CN113912019A - Production method of electronic grade hydrogen peroxide aqueous solution - Google Patents
Production method of electronic grade hydrogen peroxide aqueous solution Download PDFInfo
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- CN113912019A CN113912019A CN202111430784.8A CN202111430784A CN113912019A CN 113912019 A CN113912019 A CN 113912019A CN 202111430784 A CN202111430784 A CN 202111430784A CN 113912019 A CN113912019 A CN 113912019A
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- 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
- C01B15/0135—Purification by solid ion-exchangers or solid chelating agents
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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
Abstract
A production method of electronic grade aqueous hydrogen peroxide comprises feeding a part of aqueous hydrogen peroxide from the top of an evaporator (1), heating the aqueous hydrogen peroxide by the evaporator (1), feeding the heated aqueous hydrogen peroxide into a concentrated solution storage area (12) of the evaporator (1), gas generated in the concentrated solution storage area (12) enters a rectifying tower (2), the rest part of the hydrogen peroxide solution enters the rectifying tower (2) from a second feed inlet of the rectifying tower (2), part of the hydrogen peroxide solution which is combined after being concentrated by an evaporator (1) and the rectifying tower (2) is pumped into a heat exchanger (13), the hydrogen peroxide solution is cooled to normal temperature and then enters a first-stage reverse osmosis mechanism (16), reverse osmosis liquid obtained after reverse osmosis of the first-stage reverse osmosis mechanism (16) enters a second-stage reverse osmosis mechanism (21), and reverse osmosis liquid obtained after reverse osmosis of the second-stage reverse osmosis mechanism (21) is subjected to ion exchange by an ion exchange device (28) to prepare the electronic-grade hydrogen peroxide solution.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide production, in particular to a production method of an electronic-grade aqueous hydrogen peroxide solution.
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 membrane, freeze crystallization, resin method, 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.
The problems of high energy consumption, high cost, inflexible production and the like generally exist in the production of the conventional electronic grade hydrogen peroxide aqueous solution. Therefore, the problem to be solved by those skilled in the art is how to provide a method for producing an electronic-grade aqueous hydrogen peroxide solution with low energy consumption, flexibility to meet market demands, and convenience for adjusting the production process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a production method of electronic grade hydrogen peroxide aqueous solution, 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 technical problems, the invention provides a production method of an electronic grade hydrogen peroxide aqueous solution, which is prepared by concentrating industrial grade hydrogen peroxide through a hydrogen oxide concentration device, cooling through a heat exchanger, performing reverse osmosis through a first-stage reverse osmosis device and a second-stage reverse osmosis device, and performing ion exchange through an ion exchange device; the hydrogen peroxide concentration device comprises an evaporator, a rectifying tower, a condenser communicated with a gas phase outlet of the rectifying tower and a vacuum pump connected with the condenser, wherein a concentrated solution storage area of the evaporator is communicated with a first feed inlet of the rectifying tower, a dilute hydrogen peroxide feed pipe is communicated with a feed inlet of the evaporator and a second feed inlet of the rectifying tower, a steam ejector is arranged on a steam inlet pipe of the evaporator, and an air suction cavity of the steam ejector is communicated with the top of the rectifying tower through a pipeline; a first medium inlet of the heat exchanger is connected with the evaporator and a concentrated solution outlet pipeline of the rectifying tower; 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; a feed port of the ion exchange device is connected with a reverse osmosis liquid collecting pipe;
the production process comprises the following steps: feeding a part of 27.5-33 wt% aqueous hydrogen peroxide solution into the top of an evaporator, heating the aqueous hydrogen peroxide solution by the evaporator, feeding the heated aqueous hydrogen peroxide solution into a concentrated solution storage area of the evaporator, feeding gas generated in the concentrated solution storage area into a rectifying tower, feeding the rest 27.5-33 wt% aqueous hydrogen peroxide solution into the rectifying tower from a second feed inlet of the rectifying tower, concentrating the concentrated aqueous hydrogen peroxide solution by the evaporator and the rectifying tower to obtain a combined aqueous hydrogen peroxide solution with the concentration of not less than 50wt%, pumping a part of the aqueous hydrogen peroxide solution obtained by concentrating the evaporator and the rectifying tower into a heat exchanger, cooling the solution to normal temperature, feeding the cooled solution into a first-stage reverse osmosis mechanism, and performing reverse osmosis by the first-stage reverse osmosis mechanism to obtain a product with the Total Organic Carbon (TOC) concentration of less than 10 ppm and PO of less than 10 ppm3-The reverse osmosis liquid with the ion concentration lower than 10 ppm enters a second-stage reverse osmosis mechanism, and the Total Organic Carbon (TOC) concentration lower than 5 ppm and PO are obtained after reverse osmosis of the second-stage reverse osmosis mechanism3-Carrying out ion exchange on the reverse osmosis liquid with the ion concentration lower than 5 ppm by using an ion exchange device to prepare an electronic grade hydrogen peroxide aqueous solution; mixing the residual liquid after reverse osmosis by the first-stage reverse osmosis mechanism with the residual hydrogen peroxide aqueous solution after concentration by the evaporator and the rectifying tower, and collecting and storing; the reverse osmosis pressure of the first-stage reverse osmosis mechanism is controlled to be constant by controlling the pressure control valve.
