CN216259148U - System for producing electronic-grade hydrogen peroxide water solution - Google Patents
System for producing electronic-grade hydrogen peroxide water solution Download PDFInfo
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- CN216259148U CN216259148U CN202122955967.3U CN202122955967U CN216259148U CN 216259148 U CN216259148 U CN 216259148U CN 202122955967 U CN202122955967 U CN 202122955967U CN 216259148 U CN216259148 U CN 216259148U
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Abstract
A system for producing an electronic grade aqueous hydrogen peroxide solution comprising a heat exchanger (13) connected to a hydrogen peroxide concentration device, a primary reverse osmosis device connected to the heat exchanger (13), a secondary reverse osmosis device connected to the primary reverse osmosis device, an ion exchange device (28) connected to the secondary reverse osmosis device; the primary reverse osmosis device comprises a feeding control valve (15), a primary reverse osmosis mechanism (16), a first discharging control valve (17), a first reverse osmosis residual liquid recovery pipe (18), a first explosion-proof mechanism (19) and a first emptying pipe (20); the secondary reverse osmosis device comprises a secondary reverse osmosis mechanism (21), a second discharge control valve (22), a second reverse osmosis residual liquid recovery pipe (23), a second explosion-proof mechanism (24), a second emptying pipe (25) and a reverse osmosis liquid collecting pipe (26), an outlet pipeline (14) of the heat exchanger (13) is communicated with the first reverse osmosis residual liquid recovery pipe (18), and a pressure control valve (27) is arranged on the communicating pipeline.
Description
Technical Field
The utility model relates to the technical field of hydrogen peroxide production, in particular to a system for producing electronic-grade aqueous hydrogen peroxide.
Background
The aqueous hydrogen peroxide solution is also changed into hydrogen peroxide, is an important raw material for producing peroxides such as peroxyacetic acid, thiourea peroxide and the like, and is widely applied to industries such as medicine, textile printing and dyeing, papermaking bleaching and the like. With the development of the electronics industry, electronic grade hydrogen peroxide is used as an important cleaning agent and etching agent, and the demand of the electronic grade hydrogen peroxide is gradually increased.
Electronic grade hydrogen peroxide directly affects the performance of integrated circuits and the continuity and stability of their production. The electronic-grade aqueous hydrogen peroxide solution is generally obtained by using industrial-grade aqueous hydrogen peroxide solution as a raw material and performing a series of refining and purification. The common methods include distillation, adsorption, extraction, reverse osmosis, freeze crystallization, resin, and ultrafiltration. The single unit operation is adopted to purify the industrial hydrogen peroxide aqueous solution, although the quality of the hydrogen peroxide aqueous solution can be improved, the single method has the advantages of high production energy consumption, high cost and low efficiency, and can not meet the requirements of the electronic market on the quality of hydrogen peroxide products.
CN 112062096 a discloses a production device and a production method of electronic grade aqueous hydrogen peroxide solution. The production device of the electronic-grade hydrogen peroxide water solution comprises a rectifying device, a first delivery pump, a reverse osmosis device, a second delivery pump, an ion exchange device, a third delivery pump, an ultra-pure filtering device, a fourth delivery pump and a filling device which are sequentially connected through pipelines. Rectifying, reverse osmosis and ion exchange are carried out on industrial-grade hydrogen peroxide, and finally, an electronic-grade hydrogen peroxide water solution is obtained through ultrafiltration membrane filtration.
At present, equipment for producing electronic grade hydrogen peroxide water solution generally has the problems of high energy consumption, high cost, inflexible production and the like. Therefore, the problem to be solved by the technical personnel in the field is how to provide an electronic-grade hydrogen peroxide aqueous solution production device which has low energy consumption, can flexibly adapt to market demands and is convenient for production process adjustment.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model aims to provide a system for producing electronic-grade aqueous hydrogen peroxide, which can effectively reduce energy consumption and cooling water consumption, flexibly adapt to market demands and facilitate production and adjustment.
