CN106496011B - Oxalic acid production system - Google Patents
Oxalic acid production system Download PDFInfo
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- CN106496011B CN106496011B CN201610842381.7A CN201610842381A CN106496011B CN 106496011 B CN106496011 B CN 106496011B CN 201610842381 A CN201610842381 A CN 201610842381A CN 106496011 B CN106496011 B CN 106496011B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C55/00—Saturated compounds having more than one carboxyl group bound to acyclic carbon atoms
- C07C55/02—Dicarboxylic acids
- C07C55/06—Oxalic acid
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
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Abstract
The invention provides an oxalic acid production system, which comprises a dissolving tank, a concentrated solution delivery pump and a filtering device which are sequentially connected, wherein the back of the filtering device is also connected with at least two sets of same or different splicing and filling devices in parallel, the concentrated solution delivery pump is also in circulating connection with the dissolving tank and is used for circularly dissolving oxalic acid, the dissolving tank is provided with a feed port and is also connected with a first pure water inlet pipe, the dissolving tank is also provided with a high-position bottom valve and a low-position bottom valve, the high-position bottom valve and the low-position bottom valve are both connected with the concentrated solution delivery pump, the high-position bottom valve is used for opening when oxalic acid powder is not completely dissolved so as to realize continuous circulation of the solution, the low-position bottom valve is used for opening when the oxalic acid powder is completely dissolved so as to deliver the solution for filtering, and the low-position bottom valve is also connected with an inert gas inlet. The invention has reasonable structure, skillfully solves various problems and difficulties in the oxalic acid dissolving process, can be used for continuous production, has strong practicability and is worthy of popularization.
Description
Technical Field
The invention relates to the field of chemical production, and mainly relates to an oxalic acid production system.
Background
The Indium Tin Oxide (ITO) conductive film is a high-technology product obtained by sputtering a transparent ITO conductive film layer on a transparent organic film material by adopting a magnetron sputtering method and carrying out high-temperature annealing treatment. ITO conductive films are widely used in Liquid Crystal Displays (LCDs), solar cells, microelectronic ITO conductive film glasses, optoelectronics, and various optical fields. In the panel process of the industries such as thin film field effect transistor liquid crystal display (TFT-LCD), light emitting diode (LCD), Organic Light Emitting Diode (OLED) and the like, a hydrochloric acid/nitric acid mixed aqueous solution, a hydrochloric acid/ferric trichloride aqueous solution, an oxalic acid aqueous solution, an iodic acid aqueous solution, a phosphoric acid aqueous solution and the like are generally adopted for etching the indium tin oxide semiconductor transparent conductive film (ITO). With the continuous improvement of the technology, the oxalic acid ITO etching solution has the unique property of etching an ITO layer under a mild condition, and more manufacturers develop and research the ITO layer.
The main raw materials of oxalic acid system ITO etching solution is the oxalic acid, and the raw materials oxalic acid powder of production oxalic acid exists that the purity is lower, easy crystallization, the difficult problem of dissolving completely in the short time, directly cause the pipeline to be easily blockked up at present oxalic acid production system, filtration system need often shut down the washing, the problem of change, the production efficiency of oxalic acid has seriously been reduced, the manual demand is many, and, the addition mode of additive also easily causes the pipeline to block up, people need production efficiency higher, practice thrift the oxalic acid production system of manpower, the present case produces from this.
Disclosure of Invention
The invention aims to solve the technical problem of providing an oxalic acid production system which has reasonable integral structure and high production efficiency and can continuously produce.