As a further improved technical scheme, the production method of the electronic grade aqueous hydrogen peroxide provided by the invention 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 tower is also provided with a pure water pipe communicated with the first liquid distributor.
As a further improved technical scheme, the production method of the electronic-grade aqueous hydrogen peroxide solution provided by the invention 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 invention provides the production method of the electronic-grade aqueous hydrogen peroxide solution, wherein the number of the first-stage reverse osmosis mechanisms is more than that of the second-stage reverse osmosis mechanisms.
In the method 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 both provided with control valves.
As a further improved technical scheme, the production method of the electronic grade hydrogen peroxide water solution provided by the invention 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 invention provides a production method of the electronic grade hydrogen peroxide aqueous solution, 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 bracket and a lower annular bracket respectively connected with the inner wall of the cylindrical barrel body, a porous plate respectively positioned above the upper annular bracket and the lower annular bracket, filter cloth connected with the porous plate, a first overflow port positioned above the upper annular bracket and connected with the cylindrical barrel body, a second overflow port and at least one resin outlet positioned between the upper annular bracket and the lower annular bracket and connected with the cylindrical barrel body, a blind plate respectively detachably connected with the second overflow port and the resin outlet, a first overflow port positioned above the second overflow port and below the upper annular bracket, a second overflow port and at least one resin outlet positioned above the second overflow port and below the upper annular bracket, 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 improved technical scheme, the production method of the electronic-grade aqueous hydrogen peroxide solution further comprises a pressure relief opening and a standby opening which are connected with the top cover.
As a further improved technical scheme, the production method of the electronic-grade aqueous hydrogen peroxide solution provided by the invention is characterized in that the upper annular bracket 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 invention, the low-concentration hydrogen peroxide aqueous solution is added into the rectifying tower, the moisture of the hydrogen peroxide aqueous solution is evaporated by flash evaporation and secondary steam heat generated by the evaporator, and the secondary steam generated by the rectifying tower is absorbed by the steam ejector and mixed into the heating steam entering the evaporator, so that the purpose of energy conservation is achieved. The condensing amount of the secondary steam is reduced, so that the cooling water consumption of the condenser can be reduced. By applying a membrane separation technology and an ion exchange technology and adopting a secondary reverse osmosis mechanism, charged ions, inorganic matters, colloid particles and the like in the industrial-grade hydrogen peroxide water can be effectively removed, and the hydrogen peroxide water 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.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention. In the drawings:
FIG. 1 is a schematic flow diagram illustrating the production of 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.
When producing the electronic grade hydrogen peroxide aqueous solution, the industrial grade hydrogen peroxide aqueous solution is concentrated by a hydrogen oxide concentration device, cooled by a heat exchanger 13, subjected to reverse osmosis by a first-stage reverse osmosis device and a second-stage reverse osmosis device, and subjected to ion exchange by an ion exchange device 28. As shown in figure 1, 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 inlet of the rectifying tower 2, a dilute hydrogen peroxide feed pipe 5 is communicated with a feed inlet of the evaporator 1 and a second feed inlet of the rectifying tower 2, a steam ejector 7 is arranged on a steam inlet 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. The first medium inlet of the heat exchanger 13 is connected with the evaporator 1 and the concentrated solution outlet pipeline of the rectifying tower 2. 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.
