CN100453448C - Method and equipment for preparing high-purity chlorine dioxide - Google Patents
Method and equipment for preparing high-purity chlorine dioxide Download PDFInfo
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- CN100453448C CN100453448C CNB2006100332110A CN200610033211A CN100453448C CN 100453448 C CN100453448 C CN 100453448C CN B2006100332110 A CNB2006100332110 A CN B2006100332110A CN 200610033211 A CN200610033211 A CN 200610033211A CN 100453448 C CN100453448 C CN 100453448C
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Abstract
The present invention discloses a method for preparing high-purity chlorine dioxide and equipment thereof. The present invention solves the technical problems of tap water disinfecting cost reduction, and chlorine dioxide conversion rate and purity improvement. The method for preparing high-purity chlorine dioxide comprises the following procedures: sulphuric acid, sodium chlorate solution and hydrogen peroxide solution are heated; the sulphuric acid, the sodium chlorate solution and the hydrogen peroxide solution are mixed with the air via a venturi feeder; gas and liquid are separated, and the preparing equipment is provided with a liquid metering tank, a metering pump, the venturi feeder and a gas-liquid separator which are orderly connected by pipelines; the inlet end of the venturi feeder is connected with an air inlet; a pipeline between the metering pump and the venturi feeder is provided with a heater. Compared with the prior art, the present invention prepares the high-purity chlorine dioxide in the method of the gas-liquid separation by adopting the sulphuric acid, the sodium chlorate solution and the hydrogen peroxide solution which are heated and mixed with the air. Thereby, the present invention has the advantages of high conversion rate, high purity, safety, reliability, low disinfecting cost, and easy popularization and application.
Description
Technical field
The present invention relates to a kind of equipment of drinking water disinfect, particularly a kind of equipment for preparing chlorine dioxide with high purity.
Background technology
1977, EPA USEPA proposed with dioxide peroxide and O
3Substitute traditional liquid chlorine tap water is carried out disinfection, sterilizing agent/disinfection byproduct (DBP) etc. has been carried out risk assessment thereupon.Over more than 20 year, some economically developed countries have abolished with the technology of liquid chlorine to drinking water disinfection, adopt dioxide peroxide and O
3Sterilization, its major cause is a liquid chlorine disinfection byproduct (DBP) halohydrocarbon, as trichloromethane CHCL
3, human body is had carcinogenesis.In the later stage nineties, China brings into use dioxide peroxide to substitute liquid chlorine to the tap water purification that carries out disinfection in small-sized tap water factory.Existing dioxide peroxide preparation method mainly contains: a kind of is raw material with the Textone, prepares dioxide peroxide after acidifying, directly adds, and sees Chemical formula 1; Another kind is salt acid system (a R5 method), claims Kai Sitingfa again, carries out chemical reaction with sodium chlorate and hydrochloric acid and prepares dioxide peroxide, sees Chemical formula 2.
5NaClO
2+4HCl＝4ClO
2+NaCl+H
2O………………1
NaClO
3+2HCl＝ClO
2+1/2Cl
2+NaCl+H
2O…………2
The chlorite method causes disinfection of tap water cost height because of expensive raw material price.And salt acid system (R5 method) resulting be dioxide peroxide and Cl
2Mixed gas, NaClO
3Transformation efficiency low.
Goal of the invention
The purpose of this invention is to provide a kind of equipment for preparing chlorine dioxide with high purity, the technical problem that solve is to reduce the disinfection of tap water cost, improves dioxide peroxide transformation efficiency and purity.
The present invention is by the following technical solutions: a kind of equipment for preparing chlorine dioxide with high purity, have the first level meter measuring tank and first volume pump, the second level meter measuring tank and second volume pump that are linked in sequence by the two-way pipeline, this two-way connects the Venturi meter feeder, then to gas-liquid separator; The entrance end of Venturi meter feeder is connected with first air intlet; Be respectively equipped with primary heater and secondary heater on the pipeline between first volume pump and second volume pump and the Venturi meter feeder.