In order to solve the above technical problems, the present invention provides a system for producing an electronic-grade aqueous hydrogen peroxide solution, comprising a hydrogen peroxide concentration device, a heat exchanger connected with the hydrogen peroxide concentration device through a pipeline, a primary reverse osmosis device connected with the heat exchanger through a pipeline, a secondary reverse osmosis device connected with the primary reverse osmosis device through a pipeline, and an ion exchange device connected with the secondary reverse osmosis device through a pipeline; a first medium inlet of the heat exchanger is connected with a concentrated solution outlet pipeline of the hydrogen peroxide concentration device; the first-stage reverse osmosis device comprises a plurality of feeding control valves with inlets communicated with a first medium outlet pipeline of the heat exchanger, a first-stage reverse osmosis mechanism with a plurality of feeding ports communicated with outlets of the feeding control valves through pipelines, a plurality of first discharging control valves communicated with reverse osmosis residual liquid outlets of the first-stage reverse osmosis mechanism, a first reverse osmosis residual liquid recovery pipe communicated with the first discharging control valves, a first explosion-proof mechanism with a first end communicated with the feeding ports of the first-stage reverse osmosis mechanism through pipelines, and a first emptying pipe connected with the other end of the first explosion-proof mechanism; the second-stage reverse osmosis device comprises a second-stage reverse osmosis mechanism, a second discharging control valve, a second reverse osmosis residual liquid recovery pipe, a second explosion-proof mechanism, a second emptying pipe and a reverse osmosis liquid collecting pipe, wherein at least one feeding hole of the second-stage reverse osmosis mechanism is communicated with a penetrating liquid outlet of the first-stage reverse osmosis mechanism through a pipeline, the second discharging control valve is connected with a reverse osmosis residual liquid outlet of the second-stage reverse osmosis mechanism through a pipeline, the second reverse osmosis residual liquid recovery pipe is connected with the second discharging control valve, the first end of the second explosion-proof mechanism is communicated with a reverse osmosis residual liquid outlet of the second-stage reverse osmosis mechanism through a pipeline, the second emptying pipe is connected with the other end of the second explosion-proof mechanism, and the reverse osmosis liquid collecting pipe is communicated with a penetrating liquid outlet of the second-stage reverse osmosis mechanism; the first medium outlet pipeline is communicated with the first reverse osmosis residual liquid recovery pipe, and a pressure control valve is arranged on the communicating pipeline; the first reverse osmosis residual liquid recovery pipe is connected with a concentrated liquid collecting pipeline of the evaporator or/and the rectifying tower; and a feed inlet of the ion exchange device is connected with the reverse osmosis liquid collecting pipe.
As a further improved technical solution, the system for producing an electronic-grade aqueous hydrogen peroxide solution provided by the present invention comprises an evaporator, a rectifying tower, a condenser communicated with a gas phase outlet of the rectifying tower, and a vacuum pump connected to the condenser, wherein a concentrated solution storage area of the evaporator is communicated with a first feed port of the rectifying tower, a dilute hydrogen peroxide feed pipe is communicated with a feed port of the evaporator and a second feed port of the rectifying tower, a steam pipe of the evaporator is provided with a steam ejector, and a suction cavity of the steam ejector is communicated with a tower top of the rectifying tower through a pipeline.
As a further improved technical scheme, the system for producing the electronic-grade aqueous hydrogen peroxide provided by the utility model has the advantages that the rectifying tower is a packed tower, the top of the tower is provided with a first liquid distributor, and the system is also provided with a pure water pipe communicated with the first liquid distributor.
As a further improved technical scheme, the system for producing the electronic-grade aqueous hydrogen peroxide provided by the utility model is characterized in that the lower part of the rectifying tower is provided with a stripping section, a second liquid distributor is arranged above the stripping section, and a dilute hydrogen peroxide feeding pipe is communicated with the second liquid distributor.
As a further improvement, the present invention provides a system for producing an electronic-grade aqueous hydrogen peroxide solution, wherein the number of the first stage reverse osmosis mechanisms is greater than the number of the second stage reverse osmosis mechanisms.
In the system for producing the electronic-grade aqueous hydrogen peroxide solution, the second reverse osmosis surplus solution recovery pipe is communicated with the first reverse osmosis surplus solution recovery pipe through a bypass pipeline, and the bypass pipeline and the second reverse osmosis surplus solution recovery pipe are respectively provided with a control valve.
