CN107902630A - The production equipment and production technology of a kind of high-purity hydrogen peroxide - Google Patents
The production equipment and production technology of a kind of high-purity hydrogen peroxide Download PDFInfo
- Publication number
- CN107902630A CN107902630A CN201711440469.7A CN201711440469A CN107902630A CN 107902630 A CN107902630 A CN 107902630A CN 201711440469 A CN201711440469 A CN 201711440469A CN 107902630 A CN107902630 A CN 107902630A
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- China
- Prior art keywords
- hydrogen peroxide
- storage tank
- resin column
- exchange resin
- ion exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
- B01J47/026—Column or bed processes using columns or beds of different ion exchange materials in series
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention provides a kind of production equipment of high-purity hydrogen peroxide, it is characterised in that is provided with high-order storage tank, adsorption resin column, ion exchange resin column, intermediate storage tank, nanofiltration membrane component, finished product storage tank from top to bottom；High-order reservoir outlet is connected by pipeline with adsorption resin column upper inlet, and valve K1 is equipped with pipeline；Outlet is connected by pipeline with ion exchange resin column upper inlet K2 and is equipped with valve K2 under adsorption resin column；Outlet is connected with intermediate storage tank entrance and is equipped with valve K3 under ion exchange resin column；Intermediate storage tank is connected with vacuum pump, and blow valve K4；Intermediate storage tank outlet is connected by pipeline with hollow fiber nanofiltration membrane module inlet, and pipeline is equipped with valve K5 and booster pump；Outlet is connected with finished product storage tank entrance under hollow fiber nanofiltration membrane component, and valve K6 is equipped with connecting pipe.The present invention provides a kind of preparation method of high-purity hydrogen peroxide, solve that traditional hydrogen peroxide method of purification production cost is high, efficiency is low, ropy shortcoming.
Description
Technical field
The present invention relates to the production equipment and production technology of a kind of high-purity hydrogen peroxide, especially semiconductor and IC
With the production Technology of high-purity hydrogen peroxide.
Background technology
High-purity hydrogen peroxide plays an important role in electronic manufacturing field, is widely used in the cleaning of semiconductor and IC
Corrosion etc., higher and higher to the quality requirement of high-purity hydrogen peroxide with the development of electronics industry, demand is also increasing.I
The advantages of existing industrial grade hydrogen peroxide of state uses anthraquinone production mostly, this method is that technology maturation cost is low, but product
In contain substantial amounts of organic and inorganic impurity.It is industrial usually using distillation, reverse osmosis, ion exchange to eliminate these impurity
The methods of, but production cost is high, low production efficiency, poor product quality.
At present, industrializing the method for purifying hydrogen peroxide has two kinds：First, cation and anion exchange is added using organic carbon adsorption
Method, such as CN1285311A, it is the absorption that raw material hydrogen peroxide is carried out to organic carbon by pumping input adsorption resin column, then will
The hydrogen peroxide input anion-cation exchange resin column for removing organic carbon carries out ion exchange, then by the peroxide Jing Guo ion exchange
Change hydrogen input filter to remove granule foreign, so as to obtain ultrapure hydrogen peroxide product.Second, handed over using single zwitterion
Change and add cation and anion exchange method, such as CN1439600A.It is by industrial hydrogen peroxide solution continue to flow through anion exchange resin,
Anion exchange resin and negative and positive mixture iron exchange resin carry out ion exchange, and high-purity hydrogen peroxide product is made.The two is
It is only 85% there are raw material hydrogen peroxide utilization rate is low, the defects of production cost is high, inferior separating effect, purity does not reach requirement.
Product purity does not meet semiconductor equipment and material structure (SEMI-C8) standard, i.e., 1PPb when metal ion content is small, has
Machine carbon content is less than 20PPm.Semiconductor equipment and material structure SEMIC19-90 and SEMIC7 can only be met
5-93 standards.
CN1184138C discloses a kind of manufacturing process and equipment of ultrapure hydrogen peroxide, but its production cost compared with
Height, separating effect are also to be hoisted.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of production of high-purity hydrogen peroxide for the above-mentioned prior art
Equipment and its technique, solve that traditional hydrogen peroxide method of purification production cost is high, efficiency is low, ropy shortcoming.
