CN113735697A - Continuous production method of semiconductor grade acetone - Google Patents
Continuous production method of semiconductor grade acetone Download PDFInfo
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- CN113735697A CN113735697A CN202110979768.8A CN202110979768A CN113735697A CN 113735697 A CN113735697 A CN 113735697A CN 202110979768 A CN202110979768 A CN 202110979768A CN 113735697 A CN113735697 A CN 113735697A
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 title claims abstract description 284
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000004065 semiconductor Substances 0.000 title claims abstract description 35
- 238000010924 continuous production Methods 0.000 title claims abstract description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000000895 extractive distillation Methods 0.000 claims abstract description 61
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229920001721 polyimide Polymers 0.000 claims abstract description 31
- 150000001768 cations Chemical class 0.000 claims abstract description 27
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 26
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 23
- 239000004642 Polyimide Substances 0.000 claims abstract description 22
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 20
- 150000001450 anions Chemical class 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000008096 xylene Substances 0.000 claims abstract description 17
- 239000012528 membrane Substances 0.000 claims abstract description 12
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007800 oxidant agent Substances 0.000 claims abstract description 7
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 21
- 229920001429 chelating resin Polymers 0.000 claims description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 125000003944 tolyl group Chemical group 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000000605 extraction Methods 0.000 description 23
- 238000003860 storage Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 13
- 238000004821 distillation Methods 0.000 description 11
- 239000012535 impurity Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 235000012431 wafers Nutrition 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-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
- 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
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 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
- 239000013626 chemical specie Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 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
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012476 oxidizable substance Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 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
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
- C07C45/83—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation by extractive distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous production method of semiconductor grade acetone, which comprises the following steps of: adding industrial acetone into a first extractive distillation tower, taking ethylene glycol as a first extractant and ozone as an oxidant, carrying out reaction and extractive distillation, collecting the acetone from the top of the tower, introducing the acetone into a second extractive distillation tower, carrying out extractive distillation by using a second extractant, and collecting the acetone from the top of the tower; anion exchange resin is adopted for treatment to remove anions, and then a modified polyimide membrane is adopted for filtration to remove partial metal cations and particles; leading the acetone into a third extractive distillation tower, extracting and rectifying the acetone by using a third extractant, and extracting the acetone from the tower top; and (3) treating by using cation exchange resin to remove cations, filtering to obtain semiconductor grade acetone, wherein the second extractant and the third extractant are one or a combination of more than one selected from xylene, toluene and cyclohexane, and the method can be used for producing high-purity acetone meeting the SEMIC12 standard in a large scale.
Description
Technical Field
The invention belongs to the technical field of production of reagents for semiconductor grade, and particularly relates to a continuous production method of semiconductor grade acetone.
Background
Semiconductor grade reagents generally meet the purity requirements of electronic grade reagents according to SEMI standards, including, for example, SEMI C1 standard, SEMI C2 standard, SEMI C7 standard, SEMI C8 standard, SEMI C12 standard (corresponding to the so-called SEMI G5 standard), and the like, and require low to high impurity levels, including, but not limited to, metallic impurity levels, the higher the purity of the electronic grade reagents, the less the effect on semiconductor processing.
With the higher integration of chips, the requirements for semiconductor products are more and more strict. Semiconductor manufacturing requires the wafer surface to be as clean as possible, and many times it is difficult to do this completely, when the wafer is washed with an aqueous solution and then dried, often resulting in stains that leave undesirable residues on the surface that can cause defects in the manufacturing process, whereas semiconductor grade acetone in electronic grade reagents can now be used for moisture removal on smaller wafers (e.g., 6 "and 8" inches), and as IC storage capacity increases, the oxide film that is the insulating layer becomes thinner, alkali impurities in the electronic chemical species can dissolve into the oxide film, resulting in a decrease in the insulating voltage; heavy metal impurities adhere to the surface of the silicon wafer and lower the P-N junction withstand voltage, and therefore, the purity of the semiconductor grade acetone directly affects the electrical performance, yield, and reliability of the chip.
The main methods for producing acetone include isopropanol method, cumene method, fermentation method, acetylene hydration method and propylene direct oxidation method, and the produced crude acetone contains impurities such as alcohol, aldehyde, phenol, water, metal ions and anions (chloride ions, sulfate radicals and the like). The main methods for purifying acetone include physical and chemical methods or a combination of the two methods, however, the current methods for purifying acetone mainly have the following problems: 1. the purity requirement of semiconductor grade, especially SEMI C12 standard, can not be met; 2. a large amount of corrosive strong base, expensive metal or noble metal catalyst is used in the refining process; 3. the rectifying tower is too high to achieve high purity, the energy consumption is high, and the cost is difficult to reduce; 4. the production takes long time, which is not beneficial to controlling the cost, etc.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a continuous production method of high-purity acetone which can be produced in large scale and meets the SEMI C12 standard.