As a further improved technical scheme, the system for producing the electronic-grade aqueous hydrogen peroxide solution also comprises a sampling pipe and a sampling control valve, wherein the sampling pipe is communicated with a penetrating fluid outlet connecting pipeline of the first-stage reverse osmosis mechanism, and the sampling control valve is arranged on the sampling pipe.
As a further improvement, the utility model provides a system for producing electronic-grade aqueous hydrogen peroxide, wherein the ion exchange device comprises a cylindrical barrel body, a top cover detachably connected with the cylindrical barrel body, a vent pipe connected with the top cover, an upper annular support and a lower annular support respectively connected with the inner wall of the cylindrical barrel body, a porous plate respectively positioned above the upper annular support and the lower annular support, filter cloth connected with the porous plate, a first overflow port positioned above the upper annular support and connected with the cylindrical barrel body, a second overflow port and at least one resin outlet positioned between the upper annular support and the lower annular support and connected with the cylindrical barrel body, a blind plate respectively detachably connected with the second overflow port and the resin outlet, a blind plate positioned above the second overflow port and below the upper annular support, a blind plate positioned above the second overflow port and detachably connected with the resin outlet, The liquid inlet is connected with the cylindrical barrel body, and the liquid outlet is connected with the bottom of the cylindrical barrel body; the resin outlet is located below the second overflow.
As a further improvement technical scheme, the system for producing the electronic-grade aqueous hydrogen peroxide further comprises a pressure relief opening and a standby opening which are connected with the top cover.
As a further improvement, the utility model provides the system for producing the electronic-grade aqueous hydrogen peroxide solution, wherein the upper annular support is provided with two symmetrical openings along the diameter direction.
The aforementioned improvements can be implemented individually or in combination without conflict.
According to the technical scheme provided by the utility model, a membrane separation technology and an ion exchange technology are applied, and a secondary reverse osmosis mechanism is adopted to effectively remove charged ions, inorganic substances, colloid particles and the like in industrial-grade hydrogen peroxide water solution, so that the hydrogen peroxide water solution with the conductivity meeting the requirement of electronic-grade hydrogen peroxide is obtained. The feeding and discharging of the first-stage reverse osmosis mechanism are in a large flow mode, so that industrial-grade hydrogen peroxide aqueous solution can wash the surface of the reverse osmosis membrane of the first-stage reverse osmosis mechanism, charged ions, inorganic substances with large molecular weight and colloidal particles attached to the surface of the reverse osmosis membrane are taken away, the filtering efficiency is improved, and the maintenance workload is reduced. The reverse osmosis pressure of the first-stage reverse osmosis mechanism can be guaranteed through pressure control, production is carried out under stable reverse osmosis pressure, production efficiency can be improved, the first-stage reverse osmosis mechanism is prevented from running at overpressure, and the yield of the system can be conveniently adjusted through pressure control.
In the improvement scheme, add low concentration hydrogen peroxide aqueous solution to the rectifying column, through the flash distillation and the secondary steam heat that utilizes the evaporimeter to produce, evaporate hydrogen peroxide aqueous solution's moisture, the secondary steam that inhales the rectifying column through the steam ejector produces mixes into the heating steam that gets into the evaporimeter in, reaches energy-conserving purpose. The condensing amount of the secondary steam is reduced, so that the cooling water consumption of the condenser can be reduced.
