CN102134059A - Method and device for preparing chlorine dioxide - Google Patents
Method and device for preparing chlorine dioxide Download PDFInfo
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- CN102134059A CN102134059A CN201010103162XA CN201010103162A CN102134059A CN 102134059 A CN102134059 A CN 102134059A CN 201010103162X A CN201010103162X A CN 201010103162XA CN 201010103162 A CN201010103162 A CN 201010103162A CN 102134059 A CN102134059 A CN 102134059A
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Abstract
The invention discloses a method for preparing chlorine dioxide. The method comprises a material mixing step, a main reaction step and a finished product output step, wherein in the material mixing step, two liquid raw materials are respectively led into a charger through two material conveying pipes, and the raw materials are mixed by a Y-shaped mixing charging pipe in the charger to react primarily to form primary reaction mixed liquid which enters a reaction kettle; and in the main reaction step, the primary reaction mixed liquid falls onto a cyclone plate in the reaction kettle and forms cyclone, and passes through a multi-layer cyclone plate and a multi-layer aeration plate to form chlorine dioxide gas and reaction residual liquid. In addition, the invention also provides a device for preparing chlorine dioxide. The method and device for preparing chlorine dioxide disclosed by the invention have the advantages that a reaction system is more simplified, and the working efficiency of the system is higher.
Description
Technical field
The present invention relates to prepare the method and apparatus of dioxide peroxide, the particularly a kind of method and apparatus that can realize the preparation chlorine dioxide with high purity of high-conversion rate.
Background technology
In the last thirty years, dioxide peroxide has obtained widespread use as a kind of novel sterilization oxygenant in developed country, is a kind of good sterilization oxygenant that replaces liquid chlorine.In the water of chlorine dioxide treatment, can not produce the common carcinogens haloform that forms during with disinfection by chlorine, its security is classified as the AI level by the WHO of the World Health Organization, have wide spectrum, quick-acting, nontoxic, consumption is few, drug effect is long, sterilization effect is not subjected to plurality of advantages such as pH value restriction, can reach 100% to the killing rate of part bacterium; Use some reducing metal ion such as Fe in all right oxidizing water of disinfection by chlorine dioxide
2+, Mn
2+Deng, can remove iron, manganese element in the water.
Present stage, a lot of water factories of China also bring into use dioxide peroxide to replace liquid chlorine to the tap water disinfection.When adopting the R11 legal system to be equipped with dioxide peroxide, its reaction equation is seen Chemical formula 1:
2NaClO
3+H
2O
2+2H
2SO
4＝2ClO
2+O
2+2NaHSO
4+2H
2O 1
In actual applications, the various chlorine dioxide generators of existing employing R11 method all are with the Venturi meter feeder liquid sodium chlorate, liquid sulfuric acid, three kinds of liquid starting materials of liquid hydroperoxide and warm air at first to be carried out gas-liquid mixed, begin chemical reaction this moment and generate chlorine dioxide; Then gas-liquid mixture is sent into gas-liquid separator and carried out gas-liquid separation, the chlorine dioxide of generation is derived through pipeline, and isolated liquid imports reactor further reaction and the more chlorine dioxide of lasting generation through pipeline.Blast easily because of chlorine dioxide gas concentration surpasses at 10% o'clock, this process must be carried out under negative pressure usually, so that in time derive chlorine dioxide by pipeline.
In above process, gas-liquid mixed and gas-liquid separating step all require the efficient that reaches higher, improving the reaction efficiency and the dioxide peroxide transformation efficiency of total system, and guarantee reaction safety.The major defect of this mode is: first, the two itself is the step of mutual contradictory for gas-liquid mixed and gas-liquid separation, constitute from entire system, the efficient of Venturi meter and gas-liquid separator is high more, it is just high more to be used to the merit of cancelling each other in the total system, even use the lower deflector type gas-liquid separator of separation efficiency, also still have the merit loss of considerable part formerly to carry out gas-liquid mixed and carry out again among this process of gas-liquid separation for the consideration of cost and antiseptic property; Second, generally, system's negative pressure is to be provided by the water sprayer that dioxide peroxide is added to the water body place, drive raw material and enter the malleation that various feedstock pump/valve provided of Venturi meter not only not contribution of system pressure, also need water sprayer to provide extra negative pressure to be offseted, system's negative pressure is remained within the nominal scope, increased the demand of total system virtually for energy; The 3rd, on system architecture, this serial system of commissioning pipe/pump → Venturi meter gas liquid mixer → gas-liquid separator → reactor constitutes comparatively complicated, and the working efficiency of each subsystem all can not reach or near separately the best, and can only get the compromise under the entire system balance.
