CN111039759A - Preparation method of ultra-clean high-purity isopropanol - Google Patents
Preparation method of ultra-clean high-purity isopropanol Download PDFInfo
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- CN111039759A CN111039759A CN201911156176.5A CN201911156176A CN111039759A CN 111039759 A CN111039759 A CN 111039759A CN 201911156176 A CN201911156176 A CN 201911156176A CN 111039759 A CN111039759 A CN 111039759A
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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
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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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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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
- C07C29/76—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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- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Adding weighed industrial isopropanol into a reaction kettle, adding a certain amount of metal complexing agent and efficient drying agent, feeding the isopropanol solution containing the drying agent and complex salt into a rectifying kettle through a microporous filter after the moisture and metal content are all qualified, removing organic impurities such as acetone and the like in the isopropanol, removing the complex salt dissolved in the isopropanol, performing secondary filtration on the isopropanol from which the acetone, the organic impurities and the complex salt are removed through a filtering device, and canning the rectified ultra-clean high-purity isopropanol. The invention has the beneficial effects that: the reaction kettle which is researched and developed by self is adopted to improve the complexing and drying efficiency, the filtered product is clear and transparent, the metal and salt content is greatly reduced, the reaction kettle is stable and reliable, the requirement of high-purity isopropanol in the industry can be met, the equipment maintenance is convenient, the micropore filter element and the composite ceramic nanometer filter element can be disassembled in use, the cleaning is convenient, and the reaction kettle can be recycled for a long time.
Description
Technical Field
The invention relates to the technical field of electronic, semiconductor and optical industries, in particular to a preparation method of ultra-clean high-purity isopropanol.
Background
A reaction kettle in the prior art is basically only provided with a dispersing paddle, the transparency of a filtered product is poor, the product contains partial metal and salt, the product is unstable, the requirement of high-purity isopropanol in most industries cannot be met, the equipment is inconvenient to maintain, and a filtering device cannot be disassembled, is easy to block and is inconvenient to clean. The product can not be guaranteed not to be polluted when canning, the filling amount is also manually canned, the weight error of the product is 1%, the product is easy to leak, leak and leak, and occupational health hazards are greatly increased.
And the package has only one specification, can not satisfy different demands of different trades.
Disclosure of Invention
The invention aims to provide a method for preparing ultra-clean high-purity isopropanol, which solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of ultra-clean high-purity isopropanol comprises the following steps:
the method comprises the following steps: adding weighed industrial isopropanol into a reaction kettle;
step two: then adding a quantitative metal complexing agent and a high-efficiency drying agent;
step three: filtering for later use after the water content and the metal content (detected after being filtered by a filtering device) are all qualified;
step four: the isopropanol solution containing the drying agent and the complex salt enters a rectifying still through a microporous filter to remove organic impurities such as acetone and the like in the isopropanol and remove the complex salt dissolved in the isopropanol;
step five: then the isopropanol without acetone, organic impurities and complex salt is filtered for the second time by a filter.
Step six: and canning the rectified ultra-clean high-purity isopropanol.
Preferably, the reaction kettle is a high-efficiency reaction kettle, can quickly and efficiently complex metal ions, and can ensure that the water in the isopropanol is fully dried by the high-efficiency drying agent.
Preferably, the reaction kettle is provided with two dispersing paddles, the first dispersing paddle and the second dispersing paddle are symmetrically provided with four paddles respectively, the paddles form an included angle of 45 degrees with the horizontal plane, and the distance from the first dispersing paddle to the second dispersing paddle is 1.5 meters.
Preferably, the microporous filter adopts a double-filtering device, adopts a stainless steel 307 filter element, is convenient to maintain, efficient and environment-friendly, and is clear and transparent in the isopropanol after treatment, and suspended particles are not more than 0.2 micron.
Preferably, the rectifying still adopts two stages of towers for rectification in series, so that the load of a single tower is reduced, and the yield can be effectively improved; organic impurities such as acetone in the isopropanol can be removed by rectification, and complex salt dissolved in the isopropanol can be removed at the same time.
Preferably, the kettle of the two-stage tower series rectification tower is a stainless steel kettle with 1000 liters, and the charging coefficient is 0.7, namely the charging is about 700 liters.
Preferably, the steam pressure in the rectifying still is controlled to be 0.09-0.1 Mpa, and the temperature of the top of the two-stage tower is stabilized at 80.5 ℃.
Preferably, the two filtering devices are nano-scale filter elements, the rectified pure product is subjected to nanofiltration and then is sent to a hundred-grade automatic filling and packaging machine, the treated isopropanol is clear and transparent, and the removal rate of suspended particles is 99.999%.
Preferably, a hundred-grade automatic filling technology is adopted, so that the working efficiency is greatly improved, the subpackaging error is reduced, the local aseptic dustproof treatment is realized, and the high quality of the product is ensured.