In order to achieve the purpose, the invention adopts the technical scheme that:
a continuous production method of semiconductor grade acetone adopts industrial acetone as a starting material, and comprises the following steps in sequence:
(1) adding industrial acetone into a first extractive distillation tower, reacting and carrying out extractive distillation by using ethylene glycol as a first extracting agent and ozone as an oxidant, and extracting the acetone from the top of the tower;
(2) introducing the acetone obtained in the step (1) into a second extractive distillation tower, extracting and rectifying by adopting a second extracting agent, and extracting the acetone from the tower top; wherein the second extractant is one or more selected from xylene, toluene and cyclohexane;
(3) treating the acetone obtained in the step (2) by using anion exchange resin to remove anions, and then filtering by using a modified polyimide membrane to remove partial metal cations and particles;
(4) introducing the acetone obtained after the treatment in the step (3) into a third extractive distillation tower, carrying out extractive distillation by adopting a third extractant, and extracting the acetone from the top of the tower; wherein the third extractant is one or more selected from xylene, toluene and cyclohexane;
(5) and (3) treating the acetone obtained after the treatment in the step (4) by using a cation exchange resin to remove cations, and then filtering to obtain the semiconductor grade acetone, wherein the mass content of single metal cations in the semiconductor grade acetone is below 0.02 ppb.
The starting material in the present invention is commercially available as industrial acetone.
According to some preferred aspects of the present invention, in step (1), the first extractant and the oxidizing agent are added in the following manner: ozone is firstly dissolved in ethylene glycol to obtain a mixed solution, and then the mixed solution is added into the first extractive distillation tower.
Further, the mass fraction of ozone in the mixed solution is 5% -20%, and the addition mass of the mixed solution accounts for 10% -50% of the addition mass of the industrial acetone.
According to some preferred aspects of the present invention, in the step (1), the top temperature of the first extractive distillation column is controlled to be 53.5 to 59.5 ℃, the reflux ratio is controlled to be 2 to 8, and the bottom temperature is controlled to be 75 to 95 ℃.
According to some preferred aspects of the present invention, in the step (2), the overhead temperature of the second extractive distillation column is controlled to be 54.5 to 58.5 ℃, the reflux ratio is controlled to be 2 to 8, and the bottom temperature is controlled to be 75 to 95 ℃.
According to some preferred aspects of the present invention, in the step (4), the theoretical plate number of the third extractive distillation column is controlled to be 25 to 40, the inlet of the acetone obtained after the treatment in the step (3) is 5 to 10 stages of plates, the temperature at the top of the column is 55.5 to 57.5 ℃, the temperature at the bottom of the column is 70 to 90 ℃, and the pressure is 0.02 to 0.15 MPa.
According to some preferred aspects of the invention, in step (2), the added mass of the second extractant accounts for 5% to 35% of the mass of acetone obtained in step (1).
According to some preferred aspects of the invention, in step (4), the added mass of the third extractant accounts for 5% -35% of the mass of acetone obtained in step (3).
According to some preferred aspects of the invention, the second extractant is different from the third extractant. According to a particular aspect of the invention, the second extractant is xylene and the third extractant is toluene.
According to some preferred aspects of the invention, in step (3), the anion exchange resin is basic, including but not limited to a combination of one or more selected from DuPont Amberlite IRA 96RF, DuPont Amberlite IRA402Cl, Dusheng CXO-12.
According to some preferred aspects of the invention, in step (5), the cation exchange resin is acidic, including but not limited to a combination of one or more selected from DuPont Amberlite IR1200Na, DuPont Amberjet 1600, Langshan Lewatit TP 207.
According to some preferred aspects of the present invention, in the step (3), a plurality of modified polyimide membranes are sequentially connected in series and in parallel to form a modified polyimide module, and the anion exchange resin-treated acetone is allowed to pass at a pressure of 1 to 4MPa and a passing speed of 20 to 80L/(m) at2H) passing through the modified polyimide die set to remove a portion of the metal cations and particles.
Further, the modified polyimide film includes, but is not limited to, PW8040F from GE, Kapton FN from DuPont, Purem Flux from Wingchun, Germany.