Technical solution is used by the present invention solves the above problems：A kind of production equipment of high-purity hydrogen peroxide, it is special
Levy and be to be provided with high-order storage tank from top to bottom, adsorption resin column, ion exchange resin column, intermediate storage tank, nanofiltration membrane component, into
Product storage tank；High-order reservoir outlet is connected by pipeline with adsorption resin column upper inlet, and valve K1 is equipped with pipeline；Absorption
Outlet is connected by pipeline with ion exchange resin column upper inlet and is equipped with valve K2 under resin column；Go out under ion exchange resin column
Mouth is connected with intermediate storage tank entrance and is equipped with valve K3；Intermediate storage tank is connected with vacuum pump, and blow valve K4；Intermediate storage tank exports
It is connected by pipeline with hollow fiber nanofiltration membrane module inlet, pipeline is equipped with valve K5 and booster pump；Hollow fiber nanofiltration membrane
Outlet is connected with finished product storage tank entrance under component, and valve K6 is equipped with connecting pipe.
Further, a diameter of 200mm of adsorption resin column, is highly 1000-1200mm；The absorption resin of filling is benzene second
Alkene or divinylbenzene, or the mixture of styrene and divinylbenzene.The macropore that preferably styrene, divinylbenzene copolymerization form is inhaled
Attached resin.
Further, a diameter of 200mm of ion exchange resin column, is highly 1000-1400mm；Ion exchange resin column
The filler material at bottom 1/3rd positions is the mixture of anion-cation exchange resin equal proportion, the filling of centre 1/3rd
Expect for cation exchange resin, above 1/3rd filler material be anion exchange resin.
Further, hollow fiber nanofiltration membrane component is external-compression type component.
Present invention also offers a kind of production technology of high-purity hydrogen peroxide, it is characterised in that uses above-mentioned high-purity peroxide
Change the production equipment of hydrogen, comprise the following steps：
（1）Impurity removes the stage：Adsorb resin and remove organic carbon contaminants and ion exchange removing unit second cation impurity；Raw material
Direct storage exists in high-order storage tank after industrial hydrogen peroxide incoming inspection qualification, and K4 and K5 is closed when purification produces, is opened successively
Vacuum pump, K3, K2, K1, allow industrial hydrogen peroxide to pass sequentially through adsorption resin column, middle storage are stored in after ion exchange resin column
Tank, after the completion of close K1, K2, K3 and vacuum pump successively；
（2）In the nanofiltration membrane stage, open K4, K5, K6 booster pump successively, allows during the hydrogen peroxide in intermediate storage tank is forced through
Hollow fiber nanofiltration membrane component, removes residual impurity ion, obtains high-purity hydrogen peroxide.
Further, the running temperature that impurity removes the stage is 10-30 DEG C, and operating pressure is to vacuumize negative pressure, absolute pressure
Power is controlled in 40-50kp；The running temperature in nanofiltration membrane stage is 10-30 DEG C, and operating pressure is pressurization, and absolute pressure is
500-600kp。
Present invention process technology is divided to two sections of progress, and first segment removes part for absorption resin adsorption organic carbon and ion exchange
Zwitterion impurity.Direct storage exists in high-order storage tank after primary industry hydrogen peroxide incoming inspection qualification, and purification is closed when producing
K4 and K5 are closed, vacuum pump, K3, K2, K1 is opened successively, allows industrial hydrogen peroxide to pass sequentially through adsorption resin column, amberlite
Be stored in intermediate storage tank after fat column, after the completion of close K1, K2, K3 and vacuum pump successively.Above-mentioned adsorption resin column is a diameter of
200mm, is highly 1000-1200mm, and absorption resin used is styrene or divinylbenzene or styrene and divinylbenzene
Mixture.The above-mentioned a diameter of 200mm of ion exchange resin column, is highly 1000-1400mm, its filler is anion exchange
Resin and cation exchange resin, and the mixture that bottom 1/3rd is anion-cation exchange resin equal proportion, centre three
/ mono- is cation exchange resin, above 1/3rd be anion exchange resin.This section of production technology pressure control is in 40-
50kp, temperature control is at 10-30 degrees Celsius.Second segment is the nanofiltration membrane stage, removes residual impurity ion.Open successively
K4, K5, K6 booster pump, the hydrogen peroxide allowed in intermediate storage tank are forced through hollow fiber nanofiltration membrane component, remove foreign ion,
Obtain high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane component is external-compression type component, this section of production technology pressure control exists
500-600kp, temperature control is at 10-30 DEG C.