The invention is realized by the following technical scheme:
an oxalic acid production system is characterized by comprising a dissolving tank, a concentrated solution delivery pump and a filtering device which are connected in sequence, at least two sets of same or different matching and filling devices are connected in parallel behind the filtering device, the concentrated solution delivery pump is also circularly connected with the dissolving tank for circularly dissolving oxalic acid, the dissolving tank is provided with a feed opening for feeding oxalic acid powder, the dissolving tank is also connected with a first pure water inlet pipe, the dissolving tank is also provided with a high-level bottom valve and a low-level bottom valve, the high-position bottom valve and the low-position bottom valve are both connected with a concentrated solution delivery pump, the high-position bottom valve is used for opening when the oxalic acid powder is not completely dissolved so as to realize the continuous circulation of the solution, the low-level bottom valve is used for opening when the oxalic acid powder is completely dissolved so as to send the solution to filtration, the low-level bottom valve is also connected with an inert gas inlet and is used for filling high-purity inert gas into the dissolving tank to accelerate the dissolution of the oxalic acid powder. Preferably, the inert gas is nitrogen or argon.
Preferably, the filtering device comprises at least one group of filtering units, the number of the filtering units can be adjusted according to the requirements of customers, products with different specifications can be simultaneously produced by adjusting the filtering filter elements, and the filtering device can be connected with a plurality of matching and canning devices.
More preferably, the filter unit is an in-line filter device.
Further, online filter equipment contains casing, cross slab, the cross slab sets up in the casing and divide into upper and lower two chambeies with its inner chamber, it disposes a plurality of filter cores to go up the intracavity, be connected with feed liquor pipe and play water outlet duct on the epicoele, be connected with drain pipe and inlet tube on the lower chamber, between feed liquor pipe, play water outlet duct, drain pipe and inlet tube and the casing, all be equipped with the valve, online filtering step is: when normal filtration is carried out, the valves of the water inlet pipe and the water outlet pipe are closed, and the valves of the water inlet pipe and the water outlet pipe are opened; when filter equipment needs to wash, close the valve of feed liquor pipe and drain pipe, open the valve of inlet tube and play water outlet duct, then wash into water from the inlet tube for wash away the outer impurity of filter core, sewage is discharged from play water outlet duct again. The pressure is exerted when the inlet tube intakes for most impurity on the filter core will all be washed away from the filter core surface, and in the whole process, the backwash water consumption is few, and need not shut down the renew cartridge, has greatly protected the filter core to reduce the change frequency of filter core, has practiced thrift equipment cost, and the benefit realizes serialization and automated production, has improved production efficiency greatly.
Preferably, the filter element part is provided with a circulating filter device, and a plurality of serial and parallel structures are adopted for filtering.
Preferably, the feeding port is a feeding platform, so that the feeding and observation of the oxalic acid powder are facilitated. The upper high-precision metering equipment can accurately feed materials, is convenient to operate and can better monitor the real production flow.
Preferably, the at least one set of blending and filling device comprises a blending tank, a circulating pump, a filter cabinet and a filling machine which are sequentially connected, at least one set of feeding device is further connected between the blending tank and the circulating pump, the feeding devices can be connected in parallel or in series as required, the fed substances can be raw materials, auxiliary materials or auxiliaries and additives, can be solid or liquid, and multiple feeding devices can feed materials simultaneously or feed materials sequentially.
Furthermore, a second pure water inlet pipe and a sample sampling port are connected to the splicing tank.
Furthermore, a first valve is arranged between the splicing tank and the feeding device, a second valve is arranged on the circulating pump, the feeding device comprises a metering tank and a third valve arranged below the metering tank, the metering tank is connected between the splicing tank and the circulating pump through the third valve, and the feeding step comprises the following steps: when materials need to be added, all the valves of the first valve, the second valve and the third valve are closed, the required materials are added into the metering tank, then the first valve and the third valve are opened to enable the solution in the blending tank to be flushed into the metering tank to preliminarily dissolve the materials, and then the second valve is opened to enable the solution to be circulated for further dissolution.
Furthermore, the bottom of the metering tank is also connected with an inert gas inlet for blowing inert gas from the bottom of the metering tank, so that the dissolution of the required materials is accelerated, the feeding device is protected from air impurities, and the feeding is carried out under the protection of the inert gas. More preferably, the inert gas is nitrogen or argon.