Summary of the invention
The present invention is in order to overcome defective in the above-mentioned prior art, the method and apparatus that is used to prepare dioxide peroxide that a kind of reactive system is simplified more, system works efficient is higher to be provided.
The invention provides a kind of method for preparing dioxide peroxide, comprise batch mixing step, main reaction step and go out finished product output step, wherein,
In the described batch mixing step, two kinds of stock liquids are fed in the feeder via the two-way carrier pipe respectively, described feeder is installed on the reactor top and connects as one structure with reactor, comprise a Y type mixing filling tube in the described feeder, described Y type mixing filling tube one side has two arms that are communicated with described two-way carrier pipe respectively, its opposite side is communicated with described reactor, described two-way stock liquid carries out initial action after being pumped in the described Y type mixing filling tube, and the described initial reaction mixed solution of formation enters in the described reactor;
In the described main reaction step, described initial reaction mixed solution falls on the eddy flow plate of described reactor and forms eddy flow, after carrying out uniform mixing and reaction through multi-layer rotational flow plate and the multilayer aeration board that is positioned at described eddy flow plate below successively, form chlorine dioxide and reaction residue.
Preferably, in the described batch mixing step, described feeder also comprises the warm air input tube, and the warm air input tube is positioned at the corresponding position of Y type mixing filling tube, is used to keep the initial action desired reaction temperature and derives the chlorine dioxide that initial reaction forms; In the described main reaction step, the airway that has connection described eddy flow plate of each layer and described aeration board in the described reactor, described airway is communicated with gas output tube on the described reactor, and the dioxide peroxide that generates on described each layer eddy flow plate and the described aeration board enters described gas output tube by described airway; In the finished product output step, the chlorine dioxide of described generation is exported through the gas output tube on described reactor top by the hot gas that described aeration board provides, and described reaction residue is discharged through the Drainage pipe of described reactor bottom.
Preferably, in the described batch mixing step, described Y type mixing filling tube comprises expansion section, contraction section and synthesis stage, and at expansion section and contraction section place, liquid starting material atomizes under pressure and forms the gas-liquid mixed state; Described two arms combine the formation synthesis stage in contraction section bottom separately, and the liquid starting material after the atomizing is in described synthesis stage mixing and carry out initial action, and forms the initial reaction mixed solution; In the described main reaction step, described every layer of eddy flow plate comprises the eddy flow groove that passed through the connection of liquid mouth each other, initial reaction mixed solution formed eddy flow direction in the adjacent eddy flow groove of every layer of eddy flow plate opposite each other and flow into by eddy flow plate tremie pipe under on one deck eddy flow plate, the initial reaction mixed solution on last one deck eddy flow plate flows on the superiors' aeration board.
Preferably, in two kinds of stock liquids, a kind of is aqueous sulfuric acid, and a kind of is the sodium chlorate and the hydrogen peroxide mixture aqueous solution, and the mol ratio that adds sulfuric acid, sodium chlorate and hydrogen peroxide in the described stock liquid is (1.9～2.1): (1.9～2.1): (0.9～1.1); Described initial reaction mixed solution keeps the time of eddy flow state more than or equal to 2 hours in described reactor.
Preferably, described two carrier pipes are coated with liquid working media outward respectively so that it is heated, and corresponding, shape is twined at the heating zone place that described two carrier pipes are coated with liquid working media twist.
Preferably, described reactor is provided with urgent tapping valve, is used for breaking down or needing under the situation of emergency stop, and the liquid emptying with in the reactor no longer produces chlorine dioxide.
The present invention also provides a kind of equipment for preparing dioxide peroxide, comprises the feeder and the reactor that are communicated with in turn, wherein,
Described feeder is installed on the reactor top, and connects as one structure with reactor, comprises a Y type mixing filling tube in the described feeder, and described Y type mixing filling tube one side has two arms, is communicated with the carrier pipe that two-way is used to import stock liquid respectively; Its opposite side is communicated with described reactor;
From top to bottom be provided with the aeration board that is used to provide rising hot gas that multilayer is used to form the eddy flow plate of eddy flow and is positioned at described eddy flow plate below in the described reactor successively.