Compared with prior art, advantageous effects of the present invention：
（1）The present invention is set each device to make full use of potential energy from top to bottom by high order, and in finished product storage tank and
Intermediate storage tank is provided between high-order storage tank, makes the present invention only two pumps need to be set to drive, greatly reduces production cost；
（2）The ion exchange resin column difference from prior art of the present invention is the zwitterion of subsection filling different proportion
Exchanger resin, anion exchange resin is filled in the top, and interlude is cation exchange resin, and bottom is the moon of equal proportion
Cation exchange resin, this filling mode can carry out grading absorption, and facilitate subsequent recovery to reuse, so that significantly
Reduce cost；
（3）The present invention is designed by overall flow, greatly reduces the required pressure of production technology, raw so as to fulfill low cost
Production, and by the setting of segmented ion exchange resin column and hollow fiber nanofiltration membrane, improve the adsorption capacity to impurity, make
The product quality of preparation is more preferable.
Brief description of the drawings
Fig. 1 is the production technological process of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with attached drawing embodiment.
The present invention is illustrated with reference to embodiment.
Embodiment 1
First segment is absorption resin adsorption and ion exchange.Direct storage exists high after primary industry hydrogen peroxide incoming inspection qualification
In the storage tank of position, K4 and K5 is closed when purification produces, vacuum pump, K3, K2, K1 is opened successively, allows industrial hydrogen peroxide to pass sequentially through
Adsorption resin column, is stored in intermediate storage tank after ion exchange resin column, after the completion of close K1, K2, K3 and vacuum pump successively.It is above-mentioned
The a diameter of 200mm of adsorption resin column, is highly 1000mm, and absorption resin used is styrene.Above-mentioned ion exchange resin column
A diameter of 200mm, is highly 1000mm, its filler is anion exchange resin and cation exchange resin, and bottom
1/3rd be the mixture of anion-cation exchange resin equal proportion, and centre 1/3rd is cation exchange resin, above three
/ mono- is anion exchange resin.This section of production technology pressure is controlled in 40kp, and temperature control is at 10 DEG C.
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
Hollow fiber nanofiltration membrane component is forced through, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, this section of production technology pressure is controlled in 500kp, and temperature control is at 10 DEG C.
Embodiment 2
First segment is absorption resin adsorption and ion exchange.Direct storage exists high after primary industry hydrogen peroxide incoming inspection qualification
In the storage tank of position, K4 and K5 is closed when purification produces, vacuum pump, K3, K2, K1 is opened successively, allows industrial hydrogen peroxide to pass sequentially through
Adsorption resin column, is stored in intermediate storage tank after ion exchange resin column, after the completion of close K1, K2, K3 and vacuum pump successively.It is above-mentioned
The a diameter of 200mm of adsorption resin column, is highly 1100mm, and absorption resin used is divinylbenzene.Above-mentioned ion exchange resin
Column diameter is 200mm, is highly 1200mm, its filler is anion exchange resin and cation exchange resin, and most lower
Face 1/3rd is the mixture of anion-cation exchange resin equal proportion, and centre 1/3rd is cation exchange resin, above
1/3rd be anion exchange resin.This section of production technology pressure is controlled in 45kp, and temperature control is at 20 DEG C.
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
Hollow fiber nanofiltration membrane component is forced through, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, this section of production technology pressure is controlled in 550kp, and temperature control is at 20 DEG C.
Embodiment 3
First segment is absorption resin adsorption and ion exchange.Direct storage exists high after primary industry hydrogen peroxide incoming inspection qualification
In the storage tank of position, K4 and K5 is closed when purification produces, vacuum pump, K3, K2, K1 is opened successively, allows industrial hydrogen peroxide to pass sequentially through
Adsorption resin column, is stored in intermediate storage tank after ion exchange resin column, after the completion of close K1, K2, K3 and vacuum pump successively.It is above-mentioned
The a diameter of 200mm of adsorption resin column, is highly 1200mm, and absorption resin used is styrene and the mixture of divinylbenzene.
The above-mentioned a diameter of 200mm of ion exchange resin column, is highly 1400mm, its filler is anion exchange resin and cation
Exchanger resin, and bottom 1/3rd be anion-cation exchange resin equal proportion mixture, centre 1/3rd for sun from
Sub-exchange resin, above 1/3rd be anion exchange resin.This section of production technology pressure control exists in 50kp, temperature control
30℃。
Second segment is the nanofiltration membrane stage, opens K4, K5, K6 booster pump successively, allows hydrogen peroxide in intermediate storage tank
Hollow fiber nanofiltration membrane component is forced through, foreign ion is removed, obtains high-purity hydrogen peroxide.Above-mentioned hollow fiber nanofiltration membrane group
Part is external-compression type component, this section of production technology pressure is controlled in 600kp, and temperature control is at 30 DEG C.
Comparative example 1
It is same as Example 3, except mixing for all anion-cation exchange resin equal proportions of ion exchange resin column filler
Compound.
Comparative example 2
Produced according to the preparation process of the embodiment 1 of CN1184138C.