According to some preferred aspects of the present invention, in the step (5), the material of the filter element material used for filtration is polytetrafluoroethylene, and the pore size is 30-50 nm.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
based on the defects of the existing method for purifying acetone, the invention adopts a multi-step fractional purification process, removes oxidizable substances, alcohols and impurities with strong hydrophilicity which are close to the boiling point of acetone by selecting a specific first extracting agent and matching with ozone, then removes impurities such as hydrocarbons and the like which are close to the boiling point of acetone by adopting a specific second extracting agent, then respectively removes anions and partial metal cations and particles by combining with an anion exchange resin and a modified polyimide membrane which are sequentially arranged, and performs extractive rectification by combining with a specific third extracting agent again, and based on the treatment steps, a rectifying tower adopted by the third extractive rectification can adopt tower plates with lower numbers, thereby saving energy, finally adopts cation exchange resin to treat to remove cations, and then filters, the content of acetone in the obtained semiconductor grade acetone reaches more than 99.9 percent, the mass content of single metal cations is below 0.02ppb, the content of each single anion is below 0.1ppm, and the water content is below 800 ppm. Compared with the prior art, the product obtained by the method has stable quality, meets or even exceeds the requirements of SEMI C12 standard, and can be used for removing moisture of semiconductor wafers. Moreover, the production efficiency is high, the energy utilization efficiency is high, the energy consumption is low, and the cost is obviously reduced.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a continuous production apparatus for semiconductor grade acetone according to an embodiment of the present invention;
1. a first extractive distillation column; 2. a second extractive distillation column; 3. an anion exchange resin tank; 4. a modified polyimide film high pressure tank; 5. a third extractive distillation column; 6. a cation exchange resin tank; 7. and (4) a particle processing filter element tank.
Detailed Description
The invention takes commercially available industrial acetone as raw material to prepare the semiconductor grade acetone with purity meeting the SEMI C12 standard. The process is mainly characterized in that three-stage extractive distillation is adopted, and anion-removing resin and a modified polyimide membrane for removing metal cations are arranged between the second-stage extractive distillation and the third-stage extractive distillation, so that the energy consumption of the third-stage extractive distillation tower is greatly reduced, the load is reduced, and a foundation is laid for obtaining high-purity acetone. Meanwhile, specific extracting agents are respectively adopted in the three-stage extraction and rectification, the extracting agents are wide in source and low in price, and the extraction effect on impurities is excellent through three-stage independent step-by-step treatment. Compared with the prior art, the technical progress is mainly shown in the following aspects:
firstly, the quality of high-purity acetone is greatly improved, the content of the acetone is up to more than 99.9 percent, the mass content of single metal cations is below 0.02ppb, the content of each single anion is lower than 0.1ppm, the water content is lower than 800ppm, and the purity meets the SEMI C12 standard;
secondly, the energy consumption of the high-purity acetone is reduced, the height of the rectifying tower is reduced, expensive metal or noble metal catalyst is not needed, and the cost is reduced;
thirdly, substances such as high-corrosivity strong base and the like are avoided, and the safety production is greatly improved;
fourthly, the production time is short, the impurity removal processing time of each stage is shortened, and the cost is further reduced.
Further, the continuous production method of semiconductor grade acetone comprises the steps of sequentially carrying out primary extractive distillation (taking ethylene glycol as a first extracting agent and ozone as an oxidizing agent), secondary extractive distillation (taking one or a combination of more of xylene, toluene and cyclohexane as an extracting agent), anion removal by using an anion exchange resin, partial metal cations and particles removal by using a modified polyimide membrane, tertiary extractive distillation (taking one or a combination of more of xylene, toluene and cyclohexane as an extracting agent), cation removal by using a cation exchange resin, and filtration. As shown in FIG. 1, the process of the present invention can be carried out in a continuous production apparatus as shown in the figure.
As shown in fig. 1, the production apparatus comprises a first extractive distillation column 1, a second extractive distillation column 2, an anion exchange resin tank 3, a modified polyimide membrane high-pressure tank 4, a third extractive distillation column 5, a cation exchange resin tank 6, and a particle treatment cartridge tank 7, which are arranged in sequence; the first extractive distillation column 1, the second extractive distillation column 2 and the third extractive distillation column 5 are all plate columns.
Wherein, in the first extractive distillation tower 1, industrial grade glycol with purity not lower than 98% and no component with boiling point lower than 100 ℃ is adopted as an extracting agent, and industrial ozone with purity not lower than 99% is adopted as an oxidant, and the ozone is in a gas form, while the extracting agent glycol can better dissolve the ozone, so the ozone can be dissolved in the glycol and then added together in a solution form. Furthermore, the mass fraction of ozone in the mixed solution formed by dissolving ozone in ethylene glycol is 5% -20%, the adding mass of the mixed solution accounts for 10% -50% of the adding mass of industrial acetone, acetone is extracted from the top of the first extractive distillation tower 1, and ethylene glycol containing impurities is extracted from the bottom of the tower.