Still further, be equipped with the filtration membrane in the metering tank, more preferably, still be equipped with the level gauge in the metering tank.
Preferably, the concentrated solution delivery pump is a magnetic pump.
Preferably, a plate heat exchanger is further arranged at the front end of the first pure water inlet pipe connected to the dissolving tank and used for exchanging heat between pure water and water vapor for heating.
Preferably, the upper portion of the splicing tank is further provided with a breathing filter element for preventing the tank body from being in a pressure-building or negative pressure state and potential safety hazards caused by deformation.
Preferably, the blending tank is a PE tank for 10m ethanol harvest.
Preferably, the dissolving tank is a 3m stainless steel lined fluorine tank.
The production flow of the oxalic acid is as follows:
(1) and adding the oxalic acid powder into a dissolving tank for stirring and dissolving: putting oxalic acid powder into a dissolving tank through a feeding hole, introducing deionized water with a certain temperature through a first pure water inlet pipe, circulating by using a concentrated solution conveying pump until the oxalic acid powder is completely dissolved, circulating by using a high-position bottom valve on the dissolving tank to prevent undissolved solids settled to the bottom of the tank from entering the concentrated solution conveying pump when the oxalic acid is not completely dissolved so as to protect equipment, simultaneously filling high-purity inert gas from an inert gas inlet connected with the low-position bottom valve to assist in accelerating dissolution, closing the high-position bottom valve when the oxalic acid is completely dissolved, and opening the bottom valve to thoroughly pump the dissolved high-concentration oxalic acid solution into a blending tank through the concentrated solution conveying pump;
(2) the oxalic acid in the dissolving tank is conveyed to the blending tank through a concentrated solution conveying pump for circulation: after the oxalic acid powder is completely dissolved, the oxalic acid solution is conveyed to the blending tank by a concentrated solution conveying pump, a filtering device arranged between the concentrated solution conveying pump and the blending tank comprises at least one group of filtering units, particle impurities in the solution are filtered, the purity of the product is improved, and meanwhile, a rear-end circulating pump is protected, and the filtering units are preferably online backflushing filtering devices; deionized water is added into the blending tank in advance through a second pure water inlet pipe and is used for diluting the oxalic acid solution, and circulating operation is performed. And the convenient sample of sample connection has been designed to jar body below to and set up feeding device between blending jar and circulating pump and add required material like raw materials, auxiliary material or auxiliary agent, additive.
The feeding mode is as follows: firstly, close the valve on the circulating pump, add required material in feeding device, let oxalic acid in the blending jar rush into feeding device and dissolve the material and prevent that the material that does not dissolve gets into the circulating pump with higher speed and lead to the card in order to dissolve of material, then, open the valve on the circulating pump and circulate.
(3) And the oxalic acid after the blending is finished is filtered by a filter cabinet to a filling line.
Tank blending to filling: through the circulation blending, after the sample is qualified, carry required oxalic acid solution to the filling line through the magnetic force pump, get rid of solid particle impurity through the filter cabinet.
The invention has the beneficial effects that: the oxalic acid production system has reasonable structure, skillfully solves various problems and difficulties in the oxalic acid dissolving process by arranging the high-low bottom valve on the dissolving tank and matching with the inert gas inlet, reduces the damage of equipment and accelerates the dissolving speed; when the filtering unit in the filtering device is an online backflushing device, the filter element in the filtering device does not need to be stopped for cleaning or replaced, the production efficiency is improved, and the maintenance time and labor are greatly saved; at least two sets of same or different assembly and filling devices are connected behind the dissolving tank, so that continuous production can be realized by flexibly using at least two sets of same or different assembly and filling devices according to requirements in the production process, and the production rate and the production flexibility are greatly improved; through setting up feeding device between amalgamation jar and circulating pump, let oxalic acid in the amalgamation jar rush into feeding device and dissolve material that needs to add such as raw materials, auxiliary material or auxiliary agent, additive with the solution of material with higher speed, prevented ingeniously that the material that does not dissolve from getting into the circulating pump and leading to the problem that blocks, to sum up, whole device is rationally distributed, the optimization of a plurality of details, and the practicality is strong, is worth promoting.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a detailed view of the dissolving tank, the concentrate delivery pump, and the filtering device of FIG. 1;
FIG. 3 is a schematic view of the filter unit of FIG. 1;
fig. 4 is a detailed view of the makeup tank, charging device, and circulation pump of fig. 1.
