CN115650178A - Method for refining electronic-grade hydrogen peroxide - Google Patents
Method for refining electronic-grade hydrogen peroxide Download PDFInfo
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- CN115650178A CN115650178A CN202211461735.5A CN202211461735A CN115650178A CN 115650178 A CN115650178 A CN 115650178A CN 202211461735 A CN202211461735 A CN 202211461735A CN 115650178 A CN115650178 A CN 115650178A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
A method for refining electronic-grade hydrogen peroxide comprises the following steps: cooling hydrogen peroxide prepared by an anthraquinone method to 0-10 ℃ through a plate heat exchanger, filtering out residual organic matters through a two-stage filter, and then feeding the organic matters into a resin bed to remove metal ions in the hydrogen peroxide; then the mixture enters a raw material buffer tank; and (3) the effluent from the raw material buffer tank enters two stages of RO (reverse osmosis) filtration for desalination, the total organic carbon content in the effluent is reduced to be below 5ppm, the intermediate product enters a secondary intermediate tank and total TOC (total organic carbon) is detected, the effluent is pumped to a finished product tank after passing the inspection, and the effluent is discharged by a finished product pump. And the whole process has low cost and low energy consumption.
Description
Technical Field
The invention relates to a method for refining electronic-grade hydrogen peroxide.
Background
Hydrogen peroxide (academic name hydrogen peroxide, H) 2 O 2 ) Is mainly used for textile, knitwear, paper pulp, grass, vine, bamboo and woodBleaching the product; three-waste (especially waste water) treatment; organic and polymer synthesis (used as oxidant, catalyst, initiator, epoxidizing agent, crosslinking agent, etc.); organic and inorganic peroxides (e.g., peracetic acid, benzoyl peroxide, methyl ethyl ketone peroxide, sodium percarbonate, sodium perborate, calcium peroxide, thiourea peroxide, caprolactam, propylene oxide, etc.); purifying the electroplating solution; the product is used for disinfection, antisepsis and fresh-keeping in food industry; as surface treating agents in the electronics industry; used for disinfection in medical and pharmaceutical industries; high concentrations of hydrogen peroxide are useful in rocket propellants; other applications such as the building material industry as blowing agents; the water treatment industry is used for sterilization and algae removal; are used in the cosmetics industry as hair bleaches and dyes.
The anthraquinone process is a main industrial production method of hydrogen peroxide, hydrogen peroxide products comprise industrial grade, reagent grade, food grade, medical grade, electronic grade and the like, and the finished products are industrial grade hydrogen peroxide in the hydrogen peroxide process of the anthraquinone process, while the existing hydrogen peroxide refining method has high energy consumption and high cost, and the TOC content and the salt ion content in the refined hydrogen peroxide products are high and cannot meet the requirements of the electronic grade.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for refining electronic-grade hydrogen peroxide, which can effectively reduce the content of salt ions and TOC in industrial-grade hydrogen peroxide and refine the hydrogen peroxide into the electronic-grade hydrogen peroxide.
