeotropic distillation is as follows: introducing the dehydrated isopropanol raw material into a rectifying tower, strictly controlling the rectifying temperature, and finely separating isopropanol and water; the rectification temperature is controlled as follows: under the protection of nitrogen, starting at 50 ℃ and keeping for 2 min; then heating to 82 ℃ at the speed of 5 ℃/min, and keeping for 5 min; then raising the temperature to 82.45 ℃ at the speed of 0.05 ℃/min, rectifying and separating water, extracting and filtering: and then introducing a product subjected to azeotropic distillation into an extraction tower, wherein the bottom of the extraction tower is provided with an extraction filter membrane, the extraction filter membrane is a reverse osmosis membrane and is three layers, an ion complexing agent is filled between the lowest layer and the middle layer, calcium carbonate is filled between the middle layer and the uppermost layer, the water and ions in the fraction are further stripped, and the recovery and purification are carried out: and introducing the fraction extracted and filtered by the extraction tower into a recovery tower, cooling and condensing the fraction by a condensation system in the tower, and then introducing the fraction into a purification collector, wherein a nanofiltration membrane with the aperture of 0.5-1.5 nm is arranged at the inlet of the purification collector, so as to obtain the semiconductor grade isopropanol.
The method comprises the steps of carrying out ion purification and dehydration treatment on an industrial-grade isopropanol raw material, finely controlling the rectification temperature and strictly controlling the azeotropic point, and stripping the water in the isopropanol raw material. And the water and the plasma in the fraction are further intercepted through the extraction tower, and the concentration of the isopropanol is increased. In addition, a nanofiltration membrane is arranged at the inlet of the final purification collector, so that the cooled isopropanol is further purified of particle impurities, and the purity and quality of the isopropanol are further improved. The isopropanol obtained by the method has the main body content of 99.99 percent, the water content of less than 50ppm, the cation content of less than 0.1ppb and the anion content of less than 50ppb, meets the 12-grade standard of chemical materials established by international semiconductor equipment and material organizations, and can be used for cleaning, drying and the like in the assembling and processing processes of semiconductors and large-scale integrated circuits. TABLE 1
| Item | Unit of | SEMI C12 Standard | Examples | Remarks for note |
| Color intensity | APHA | 10 | 1 | |
| Content of isopropyl alcohol | ％ | ＞99.8 | 99.99 | |
| Water content | ppm | ＜50 | 30 | |
| Evaporation of residue | ppm | ＜1 | 0.3 | |
| Chloride (CL) | ppb | ＜50 | 5 | |
| Nitrate salt | ppb | ＜50 | 15 | |
| (phosphoric) acid salt | ppb | ＜50 | 20 | |
| (thio) acid salt | ppb | ＜50 | 20 | |
| (aluminum (A) l) | ppb | ＜0.1 | 0.03 | |
| Lithium (Li) | ppb | ＜0.1 | 0.05 | |
| Sodium ((Na) | ppb | ＜0.1 | 0.06 | |
| Magnesium (Mg) | ppb | ＜0.1 | 0.05 | |
| Aluminum (Al) | ppb | ＜0.1 | 0.03 | |
| Potassium (K) | ppb | ＜0.1 | 0.04 | |
| Calcium (Ca) | ppb | ＜0.1 | 0.08 | |
| Chromium (Cr) | ppb | ＜0.1 | 0.05 | |
| Manganese (Mn) | ppb | ＜0.1 | 0.03 | |
| Iron (Fe) | ppb | ＜0.1 | 0.08 | |
| Nickel (Ni) | ppb | ＜0.1 | 0.01 | |
| Cobalt (Co) | ppb | ＜0.1 | 0.01 | |
| Copper (Cu) | ppb | ＜0.1 | 0.01 | |
| Zinc (Zn) | ppb | ＜0.1 | 0.03 | |
| Molybdenum (Mo) | ppb | ＜0.1 | 0.02 | |
| Cadmium (Cd) | ppb | ＜0.1 | 0.02 | |
| Lead ((Pb) | ppb | ＜0.1 | 0.04 | |
| Silver (Ag) | ppb | ＜0.1 | 0.02 |
The terms "central," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used for indicating orientations that are merely used for simplifying the description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the scope of the present invention.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method of purifying semiconductor grade isopropanol, characterized by: the method comprises the following steps:
s1, adjusting the pH value: adjusting the pH value of an industrial grade isopropanol raw material with the content of 98% to 5.5-7.5 by using carbonate;
s2, ion purification treatment: adding a metal ion purifying agent accounting for 0.5-5 wt% of the weight of the isopropanol raw material into a purifying processor for purification reaction for 30-120 min;
s3, dehydration treatment: adding a dehydrating agent into the purified isopropanol raw material, and then carrying out dehydration reaction for 4 hours under a reflux state;
s4, azeotropic distillation: introducing the dehydrated isopropanol raw material into a rectifying tower, strictly controlling the rectifying temperature, and finely separating isopropanol and water;
s5, extraction and filtration: introducing a product subjected to azeotropic distillation into an extraction tower, wherein an extraction filter membrane is arranged at the bottom of the extraction tower, and further stripping moisture and ions in the fraction;
s6, recovery and purification: and introducing the fraction extracted and filtered by the extraction tower into a recovery tower, cooling and condensing the fraction by a condensing system in the tower, and then introducing the fraction into a purification collector to obtain the semiconductor grade isopropanol.
2. The method of claim 1, wherein the purification process comprises: the carbonate is sodium carbonate or sodium bicarbonate or a mixture of the two.
3. The method of claim 1, wherein the purification process comprises: the carbonate is a mixture of sodium carbonate and sodium bicarbonate, and the mass ratio of the mixture of the sodium carbonate and the sodium bicarbonate is as follows: 1:1.5.
4. The method of claim 1, wherein the purification process comprises: and adjusting the pH value of the isopropanol raw material to be 6-7.
5. The method of claim 2, wherein the purification process comprises: the ion purifying agent is an organic phosphonate ion complexing agent.
6. The method of claim 5, wherein the purification process comprises: the organic phosphonate ion complexing agent is one of ethylene diamine tetra methylene sodium phosphate, diethylene triamine penta methylene phosphonate or amine trimethyl phosphate.
7. The method of claim 3, wherein the purification process comprises: the dehydrating agent is a mixture of silica gel and magnesium sulfate, and the mass ratio of the mixture of the silica gel and the magnesium sulfate is as follows: 1:2.
8. The method of claim 4, wherein the purification process comprises: the rectification temperature is controlled as follows: under the protection of nitrogen, starting at 50 ℃ and keeping for 2 min; then heating to 82 ℃ at the speed of 5 ℃/min, and keeping for 5 min; then raising the temperature to 82.45 ℃ at the speed of 0.05 ℃/min, and rectifying and separating the water.
9. The method of claim 5, wherein the purification process comprises: the extraction filter membrane at the bottom of the extraction tower is a reverse osmosis membrane which is three layers, an ion complexing agent is filled between the lowest layer and the middle layer, and calcium carbonate is filled between the middle layer and the uppermost layer.
10. The method of claim 6, wherein the purification process comprises: and a nanofiltration membrane with the aperture of 0.5-1.5 nm is arranged at the inlet of the purification collector.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113968773A (en) * | 2021-11-15 | 2022-01-25 | 江苏三贵资源再生有限公司 | Method for separating isopropanol and water by extractive distillation |
| CN114470958A (en) * | 2022-02-15 | 2022-05-13 | 北京袭明科技有限公司 | Production method and device of high-purity electronic grade methanol |
| CN114748885A (en) * | 2022-05-20 | 2022-07-15 | 北京化工大学 | Production device and production process of electronic grade isopropanol |
| CN114870420A (en) * | 2022-02-15 | 2022-08-09 | 北京袭明科技有限公司 | Method and device for producing high-purity electronic grade isopropanol |
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Application publication date: 20210430 |