Preferably, the airway that has connection described eddy flow plate of each layer and described aeration board in the described reactor with the derivation chlorine dioxide, described airway is communicated with gas output tube on the described reactor, and the reactor bottom is provided with the Drainage pipe of discharging reaction residue.
Preferably, described every layer of eddy flow plate comprises eddy flow plate base plate, is positioned at the eddy flow plate outer wall at outer rim place, described eddy flow plate base plate upper surface, and the gas port that is positioned at the described airway of formation at described base plate middle part, described plate upper surface is provided with eddy flow plate baffle plate and multiple tracks begins from inside to outside the eddy flow cell wall of setting in turn from the gas port periphery, and described eddy flow plate baffle plate radially extends to eddy flow plate outer wall place by the most inboard eddy flow cell wall; Form the eddy flow groove between the adjacent eddy flow cell wall and between outermost eddy flow cell wall and eddy flow plate outer wall; Offered the liquid mouth on the eddy flow cell wall between adjacent eddy flow groove, the described liquid mouth of crossing alternately is divided into the eddy flow baffle plate both sides, so that the formed eddy flow direction of adjacent eddy flow groove is opposite, the base plate of described eddy flow groove correspondence is provided with the tremie pipe of downward one deck eddy flow plate or aeration board extension, and the base plate of the eddy flow groove correspondence on last one deck eddy flow plate is provided with the tremie pipe that extends to the superiors' aeration board.
Preferably, in the described reactor, the eddy flow plate structure of alternate setting is identical, and the described tremie pipe on two eddy flow plates of adjacent setting is arranged at the eddy flow groove place of different positions.
The present invention has following beneficial effect:
(1) (as open day was on July 19th, 2006 for the equipment of the preparation dioxide peroxide of realization high-conversion rate of the present invention and prior art, publication number is the method and apparatus of the disclosed preparation chlorine dioxide with high purity of Chinese invention patent ublic specification of application of CN1803581) compare, Venturi meter feeder and gas-liquid separator have been cancelled, rely on Y type mixing filling tube to feed in raw material and gas-liquid mixed, effective simplification system architecture, reduce equipment cost, avoided energy wastage.
(2) its multi-layer rotational flow aeration design can fully be reacted reaction raw materials, has dioxide peroxide transformation efficiency height, and equipment cost and running energy consumption are low, advantages of simple operation; Water or agricultural water treatment occasion in the open air, the present invention can be set to work under positive pressure, under the situation that is not equipped with water sprayer, rely on easy blast apparatus just the chlorine dioxide that produces can be added to staying water, therefore have advantage of wide range of application, be easy to large-scale promotion and use.
Description of drawings
Fig. 1 is the one-piece construction synoptic diagram of equipment of the preparation dioxide peroxide of realization high-conversion rate of the present invention;
Fig. 2 be reactor shown in Figure 1 and feeder be connected to vertical section structure figure after the integral body;
Fig. 3 be reactor shown in Figure 1 and feeder be connected to top view after the integral body;
Fig. 4 a and 4b are respectively the interior one deck of reactor shown in Figure 2 and horizontal stroke, the longitudinal diagram of three layers of eddy flow plate;
Fig. 5 a and 5b are respectively horizontal stroke, the longitudinal diagrams of two layers and four layers eddy flow plate in the reactor shown in Figure 2;
Fig. 6 a and 6b are respectively horizontal stroke, the longitudinal diagrams of five layers of aeration board in the reactor shown in Figure 2;
Fig. 7 a and 7b are respectively the longitudinal and transverse sectional views of six layers of aeration board in the reactor shown in Figure 2;
Fig. 8 is the structure iron of the first and second water-bath warmers shown in Figure 1;
Fig. 9 is the top view of the type of Y shown in Fig. 1 mixing filling tube;
Figure 10 is the fish-eye view of the type of Y shown in Fig. 1 mixing filling tube;
Figure 11 is the frontview of the type of Y shown in Fig. 1 mixing filling tube;
Figure 12 is the rear view of the type of Y shown in Fig. 1 mixing filling tube;
Figure 13 is the right view of the type of Y shown in Fig. 1 mixing filling tube;
Figure 14 is the left view of the type of Y shown in Fig. 1 mixing filling tube.