Drawings
The accompanying drawings are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the utility model and together with the description serve to explain the utility model without limiting the utility model. In the drawings:
FIG. 1 is a schematic structural diagram of a system for producing an electronic-grade aqueous hydrogen peroxide solution according to an embodiment;
FIG. 2 is a schematic structural view of an ion exchange apparatus in an embodiment;
FIG. 3 is a schematic view of the structure of FIG. 2 along line A-A;
FIG. 4 is a schematic view of the structure of FIG. 2 along the line B-B;
FIG. 5 is a schematic view showing the structure of the ion exchange unit according to the embodiment after the upper ring support, the porous plate and the filter cloth are combined;
FIG. 6 is a schematic structural diagram of an upper ring support of the ion exchange device in accordance with an embodiment.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
The system for producing an electronic-grade aqueous hydrogen peroxide solution as shown in fig. 1 comprises a hydrogen peroxide concentration device, a heat exchanger 13 connected to the hydrogen peroxide concentration device through a pipeline, a primary reverse osmosis device connected to the heat exchanger 13 through a pipeline, a secondary reverse osmosis device connected to the primary reverse osmosis device through a pipeline, and an ion exchange device 28 connected to the secondary reverse osmosis device through a pipeline. The first medium inlet of the heat exchanger 13 is connected with the concentrated solution outlet pipeline of the hydrogen peroxide concentration device. The first-stage reverse osmosis device comprises a plurality of feeding control valves 15, a plurality of feeding ports of which are communicated with a first medium outlet pipeline 14 of a heat exchanger 13, a first-stage reverse osmosis mechanism 16, a plurality of first discharging control valves 17, a first reverse osmosis residual liquid recovery pipe 18, a first explosion-proof mechanism 19 and a first emptying pipe 20, wherein the feeding ports of the first-stage reverse osmosis mechanism 16 are respectively communicated with the outlet of the feeding control valve 15 through pipelines, the first discharging control valves 17 are respectively communicated with the reverse osmosis residual liquid outlet of the first-stage reverse osmosis mechanism 16, the first reverse osmosis residual liquid recovery pipe 18 is communicated with the first discharging control valves 17, the first end of the first explosion-proof mechanism 19 is communicated with the feeding ports of the first-stage reverse osmosis mechanism 16 through pipelines, and the first emptying pipe 20 is connected with the other end of the first explosion-proof mechanism 19; the second-stage reverse osmosis device comprises a second-stage reverse osmosis mechanism 21 with at least one feed inlet communicated with a penetrating fluid outlet of the first-stage reverse osmosis mechanism 16 through a pipeline, a second discharge control valve 22 connected with a reverse osmosis residual fluid outlet of the second-stage reverse osmosis mechanism 21 through a pipeline, a second reverse osmosis residual fluid recovery pipe 23 connected with the second discharge control valve 22, a second anti-explosion mechanism 24 with a first end communicated with the reverse osmosis residual fluid outlet of the second-stage reverse osmosis mechanism 21 through a pipeline, a second emptying pipe 25 connected with the other end of the second anti-explosion mechanism 24, and a reverse osmosis fluid collection pipe 26 communicated with a penetrating fluid outlet of the second-stage reverse osmosis mechanism 21; a first medium outlet pipeline 14 of the heat exchanger 13 is communicated with a first reverse osmosis residual liquid recovery pipe 18, and a pressure control valve 27 is arranged on a communication pipeline of the first medium outlet pipeline and the first reverse osmosis residual liquid recovery pipe; the first reverse osmosis residual liquid recovery pipe 18 is connected with a concentrated liquid collecting pipeline of the evaporator 1 or/and the rectifying tower 2; the feed inlet of the ion exchange unit 28 is connected to the reverse osmosis liquid collecting pipe 26.
Pumping the hydrogen peroxide water solution obtained by the concentration of the hydrogen oxide concentration device into a heat exchanger 13, cooling to normal temperature, then entering a first-stage reverse osmosis mechanism 16, entering a second-stage reverse osmosis mechanism 21 by using a reverse osmosis liquid obtained by the reverse osmosis of the first-stage reverse osmosis mechanism 16, and carrying out ion exchange on a reverse osmosis liquid obtained by the reverse osmosis of the second-stage reverse osmosis mechanism 21 by using an ion exchange device 28 to prepare an electronic-stage hydrogen peroxide water solution; mixing the residual liquid after reverse osmosis by the first-stage reverse osmosis mechanism 16 with the residual part of the aqueous hydrogen peroxide solution after concentration by the evaporator 1 and the rectifying tower 2, and collecting and storing; the reverse osmosis pressure of the first stage reverse osmosis mechanism 16 is controlled to be constant by controlling the pressure control valve 27, and the reverse osmosis pressure of the first stage reverse osmosis mechanism 16 is controlled by controlling the pressure control valve 27, so that the yield in the production process can be adjusted.