The air outlet of gas-liquid separator of the present invention connects the import of scum dredger, liquid outlet connects the opening for feed of producer, the air outlet of producer connects the import of scum dredger, traverse baffle in the producer is connected with the mother liquor collecting tank through pipeline, second valve, the producer bottom connects the mother liquor collecting tank through liquid discharge pipe, top first valve of producer connects water source from the beginning, and the bottom is connected with second air intlet, and every layer of traverse baffle in the producer is connected with first explosion trap through pipeline.
The air outlet of scum dredger of the present invention is connected with second hydraulic ejector with first hydraulic ejector respectively, the water-in of first hydraulic ejector and second hydraulic ejector connects water source from the beginning through first water pump and second water pump respectively, water outlet connects the coagulation basin and the clean water basin of former water treating pond respectively, and the air outlet of scum dredger is connected with second explosion trap.
First air intlet of the present invention and the second air intlet place are provided with well heater respectively.
On the heater outlet pipe of the present invention temperature probe is housed, the air outlet of scum dredger is provided with pressure transmitter, second pumping line is equipped with the chlorine dioxide concentration transmitter, and temperature probe, pressure transmitter and chlorine dioxide concentration transmitter are connected with the computer primary controller.
Traverse baffle in the producer of the present invention is one to five layer, every layer of staggered dividing plate that is provided with; The first level meter measuring tank and the second level meter measuring tank are the PVC cylindrical container of band graduated scale, first volume pump and second volume pump are selected EH/E55VC-20EPE6 for use, the Venturi meter feeder is the Venturi tube feeder, gas-liquid separator is band grid type glass reinforced plastic container, well heater is that electric heater capacity is 500W or 2000W, first valve and second valve are electrical ball valve KLD20-QZI-10T, scum dredger is the glass reinforced plastic container of band tapering, first hydraulic ejector and second hydraulic ejector are selected WNP-3023 for use, first water pump and second water pump are selected 65FB32 for use, first explosion trap and second explosion trap are the pvc pipe and the mating plane lid of band sealing-ring, and the computer primary controller is selected CPU224 for use.。
The present invention compared with prior art, adopt sulfuric acid, sodium chlorate solution, superoxol heating, in molar ratio through Venturi meter feeder and air mixed, the method of carrying out gas-liquid separation prepares highly purified dioxide peroxide, and the level meter measuring tank, volume pump, Venturi meter feeder and the gas-liquid separator that are linked in sequence by pipeline prepare dioxide peroxide, the transformation efficiency height, the purity height, safe and reliable, disinfection cost is low, is easy to apply.
Description of drawings
Fig. 1 is the structural representation that the present invention prepares the apparatus embodiments of chlorine dioxide with high purity.
Fig. 2 is an A-A sectional view among Fig. 1.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Be on the rise in that China's water resources is contaminated, the surface water eutrophication under the Chemical Composition complicated situations such as heavy metal organism, inorganics, is selected a kind of new production technique and corresponding dioxide peroxide generation equipment, improves transformation efficiency and purity, is necessary.
The present invention adopts sulfuric acid, sodium chlorate solution, hydrogen peroxide liquid molten by 3.8～4.3: 1.5～1.75: 0.8～1.2 mol ratio is reacted by department of chemistry's formula 3 through Venturi meter feeder and equipment such as gas-liquid separator, producer:
2NaClO
3+H
2O
2+2H
2SO
4＝2ClO
2+O
2+2NaHSO
4+2H
2O…………3
When the present invention produces in dioxide peroxide preparation, at first be that the dilute sulphuric acid of 65%～75% concentration is packed in the scale tank with diluting concentrated sulfuric acid, sodium chlorate is mixed with mixed solution another scale tank of packing into by the concentration of 35%～45% concentration and hydrogen peroxide 5%～10%.The mixed solution of sulfuric acid and sodium chlorate and hydrogen peroxide presses 3.8～4.3: 1.5～1.75 by volume pump respectively: 0.8～1.2 mol ratio is continuously to Venturi meter feeder feed, two kinds of liquid materials are equipped with well heater separately on the volume pump outlet pipe, preheating reaches after 65～85 ℃ of temperature the air mixed 45～80 ℃ of the trunnion position of Venturi meter and heater via heating.This feeder is the uniform mixing reaction mass fast, effectively avoids generating because of Dilution of sulphuric acid heat causes the too high side reaction that causes of local temperature rise, can obtain highly purified chlorine dioxide.Gases such as the dioxide peroxide that is come out by Wen's feeder and reaction solution enter gas-liquid separation, and the gas after the separation enters the dioxide peroxide escape pipe by top, and reaction solution then enters producer by the bottom.Producer is made up of housing and traverse baffle, and reaction solution forms plug-flow between traverse baffle, and the reaction solution that enters producer is carried out sequentially, keeps the concentration gradient of reaction solution.The producer number of baffles, can according to reactant and generating tube what, the length in reaction times decides.In the bottom of producer one blast main is housed, warm air is to enter producer after the airheater preheating, warm air from bottom to top with every traverse baffle from top to bottom reaction solution form counter current contact, one of effect for warm air can will be dissolved in chlorine dioxide in the reaction solution take off suction and blow out, two of effect is to keep producer internal reaction liquid temp.The preparation process of dioxide peroxide is to carry out under negative pressure state, and it is that the vacuum of leaning on hydraulic ejector to form is kept that negative pressure forms.