Mark the following drawings mark thereon in conjunction with the accompanying drawings:
The 1-reactor, 2-feeder, 3-communicating pipe, (wherein 4-1 is an expansion section to 4-Y type mixing filling tube, and 4-2 is a contraction section, and 4-3 is a synthesis stage, 4-4 is a breather hole), 6-warm air input tube, 7-one deck eddy flow plate, two layers of eddy flow plate of 8-, three layers of eddy flow plate of 9-, four layers of eddy flow plate of 10-, five layers of aeration board of 11-, six layers of aeration board of 12-, the urgent leakage fluid dram of 13-, the 14-aeration tube, the 15-solarization air cap, (wherein 16-2 is the aeration board tremie pipe to 16-eddy flow plate tremie pipe, 16-3 is the top tremie pipe), (wherein 17-1 is the middle part airway to the 17-airway, and 17-2 is the bottom airway, 17-3 is the top airway), 18-eddy flow plate baffle plate, 18-2 is the aeration board baffle plate, 19-eddy flow cell wall, 20-crosses the liquid mouth, 21-leakage fluid dram, 22-housing, the 23-temperature controlled switch, the 24-heating tube, 25-top liquid-inlet pipe, 26-top drain pipe, the 27-sheath, the 28-louvre, the urgent tapping valve of 29-, 30-water-bath warmer, the 32-feedstock pump, the 34-vacuum breaker, 36-airheater, 37-well heater temperature control unit, the 38-temperature control unit, the 40-pressure transmitter, 41-safety valve, 42-Drainage pipe, the 43-hot air delivery pipe, 44-sulfuric acid carrier pipe, 45-sodium chlorate mixed solution carrier pipe, 46-gas output tube.
Embodiment
Below in conjunction with accompanying drawing, a specific embodiment of the present invention is described in detail, but is to be understood that protection scope of the present invention is not subjected to the restriction of embodiment.Should be noted that the orientation qualifier such as upper and lower that occurs among the present invention is reference with position shown in the accompanying drawing all,, do not limit the protection domain of technical solution of the present invention so that more clearly understand its structure.
The present invention adopts sodium chlorate and sulfuric acid as raw material, and hydrogen peroxide prepares dioxide peroxide as reductive agent, usually sodium chlorate and hydrogen peroxide is configured to the sodium chlorate mixed solution during preparation raw material.
Shown in Fig. 1,2 and 3, the equipment of the preparation dioxide peroxide of realization high-conversion rate of the present invention comprises two transport pipes, every transport pipe be linked in sequence feedstock pump 32, water-bath warmer 30 and vacuum breaker 34; Article two, transport pipe in application respectively as sulfuric acid carrier pipe 44 and sodium chlorate mixed solution carrier pipe 45.Feeder 2 is installed in reactor 1 top, and with reactor 1 structure in aggregates, has a warm air input tube 6 on the feeder 2, be provided with Y type mixing filling tube 4 in the feeder 2, two arms of Y type mixing filling tube 4 connect the exit end of the vacuum breaker 34 of sulfuric acid carrier pipe 44 and sodium chlorate mixed solution carrier pipe 45 respectively.Shown in Fig. 9 to 14, the arm of Y type mixing filling tube 4 comprises expansion section 4-1 and contraction section 4-2, article two, arm combines in the bottom of separately contraction section 4-2 and forms synthesis stage 4-3, all have some breather hole 4-4 on the tube wall of the synthesis stage 4-3 of Y type mixing filling tube 4, so that derive the chlorine dioxide that produces in the Y type mixing filling tube 4.The top of reactor 1 is provided with the top tremie pipe 16-3 that is communicated with blanking device 2.
As shown in Figure 2, described reactor 1 comprises four layers of eddy flow plate that connects in turn from top to bottom, be respectively one deck eddy flow plate 7, two layers of eddy flow plate 8, three layers of eddy flow plate 9 and four layers of eddy flow plate 10, and the two-layer aeration board that connects in turn from top to bottom that is connected four layers of eddy flow plate 10 below, be respectively five layers of aeration board 11 and six layers of aeration board 12.