The working principle is as follows: during production, a part of 27.5wt% -33 wt% of aqueous hydrogen peroxide enters from the top of the evaporator 1, the aqueous hydrogen peroxide enters into 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 into the rectifying tower 2, the rest part of 27.5wt% -33 wt% of aqueous hydrogen peroxide enters into the rectifying tower 2 from the second feeding hole of the rectifying tower 2, and the aqueous hydrogen peroxide concentrated by the concentrated solution storage area 12 is taken out from the bottom of the evaporator 1. The low-concentration hydrogen peroxide aqueous solution is added into the rectifying tower 2, the moisture of the hydrogen peroxide aqueous solution is evaporated by flash evaporation and the heat of secondary steam generated by an evaporator, and the secondary steam generated by the rectifying tower 2 is absorbed by the steam ejector 7 and is mixed into the heating steam entering the evaporator 1, so that the purpose of energy conservation is achieved. The amount of cooling water used in the condenser 3 can be reduced by reducing the amount of condensation of the secondary steam. 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. The concentration of the combined aqueous hydrogen peroxide solution concentrated by the evaporator 1 and the rectifying tower 2 is not less than 50wt%, and a part of the aqueous hydrogen peroxide solution concentrated by the evaporator 1 and the rectifying tower 2 is pumped into a heat exchanger 13 to be cooledCooling to normal temperature, entering a first stage reverse osmosis mechanism 16, and performing reverse osmosis by the first stage reverse osmosis mechanism 16 to obtain Total Organic Carbon (TOC) with concentration lower than 10 ppm and PO3-The reverse osmosis liquid with the ion concentration lower than 10 ppm enters a second-stage reverse osmosis mechanism 21, and the Total Organic Carbon (TOC) concentration lower than 5 ppm and PO are obtained after reverse osmosis of the second-stage reverse osmosis mechanism 213-The reverse osmosis solution with the ion concentration lower than 5 ppm is subjected to ion exchange by an ion exchange device 28 to prepare an electronic grade hydrogen peroxide aqueous 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.
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 aqueous 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 aqueous 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 reverse osmosis resistance is reduced, the filtration 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 reverse osmosis pressure of the first stage reverse osmosis mechanism 16 is controlled by the pressure control valve 27 within the bearable pressure range of the first stage reverse osmosis mechanism 16, and the yield in the production process can be adjusted.
In one embodiment, the present invention provides a method for producing an electronic-grade aqueous hydrogen peroxide solution, in which the rectifying tower 2 of the hydrogen peroxide concentration apparatus is a packed tower, the top of the tower is provided with a first liquid distributor 8, and the tower further comprises a purified water pipe 9 communicating with 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 embodiment, based on the above, the present invention provides a method for producing an electronic-grade aqueous hydrogen peroxide solution, wherein the rectifying tower 2 has a stripping section 10 at the lower part, a second liquid distributor 11 is arranged above the stripping section 10, and the dilute hydrogen peroxide feeding pipe 5 is communicated with the second liquid distributor 11.
As an example, on the basis of the foregoing, the present invention provides a method 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 embodiment, based on the above, the second reverse osmosis surplus liquid recovery pipe 23 is further communicated with the first reverse osmosis surplus liquid recovery pipe 18 through a bypass pipe, and the bypass pipe and the second reverse osmosis surplus liquid recovery pipe 23 are both 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 method for producing an electronic-grade aqueous hydrogen peroxide solution according to the present invention further comprises 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 amount 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 (9)
1. A production method of electronic grade hydrogen peroxide water solution is characterized in that industrial grade hydrogen peroxide is concentrated by a hydrogen peroxide concentration device, a heat exchanger (13) is cooled, a first-stage reverse osmosis device and a second-stage reverse osmosis device are used for reverse osmosis, and an ion exchange device (28) is used for ion exchange to obtain the electronic grade hydrogen peroxide water solution; the hydrogen peroxide concentration device is characterized by comprising an evaporator (1), a rectifying tower (2), a condenser (3) communicated with a gas phase outlet of the rectifying tower (2), and a vacuum pump (4) connected with the condenser (3), wherein a concentrated solution storage area (12) of the evaporator (1) is communicated with a first feed inlet of the rectifying tower (2), a dilute hydrogen peroxide feed pipe (5) is communicated with a feed inlet of the evaporator (1) and a second feed inlet of the rectifying tower (2), a steam inlet pipe (6) of the evaporator (1) is provided with a steam ejector (7), and a suction cavity of the steam ejector (7) is communicated with the top of the rectifying tower (2) through a pipeline; a first medium inlet of the heat exchanger (13) is connected with the evaporator (1) and a concentrated solution outlet pipeline of the rectifying tower (2); 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 a reverse osmosis liquid collecting pipe (26);
the production process comprises the following steps: a part of 27.5wt% -33 wt% of aqueous hydrogen peroxide enters from the top of an evaporator (1), the aqueous hydrogen peroxide enters a 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 a rectifying tower (2), the rest part of 27.5wt% -33 wt% of aqueous hydrogen peroxide enters the rectifying tower (2) from a second feeding hole of the rectifying tower (2), the concentration of the aqueous hydrogen peroxide combined after being concentrated by the evaporator (1) and the rectifying tower (2) is not less than 50wt%, the aqueous hydrogen peroxide obtained by concentrating a part of aqueous hydrogen peroxide obtained by the evaporator (1) and the rectifying tower (2) is pumped into a heat exchanger (13), the aqueous hydrogen peroxide enters a first-stage reverse osmosis mechanism (16) after being cooled to normal temperature, and reverse osmosis total organic carbon concentration of less than 10 ppm and PO is obtained after passing through the first-stage reverse osmosis mechanism (16)3-The reverse osmosis liquid with the ion concentration lower than 10 ppm enters a second-stage reverse osmosis mechanism (21), and the total organic carbon concentration lower than 5 ppm and PO are obtained after reverse osmosis of the second-stage reverse osmosis mechanism (21)3-The reverse osmosis solution with the ion concentration lower than 5 ppm is subjected to ion exchange by an ion exchange device (28) to prepare an electronic grade hydrogen peroxide aqueous solution; mixing the residual liquid after reverse osmosis by the first-stage reverse osmosis mechanism (16) with the part of the hydrogen peroxide aqueous solution left 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 pressure by controlling a pressure control valve (27).