Advantageous effects
The invention adopts a self-developed patent technology reaction kettle to greatly improve the complexing and drying efficiency, greatly improve the product quality, the product after microfiltration and nanofiltration is clear and transparent, the content of partial metal and salt thereof is greatly reduced, the product is stable and reliable, the requirement of high-purity isopropanol in most industries can be met, the equipment maintenance is convenient, the detachable microporous filter core and the composite ceramic nano filter core are used, the blockage is not easy, the cleaning is convenient, the product can be recycled for a long time, the hundred-level automatic filling technology is used for improving the working efficiency to ensure that the product is not polluted, the filling amount is improved to 120 barrels from 20 barrels per hour of the original manpower, the product weight error is reduced to be below 0.5 percent from the original 1 percent, the safety and the reliability are realized, the leakage phenomenon is avoided, the occupational health hazard is greatly reduced, the environment is friendly, the quality is reliable after purification, nanofiltration and aseptic packaging, and the electronic, the demand of a plurality of fields such as chromatogram, medicine to ultra-clean high-purity isopropyl alcohol, packing specification is from 500ML to 200L moreover, can satisfy the different demands of different trades, avoids extravagant and secondary use pollution.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Examples
A preparation method of ultra-clean high-purity isopropanol comprises the following steps:
the method comprises the following steps: adding weighed industrial isopropanol into a reaction kettle;
step two: then adding a quantitative metal complexing agent and a high-efficiency drying agent;
step three: filtering for later use after the water content and the metal content (detected after being filtered by a filtering device) are all qualified;
step four: the isopropanol solution containing the drying agent and the complex salt enters a rectifying still through a microporous filter to remove organic impurities such as acetone and the like in the isopropanol and remove the complex salt dissolved in the isopropanol;
step five: then the isopropanol without acetone, organic impurities and complex salt is filtered for the second time by a filter.
Step six: and canning the rectified ultra-clean high-purity isopropanol.
Preferably, the reaction kettle is a high-efficiency reaction kettle, can quickly and efficiently complex metal ions, and can ensure that the water in the isopropanol is fully dried by the high-efficiency drying agent.
Preferably, the reaction kettle is provided with two dispersing paddles, the first dispersing paddle and the second dispersing paddle are symmetrically provided with four paddles respectively, the paddles form an included angle of 45 degrees with the horizontal plane, and the distance from the first dispersing paddle to the second dispersing paddle is 1.5 meters.
Preferably, the microporous filter adopts a double-filtering device, adopts a stainless steel 307 filter element, is convenient to maintain, efficient and environment-friendly, and is clear and transparent in the isopropanol after treatment, and suspended particles are not more than 0.2 micron.
Preferably, the rectifying still adopts two stages of towers for rectification in series, so that the load of a single tower is reduced, and the yield can be effectively improved; organic impurities such as acetone in the isopropanol can be removed by rectification, and complex salt dissolved in the isopropanol can be removed at the same time.
Preferably, the kettle of the two-stage tower series rectification tower is a stainless steel kettle with 1000 liters, and the charging coefficient is 0.7, namely the charging is about 700 liters.
Preferably, the steam pressure in the rectifying still is controlled to be 0.09-0.1 Mpa, and the temperature of the top of the two-stage tower is stabilized at 80.5 ℃.
Preferably, the two filtering devices are nano-scale filter elements, the rectified pure product is subjected to nanofiltration and then is sent to a hundred-grade automatic filling and packaging machine, the treated isopropanol is clear and transparent, and the removal rate of suspended particles is 99.999%.
Preferably, a hundred-grade automatic filling technology is adopted, so that the working efficiency is greatly improved, the subpackaging error is reduced, the local aseptic dustproof treatment is realized, and the high quality of the product is ensured.
The raw material isopropanol is pumped into an isopropanol raw material tank and then pumped into a tower kettle of an isopropanol rectification tower by an isopropanol raw material pump, wherein the tower kettle is a 1000-liter stainless steel kettle, the charging coefficient is 0.7, and the charging is about 700 liters. The continuous rectification is carried out, so that the isopropanol is distilled from the top of the tower, and impurities such as moisture, calcium and the like contained in the isopropanol raw material are removed to produce the high-quality isopropanol. The continuous distillation process comprises the following steps: and opening a steam valve of the heating rectifying tower kettle, heating the materials in the kettle, and gradually increasing the temperature. The steam pressure is controlled to be generally 0.09-0.1 Mpa, and the accurate value is determined according to the size of the reflux quantity. When the isopropanol in the rectifying tower kettle is distilled to the top of the rectifying tower, the isopropanol flows into a gas-liquid separator for reflux after being condensed by a condenser at the top of the rectifying tower, the total reflux operation is kept for about 30 minutes, and the temperature at the top of the rectifying tower is stabilized at about 80.5 ℃. Then, the ratio of 10: discharging the material to an isopropanol finished product tank at a reflux ratio of about 1, opening a raw material isopropanol feed valve on a rectifying tower kettle to continuously feed, and adjusting the accurate value of the raw material isopropanol feed valve according to the discharge amount and the residual liquid discharge amount of the high-quality isopropanol. After 3 hours of high-quality isopropanol discharge in the rectification operation, the residual liquid in the bottom of the isopropanol rectification tower can be cooled by a residual liquid cooler, a certain amount of the residual liquid is controlled to be put into a residual liquid tank, and when the liquid level of the residual liquid tank is higher, the residual liquid is pumped into an isopropanol treatment tank by a residual liquid pump.