As Fig. 4 a and 4b, and shown in 5a and the 5b, described eddy flow plate comprises (the not indication among the figure of eddy flow plate base plate, it is positioned at eddy flow plate bottom, be used for support liquid) and (figure does not indicate to be positioned at the eddy flow plate outer wall of described eddy flow plate base plate upper surface outer rim, itself and eddy flow plate bottom constitute the circular groove type that opening makes progress), the middle part of eddy flow plate base plate is provided with gas port (not indication among the figure, it constitutes middle part airway 17-1 with the most inboard eddy flow cell wall 19 that is positioned at its periphery), eddy flow plate base plate is provided with the eddy flow cell wall 19 that eddy flow plate baffle plate 18 and multiple tracks begin to be provided with in turn from inside to outside from the periphery of gas port, and outermost layer eddy flow cell wall 19 is positioned at eddy flow plate outer wall inboard; One end of described eddy flow plate baffle plate 18 is connected to and is positioned at the most inboard eddy flow cell wall 19, and its other end is connected to eddy flow plate outer wall.Form the eddy flow groove between the adjacent eddy flow cell wall 19 and between outermost eddy flow cell wall 19 and eddy flow plate outer wall, be provided with three eddy flow grooves in the present embodiment.Except that being positioned at the most inboard eddy flow cell wall 19, all had liquid mouth 20 on all the other eddy flow cell walls 19, described two mistake liquid mouths 20 alternately are divided into the eddy flow baffle plate both sides, so that each road eddy flow groove is opposite with the formed eddy flow direction of adjacent eddy flow groove, liquid material (mixing the initial reaction mixed solution that forms behind the initial action in feeder 2) forms eddy flow in the eddy flow groove, and flows into one deck eddy flow plate or aeration board down by being positioned at eddy flow plate tremie pipe 16 an eddy flow groove and that be installed on the eddy flow plate base plate.The most inboard eddy flow cell wall 19 cooperates gas port to form middle part airway 17-1.
Wherein, the structure of one deck eddy flow plate 7 and three layers of eddy flow plate 9 is identical, as shown in Figs. 4a and 4b, and its eddy flow plate tremie pipe 16 is arranged in the most inboard eddy flow groove; The structure of two layers of eddy flow plate 8 and four layers of eddy flow plate 10 is also identical, and shown in Fig. 5 a and 5b, its eddy flow plate tremie pipe 16 is arranged in outermost eddy flow groove.During works better, liquid starting material (initial reaction mixed solution) forms eddy flow in reactor 1, and the time that keeps the eddy flow state more than or equal to 2 hours, liquid starting material can fully be reacted.
As Fig. 6 a and 6b, and shown in 7a and the 7b, aeration board comprises aeration board outer wall and the aeration board base plate that is connected thereon, the aeration board base plate is provided with the aeration tube 14 with many take-off pipes, has several solarization air caps 15 (being located at each bar take-off pipe top shown in Fig. 6 a) on the tube wall of aeration tube 14; Aeration tube 14 and described warm air input tube 6 required warm airs are provided by hot air delivery pipe shown in Figure 1 43, and airheater 36 is housed on the hot air delivery pipe 43.Shown in Fig. 6 a and 6b, the aeration board base plate of five layers of aeration board 11 is provided with bottom airway 17-2; One aeration board baffle plate 18-2 is connected between bottom airway 17-2 and the aeration board outer wall; The aeration board base plate is provided with the aeration board tremie pipe 16-2 that flows into six layers of aeration board 12.Shown in Fig. 7 a and 7b, the aeration board of six layers of aeration board 12 does not have airway 17-2 and aeration board tremie pipe 16-2, but its aeration board outer wall is provided with the leakage fluid dram 21 that is used to discharge reaction residue, and leakage fluid dram 21 is provided with tapping valve.Connect on eddy flow plate outer wall and the aeration board outer wall and be provided with urgent leakage fluid dram 13, be provided with urgent tapping valve 29 on each urgent leakage fluid dram 13, described leakage fluid dram 21 and all urgent leakage fluid dram 13 all are communicated with as shown in Figure 1 Drainage pipe 42, can discharge the interior liquid starting material of reactor 1 whenever necessary rapidly.
Link together by eddy flow plate outer wall between the adjacent eddy flow plate, connect by the aeration board outer wall between the adjacent aeration board, be connected with the aeration board outer wall by eddy flow plate outer wall between adjacent eddy flow plate and the aeration board.