According to some embodiments of the invention, the top temperature of the first extractive distillation column is controlled to be 57.5-58.5 ℃, the reflux ratio is controlled to be 2-8, and the bottom temperature is controlled to be 82-90 ℃. When the mixed solution formed by dissolving ozone in ethylene glycol is added into the first extraction and rectification tower 1, the total reflux is carried out for 0.5-2h, the fraction at the top of the tower is extracted, the fraction with the required temperature for extraction enters the second extraction and rectification tower 2, and other fractions can be stored in a material storage tank or returned to an acetone raw material storage tank to be combined with the acetone raw material for use.
The second extractive distillation tower 2 adopts one or more of xylene, toluene and cyclohexane as an extracting agent, preferably, in a specific aspect of the invention, xylene is adopted as the extracting agent adopted by the second extractive distillation tower 2, the xylene is industrial xylene with purity not lower than 99% and no component with boiling point lower than that of xylene, the adding amount of the industrial xylene accounts for 5% -35% of the mass of acetone obtained after the treatment of the first extractive distillation tower 1, acetone is adopted at the tower top of the second extractive distillation tower 2, and xylene containing impurities is extracted from the tower bottom.
According to some embodiments of the invention, the overhead temperature of the second extractive distillation column is controlled to be 56.5-57.5 ℃, the reflux ratio is 3-5, the temperature of the bottom of the column is 80-90 ℃, the total reflux is 0.5-2h, the overhead fraction is extracted, the temperature fraction required by extraction is fed into an anion exchange resin tank 3 to remove anions, and then acetone treated by anion exchange resin is led to pass through the anion exchange resin at the pressure of 1-4MPa and the passing speed of 20-80L/(m & lt/m & gt2H) through a modified polyimide film high pressure tank 4 (provided with a modified polyimide module formed by connecting a plurality of modified polyimide films in series and in parallel in sequence), and removing part of metal cations and particles. Further, the anion exchange resin is selected from basic anion exchange resins, and specifically can be selected from the following, but not limited to: amberlite IRA 96RF, DuPont Amberlite IRA402Cl, Dusheng CXO-12; the modified polyimide film may be selected from the group including, but not limited to, the following: PW8040F from GE, USA, Kapton FN from DuPont, Germany, Purem Flux from Wingchun.
The third extractive distillation tower 5 adopts one or more of xylene, toluene and cyclohexane as an extracting agent, and preferably, in one specific aspect of the invention, toluene is adopted as the extracting agent adopted by the third extractive distillation tower 5, the toluene is industrial toluene with the purity of not less than 99% and no component with the boiling point lower than that of the toluene, and the adding amount of the industrial toluene accounts for 5% -35% of the mass of acetone obtained after the treatment of the modified polyimide film high-pressure tank 4. Furthermore, the third extractive distillation tower 5 can realize the purification of acetone only by adopting 25-40 theoretical plates, and has excellent purification effect, meanwhile, in the invention, the acetone obtained after the treatment of the modified polyimide film high-pressure tank 4 enters from the 5-10 stages of plates of the third extractive distillation tower 5, the temperature of the tower top is 55.5-57.5 ℃, the temperature of the tower bottom is 70-90 ℃, and the pressure is 0.02-0.15 MPa.
In the invention, the second extractant and the third extractant are preferably controlled to be different, so that different extractants are respectively adopted in the three-stage extractive distillation, thereby realizing equivalent variable-pressure distillation effect to a certain extent and improving the purification effect.
According to some embodiments of the present invention, the acetone obtained after the treatment in the third extractive distillation column 5 is treated with a cation exchange resin tank, preferably an acidic cation exchange resin, which may contain strongly acidic reactive groups such as sulfonic acid groups (-SO), for further removal of metal cations3H) And the like, and particularly, the cation exchange resin may be selected from the following, including but not limited to: amberlite IR1200Na, dupont Amberjet 1600, lang Lewatit TP 207.
According to some embodiments of the present invention, the acetone treated by the cation exchange resin is subjected to particle removal by using a particle treatment filter cartridge tank, wherein the material of the filter cartridge used in the particle treatment filter cartridge tank is Polytetrafluoroethylene (PTFE), and the pore diameter is preferably 30-50nm, and further can be 40 nm.
In the invention, the sequence of the steps can not be changed, and practice proves that the acetone can be purified according to the sequence of the invention to obtain better effect.