As shown in Figure 1, the equipment of preparation chlorine dioxide with high purity of the present invention, comprise that the PVC of the band graduated scale that is linked in sequence by pipeline is shaped as the first level meter measuring tank 1, the second level meter measuring tank 2 of Cylinder container, first volume pump 3, second volume pump 4 (Japanese Yi Weiqi company, the EH/E55VC-20EPE6 type), Venturi meter feeder 8 (Venturi feeder) and gas-liquid separator 12 (band grid type glass reinforced plastic container).The entrance end of Venturi meter feeder 8 is connected with first air intlet 7, and first air intlet 7, second air intlet, 9 places are provided with well heater (electric minister electricradiator industry (Long Gang) branch office is liked by the Shenzhen, 500W).Pipeline between first volume pump 3, second volume pump 4 and the Venturi meter feeder 8 be provided with primary heater 5, secondary heater 6 (Guangzhou Haizhu District Ward products factory, 2000W).The air outlet of gas-liquid separator 12 connects the import of scum dredger 13, scum dredger 13 is the glass reinforced plastic container of band tapering, liquid outlet connects the opening for feed of producer 10, the air outlet of producer 10 connects the import of scum dredger 13, traverse baffle 11 in the producer 10 is through pipeline, (sharp extraordinary valve Manufacturing Co., Ltd is opened in Shanghai to second valve 19, the KLD20-QZI-10T type) is connected with mother liquor collecting tank 21, mother liquor collecting tank 21 is the rectangular cell body of PVC, every layer of traverse baffle 11 in the producer 10 is connected with first explosion trap 141 through pipeline, producer 10 bottoms connect mother liquor collecting tank 21 through liquid discharge pipe, (sharp extraordinary valve Manufacturing Co., Ltd is opened in Shanghai to top first valve 17 of producer 10, the KLD20-QZI-10T type) connects water source from the beginning, (electric minister electricradiator industry (Long Gang) branch office is liked by the Shenzhen for the bottom and second air intlet 9,500W) connect, traverse baffle 11 in the producer 10 is one to five layer, every layer of staggered dividing plate that is provided with.The air outlet of scum dredger 13 respectively with first hydraulic ejector 16, second hydraulic ejector 18 (electrochemical worker's anticorrosion equipment factory in the Wuxi City, the WNP-3023 type) connects, the water-in of first hydraulic ejector 16, second hydraulic ejector 18 is through first water pump 15, second water pump 20 (Zhaoqing outstanding one-tenth hardware machinery factory, the 65FB32 type) connects water source from the beginning, water outlet connects the coagulation basin and the clean water basin of former water treating pond respectively, and the air outlet of scum dredger 13 is connected with second explosion trap 142 with the pvc pipe of sweet seal and mating plane lid.Temperature probe (Xi'an Xin Min Science and Technology Ltd. is housed on each heater outlet pipe, K-0～400 ℃), the air outlet of scum dredger 13 is provided with pressure transmitter (Xi'an Xin Min Science and Technology Ltd., CYB13), second water pump 20 goes out pipe chlorine dioxide concentration transmitter (German general sieve name spy is housed, 0～2mg/L), temperature probe, pressure transmitter and chlorine dioxide concentration transmitter are connected with computer primary controller 22 (CPU224).