In order to solve the technical problems, the invention provides a method for refining electronic-grade hydrogen peroxide, which comprises the following steps:
(1) Reducing the temperature of 35-50% hydrogen peroxide produced in a concentration working section for preparing hydrogen peroxide by an anthraquinone method to 0-10 ℃ through a primary plate heat exchanger, filtering out residual organic matters through a primary filter, filtering out the hydrogen peroxide which is transparent in appearance and free of macroscopic oily substances, and feeding the hydrogen peroxide into a raw material tank after filtering;
(2) Hydrogen peroxide in the raw material groove is pumped to a secondary filter by a raw material pump, the hydrogen peroxide filtered by the secondary filter is kept at 0-10 ℃ by a secondary plate heat exchanger and then enters a resin bed, and cation exchange resin is filled in the resin bed and used for removing metal ions in the hydrogen peroxide;
(3) Hydrogen peroxide absorbed and filtered by the resin bed enters a raw material buffer tank;
(4) Hydrogen peroxide in a raw material buffer tank enters a primary RO (reverse osmosis) filter, a first high-pressure pump is arranged in the primary RO filter, the hydrogen peroxide in the raw material buffer tank is desalted through primary reverse osmosis filtration under the action of the first high-pressure pump, the content of total organic carbon in the hydrogen peroxide is reduced to be below 10ppm, a primary intermediate product and first waste liquid are produced at an outlet, the primary intermediate product enters a primary intermediate tank, the first waste liquid enters a waste liquid recovery tank, the first waste liquid in the waste liquid recovery tank is pumped to a dilute product tank through a waste liquid pump, and the flow ratio of the primary intermediate product to the primary waste liquid is 1:4;
(5) The first-stage intermediate product in the first-stage intermediate tank enters a second-stage RO reverse osmosis filter, a second high-pressure pump is arranged in the second-stage RO reverse osmosis filter, the first-stage intermediate product in the first-stage intermediate tank is subjected to second-stage reverse osmosis filtration and secondary desalination under the action of the second high-pressure pump, the total organic carbon content of the first-stage intermediate product is reduced to be below 5ppm, a second-stage intermediate product and second waste liquid are produced at an outlet, the second-stage intermediate product enters the second-stage intermediate tank and is used for detecting total TOC, the second waste liquid enters a raw material buffer tank or a raw material tank, and the flow ratio of the second-stage intermediate product to the second waste liquid is 5:4;
(6) And after the second-stage intermediate products in the second-stage intermediate tank are qualified through inspection, the second-stage intermediate products are pumped to the finished product tank through a second-stage intermediate pump and discharged through a finished product pump, and when the second-stage intermediate products in the second-stage intermediate tank are unqualified through inspection, the second-stage intermediate products and the second waste liquid are combined and enter the raw material buffer tank or the raw material tank.
Preferably, the inlet of the secondary filter, the inlet of the primary RO reverse osmosis filter and the inlet of the secondary RO reverse osmosis filter are provided with pure water lines for cleaning, and when the resin in the resin bed and the RO reverse osmosis membrane are exchanged, the pure water is used for cleaning.
Preferably, the thin product tank is connected to the raw material buffer tank through a thin product pump, and when the liquid level of the raw material buffer tank is low, the thin product pump introduces the liquid in the thin product tank into the raw material buffer tank.
Preferably, the primary filter, the secondary filter, the primary RO reverse osmosis filter and the secondary RO reverse osmosis filter are all provided with exhaust devices, the exhaust devices are started by adopting a grounding sleeve electromagnetic valve, all the exhaust devices are started to exhaust air in the system within 1-2min after the system starts to operate, exhaust pipes of the exhaust devices intensively pass through a gas-liquid separator, gas phase is discharged, and liquid phase returns to the raw material tank.
The invention has the advantages that: the method for refining the electronic-grade hydrogen peroxide can effectively reduce the content of salt ions and TOC in industrial-grade hydrogen peroxide and refine the hydrogen peroxide into the electronic-grade hydrogen peroxide. And the whole process has low cost and low energy consumption.
The pure water pipeline can wash related parts when the resin in the resin bed and the RO reverse osmosis membrane are replaced, so that a better refining effect is ensured; the dilute product tank can be used for supplementing materials for the raw material buffer tank, so that the condition that the operation of the system is influenced by low liquid level of the raw material buffer tank (air can be brought in due to too low liquid level) is prevented; the exhaust device can avoid the pump evacuation phenomenon from occurring, and the whole operation efficiency is influenced.