Detailed Description
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
As shown in fig. 1-4, an oxalic acid production system is characterized by comprising a dissolving tank 1, a concentrated solution delivery pump 2 and a filtering device 3 which are sequentially connected, wherein two identical blending tanks are connected behind the filtering device 3 in parallel, each blending tank comprises a blending tank 4, a circulating pump 5, a filtering cabinet 7 and a filling machine 8 which are sequentially connected, the circulating pump 5 is also circularly connected with the blending tank and used for circulating oxalic acid in the blending tank 4, a group of feeding devices are further connected between the blending tank 4 and the circulating pump 5, and the fed substances can be raw materials, auxiliary materials or additives and additives, and can be solid or liquid.
The oxalic acid powder dissolving device is characterized in that a feed port 1.1 is formed in the dissolving tank 1 and used for feeding oxalic acid powder, the dissolving tank is further connected with a first pure water inlet pipe 1.2, a high-position bottom valve 1.3 and a low-position bottom valve 1.4 are further arranged on the dissolving tank 1, the high-position bottom valve 1.3 and the low-position bottom valve 1.4 are both connected with a concentrated solution conveying pump 2, the concentrated solution conveying pump 2 is further connected with the dissolving tank 1 in a circulating mode and used for circularly dissolving oxalic acid, the low-position bottom valve 1.4 is further connected with a nitrogen inlet 1.5 and used for filling high-purity nitrogen into the dissolving tank to accelerate dissolution of the oxalic acid powder, and a second pure water inlet pipe 4.1 and a sample sampling port 4.2 are further connected to the blending tank.
The dog-house 1.1 is for throwing the material platform, considers the convenience and the convenient observation that the oxalic acid powder was thrown the material, so designs the dissolving tank and goes up to throw the material platform. The upper high-precision metering equipment can accurately feed materials, is convenient to operate and can better monitor the whole production flow.
Between tank 4 and feeding device 6, be equipped with first valve 4.4, be equipped with second valve 5.1 on the circulating pump 5, feeding device 6 contains metering tank 6.1 and sets up third valve 6.2 in metering tank 6.1 below, metering tank 6.1 is gone into through third valve 6.2 and is pieced together between tank 4 and the circulating pump 5, and reinforced step is: when materials need to be added, all the valves of the first valve, the second valve and the third valve are closed, the required materials are added into the metering tank 6.1, then the first valve 4.4 and the third valve 6.2 are opened to enable the solution in the splicing tank 4 to be flushed into the metering tank 6.1 to preliminarily dissolve the materials, and then the second valve 5.1 is opened to enable the solution to be circulated for further dissolution. The bottom of the metering tank is also connected with an inert gas inlet for blowing inert gas from the bottom of the metering tank, so that the dissolution of the material is accelerated, the feeding device is protected from entering air impurities, and the feeding is carried out under the protection of the inert gas. The inert gas is nitrogen. And a filtering membrane is arranged in the metering tank, and a liquid level meter is also arranged in the metering tank.
The concentrated solution delivery pump 2 is a magnetic pump. And the front end of the water inlet pipe connected to the dissolving tank 1 is also provided with a plate heat exchanger 9 for exchanging heat between water and steam to heat. The upper portion of the splicing tank 4 is also provided with a breathing filter element 4.3 for preventing the tank body from being in a pressure-building or negative pressure state and potential safety hazards caused by deformation. And the splicing tank 4 is a PE tank for 10m cultivation. Dissolving tank 1 is 3m stainless steel storage tank lined with fluorine.