The present invention adopts computer programming control to the technical parameter that relates in the preparation of dioxide peroxide and the use.On sterilizing and purifying to tap water, adopt gas-liquid separation, gas adds the mother liquor comprehensive utilization method, can stop the secondary pollution of tap water and reduces chlorite and chlorate content in the output water, guarantees water quality reaching standard.
The present invention prepares the equipment of dioxide peroxide and the dosage of temperature, pressure, concentration and the reaction mass of dioxide peroxide in the tap water dosing system is equipped with transmitter, the signal input computer that is produced, and each heater current is pressed the PLC time variable control; The regulation and control of negative pressure, force (forcing) pump motor frequency conversion device are pressed the PLC time variable control; The flow of diaphragm metering pump (stroke) is pressed the PLC time variable control by chlorine dioxide concentration determinator, computer in the output water.In addition temperature, pressure all there is overload alarm, sfgd.s such as superelevation limit shutdown.Orderly closedown is provided with delay function, just prepares to shut down, can stop feed in advance, outage again after question response liquid reacts completely, security measuress such as bath like this, discharge opeing, emptying can reduce loss of material.
The method and apparatus that the present invention prepares chlorine dioxide with high purity can obtain 95% above chlorine dioxide, NaClO
3The transformation efficiency that is converted into chlorine dioxide is greater than 92%, and the purity of dioxide peroxide reaches 95%.In the sterilizing and purifying of tap water, reduce by product, guarantee that tap water reaches national cities and towns tap water industry standard CJ/T206-2005.
The aqueous solution of the chlorine dioxide that the foregoing description makes adopts five step allusion quotation amount methods to measure, measuring method is defended method prison according to Ministry of Health of the People's Republic of China and is sent out in " disinfection technology standard " (version in 2002) of [2002] No. 282 files " Ministry of Health is about printing and distributing the notice of disinfection technology standard (version in 2002) " the 112nd page five step iodimetry,iodometry, measures and experimental data sees attached list one.
Safety in production of the present invention is guaranteed by following control method: 1, selected sulfuric acid, hydrogen peroxide, and in reaction, itself just follow aerobic gas to generate by chemical formula 3, can dilute the chlorine dioxide of generation.2, in the preparation of chlorine dioxide, adopt the negative pressure operation, the external Vent of chlorine dioxide can not appear in system-wide equipment and pipeline.The air that enters producer by Venturi meter feeder and producer bottom can effectively be controlled chlorine dioxide gas concentration in addition, guarantees in the preparation process that the concentration of chlorine dioxide can not set off an explosion because of surpassing 10% in any equipment and pipeline.3, when power supply system power failure suddenly and tripping operation, the producer motorized valve is opened reaction solution is drained, and the power supply of motorized valve is supplied with by store battery; Reactor is equipped with the emptying of automatic burst-preventing valve; Bath magnetic valve on the generator exports pipe is opened, and to the inner bath of producer, makes the reaction solution dilution reduce chemical reaction velocity.
Subordinate list one is measured and experimental data
Add 200ml distilled water in the iodine flask of 500ml, the 1ml phosphate buffered saline buffer is drawn 5.0ml dioxide peroxide sample, adds the 10ml liquor kalii iodide again, mixing.With 0.0105mol/L Sulfothiorine titration end point.
| |
|
|
|
| Reading A | 2.70 | 2.60 | 2.64 |
| Reading B | 10.06 | 10.42 | 10.50 |
| Reading C | 0.20 | 0.20 | 0.20 |
| Reading D | 0.40 | 0.60 | 0.50 |
| Reading E | 12.80 | 13.04 | 13.16 |
| ClO 2 | 342.1 | 347.7 | 354.1 |
| ClO 2 - | 14.16 | 21.25 | 17.71 |
| ClO 3 - | 1.2 | 0.58 | 0.58 |
| Cl 2 | 11.20 | 10.8 | 10.4 |
Claims (6)
1. equipment for preparing chlorine dioxide with high purity, it is characterized in that: have the first level meter measuring tank (1) and first volume pump (3), the second level meter measuring tank (2) and second volume pump (4) that are linked in sequence by the two-way pipeline, this two-way connects Venturi meter feeder (8), then to gas-liquid separator (12); The entrance end of Venturi meter feeder (8) is connected with first air intlet (7); Be respectively equipped with primary heater (5) and secondary heater (6) on the pipeline between first volume pump (3) and second volume pump (4) and the Venturi meter feeder (8).