The method for detecting the content of acetone in the semiconductor grade acetone adopts Shimadzu gas chromatography; the moisture detection is carried out by using a Karl-Fischer moisture meter of Mettler-Torlo; the metal ion test is completed by ICP-MS8900 of Agilent, and the anions are detected by Agilent anion detection equipment.
The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or may be prepared by methods conventional in the art. The results of the detection of industrial acetone used in the following examples are shown in table 1 below.
TABLE 1
| Detecting items | Unit of | The result of the detection | Detecting items | Unit of | The result of the detection |
| Content (wt.) | ％ | 98.5 | Copper (Cu) | ppb | 0.2 |
| Water (W) | ppm | 2578 | Zinc (Zn) | ppb | 0.1 |
| Cl- | ppb | 1690 | Gallium (Ga) | ppb | 0.01 |
| SO4 2- | ppb | 1320 | Germanium (Ge) | ppb | 0.02 |
| Sodium (Na) | ppb | 2.5 | Arsenic (As) | ppb | 0.08 |
| Magnesium (Mg) | ppb | 0.5 | Strontium (Sr) | ppb | 0.01 |
| Aluminum (Al) | ppb | 0.1 | Zirconium (Zr) | ppb | 0.01 |
| Potassium (K) | ppb | 0.4 | Niobium (Nb) | ppb | 0.01 |
| Calcium (Ca) | ppb | 0.6 | Molybdenum (Mo) | ppb | 0.03 |
| Titanium (Ti) | ppb | 0.9 | Silver (Ag) | ppb | 0.01 |
| Vanadium (V) | ppb | 0.1 | Cadmium (Cd) | ppb | 0.01 |
| Chromium (Cr) | ppb | 0.2 | Tin (Sn) | ppb | 0.05 |
| Manganese (Mn) | ppb | 0.01 | Antimony (Sb) | ppb | 0.03 |
| Iron (Fe) | ppb | 0.7 | Barium (Ba) | ppb | 0.01 |
| Cobalt (Co) | ppb | 0.02 | Thallium (Tl) | ppb | 0.01 |
| Nickel (Ni) | ppb | 0.4 | Lead (Pb) | ppb | 0.02 |
Example 1
500 kg of industrial acetone is added into a first extractive distillation tower, and simultaneously ozone is dissolved in glycol to obtain a mixed solution (the mixed solution comprises glycol accounting for 25 percent of the mass of the industrial acetone)125 kg and 12.5 kg of ozone) is added into the first extraction and rectification tower, the temperature at the top of the tower is controlled at 58.0 ℃, the distillate at the top of the tower is extracted after the total reflux is carried out for 1 hour, the reflux ratio is 6, and the temperature at the bottom of the tower is 85 ℃. Fractions with the temperature below 56.5 ℃ are extracted and returned to the raw material storage tank. 425 kg of fractions at the temperature of between 56.5 and 58.0 ℃ are extracted and enter a second extraction rectifying tower, 50 kg of dimethylbenzene is added into the second extraction rectifying tower, the tower top temperature is controlled at 57.0 ℃, after total reflux is carried out for 1 hour, the fractions at the tower top are extracted, the reflux ratio is 5, and the tower kettle temperature is 80 ℃. Collecting fractions below 56.5 deg.C, and returning to raw material storage tank. 360 kilograms of distillate acetone products with the temperature of 56.5 to 57.5 ℃ are extracted; the acetone product extracted from the tower top enters an anion exchange resin treatment tank (the anion exchange resin is Amberlite IRA 96RF), after anions are removed, the acetone product enters a modified polyimide module (the modified polyimide membrane adopts PW8040F of GE company of America) through a high-pressure pump, the pressure is 2.5 +/-1 MPa, and the pressure is 30-60L/(m2H), then entering a third extractive distillation tower with 29 stages of tower plates, wherein the inlet is the 6 th stage tower plate, the temperature of the tower bottom of the distillation tower is 80 ℃, the pressure is 0.08MPa, the temperature of the distillation outlet (the tower top) is 56.5 ℃, the extracting agent is toluene, the adding amount is 10 kg, the distilled acetone solution enters a cation resin exchange tank (the cation exchange resin is DuPont Amberlite IR1200Na), after removing cations in acetone, enters a particle control tank (the filter core aperture is 40nm) provided with a PTFE filter core, and after controlling particles, the finally needed high-purity acetone product is obtained, and the detection result of the high-purity acetone product is shown in Table 2.