2. The method for the production of an electronic-grade aqueous hydrogen peroxide solution according to claim 1, characterized in that the rectification column (2) is a packed column, the top of which is provided with a first liquid distributor (8) and has a plain water pipe (9) communicating with the first liquid distributor (8).
3. The method for the production of an aqueous solution of electronic grade hydrogen peroxide according to claim 2, characterized in that the lower part of the rectification column (2) has a stripping section (10), a second liquid distributor (11) is arranged above the stripping section (10), and the dilute hydrogen peroxide feed pipe (5) is in communication with the second liquid distributor (11).
4. Method for the production of 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).
5. The method for the production of an aqueous solution of electronic grade hydrogen peroxide according to claim 1, wherein the second reverse osmosis retentate recovery line (23) is further in communication with the first reverse osmosis retentate recovery line (18) via a bypass line, wherein the bypass line and the second reverse osmosis retentate recovery line (23) are each provided with a control valve.
6. The method for producing an electronic-grade aqueous hydrogen peroxide solution according to claim 1, further comprising a sampling pipe (29) connected to the permeate outlet connection line of the first-stage reverse osmosis mechanism (16), and a sampling control valve (30) provided on the sampling pipe (29).
7. The method for the production of an electronic-grade aqueous hydrogen peroxide solution according to claim 1, characterized in that the ion exchange device comprises a cylindrical tub body (31), a top cover (32) detachably connected to the cylindrical tub body (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 the inner wall of the cylindrical tub body (31), a porous plate (36) respectively located 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 opening (38) located above the upper ring support (35) and connected to the cylindrical tub body (31), a second overflow opening (40) and at least one resin outlet (41) located between the upper ring support (35) and the lower ring support (39) and connected to the cylindrical tub body (31), 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).
8. The method for the production of an electronic-grade aqueous hydrogen peroxide solution according to claim 7, further comprising a pressure relief port (34) and a back-up port (44) connected to the top cover (32).
9. Process for the production of an electronic-grade aqueous hydrogen peroxide solution according to claim 7, characterized in that said upper annular support (35) is provided with two diametrically symmetrical openings (45).
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| CN115521197A (en) * | 2022-10-28 | 2022-12-27 | 江苏扬农化工集团有限公司 | Method for concentrating 3-hydroxypropionaldehyde aqueous solution |
| CN115557470A (en) * | 2022-10-31 | 2023-01-03 | 湖南双阳高科化工有限公司 | Production method and production device of electronic-grade hydrogen peroxide |
| CN115744832A (en) * | 2022-11-15 | 2023-03-07 | 湖南双阳高科化工有限公司 | Hydrogen peroxide purification device and purification method |
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| 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 |
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| 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115521197A (en) * | 2022-10-28 | 2022-12-27 | 江苏扬农化工集团有限公司 | Method for concentrating 3-hydroxypropionaldehyde aqueous solution |
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| CN115557470B (en) * | 2022-10-31 | 2023-10-17 | 湖南双阳高科化工有限公司 | Production method and production device of electronic grade hydrogen peroxide |
| CN115744832A (en) * | 2022-11-15 | 2023-03-07 | 湖南双阳高科化工有限公司 | Hydrogen peroxide purification device and purification method |
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