CN113429262A - Preparation method of high-purity isopropanol - Google Patents
Preparation method of high-purity isopropanol Download PDFInfo
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- CN113429262A CN113429262A CN202110667406.5A CN202110667406A CN113429262A CN 113429262 A CN113429262 A CN 113429262A CN 202110667406 A CN202110667406 A CN 202110667406A CN 113429262 A CN113429262 A CN 113429262A
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- raw material
- isopropanol
- complexing agent
- positive pressure
- material tank
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 58
- 239000008139 complexing agent Substances 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 38
- 208000005156 Dehydration Diseases 0.000 claims description 18
- 230000018044 dehydration Effects 0.000 claims description 18
- 238000006297 dehydration reaction Methods 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 238000005086 pumping Methods 0.000 description 10
- 239000012024 dehydrating agents Substances 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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- 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
- C07C29/94—Use of additives, e.g. for stabilisation
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a high-purity isopropanol preparation method, which comprises adhering metal ions in isopropanol by complexing agent to make them settle, sucking complexing agent into automatic piston assembly from the outer side of raw material tank, pushing complexing agent quantitatively into raw material tank by automatic piston assembly to combine with isopropanol raw material, adding complexing agent into operation process by automatic piston assembly to avoid mixing with external impurities, providing reliable and convenient conditions for preparing high-purity isopropanol, mixing complexing agent by positive pressure mixer, generating positive pressure in the mixture of raw material tank by positive pressure mixer to make the mixture flow continuously to realize uniform mixing, and mixing with stirring paddle type mechanical mixing, can ensure that other impurities are not introduced into the raw material tank, and further provides reliable convenient conditions for preparing the high-purity isopropanol.
Description
Technical Field
The invention relates to the technical field of preparation methods of high-purity isopropanol, in particular to a preparation method of high-purity isopropanol.
Background
With the rapid development of semiconductor technology, the requirement for ultra-clean and high-purity reagents is higher and higher. In the process of processing an integrated circuit, the ultra-clean high-purity reagent is mainly used for cleaning and etching the surfaces of a chip and a silicon wafer, and the purity and the cleanliness of the ultra-clean high-purity reagent have great influence on the yield, the electrical property and the reliability of the integrated circuit. As an important microelectronic chemical, ultra-clean and high-purity isopropanol is widely used for cleaning, drying and the like in the processes of semiconductors and large-scale integrated circuits. As the processing size of the integrated circuit enters the submicron deep submicron era, higher requirements are put on the matched ultra-clean high-purity isopropanol.
At present, ultra-clean high-purity isopropanol is usually prepared by purifying and refining industrial grade isopropanol serving as a raw material, and rectification is a main method for industrially purifying the isopropanol and comprises azeotropic rectification, extractive rectification and the like. But for micro
The requirements of ultra-clean high-purity isopropanol in the electronic chemical industry on the particle size content of metal impurities and anions are very strict, and the rectification process can not meet the requirements, so that the preparation method of the high-purity isopropanol is provided.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity isopropanol, which comprises the following steps:
1) inputting an industrial grade isopropanol raw material into a raw material tank, and inputting a complexing agent into the raw material tank, wherein the complexing agent is input in a mode of adopting an automatic piston assembly, the complexing agent is sucked into the automatic piston assembly from the outer side of the raw material tank, and the complexing agent is quantitatively pushed out into the raw material tank by the automatic piston assembly in a mode of pushing a piston to be combined with the isopropanol raw material;
2) a positive pressure mixer is arranged in the raw material tank, positive pressure is generated in the mixture in the raw material tank through the work of the positive pressure mixer, the mixture is enabled to continuously flow to realize uniform mixing of the mixture, the mixture is kept stand after being mixed, part of complex compounds descend to the bottom of the raw material tank, and the mixture at the upper part is input into a dehydration processor for dehydration treatment;
3) after the dehydration is finished, the material continues to enter a micro filter for filtration, and after the material is filtered by the micro filter, the material enters a rectifying tower for rectification;
4) after the rectification, the material enters a nano-filter for filtration, and high-purity isopropanol is obtained after the filtration by the nano-filter.