Example 2
500 kg of industrial acetone is added into a first extraction and rectification tower, and simultaneously, a mixed solution obtained by dissolving ozone in ethylene glycol (the mixed solution comprises 100 kg of ethylene glycol accounting for 20% of the mass of the industrial acetone and 10 kg of ozone) is added into the first extraction and rectification tower, the temperature of the tower top is controlled at 58.5 ℃, after total reflux is carried out for 1 hour, fraction at the tower top is extracted, the reflux ratio is 6, and the temperature of a tower kettle is 90 ℃. Fractions with the temperature below 56.5 ℃ are extracted and returned to the raw material storage tank. 400 kg of fractions at the temperature of 56.5-58.5 ℃ are extracted and enter a second extraction and rectification tower: 30 kg of dimethylbenzene is added into the second extractive distillation tower. Tower with a tower bodyThe top temperature is controlled at 57.5 ℃, after one hour of total reflux, fraction at the top of the tower is extracted, the reflux ratio is 5, and the temperature of the bottom of the tower is 80 ℃. Collecting fractions below 56.5 deg.C, and returning to raw material storage tank. 320 kilograms of distillate acetone products with the temperature of 56.5 to 57.5 ℃ are extracted; the acetone product extracted from the tower top enters a storage tank (DuPont Amberlite IRA402Cl) filled with anion exchange resin, after anion is removed, the acetone product enters a modified polyimide module (the modified polyimide membrane adopts Kapton FN of DuPont company in America) through a high-pressure pump, the pressure is 2.5 +/-1 Mpa, and the pressure is 40-70L/(m)2H) and then enters a third extractive distillation tower with 32 stages of tower plates, wherein the extracting agent is toluene, the inlet is the 7 th stage of tower plate, the temperature of the tower bottom of the distillation tower is set to be 80 ℃, the pressure is 0.07MPa, and the temperature of the distillation outlet (tower top) is set to be 56.5 ℃. The rectified acetone solution passes through a storage tank filled with cation exchange resin (DuPont Amberjet 1600 is the cation exchange resin), after cations are removed, the acetone solution enters a particle control tank filled with a PTFE filter element (the aperture of the filter element is 40nm), and after particles are controlled, the finally needed high-purity acetone product is obtained, and the detection result of the high-purity acetone product is shown in Table 2.
Example 3
Adding 500 kg of industrial acetone into a first extraction and rectification tower, simultaneously adding a mixed solution (the mixed solution comprises 75 kg of ethylene glycol accounting for 15% of the mass of the industrial acetone and 7.5 kg of ozone) obtained by dissolving the ozone in the ethylene glycol into the first extraction and rectification tower, controlling the temperature at the top of the tower at 57.5 ℃, carrying out total reflux for 1 hour, and then starting to extract fraction at the top of the tower, wherein the reflux ratio is 6, and the temperature at the bottom of the tower is 88 ℃. Fractions with the temperature below 56.5 ℃ are extracted and returned to the raw material storage tank. And (3) extracting 350 kg of fractions at the temperature of between 56.5 and 57.5 ℃, and feeding the fractions into a second extraction and rectification tower: adding 50 kg of dimethylbenzene into the second extractive distillation tower, controlling the temperature at the top of the tower to be 57.0 ℃, fully refluxing for one hour, then starting to extract the fraction at the top of the tower, wherein the reflux ratio is 5, the temperature at the bottom of the tower is 85 ℃, extracting the fraction below 56.5 ℃, and returning the fraction to the raw material storage tank. 280 kg of fraction acetone products at the temperature of between 56.5 and 57.5 ℃ are extracted; the acetone product extracted from the tower top enters an anion exchange resin tank (anion exchange resin is DuPont Amberlite IRA402Cl), after the anion is removed, the acetone product enters a modified polyimide through a high-pressure pumpThe amine module (the modified polyimide film adopts PureMem Flux of Germany winning and creating company), the pressure is 2.5 +/-1 Mpa, and the pressure is 30-60L/(m)2H) and then entering a third extractive distillation tower with 35 stages, wherein the extracting agent is toluene, the inlet is a 9 th stage tower plate, the temperature of the distillation tower (tower bottom) is set to be 85 ℃, the pressure is 0.07MPa, and the temperature of the distillation outlet (tower top) is set to be 57.0 ℃. And (3) feeding the rectified acetone solution into a cation exchange resin tank (DuPont Amberjet 1600), removing cations, and finally feeding the acetone solution into a particle control tank (the aperture of a filter element is 40nm) provided with a PTFE filter element, and removing particles to obtain the finally required high-purity acetone product, wherein the detection result of the high-purity acetone product is shown in Table 2.