2. the equipment of preparation chlorine dioxide with high purity according to claim 1, it is characterized in that: the air outlet of described gas-liquid separator (12) connects the import of scum dredger (13), liquid outlet connects the opening for feed of producer (10), the air outlet of producer (10) connects the import of scum dredger (13), traverse baffle (11) in the producer (10) is through pipeline, second valve (19) is connected with mother liquor collecting tank (21), producer (10) bottom connects mother liquor collecting tank (21) through liquid discharge pipe, top first valve (17) of producer (10) connects water source from the beginning, the bottom is connected with second air intlet (9), and the every layer of traverse baffle (11) in the producer (10) is connected with first explosion trap (141) through pipeline.
3. the equipment of preparation chlorine dioxide with high purity according to claim 2, it is characterized in that: the air outlet of described scum dredger (13) is connected with second hydraulic ejector (18) with first hydraulic ejector (16) respectively, the water-in of first hydraulic ejector (16) and second hydraulic ejector (18) connects water source from the beginning through first water pump (15) and second water pump (20) respectively, water outlet connects the coagulation basin and the clean water basin of former water treating pond respectively, and the air outlet of scum dredger (13) is connected with second explosion trap (142).
4. the equipment of preparation chlorine dioxide with high purity according to claim 3 is characterized in that: described first air intlet (7) and second air intlet (9) locate to be provided with respectively well heater.
5. the equipment of preparation chlorine dioxide with high purity according to claim 4, it is characterized in that: on the described heater outlet pipe temperature probe is housed, the air outlet of scum dredger (13) is provided with pressure transmitter, second water pump (20) rising pipe is equipped with the chlorine dioxide concentration transmitter, and temperature probe, pressure transmitter and chlorine dioxide concentration transmitter are connected with computer primary controller (22).
6. the equipment of preparation chlorine dioxide with high purity according to claim 5 is characterized in that: the traverse baffle (11) in the described producer (10) is one to five layer, every layer of staggered dividing plate that is provided with; The first level meter measuring tank (1) and the second level meter measuring tank (2) are the PVC cylindrical container of band graduated scale, first volume pump (3) and second volume pump (4) are selected EH/E55VC-20EPE6 for use, Venturi meter feeder (8) is the Venturi tube feeder, gas-liquid separator (12) is band grid type glass reinforced plastic container, well heater is that electric heater capacity is 500W or 2000W, first valve (17) and second valve (19) are electrical ball valve KLD20-QZI-10T, scum dredger (13) is the glass reinforced plastic container of band tapering, first hydraulic ejector (16) and second hydraulic ejector (18) are selected WNP-3023 for use, first water pump (15) and second water pump (20) are selected 65FB32 for use, first explosion trap (141) and second explosion trap (142) are the pvc pipe and the mating plane lid of band sealing-ring, and computer primary controller (22) is selected CPU224 for use.
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Families Citing this family (4)
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| CN102167287B (en) * | 2011-05-19 | 2016-01-20 | 李达 | Multifunction efficient energy-saving chlorine dioxide generator |
| CN104090594B (en) * | 2014-07-27 | 2017-08-25 | 杭州凡腾科技有限公司 | A kind of solution concentration on-line monitoring and control system and method |
| CN105568659B (en) * | 2015-11-20 | 2019-08-09 | 北京鹏盛天纤科技有限公司 | A kind of method of the device and gas phase ClO 2 bleaching floccule of gas phase ClO 2 bleaching floccule |
| CN105525463B (en) * | 2015-11-20 | 2019-02-22 | 北京鹏盛天纤科技有限公司 | A kind of method of the device and gas phase ClO 2 bleaching waste textile of gas phase ClO 2 bleaching waste textile |
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