Preferably, the automatic piston assembly comprises a material pumping pipe, the material pumping pipe fixedly penetrates through the upper wall of the raw material tank, a piston is arranged in the material pumping pipe, one end of a piston rod is fixedly connected to the side wall of the piston, the other end of the piston rod is fixedly connected with the output end of an electric telescopic rod, the fixed end of the electric telescopic rod is fixed to the upper side of the material pumping pipe through a support, the output end of the material pumping pipe is connected with a material inlet pipe, the material pumping pipe and the material inlet pipe are both provided with electric control valves, when a complexing agent needs to be input into the raw material tank, the electric control valve at the output end of the material pumping pipe is firstly closed, the piston rod and the piston are driven to move upwards through the work of the electric telescopic rod, the complexing agent enters the material pumping pipe along the material inlet pipe, then the electric control valve on the material inlet pipe is closed, and the electric control valve at the output end of the material pumping pipe is opened, through electric telescopic handle work drives piston rod and piston move down, push the complexing agent in the raw materials jar, automatic piston assembly makes the complexing agent pan feeding process sealed relatively, prevents effectively that external impurity from sneaking into.
Preferably, the malleation blender includes annular pipe fitting, annular pipe fitting fixed connection in on the inside wall of head tank, the venthole has evenly been seted up on the annular pipe fitting, the one end of intake pipe is still connected on the annular pipe fitting, the other end of intake pipe is located the outside of head tank, with inert gas source with intake-tube connection, gaseous edge the intake pipe gets into annular pipe fitting discharges along the venthole, stirs mixture intensive mixing in the head tank, this kind of mixed mode compares in the mechanical mixing of stirring paddle formula, can guarantee not to introduce other impurity in the head tank, further provides reliable convenient condition for preparing high-purity isopropanol.
Preferably, the positive pressure gas used in the positive pressure mixer is an inert gas.
The invention has the beneficial effects that: the complexing agent is used for adhering metal ions in the isopropanol to enable the metal ions to be settled, the content of the metal ions in the isopropanol is effectively removed, the complexing agent is added by adopting an automatic piston assembly, the complexing agent is sucked into the automatic piston assembly from the outer side of a raw material tank, the automatic piston assembly quantitatively pushes the complexing agent out of the raw material tank in a piston pushing mode to be combined with the isopropanol raw material, the automatic piston assembly enables the adding operation process of the complexing agent to be free from mixing of external impurities, reliable and convenient conditions are provided for preparing high-purity isopropanol, a positive pressure mixer is adopted in the mixing mode of the complexing agent, and the positive pressure mixer works, produce the malleation in the head tank mixture, make the mixture constantly flow in order to realize the even mixture of mixture, this kind of mixing mode contrast in the mechanical mixing of stirring paddle formula, can guarantee not to introduce other impurity in to the head tank, further provide reliable convenient condition for preparing high-purity isopropanol.
Drawings
FIG. 1 is a flow chart of the process for the preparation of high purity isopropanol of the present invention.
In the figure: 1-raw material tank, 2-automatic piston assembly, 201-pumping pipe, 202-piston, 203-piston rod, 204-electric telescopic rod, 205-bracket, 206-feeding pipe, 3-positive pressure mixer, 301-annular pipe fitting, 302-air inlet pipe, 4-dewatering processor, 5-micro filter, 6-rectifying tower, 7-nano filter, water outlet pipe, and water outlet pipe,
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1:
1) inputting 100 parts of industrial grade isopropanol raw material into a raw material tank 1, and then inputting 0.5 part of complexing agent into the raw material tank 1, wherein the complexing agent is input in a mode of adopting an automatic piston assembly 2, the complexing agent is sucked into the automatic piston assembly 2 from the outer side of the raw material tank, and the automatic piston assembly 2 quantitatively pushes the complexing agent out of the raw material tank 1 in a mode of pushing a piston to be combined with the isopropanol raw material;
2) a positive pressure mixer 3 is arranged in the raw material tank 1, positive pressure is generated in a mixture in the raw material tank 1 by the operation of the positive pressure mixer 3, the mixture is enabled to continuously flow to realize uniform mixing of the mixture, the mixing time is 10min, the mixture is kept stand after being mixed, part of complex compound is reduced to the bottom of the raw material tank, the mixture at the upper part is input into a dehydration processor 4 for dehydration, the addition amount of a dehydrating agent is 1 part, the used dehydrating agent is a molecular sieve, and the temperature of the dehydration processor 4 is 60 ℃;
3) after the dehydration is finished, the material continuously enters a micro-filter 5 for filtration under the pressure condition of 0.15Mpa, the aperture of the micro-filter is 0.5 mu m in the micro-filter 5, the material is rectified in a rectifying tower 6 after being filtered by the micro-filter 5, the material used in the rectifying tower is high-purity quartz, the rectifying pressure is 0.1Ppa, the temperature is 50 ℃, and the reflux ratio is 0.5;
4) after the rectification, the material enters a nano filter 7 under the pressure of 0.5Mpa for filtration, and high-purity isopropanol is obtained after the filtration by the nano filter 7, wherein the aperture of a nano filter membrane in the nano filter 7 is 0.5 nm.