Comparative example 1
500 kg of industrial acetone is added into a first extraction and rectification tower, a mixed solution obtained by dissolving ozone in toluene (the mixed solution comprises 125 kg of toluene accounting for 25% of the mass of the industrial acetone and 12.5 kg of ozone) is added into the first extraction and rectification tower, the tower top temperature is controlled at 58.0 ℃, after total reflux is carried out for 1 hour, fraction at the tower top is extracted, the reflux ratio is 6, and the tower kettle temperature is 85 ℃. Fractions with the temperature below 56.5 ℃ are extracted and returned to the raw material storage tank. 420 kg of fractions at the temperature of 56.5-58.0 ℃ are extracted and enter a second extraction rectifying tower, 50 kg of methylbenzene is added into the second extraction rectifying tower, the tower top temperature is controlled at 57.0 ℃, after total reflux is carried out for 1 hour, the fractions at the tower top are extracted, the reflux ratio is 5, and the tower kettle temperature is 80 ℃. Collecting fractions below 56.5 deg.C, and returning to raw material storage tank. 320 kilograms of distillate acetone products with the temperature of 56.5 to 57.5 ℃ are extracted; the acetone product extracted from the tower top enters an anion exchange resin treatment tank (the anion exchange resin is Amberlite IRA 96RF), after anions are removed, the acetone product enters a modified polyimide module (the modified polyimide membrane adopts PW8040F of GE company of America) through a high-pressure pump, the pressure is 2.5 +/-1 MPa, and the pressure is 30-60L/(m2H), then enters a third extractive distillation tower with 29 stages of tower plates, the inlet is a 6 th stage tower plate, the temperature of the tower bottom of the distillation tower is set to be 80 ℃, the pressure is 0.08MPa, the temperature of the distillation outlet (tower top) is set to be 56.5 ℃, the extractant is toluene, the adding amount is 10 kg, and the rectified acetone solution enters a cation resin exchange tank (cation exchange resin)Dupont Amberlite IR1200Na), removing cations in acetone, entering a particle control tank (with filter element aperture of 40nm) equipped with a PTFE filter element, controlling particles, and obtaining the final required high-purity acetone product, wherein the detection results of the high-purity acetone product are shown in Table 2.
Comparative example 2
500 kg of industrial acetone is added into a first extraction and rectification tower, a mixed solution (the mixed solution comprises 125 kg of glycol accounting for 25 percent of the mass of the industrial acetone and 12.5 kg of ozone) obtained by dissolving the ozone in toluene is added into the first extraction and rectification tower, the temperature of the tower top is controlled at 58.0 ℃, after total reflux is carried out for 1 hour, fraction at the tower top is extracted, the reflux ratio is 6, and the temperature of a tower kettle is 85 ℃. Fractions with the temperature below 56.5 ℃ are extracted and returned to the raw material storage tank. 425 kg of fractions at the temperature of between 56.5 and 58.0 ℃ are extracted and enter a second extraction rectifying tower, 50 kg of ethylene glycol is added into the second extraction rectifying tower, the tower top temperature is controlled at 57.0 ℃, after total reflux is carried out for 1 hour, the fractions at the tower top are extracted, the reflux ratio is 5, and the tower kettle temperature is 80 ℃. Collecting fractions below 56.5 deg.C, and returning to raw material storage tank. 350 kg of distillate acetone products with the temperature of 56.5-57.5 ℃ are extracted; the acetone product extracted from the tower top enters an anion exchange resin treatment tank (the anion exchange resin is Amberlite IRA 96RF), after anions are removed, the acetone product enters a modified polyimide module (the modified polyimide membrane adopts PW8040F of GE company of America) through a high-pressure pump, the pressure is 2.5 +/-1 MPa, and the pressure is 30-60L/(m2H), then entering a third extractive distillation tower with 29 stages of tower plates, wherein the inlet is the 6 th stage tower plate, the temperature of the tower bottom of the distillation tower is set to be 80 ℃, the pressure is 0.08MPa, the temperature of the distillation outlet (the tower top) is set to be 56.5 ℃, the extracting agent is ethylene glycol, the adding amount is 10 kg, the distilled acetone solution enters a cation resin exchange tank (the cation exchange resin is DuPont Amberlite IR1200Na), after removing cations in acetone, enters a particle control tank (the pore diameter of a filter element is 40nm) provided with a PTFE filter element, and after controlling particles, the finally needed high-purity acetone product is obtained, and the detection result of the high-purity acetone product is shown in Table 2.