Test result is as shown in the table：
The content for analyzing impurity in raw material and each embodiment in above table is understood：The present invention can be removed effectively in hydrogen peroxide
Organic carbon and zwitterion impurity, and cost is lower, more efficient.In addition to the implementation, present invention additionally comprises have it
His embodiment, all technical solutions formed using equivalent transformation or equivalent replacement mode, should all fall into right of the present invention will
Within the protection domain asked.
Claims (6)
- A kind of 1. production equipment of high-purity hydrogen peroxide, it is characterised in that it is provided with high-order storage tank from top to bottom, adsorption resin column, Ion exchange resin column, intermediate storage tank, hollow fiber nanofiltration membrane component, finished product storage tank；High-order reservoir outlet by pipeline with Adsorption resin column upper inlet connects, and valve K1 is equipped with pipeline；Under adsorption resin column in outlet and ion exchange resin column Entrance is connected by pipeline and is equipped with valve K2；Outlet is connected with intermediate storage tank entrance and is equipped with valve under ion exchange resin column K3；Intermediate storage tank is connected with vacuum pump, and blow valve K4；Intermediate storage tank outlet is entered by pipeline and hollow fiber nanofiltration membrane component Mouth is connected, and pipeline is equipped with valve K5 and booster pump；Outlet is connected with finished product storage tank entrance under hollow fiber nanofiltration membrane component, and Valve K6 is equipped with connecting pipe.
- 2. the production equipment of high-purity hydrogen peroxide according to claim 1, it is characterised in that adsorption resin column is a diameter of 200mm, is highly 1000-1200mm；The absorption resin of filling is styrene or divinylbenzene, or styrene and divinylbenzene Mixture.
- 3. the production equipment of high-purity hydrogen peroxide according to claim 1, it is characterised in that ion exchange resin column diameter It is highly 1000-1400mm for 200mm；The filler material at 1/3rd position of bottom of ion exchange resin column for negative and positive from The mixture of sub-exchange resin equal proportion, the filler material of centre 1/3rd is cation exchange resin, above 1/3rd Filler material is anion exchange resin.
- 4. the production equipment of high-purity hydrogen peroxide according to claim 1, it is characterised in that hollow fiber nanofiltration membrane component For external-compression type component.
- 5. a kind of production technology of high-purity hydrogen peroxide, it is characterised in that usage right requires the high-purity hydrogen peroxide described in 1 Production equipment, comprises the following steps：（1）Impurity removes the stage：Adsorb resin and remove organic carbon contaminants and ion exchange removing unit second cation impurity；Raw material Direct storage exists in high-order storage tank after industrial hydrogen peroxide incoming inspection qualification, and K4 and K5 is closed when purification produces, is opened successively Vacuum pump, K3, K2, K1, allow industrial hydrogen peroxide to pass sequentially through adsorption resin column, middle storage are stored in after ion exchange resin column Tank, after the completion of close K1, K2, K3 and vacuum pump successively；（2）In the nanofiltration membrane stage, open K4, K5, K6 booster pump successively, allows during the hydrogen peroxide in intermediate storage tank is forced through Hollow fiber nanofiltration membrane component, removes residual impurity ion, obtains high-purity hydrogen peroxide.
- 6. the production technology of high-purity hydrogen peroxide according to claim 2, it is characterised in that impurity removes the operation in stage Temperature is 10-30 DEG C, and to vacuumize negative pressure, absolute pressure is controlled in 40-50kp operating pressure；The operation in nanofiltration membrane stage Temperature is 10-30 DEG C, and operating pressure is pressurizes, absolute pressure 500-600kp.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711440469.7A CN107902630A (en) | 2017-12-27 | 2017-12-27 | The production equipment and production technology of a kind of high-purity hydrogen peroxide |
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| CN201711440469.7A CN107902630A (en) | 2017-12-27 | 2017-12-27 | The production equipment and production technology of a kind of high-purity hydrogen peroxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102730897B1 (en) * | 2023-07-31 | 2024-11-18 | 동우 화인켐 주식회사 | Purification method and apparatus for aqueous hydrogen peroxide solution |
| KR102730899B1 (en) * | 2023-07-31 | 2024-11-18 | 동우 화인켐 주식회사 | Purification method and system aqueous hydrogen peroxide solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102730897B1 (en) * | 2023-07-31 | 2024-11-18 | 동우 화인켐 주식회사 | Purification method and apparatus for aqueous hydrogen peroxide solution |
| KR102730899B1 (en) * | 2023-07-31 | 2024-11-18 | 동우 화인켐 주식회사 | Purification method and system aqueous hydrogen peroxide solution |
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