Example 2:
1) inputting 100 parts of industrial grade isopropanol raw material into a raw material tank 1, and then inputting 0.4 part of complexing agent into the raw material tank 1, wherein the complexing agent is input in a mode of adopting an automatic piston assembly 2, the complexing agent is sucked into the automatic piston assembly 2 from the outer side of the raw material tank, and the automatic piston assembly 2 quantitatively pushes the complexing agent out of the raw material tank 1 in a mode of pushing a piston to be combined with the isopropanol raw material;
2) a positive pressure mixer 3 is arranged in the raw material tank 1, positive pressure is generated in a mixture in the raw material tank 1 by the operation of the positive pressure mixer 3, the mixture is enabled to continuously flow to realize uniform mixing of the mixture, the mixing time is 12min, the mixture is kept stand after being mixed, part of complex compound is reduced to the bottom of the raw material tank, the mixture at the upper part is input into a dehydration processor 4 for dehydration, the addition amount of a dehydrating agent is 1 part, the used dehydrating agent is a molecular sieve, and the temperature of the dehydration processor 4 is 80 ℃;
3) after the dehydration is finished, the material continuously enters a micro-filter 5 for filtration under the pressure condition of 0.1Mpa, the aperture of the micro-filter is 0.5 mu m in the micro-filter 5, the material is rectified in a rectifying tower 6 after being filtered by the micro-filter 5, the material used in the rectifying tower is high-purity quartz, the rectifying pressure is 0.1Ppa, the temperature is 50 ℃, and the reflux ratio is 0.5;
4) after the rectification, the material enters a nano filter 7 under the pressure of 0.6Mpa for filtration, and high-purity isopropanol is obtained after the filtration by the nano filter 7, wherein the aperture of a nano filter membrane in the nano filter 7 is 0.5 nm.
Example 3
1) Inputting 100 parts of industrial grade isopropanol raw material into a raw material tank 1, and then inputting 0.6 part of complexing agent into the raw material tank 1, wherein the complexing agent is input in a mode of adopting an automatic piston assembly 2, the complexing agent is sucked into the automatic piston assembly 2 from the outer side of the raw material tank, and the automatic piston assembly 2 quantitatively pushes the complexing agent out of the raw material tank 1 in a mode of pushing a piston to be combined with the isopropanol raw material;
2) a positive pressure mixer 3 is arranged in the raw material tank 1, positive pressure is generated in a mixture in the raw material tank 1 by the operation of the positive pressure mixer 3, the mixture is enabled to continuously flow to realize uniform mixing of the mixture, the mixing time is 15min, the mixture is kept stand after being mixed, part of complex compound is reduced to the bottom of the raw material tank, the mixture at the upper part is input into a dehydration processor 4 for dehydration, the addition amount of a dehydrating agent is 1 part, the used dehydrating agent is a molecular sieve, and the temperature of the dehydration processor 4 is 70 ℃;
3) after the dehydration is finished, the material continuously enters a micro-filter 5 for filtration under the pressure condition of 0.12Mpa, the aperture of the micro-filter is 0.5 mu m in the micro-filter 5, the material is rectified in a rectifying tower 6 after being filtered by the micro-filter 5, the material used in the rectifying tower is high-purity quartz, the rectifying pressure is 0.1Ppa, the temperature is 50 ℃, and the reflux ratio is 0.5;
4) after the rectification, the material enters a nano filter 7 under the pressure of 0.7Mpa for filtration, and high-purity isopropanol is obtained after the filtration by the nano filter 7, wherein the aperture of a nano filter membrane in the nano filter 7 is 0.5 nm.