The production flow of the oxalic acid is as follows:
(1) and adding the oxalic acid powder into a dissolving tank for stirring and dissolving: putting oxalic acid powder into a dissolving tank through a feeding hole, introducing deionized water with a certain temperature through a first pure water inlet pipe, circulating by using a concentrated solution conveying pump until the oxalic acid powder is completely dissolved, circulating by using a high-position bottom valve on the dissolving tank to prevent undissolved solids settled to the bottom of the tank from entering the concentrated solution conveying pump when the oxalic acid is not completely dissolved so as to protect equipment, simultaneously filling high-purity nitrogen from a nitrogen inlet connected with the low-position bottom valve to assist in accelerating dissolution, closing the high-position bottom valve when the oxalic acid is completely dissolved, and opening the bottom valve to thoroughly pump the dissolved high-concentration oxalic acid solution into a blending tank through the concentrated solution conveying pump;
(2) the oxalic acid in the dissolving tank is conveyed to the blending tank through a concentrated solution conveying pump for circulation: after the oxalic acid powder is completely dissolved, the oxalic acid solution is conveyed to the blending tank by a concentrated solution conveying pump, a filtering unit is added between the concentrated solution conveying pump and the blending tank to filter particle impurities in the solution, so that the rear-end circulating pump is protected while the product purity is improved, and the filtering unit is an online backflushing filtering device; deionized water is added into the blending tank in advance through a second pure water inlet pipe and is used for diluting the oxalic acid solution, and circulating operation is performed. And the convenient sample of sample connection has been designed to jar body below to and set up feeding device between blending jar and circulating pump and add required material like raw materials, auxiliary material or auxiliary agent, additive.
The feeding mode is as follows: firstly, a valve on the circulating pump is closed, the required materials are added into the feeding device, and the oxalic acid in the blending tank is flushed into the feeding device to dissolve the materials so as to accelerate the dissolution of the materials and prevent the materials from being not dissolved.
(3) And the oxalic acid after the blending is finished is filtered by a filter cabinet to a filling line.
Tank blending to filling: through the circulation blending, after the sample is qualified, carry required oxalic acid solution to the filling line through the magnetic force pump, get rid of solid particle impurity through the filter cabinet.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (6)
1. The oxalic acid production equipment is characterized by comprising a dissolving tank (1), a concentrated solution delivery pump (2) and a filtering device (3) which are sequentially connected, wherein at least two sets of same or different matching and filling devices are connected behind the filtering device (3) in parallel, the concentrated solution delivery pump (2) is also connected with the dissolving tank (1) in a circulating manner and used for circularly dissolving oxalic acid, a feeding port (1.1) is formed in the dissolving tank (1) and used for feeding oxalic acid powder, the dissolving tank is also connected with a first pure water inlet pipe (1.2), a high-position bottom valve (1.3) and a low-position bottom valve (1.4) are also arranged on the dissolving tank (1), the high-position bottom valve (1.3) and the low-position bottom valve (1.4) are both connected with the concentrated solution delivery pump (2), and the high-position bottom valve (1.3) is used for opening when the oxalic acid powder is not completely dissolved so as to realize continuous circulation of the solution, the low-level bottom valve (1.4) is used for opening when the oxalic acid powder is completely dissolved so as to send the solution to be filtered, and the low-level bottom valve (1.4) is also connected with an inert gas inlet (1.5) for filling high-purity inert gas into the dissolving tank so as to accelerate the dissolution of the oxalic acid powder; the filtering device comprises at least one group of filtering units; the filter unit is an online filter device, the at least one set of matching and filling device comprises a matching tank (4), a circulating pump (5), a filter cabinet (7) and a filling machine (8) which are sequentially connected, and at least one set of feeding device (6) is connected between the matching tank (4) and the circulating pump (5); between tank (4) and feeding device (6) are pieced together, are equipped with first valve (4.4), be equipped with second valve (5.1) on circulating pump (5), feeding device (6) contain metering tank (6.1) and third valve (6.2) of setting in metering tank (6.1) below, metering tank (6.1) are even gone into through third valve (6.2) and are pieced together between tank (4) and circulating pump (5), and reinforced step is: when materials need to be added, all the valves of the first valve, the second valve and the third valve are closed, the required materials are added into the metering tank (6.1), then the first valve (4.4) and the third valve (6.2) are opened to enable the solution in the splicing tank (4) to be flushed into the metering tank (6.1) to preliminarily dissolve the materials, and then the second valve (5.1) is opened to enable the solution to be circulated for further dissolution.