The reverse osmosis membranes in the first stage reverse osmosis mechanism 16 and the second stage reverse osmosis mechanism 21 can be aromatic polyamide membranes, polyamide piperazine membranes, polysulfone membranes, polyvinyl chloride membranes and the like, under the action of pressure, water and small molecular substances of hydrogen peroxide can pass through the reverse osmosis membranes, while charged ions, inorganic substances with large molecular weight and colloidal particles cannot pass through the reverse osmosis membranes, so that the hydrogen peroxide solution at the penetrating fluid outlet of the reverse osmosis mechanism can effectively remove the charged ions, the inorganic substances with large molecular weight and the colloidal particles, thereby improving the purity of the hydrogen peroxide solution and reducing the conductivity. In the production process, different grades of products can be obtained by changing the material of the reverse osmosis membrane, the layer number of the membrane and the type of the ion exchange resin, and different grades of products can also be obtained from the penetrating fluid outlets of the first-stage reverse osmosis mechanism 16 and the second-stage reverse osmosis mechanism 21.
The residual concentrated solution after reverse osmosis by the first-stage reverse osmosis mechanism 16 is collected by the first reverse osmosis residual solution recovery pipe 18 to obtain a hydrogen peroxide byproduct, and the hydrogen peroxide byproduct can be mixed into an industrial-grade hydrogen peroxide product for sale, and the residual concentrated solution after reverse osmosis by the second-stage reverse osmosis mechanism 21 is collected by the second reverse osmosis residual solution recovery pipe 23 to obtain the hydrogen peroxide byproduct, and can also be mixed into the industrial-grade hydrogen peroxide product for sale. When the pressure in the first-stage reverse osmosis mechanism 16 exceeds the safety pressure, the explosion-proof sheet of the first explosion-proof mechanism 19 is broken, and the hydrogen peroxide water enters the first exhaust pipe 20 to release the pressure of the first-stage reverse osmosis mechanism 16; when the pressure in the second-stage reverse osmosis mechanism 21 exceeds the safety pressure, the explosion-proof sheet of the second explosion-proof mechanism 24 is broken, and the hydrogen peroxide water solution enters the second emptying pipe 25 to release the pressure of the second-stage reverse osmosis mechanism 21, so that the reverse osmosis membranes of the first-stage reverse osmosis mechanism 16 and the second-stage reverse osmosis mechanism 21 are protected. The first medium outlet pipeline 14 of the heat exchanger 13 is communicated with the first reverse osmosis residual liquid recovery pipe 18, a pressure control valve 27 is arranged on a communication pipeline, a large-flow mode is adopted for feeding and discharging of the first-stage reverse osmosis mechanism 16 in the production process, and the surface of a reverse osmosis membrane of the first-stage reverse osmosis mechanism 16 is washed by the aqueous hydrogen peroxide solution, so that charged ions attached to the surface of the reverse osmosis membrane, inorganic substances with large molecular weight and colloidal particles can be taken away, the filtering efficiency is improved, and the maintenance workload is reduced. The reverse osmosis pressure of the first-stage reverse osmosis mechanism 16 is controlled to be constant by controlling the pressure control valve 27, so that the reverse osmosis working pressure of the first-stage reverse osmosis mechanism 16 is guaranteed, production is performed under the stable reverse osmosis pressure, the production efficiency can be improved, and the first-stage reverse osmosis mechanism 16 is prevented from running under overpressure. The production rate during production can be adjusted by adjusting the reverse osmosis pressure within the range of the pressure that can be carried by the first stage reverse osmosis mechanism 16.
As an example, as shown in fig. 1, the hydrogen peroxide concentration apparatus includes an evaporator 1, a rectifying tower 2, a condenser 3 communicating with a gas phase outlet of the rectifying tower 2, and a vacuum pump 4 connected to the condenser 3. The concentrated solution storage area 12 of the evaporator 1 is communicated with the first feed inlet of the rectifying tower 2, the dilute hydrogen peroxide feed pipe 5 is communicated with the feed inlet of the evaporator 1 and the second feed inlet of the rectifying tower 2, the steam pipe 6 of the evaporator 1 is provided with a steam ejector 7, and the air suction cavity of the steam ejector 7 is communicated with the top of the rectifying tower 2 through a pipeline.