The impurities in the high-purity isopropanol in the examples were analyzed, and the technical indexes are shown in the following table
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A preparation method of high-purity isopropanol is characterized by comprising the following steps: the preparation method comprises the following steps:
1) inputting an industrial grade isopropanol raw material into a raw material tank (1), and then inputting a complexing agent into the raw material tank (1), wherein the complexing agent is input in a mode of adopting an automatic piston assembly (2), the complexing agent is sucked into the automatic piston assembly (2) from the outer side of the raw material tank, and the complexing agent is quantitatively pushed out into the raw material tank (1) by the automatic piston assembly (2) in a mode of pushing a piston to be combined with the isopropanol raw material;
2) a positive pressure mixer (3) is arranged in the raw material tank (1), positive pressure is generated in the mixture of the raw material tank (1) by the work of the positive pressure mixer (3), the mixture continuously flows to realize the uniform mixing of the mixture, the mixture is kept stand after being mixed, part of the complex compound descends to the bottom of the raw material tank, and the upper mixture is input into a dehydration processor (4) for dehydration treatment;
3) after the dehydration is finished, the material continues to enter a micro filter (5) for filtration, and after being filtered by the micro filter (5), the material enters a rectifying tower (6) for rectification;
4) after the rectification, the material enters a nano filter (7) for filtration, and high-purity isopropanol is obtained after the filtration of the nano filter (7).
2. The method for preparing high-purity isopropanol according to claim 1, wherein: automatic piston assembly (2) are including drawing material pipe (201), draw material pipe (201) fixed run through in the upper wall of head tank (1), the inside of drawing material pipe (201) sets up piston (202), the one end of fixed connection piston rod (203) on the lateral wall of piston (202), the other end of piston rod (203) and the output fixed connection of electric telescopic handle (204), the stiff end of electric telescopic handle (204) is fixed in through support (205) the upside of drawing material pipe (201), the output of drawing material pipe (201) is connected with inlet pipe (206), draw material pipe (201) with all be provided with electric control valve on inlet pipe (206).
3. The method for preparing high-purity isopropanol according to claim 2, wherein: malleation blender (3) include annular pipe fitting (301), annular pipe fitting (301) fixed connection in on the inside wall of head tank (1), the venthole has evenly been seted up on annular pipe fitting (301), the one end of intake pipe (302) is still connected on annular pipe fitting (301), the other end of intake pipe (302) is located the outside of head tank (1).
4. The method for preparing high-purity isopropyl alcohol according to claim 3, wherein: the positive pressure gas used in the positive pressure mixer (3) is inert gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110667406.5A CN113429262A (en) | 2021-06-16 | 2021-06-16 | Preparation method of high-purity isopropanol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110667406.5A CN113429262A (en) | 2021-06-16 | 2021-06-16 | Preparation method of high-purity isopropanol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114570257A (en) * | 2022-03-07 | 2022-06-03 | 湖南汇虹试剂有限公司 | Ultra-clean high-purity isopropanol preparation equipment |
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| CN101362675A (en) * | 2008-09-16 | 2009-02-11 | 江阴市润玛电子材料有限公司 | Method for preparing super-clean and high-purity isopropanol and apparatus thereof |
| CN103360267A (en) * | 2013-07-23 | 2013-10-23 | 淮安嘉诚高新化工股份有限公司 | Continuous liquid-phase catalytic hydrogenation reduction method for production of o-chloroaniline |
| CN209406220U (en) * | 2018-11-23 | 2019-09-20 | 广东双塔新材料有限公司 | One kind of multiple liquid charging stock hybrid systems |
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2021
- 2021-06-16 CN CN202110667406.5A patent/CN113429262A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362675A (en) * | 2008-09-16 | 2009-02-11 | 江阴市润玛电子材料有限公司 | Method for preparing super-clean and high-purity isopropanol and apparatus thereof |
| CN103360267A (en) * | 2013-07-23 | 2013-10-23 | 淮安嘉诚高新化工股份有限公司 | Continuous liquid-phase catalytic hydrogenation reduction method for production of o-chloroaniline |
| CN209406220U (en) * | 2018-11-23 | 2019-09-20 | 广东双塔新材料有限公司 | One kind of multiple liquid charging stock hybrid systems |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN114570257A (en) * | 2022-03-07 | 2022-06-03 | 湖南汇虹试剂有限公司 | Ultra-clean high-purity isopropanol preparation equipment |
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Application publication date: 20210924 |