TABLE 2 examination results of the high purity acetone products obtained in examples 1 to 3 and comparative examples 1 to 2
As can be seen from Table 2, the high purity acetone product prepared by the method of the present invention has an acetone content of 99.9% or more, a mass content of single metal cations of 0.02ppb or less, a content of each single anion of less than 0.1ppm, a water content of less than 800ppm, and a purity meeting the SEMI C12 standard.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (10)
1. A continuous production method of semiconductor grade acetone adopts industrial acetone as a starting material, and is characterized by comprising the following steps of:
(1) adding industrial acetone into a first extractive distillation tower, reacting and carrying out extractive distillation by using ethylene glycol as a first extracting agent and ozone as an oxidant, and extracting the acetone from the top of the tower;
(2) introducing the acetone obtained in the step (1) into a second extractive distillation tower, extracting and rectifying by adopting a second extracting agent, and extracting the acetone from the tower top; wherein the second extractant is one or more selected from xylene, toluene and cyclohexane;
(3) treating the acetone obtained in the step (2) by using anion exchange resin to remove anions, and then filtering by using a modified polyimide membrane to remove partial metal cations and particles;
(4) introducing the acetone obtained after the treatment in the step (3) into a third extractive distillation tower, carrying out extractive distillation by adopting a third extractant, and extracting the acetone from the top of the tower; wherein the third extractant is one or more selected from xylene, toluene and cyclohexane;
(5) and (3) treating the acetone obtained after the treatment in the step (4) by using a cation exchange resin to remove cations, and then filtering to obtain the semiconductor grade acetone, wherein the mass content of single metal cations in the semiconductor grade acetone is below 0.02 ppb.
2. The continuous production method of semiconductor grade acetone according to claim 1, wherein in step (1), the first extractant and the oxidant are added in a manner that: ozone is firstly dissolved in ethylene glycol to obtain a mixed solution, and then the mixed solution is added into the first extractive distillation tower.
3. The continuous production method of semiconductor grade acetone according to claim 2, wherein the mass fraction of ozone in the mixed solution is 5% -20%, and the addition mass of the mixed solution accounts for 10% -50% of the addition mass of industrial acetone.
4. The continuous production method of semiconductor grade acetone according to claim 1, wherein in the step (1), the top temperature of the first extractive distillation column is controlled to be 53.5-59.5 ℃, the reflux ratio is controlled to be 2-8, and the bottom temperature of the column is controlled to be 75-95 ℃;
in the step (2), the tower top temperature of the second extractive distillation tower is controlled to be 54.5-58.5 ℃, the reflux ratio is controlled to be 2-8, and the tower kettle temperature is controlled to be 75-95 ℃;
in the step (4), the theoretical plate number of the third extractive distillation tower is controlled to be 25-40, the inlet of the acetone obtained after the treatment in the step (3) is a 5-10-stage plate, the tower top temperature is 55.5-57.5 ℃, the tower bottom temperature is 70-90 ℃, and the pressure is 0.02-0.15 MPa.
5. The continuous production method of semiconductor grade acetone according to claim 1, wherein in the step (2), the added mass of the second extractant accounts for 5-35% of the mass of acetone obtained in the step (1);
in the step (4), the adding mass of the third extracting agent accounts for 5-35% of the mass of the acetone obtained in the step (3).
6. The continuous production method of semiconductor grade acetone according to claim 1, wherein the second extractant is different from the third extractant.
7. The continuous production method of semiconductor grade acetone according to claim 1 or 6, wherein the second extractant is xylene and the third extractant is toluene.
8. The continuous production method of semiconductor grade acetone according to claim 1, wherein in step (3), the anion exchange resin is weakly basic, and the anion exchange resin is one or more selected from DuPont Amberlite IRA 96RF, DuPont Amberlite IRA402Cl, and Dusheng CXO-12; in the step (5), the cation exchange resin is strongly acidic, and the cation exchange resin is one or more of DuPont Amberlite IR1200Na, DuPont Amberjet 1600 and Langshan Lewatit TP 207; in the step (5), the material of the filter element material adopted for filtering is polytetrafluoroethylene, and the aperture is 30-50 nm.
9. The continuous production method of semiconductor grade acetone according to claim 1, wherein in the step (3), the modified polyimide modules are prepared by sequentially stacking a plurality of modified polyimide films, and the acetone treated with the anion exchange resin is subjected to a treatment under a pressure of 1 to 4MPa,The passing speed is 20-80L/(m)2H) passing through the modified polyimide die set to remove a portion of the metal cations and particles.
10. The continuous production method of semiconductor grade acetone according to claim 1, wherein the semiconductor grade acetone is produced with a water content of less than 800ppm and a content of individual anions of less than 0.1 ppm.
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