During production, a part of dilute aqueous hydrogen peroxide enters from the top of the evaporator 1, the dilute aqueous hydrogen peroxide enters the concentrated solution storage area 12 of the evaporator 1 after being heated by the evaporator 1, gas generated in the concentrated solution storage area 12 enters the rectifying tower 2, the rest part of dilute aqueous hydrogen peroxide enters the rectifying tower 2 from the second feeding hole of the rectifying tower 2, and the concentrated aqueous hydrogen peroxide in the concentrated solution storage area 12 is taken out from the bottom of the evaporator 1. The vaporous liquid drops are removed when the gas-phase material in the rectifying tower 2 passes through the packing layer, the liquid phase flows back to the bottom of the rectifying tower 2, the gas phase enters the condenser 3 and is condensed by the condenser 3, and part of the gas phase can be sucked by the steam ejector 7 and doped into steam for a heating source of the evaporator 1. Adding low-concentration hydrogen peroxide solution into the rectifying tower 2, evaporating the water content of the hydrogen peroxide solution by flash evaporation and utilizing the heat of secondary steam generated by the evaporator, sucking the secondary steam generated by the rectifying tower 2 through the steam ejector 7 and mixing the secondary steam into the heating steam entering the evaporator 1, thereby achieving the purpose of energy conservation. The amount of cooling water used in the condenser 3 can be reduced by reducing the amount of condensation of the secondary steam.
In the system for producing an electronic-grade aqueous hydrogen peroxide solution according to the present invention, the rectifying tower 2 is a packed tower, and the top of the tower is provided with a first liquid distributor 8 and a pure water pipe 9 connected to the first liquid distributor 8. By injecting pure water into the rectifying tower 2, the secondary steam generated by the rectifying tower 2 can be cooled and the concentration of the hydrogen peroxide discharged from the rectifying tower 2 can be adjusted. The load of the condenser 3 and the amount of cooling water can be reduced by cooling the secondary steam generated in the rectifying tower 2 with pure water.
In the system for producing an electronic-grade aqueous hydrogen peroxide solution according to the present invention, the lower portion of the rectifying tower 2 has a stripping section 10, a second liquid distributor 11 is disposed above the stripping section 10, and the dilute hydrogen peroxide feeding pipe 5 is connected to the second liquid distributor 11.
As an example, based on the foregoing, the present invention provides a system for producing an electronic-grade aqueous hydrogen peroxide solution, wherein the number of the first-stage reverse osmosis mechanisms 16 is greater than the number of the second-stage reverse osmosis mechanisms 21. For example, the ratio of the number of first stage reverse osmosis mechanisms 16 to the number of second stage reverse osmosis mechanisms 21 is 2: 1. The amount of permeate obtained by the first stage reverse osmosis mechanism 16 is less than the amount of hydrogen peroxide entering the first stage reverse osmosis mechanism 16, and the second stage reverse osmosis mechanism 21 adopts a smaller amount, which is beneficial to reducing the investment cost and maintaining the working pressure of the second stage reverse osmosis mechanism 21.
In the system for producing an electronic-grade aqueous hydrogen peroxide solution according to the present invention, the second reverse osmosis raffinate recovery pipe 23 is further connected to the first reverse osmosis raffinate recovery pipe 18 via a bypass line, and the bypass line and the second reverse osmosis raffinate recovery pipe 23 are provided with control valves. The concentrated solution passing through the second reverse osmosis raffinate recovery pipe 23 may be mixed into an industrial-grade hydrogen peroxide product for sale, and the aqueous hydrogen peroxide solution collected by the second reverse osmosis raffinate recovery pipe 23 may be separately sold or mixed into an industrial-grade hydrogen peroxide product for sale, as required.
In one embodiment, the present invention provides a system for producing an electronic-grade aqueous hydrogen peroxide solution, further comprising a sampling pipe 29 connected to the permeate outlet connection line of the first-stage reverse osmosis unit 16, and a sampling control valve 30 provided on the sampling pipe 29. The sampling pipe 29 can be used for sampling and detecting the penetrating fluid of the first-stage reverse osmosis mechanism 16, and has the main function of acquiring the penetrating fluid with corresponding quality requirements from the sampling pipe 29 so as to meet different requirements.