2. An oxalic acid production apparatus according to claim 1, characterized in that the said tank assembly (4) is also connected with a second pure water inlet pipe (4.1) and a sample sampling port (4.2).
3. An oxalic acid production plant according to claim 1, characterized in that the bottom of the metering tank (6.1) is also connected with an inert gas inlet.
4. The oxalic acid production equipment of claim 1, wherein the online filtering device comprises a housing (3.1), a diaphragm plate (3.2), the diaphragm plate (3.2) is arranged in the housing (3.1) and divides the inner cavity into an upper cavity and a lower cavity, a plurality of filter elements (3.3) are arranged in the upper cavity, the upper cavity is connected with a liquid inlet pipe (3.4) and a water outlet pipe (3.5), the lower cavity is connected with a liquid outlet pipe (3.6) and a water inlet pipe (3.7), the liquid inlet pipe (3.4), the water outlet pipe (3.5), the liquid outlet pipe (3.6) and the water inlet pipe (3.7) are arranged between the housing (3.1), valves are arranged, and the online filtering step is: when normal filtration is carried out, the valves of the water inlet pipe (3.7) and the water outlet pipe (3.5) are closed, and the valves of the water inlet pipe (3.4) and the water outlet pipe (3.6) are opened; when the filter device needs cleaning, the valves of the liquid inlet pipe (3.4) and the liquid outlet pipe (3.6) are closed, the valves of the water inlet pipe (3.7) and the water outlet pipe (3.5) are opened, then water is flushed from the water inlet pipe (3.7) for flushing away impurities outside the filter element, and sewage is discharged from the water outlet pipe (3.5).
5. An oxalic acid production apparatus according to claim 1, characterized in that the front end of the first pure water inlet pipe (1.2) connected to the dissolving tank (1) is further provided with a plate heat exchanger (9) for heating pure water and steam by heat exchange.
6. An oxalic acid production apparatus according to claim 1, characterized in that, the upper part of the tank (4) is also provided with a breathing filter element (4.3).
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Citations (3)
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EP0469487A1 (en) * | 1990-07-30 | 1992-02-05 | Nikkiso Co., Ltd. | Apparatus for dissolving an adjusting agent of a dialytic solution |
CN102513000A (en) * | 2011-12-01 | 2012-06-27 | 清华大学 | Dissolving system |
CN203990469U (en) * | 2014-06-26 | 2014-12-10 | 江阴江化微电子材料股份有限公司 | The device for formulating of oxalic acid solution for ITO etching |
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2016
- 2016-09-23 CN CN201610842381.7A patent/CN106496011B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0469487A1 (en) * | 1990-07-30 | 1992-02-05 | Nikkiso Co., Ltd. | Apparatus for dissolving an adjusting agent of a dialytic solution |
CN102513000A (en) * | 2011-12-01 | 2012-06-27 | 清华大学 | Dissolving system |
CN203990469U (en) * | 2014-06-26 | 2014-12-10 | 江阴江化微电子材料股份有限公司 | The device for formulating of oxalic acid solution for ITO etching |
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