Drawings
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
Referring to fig. 1, a method for refining electronic-grade hydrogen peroxide comprises the following steps:
(1) The concentration of 35-50% hydrogen peroxide produced in the concentration working section for preparing hydrogen peroxide by an anthraquinone method is reduced to 0-10 ℃ through a primary plate heat exchanger 11, residual organic matters are filtered out through a primary filter 21, the filtered hydrogen peroxide is transparent in appearance and free of macroscopic oily substances, and the filtered hydrogen peroxide enters a raw material tank 3;
(2) Hydrogen peroxide in the raw material tank 3 is pumped to a secondary filter 22 through a raw material pump 31, the hydrogen peroxide filtered by the secondary filter 22 is kept at 0-10 ℃ through a secondary plate heat exchanger 12, and then enters a resin bed 23 connected in parallel, and cation exchange resin is filled in the resin bed 23 and used for removing metal ions in the hydrogen peroxide;
(3) Hydrogen peroxide absorbed and filtered by the resin bed 23 enters the raw material buffer tank 4;
(4) Hydrogen peroxide in the raw material buffer tank 4 enters a primary RO (reverse osmosis) filter 51, a first high-pressure pump is arranged in the primary RO filter 51, under the action of the first high-pressure pump, hydrogen peroxide in the raw material buffer tank 4 is desalted through primary RO, the total organic carbon content in the hydrogen peroxide is reduced to be below 10ppm, a primary intermediate product and first waste liquid are produced at an outlet, the primary intermediate product enters a primary intermediate tank 71, the first waste liquid enters a waste liquid recovery tank 6, the first waste liquid in the waste liquid recovery tank 6 is pumped to a thin product tank 62 through a waste liquid pump 61, and the flow ratio of the primary intermediate product to the primary waste liquid is 1:4;
(5) The first-stage intermediate product in the first-stage intermediate tank 71 enters a second-stage RO reverse osmosis filter 52, a second high-pressure pump is arranged in the second-stage RO reverse osmosis filter 52, the first-stage intermediate product in the first-stage intermediate tank 71 is subjected to second-stage reverse osmosis filtration and secondary desalination under the action of the second high-pressure pump, the total organic carbon content is reduced to be below 5ppm, a second-stage intermediate product and second waste liquid are produced at an outlet, the second-stage intermediate product enters a second-stage intermediate tank 72 and is detected for total TOC, the second waste liquid enters a raw material buffer tank 4 or a raw material tank 3, and the flow ratio of the second-stage intermediate product to the second waste liquid is 5:4;
(6) And after the second-stage intermediate products in the second-stage intermediate tank 72 are inspected to be qualified, the second-stage intermediate products are pumped to the finished product tank 8 through the second-stage intermediate pump 73 and discharged through the finished product pump 81, and when the second-stage intermediate products in the second-stage intermediate tank 72 are inspected to be unqualified, the second-stage intermediate products and the second waste liquid are combined and enter the raw material buffer tank 4 or the raw material tank 3.
The inlet of the secondary filter 22, the inlet of the primary RO reverse osmosis filter 51 and the inlet of the secondary RO reverse osmosis filter 52 are provided with pure water lines for cleaning (the structure of flushing the pure water lines per se is well known to those skilled in the art and is not shown again), and when the resin and RO reverse osmosis membranes in the resin bed 23 are replaced, the pure water is used for cleaning.
The thin product groove 62 is connected with the raw material buffer tank 4 through a thin product pump, and when the liquid level of the raw material buffer tank 4 is low, the thin product pump guides the liquid in the thin product groove 62 into the raw material buffer tank 4.
The primary filter 21, the secondary filter 22, the primary RO filter 51 and the secondary RO filter 52 are all provided with exhaust devices, the exhaust devices are started by adopting a grounding sleeve electromagnetic valve, when the system starts to operate within 1-2min, all the exhaust devices are started to exhaust air in the system, exhaust pipes of the exhaust devices intensively pass through a gas-liquid separator, gas phase is discharged, and liquid phase returns to the raw material tank 3.
It is also well known in the art that exhaust devices are not described in detail in this application.