The rectification control method comprises the following steps:
finally, it should be noted that: 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 changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the content of the present invention within the scope of the protection of the present invention.
Claims (9)
1. The preparation method of the ultra-clean high-purity isopropanol is characterized by comprising the following steps:
the method comprises the following steps: adding weighed industrial isopropanol into a reaction kettle;
step two: then adding a quantitative metal complexing agent and a high-efficiency drying agent;
step three: filtering for later use after the water content and the metal content (detected after being filtered by a filtering device) are all qualified;
step four: the isopropanol solution containing the drying agent and the complex salt enters a rectifying still through a microporous filter to remove organic impurities such as acetone and the like in the isopropanol and remove the complex salt dissolved in the isopropanol;
step five: then the isopropanol without acetone, organic impurities and complex salt is filtered for the second time by a filter.
Step six: and canning the rectified ultra-clean high-purity isopropanol.
2. The method for preparing ultra-clean high-purity isopropanol according to claim 1, characterized in that: the reaction kettle is a high-efficiency reaction kettle, can quickly and efficiently complex metal ions, and can ensure that the water in the isopropanol is fully dried by the high-efficiency drying agent.
3. The method for preparing ultra-clean high-purity isopropanol according to claim 2, characterized in that: the reaction kettle is provided with two dispersing paddles, the first dispersing paddle and the second dispersing paddle are symmetrically provided with four paddles respectively, the paddles form an included angle of 45 degrees with the horizontal plane, and the distance from the first dispersing paddle to the second dispersing paddle is 1.5 m.
4. The method for preparing ultra-clean high-purity isopropanol according to claim 1, characterized in that: the microporous filter adopts a double-filtering device and a stainless steel 307 filter element, so that the maintenance is convenient, the efficiency and the environmental protection are realized, the treated isopropanol is clear and transparent, and the suspended particles are not more than 0.2 micron.
5. The method for preparing ultra-clean high-purity isopropanol according to claim 1, characterized in that: the rectifying still adopts two stages of towers for rectification in series, so that the burden of a single tower is reduced, and the yield can be effectively improved; organic impurities such as acetone in the isopropanol can be removed by rectification, and complex salt dissolved in the isopropanol can be removed at the same time.
6. The method for preparing ultra-clean high-purity isopropanol according to claim 5, characterized in that: the kettle of the two-stage tower series rectification tower is a 1000 liter stainless steel kettle, and the charging coefficient is 0.7, namely the charging is about 700 liters.
7. The method for preparing ultra-clean high-purity isopropanol according to claim 5, characterized in that: the steam pressure in the rectifying kettle is controlled to be 0.09-0.1 Mpa, and the temperature of the top of the two-stage tower is stabilized at 80.5 ℃.
8. The method for preparing ultra-clean high-purity isopropanol according to claim 1, characterized in that: and the two filtering devices are nano-scale filter elements, the purified product distilled by rectification is subjected to nanofiltration and then is sent to a hundred-grade automatic filling and packaging machine, the treated isopropanol is clear and transparent, and the removal rate of suspended particles is 99.999%.
9. The method for preparing ultra-clean high-purity isopropanol according to claim 1, characterized in that: by adopting a hundred-grade automatic filling technology, the working efficiency is greatly improved, the subpackaging error is reduced, the local aseptic dustproof treatment is realized, and the high quality of the product is ensured.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911156176.5A CN111039759A (en) | 2019-11-22 | 2019-11-22 | Preparation method of ultra-clean high-purity isopropanol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911156176.5A CN111039759A (en) | 2019-11-22 | 2019-11-22 | Preparation method of ultra-clean high-purity isopropanol |
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| CN111039759A true CN111039759A (en) | 2020-04-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773173A (en) * | 2021-08-31 | 2021-12-10 | 常州大学 | Production process and device of ultrapure isopropanol |
| 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 |
| CN115521191A (en) * | 2022-06-27 | 2022-12-27 | 江苏达诺尔科技股份有限公司 | Method for effectively purifying ultrapure isopropanol |
Citations (2)
| 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 |
| CN203030278U (en) * | 2012-12-27 | 2013-07-03 | 苏州市博洋化学品有限公司 | Reaction kettle |
-
2019
- 2019-11-22 CN CN201911156176.5A patent/CN111039759A/en active Pending
Patent Citations (2)
| 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 |
| CN203030278U (en) * | 2012-12-27 | 2013-07-03 | 苏州市博洋化学品有限公司 | Reaction kettle |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773173A (en) * | 2021-08-31 | 2021-12-10 | 常州大学 | Production process and device of ultrapure isopropanol |
| 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 |
| CN115521191A (en) * | 2022-06-27 | 2022-12-27 | 江苏达诺尔科技股份有限公司 | Method for effectively purifying ultrapure isopropanol |
| CN115521191B (en) * | 2022-06-27 | 2023-12-22 | 江苏达诺尔科技股份有限公司 | Method for purifying isopropanol |
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Application publication date: 20200421 |