As one example, as shown in FIGS. 2 to 6, an ion exchange apparatus according to the present invention includes a cylindrical tub 31, a top cover 32 detachably connected to the cylindrical tub 31, a blow-off pipe 33 connected to the top cover 32, an upper ring support 35 and a lower ring support 39 respectively connected to an inner wall of the cylindrical tub 31, a porous plate 36 respectively positioned above the upper ring support 35 and the lower ring support 39, a filter cloth 37 connected to the porous plate 36, a first overflow port 38 positioned above the upper ring support 35 and connected to the cylindrical tub 31, a second overflow port 40 and at least one resin outlet 41 positioned between the upper ring support 35 and the lower ring support 39 and connected to the cylindrical tub 31, a blind plate detachably connected to the second overflow port 40 and the resin outlet 41, a blind plate positioned above the second overflow port 40 and positioned below the upper ring support 35, A liquid inlet 42 connected to the cylindrical barrel body 31, a liquid outlet 43 connected to the bottom of the cylindrical barrel body 31; the resin outlet 41 is located below the second overflow outlet 40. And includes a pressure relief vent 34 and a backup vent 44 connected to the top cover 32. The upper annular support 35 is provided with two diametrically symmetrical openings 45.
The ion exchange resin can be added from the second overflow port 40, and when the ion exchange resin is added to be level with the second overflow port 40, the addition of the ion exchange resin is enough, and the addition is stopped. When the resin is replaced or cleaned, the ion exchange resin can be discharged by removing the blind plate of the resin outlet 41. Two symmetrical openings 45 are formed in the upper annular support 35 along the diameter direction, so that the lower porous plate 36 can be conveniently taken and placed. The obtained reverse osmosis hydrogen oxide water solution enters the cylindrical barrel body 31 from the liquid inlet 42, after ion exchange is carried out by ion exchange resin, the obtained reverse osmosis hydrogen oxide water solution flows out from the liquid outlet 43, the ion exchange resin is positioned between the upper filter cloth 37 and the lower filter cloth 37, and even if the ion exchange resin is disturbed by the liquid inlet, the ion exchange resin layer can not float greatly, so that the resin is prevented from returning and the exchange mass transfer process is enhanced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention in any way, and various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A system for producing an electronic grade aqueous hydrogen peroxide solution comprising a hydrogen peroxide concentration device, a heat exchanger (13) connected to the hydrogen peroxide concentration device by a pipeline, a primary reverse osmosis device connected to the heat exchanger (13) by a pipeline, a secondary reverse osmosis device connected to the primary reverse osmosis device by a pipeline, an ion exchange device (28) connected to the secondary reverse osmosis device by a pipeline; the device is characterized in that a first medium inlet of the heat exchanger (13) is connected with a concentrated solution outlet pipeline of the hydrogen peroxide concentration device; the primary reverse osmosis device comprises a plurality of feeding control valves (15) with inlets communicated with a first medium outlet pipeline (14) of the heat exchanger (13), a plurality of primary reverse osmosis mechanisms (16) with inlets communicated with outlets of the feeding control valves (15) through pipelines, a plurality of primary discharging control valves (17) communicated with reverse osmosis residual liquid outlets of the primary reverse osmosis mechanisms (16), first reverse osmosis residual liquid recovery pipes (18) communicated with the primary discharging control valves (17), first explosion-proof mechanisms (19) with first ends communicated with the feeding inlets of the primary reverse osmosis mechanisms (16) through pipelines, and first emptying pipes (20) connected with the other ends of the first explosion-proof mechanisms (19); the second-stage reverse osmosis device comprises a second-stage reverse osmosis mechanism (21) with at least one feed inlet communicated with a penetrating fluid outlet of the first-stage reverse osmosis mechanism (16) through a pipeline, a second discharge control valve (22) connected with a reverse osmosis residual fluid outlet of the second-stage reverse osmosis mechanism (21) through a pipeline, a second reverse osmosis residual fluid recovery pipe (23) connected with the second discharge control valve (22), a second explosion-proof mechanism (24) with a first end communicated with the reverse osmosis residual fluid outlet of the second-stage reverse osmosis mechanism (21) through a pipeline, a second emptying pipe (25) connected with the other end of the second explosion-proof mechanism (24), and a reverse osmosis fluid collecting pipe (26) communicated with the penetrating fluid outlet of the second-stage reverse osmosis mechanism (21); the first medium outlet pipeline (14) is communicated with a first reverse osmosis residual liquid recovery pipe (18), and a pressure control valve (27) is arranged on a communication pipeline of the first medium outlet pipeline; the first reverse osmosis residual liquid recovery pipe (18) is connected with a concentrated liquid collecting pipeline of the evaporator (1) or/and the rectifying tower (2); the feed inlet of the ion exchange device (28) is connected with the reverse osmosis liquid collecting pipe (26).