Through detection, the contents of partial ions and total carbon in the prepared hydrogen peroxide are as follows:
the concentration of hydrogen peroxide is 37.24 percent
8.4ppm of total carbon, no aluminum ion, 2.28ppm of potassium ion, 3.99ppm of calcium ion, 4.32 ppm of sodium ion and 0.02 ppm of iron ion.
Claims (4)
1. A method for refining electronic-grade hydrogen peroxide is characterized by comprising the following steps:
(1) Reducing the temperature of 35-50% hydrogen peroxide produced in a concentration working section for preparing hydrogen peroxide by an anthraquinone method to 0-10 ℃ through a primary plate heat exchanger, filtering out residual organic matters through a primary filter, enabling the filtered hydrogen peroxide to be transparent in appearance and free of macroscopic oily substances, and enabling the filtered hydrogen peroxide to enter a raw material tank;
(2) Hydrogen peroxide in the raw material groove is pumped to a secondary filter through a raw material pump, the temperature of the hydrogen peroxide filtered by the secondary filter is kept at 0-10 ℃ through a secondary plate heat exchanger, and then the hydrogen peroxide enters a resin bed, and cation exchange resin is filled in the resin bed and used for removing metal ions in the hydrogen peroxide;
(3) Hydrogen peroxide absorbed and filtered by the resin bed enters a raw material buffer tank;
(4) Hydrogen peroxide in a raw material buffer tank enters a primary RO (reverse osmosis) filter, a first high-pressure pump is arranged in the primary RO filter, the hydrogen peroxide in the raw material buffer tank is desalted through primary reverse osmosis filtration under the action of the first high-pressure pump, the total organic carbon content in the hydrogen peroxide is reduced to be below 10ppm, a primary intermediate product and first waste liquid are produced at an outlet, the primary intermediate product enters a primary intermediate tank, the first waste liquid enters a waste liquid recovery tank, the first waste liquid in the waste liquid recovery tank is pumped to a dilute product tank through a waste liquid pump, and the flow ratio of the primary intermediate product to the primary waste liquid is 1:4;
(5) The first-stage intermediate product in the first-stage intermediate tank enters a second-stage RO reverse osmosis filter, a second high-pressure pump is arranged in the second-stage RO reverse osmosis filter, the first-stage intermediate product in the first-stage intermediate tank is subjected to second-stage reverse osmosis filtration and secondary desalination under the action of the second high-pressure pump, the total organic carbon content of the first-stage intermediate product is reduced to be below 5ppm, a second-stage intermediate product and second waste liquid are produced at an outlet, the second-stage intermediate product enters the second-stage intermediate tank and is used for detecting total TOC, the second waste liquid enters a raw material buffer tank or a raw material tank, and the flow ratio of the second-stage intermediate product to the second waste liquid is 5:4;
(6) And after the second-stage intermediate products in the second-stage intermediate tank are qualified through inspection, the second-stage intermediate products are pumped to the finished product tank through a second-stage intermediate pump and discharged through a finished product pump, and when the second-stage intermediate products in the second-stage intermediate tank are unqualified through inspection, the second-stage intermediate products and the second waste liquid are combined and enter the raw material buffer tank or the raw material tank.
2. The method for refining electronic-grade hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the inlet of the secondary filter, the inlet of the primary RO reverse osmosis filter and the inlet of the secondary RO reverse osmosis filter are all provided with pure water pipelines for cleaning, and when the resin in the resin bed and the RO reverse osmosis membrane are replaced, the pure water is used for cleaning.
3. The method for refining electronic-grade hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the thin product groove is connected with the raw material buffer tank through the thin product pump, and when the liquid level of the raw material buffer tank is lower, the thin product pump guides liquid in the thin product groove into the raw material buffer tank.
4. The method for refining electronic-grade hydrogen peroxide according to claim 1, wherein the method comprises the following steps: and the primary filter, the secondary filter, the primary RO reverse osmosis filter and the secondary RO reverse osmosis filter are all provided with exhaust devices, the exhaust devices are started by adopting a grounding sleeve electromagnetic valve, all the exhaust devices are started to exhaust air in the system within 1-2min after the system starts to operate, exhaust pipes of the exhaust devices intensively pass through a gas-liquid separator, gas phase is discharged, and liquid phase returns to a raw material tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211461735.5A CN115650178A (en) | 2022-11-17 | 2022-11-17 | Method for refining electronic-grade hydrogen peroxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211461735.5A CN115650178A (en) | 2022-11-17 | 2022-11-17 | Method for refining electronic-grade hydrogen peroxide |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0733408A (en) * | 1993-07-14 | 1995-02-03 | Sumitomo Chem Co Ltd | Method for purifying hydrogen reroxide solution |
| JP2003001070A (en) * | 2001-06-21 | 2003-01-07 | Mitsubishi Gas Chem Co Inc | Method of refining hydrogen peroxide water |
| JP2003119008A (en) * | 2001-10-10 | 2003-04-23 | Santoku Kagaku Kogyo Kk | Method for producing refined hydrogen peroxide solution |
| US20140341800A1 (en) * | 2011-09-30 | 2014-11-20 | Mitsubishi Gas Chemical Company, Inc. | Method for producing aqueous hydrogen peroxide solution |
| KR20150089465A (en) * | 2014-01-28 | 2015-08-05 | 주식회사 한솔케미칼 | Hydrogen peroxide refined system using reverse osmosis and hydrogen peroxide produced thereof |
| CN112062096A (en) * | 2020-08-31 | 2020-12-11 | 北京化工大学 | Production device and production method of electronic-grade hydrogen peroxide aqueous solution |
| CN216259148U (en) * | 2021-11-29 | 2022-04-12 | 湖南双阳高科化工有限公司 | System for producing electronic-grade hydrogen peroxide water solution |
| CN114852968A (en) * | 2022-04-24 | 2022-08-05 | 飞潮（无锡）过滤技术有限公司 | Method for preparing electronic grade hydrogen peroxide from anthraquinone process industrial grade hydrogen peroxide |
-
2022
- 2022-11-17 CN CN202211461735.5A patent/CN115650178A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0733408A (en) * | 1993-07-14 | 1995-02-03 | Sumitomo Chem Co Ltd | Method for purifying hydrogen reroxide solution |
| JP2003001070A (en) * | 2001-06-21 | 2003-01-07 | Mitsubishi Gas Chem Co Inc | Method of refining hydrogen peroxide water |
| JP2003119008A (en) * | 2001-10-10 | 2003-04-23 | Santoku Kagaku Kogyo Kk | Method for producing refined hydrogen peroxide solution |
| US20140341800A1 (en) * | 2011-09-30 | 2014-11-20 | Mitsubishi Gas Chemical Company, Inc. | Method for producing aqueous hydrogen peroxide solution |
| KR20150089465A (en) * | 2014-01-28 | 2015-08-05 | 주식회사 한솔케미칼 | Hydrogen peroxide refined system using reverse osmosis and hydrogen peroxide produced thereof |
| CN112062096A (en) * | 2020-08-31 | 2020-12-11 | 北京化工大学 | Production device and production method of electronic-grade hydrogen peroxide aqueous solution |
| US20210009417A1 (en) * | 2020-08-31 | 2021-01-14 | Beijing University Of Chemical Technology | Production device and production method of electronic grade hydrogen peroxide aqueous solution |
| CN216259148U (en) * | 2021-11-29 | 2022-04-12 | 湖南双阳高科化工有限公司 | System for producing electronic-grade hydrogen peroxide water solution |
| CN114852968A (en) * | 2022-04-24 | 2022-08-05 | 飞潮（无锡）过滤技术有限公司 | Method for preparing electronic grade hydrogen peroxide from anthraquinone process industrial grade hydrogen peroxide |
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