2. The system for producing an electronic-grade aqueous hydrogen peroxide solution according to claim 1, wherein the hydrogen peroxide concentration device comprises an evaporator (1), a rectifying tower (2), a condenser (3) communicated with a gas phase outlet of the rectifying tower (2), a vacuum pump (4) connected with the condenser (3), a concentrated solution storage area (12) of the evaporator (1) is communicated with a first feed port of the rectifying tower (2), a dilute hydrogen peroxide feed pipe (5) is communicated with a feed port of the evaporator (1) and a second feed port of the rectifying tower (2), a steam ejector (7) is arranged on a steam pipe (6) of the evaporator (1), and a suction cavity of the steam ejector (7) is communicated with the top of the rectifying tower (2) through a pipeline.
3. System for producing an electronic grade aqueous hydrogen peroxide solution according to claim 2, characterized in that the rectification column (2) is a packed column, the top of which is provided with a first liquid distributor (8) and further having a plain water pipe (9) communicating with the first liquid distributor (8).
4. System for producing an aqueous solution of electronic grade hydrogen peroxide according to claim 3, characterized in that the lower part of the rectification column (2) has a stripping section (10), a second liquid distributor (11) is provided above the stripping section (10), and the dilute hydrogen peroxide feeding pipe (5) communicates with the second liquid distributor (11).
5. A system for producing an electronic-grade aqueous hydrogen peroxide solution according to claim 1, characterized in that the number of first-stage reverse osmosis mechanisms (16) is greater than the number of second-stage reverse osmosis mechanisms (21).
6. A system for producing an aqueous solution of electronic grade hydrogen peroxide according to claim 1, characterized in that the second reverse osmosis retentate recovery tube (23) is further in communication with the first reverse osmosis retentate recovery tube (18) via a bypass line, wherein a control valve is provided on both the bypass line and the second reverse osmosis retentate recovery tube (23).
7. A system for the production of an aqueous solution of electronic grade hydrogen peroxide according to claim 1, characterized by a sampling pipe (29) communicating with the permeate outlet connection of the first stage reverse osmosis mechanism (16), a sampling control valve (30) being provided on said sampling pipe (29).
8. The system for producing an electronic-grade aqueous hydrogen peroxide solution according to claim 1, wherein the ion exchange device comprises a cylindrical barrel body (31), a top cover (32) detachably connected to the cylindrical barrel body (31), a vent pipe (33) connected to the top cover (32), an upper annular support (35) and a lower annular support (39) respectively connected to the inner wall of the cylindrical barrel body (31), a porous plate (36) respectively located above the upper annular support (35) and the lower annular support (39), a filter cloth (37) connected to the porous plate (36), a first overflow port (38) located above the upper annular support (35) and connected to the cylindrical barrel body (31), a second overflow port (40) located between the upper annular support (35) and the lower annular support (39) and connected to the cylindrical barrel body (31), and at least one resin outlet (41), a blind plate detachably connected with the second overflow port (40) and the resin outlet (41), a liquid inlet (42) located above the second overflow port (40) and below the upper annular support (35) and connected with the cylindrical barrel body (31), and a liquid outlet (43) connected with the bottom of the cylindrical barrel body (31); the resin outlet (41) is located below the second overflow outlet (40).
9. The system for producing an electronic-grade aqueous hydrogen peroxide solution according to claim 8, further comprising a pressure relief port (34) and a back-up port (44) connected to the top cap (32).
10. System for producing an aqueous solution of electronic grade hydrogen peroxide according to claim 8, characterized in that said upper annular support (35) is provided with two diametrically symmetrical openings (45).
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| CN115650178A (en) * | 2022-11-17 | 2023-01-31 | 安徽金禾实业股份有限公司 | Method for refining electronic-grade hydrogen peroxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650178A (en) * | 2022-11-17 | 2023-01-31 | 安徽金禾实业股份有限公司 | Method for refining electronic-grade hydrogen peroxide |
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