The top of described reactor 1 is provided with top airway 17-3, and what top airway 17-3, a plurality of middle part airway 17-1 and bottom airway 17-2 formed reactor 1 is positioned at intermediary airway 17, is used to derive the chlorine dioxide that generates in the reactor 1.Be communicated with by a connecting pipe 3 between airway 17 and the feeder 2, to derive the chlorine dioxide of Y type mixings filling tube 4 places generation.As shown in Figure 1, airway 17 is connected to gas output tube 46, and gas output tube 46 is provided with pressure transmitter 40 and safety valve 41, and safety valve 41 can guarantee in time to discharge under the unforeseen circumstances chlorine dioxide in the reactor 1.
Be separately installed with temperature control unit 38 and well heater temperature control unit 37 on water-bath warmer 30 as shown in Figure 1 and the airheater 36, be heated to suitable temperature of reaction to guarantee liquid starting material and air.
Described water-bath warmer 30 comprises housing 22, and its shape can be right cylinder, and material can be PVC; Centre in the housing 22 is provided with heating tube 24, select quartz heating-pipe in the present embodiment, heating tube 24 can be coated by sheath 27, in the present embodiment, sheath 27 is the CPVC material, shape is all cylindrical, has louvre 28 on the outer wall of sheath 27, to transmit the heat that heating tube 24 sends evenly and rapidly.Liquid conducting pipes is imported by the top of water-bath warmer 30, and begins the outside that curl is wrapped in sheath 27 from the bottom of sheath 27, is finally still derived by the top of water-bath warmer 30.Be provided with temperature controlled switch 23 in the housing 22.During work, fill with liquid working media in the housing 22, can be water or oil, liquid starting material to be heated (sodium chlorate mixed solution or sulfuric acid) is by 25 inputs of top liquid-inlet pipe, the fluid pipeline that the lopping of flowing through under the pressure effect of feedstock pump 32 is twined, in this process, be heated to temperature requiredly, and derive by top drain pipe 26.The characteristics of this water-bath warmer 30 are: (1) is heated liquid and flows in sealing-duct, and ducted liquid pressure is not influenced by external pressure by infusion pressure and Heating temperature decision; (2) fluid pipeline that twines of its volution and liquid warming medium make this water-bath warmer can be fast, evenly, stably liquid starting material is heated, and keep steady temperature; (3) by heated liquid starting material with the heating original paper directly do not contact, but in sealing-duct by working medium (water/oil) even heating, can avoid raw material uneven local superheating, bubble and even the volatilization etc. that produce of being heated influence the unfavoured state of material concentration (hydrogen peroxide be heated easily decomposition and cause heating the material loss of link).
During the equipment work of the preparation dioxide peroxide of realization high-conversion rate of the present invention, at first the feedstock pump 32 by separately pumps into separately water-bath warmer 30 through sulfuric acid carrier pipe 44 and sodium chlorate mixed solution carrier pipe 45 with two kinds of liquid starting materials, is heated to the corresponding liquid raw material temperature required; Carry to feeder 2 through vacuum breaker 34 separately then.This vacuum breaker 34 is a back pressure valve, on the one hand, can stop that liquid starting material refluxes under the unforeseen circumstances; On the other hand, can keep pressure in carrier pipe and the reactor 1 within the scope of setting.After liquid starting material entered feeder 2, during through expansion section 4-1 in Y type mixing filling tube 4 arms and contraction section 4-2, atomizing rapidly became the gas-liquid mixed state under the effect of pressure.The liquid starting material of two kinds of atomizings is in the synthesis stage 4-3 of Y type mixing filling tube 4 mixing and begin reaction, the breather hole 4-4 that offers on the tube wall of the chlorine dioxide that is produced by synthesis stage 4-3 imports in the feeder 2, and taken out of feeder 2 by the warm air that is imported through warm air input tube 6, send into gas output tube 46 by airway 17.
Liquid starting material through initial reaction enters the reactor 1 from feeder 2 through top tremie pipe 16-3, and drop on one deck eddy flow plate 7, begin to form eddy flow, liquid starting material by eddy flow plate tremie pipe 16 and aeration board tremie pipe 16-2 successively through two layers of eddy flow plate 8, three layers of eddy flow plate 9, four layers of eddy flow plate 10, five layers of aeration board 11 and six layers of aeration board 12, the liquid starting material eddy flow forms in reactor 1 and keeps the time of eddy flow state is more than or equal to 2 hours, makes liquid starting material carry out sufficient uniform mixing and reaction.
The warm air that aeration tube 14 is imported is in solarization air cap 15 enters reactor 1, the temperature of reaction that maintenance suits in making reactor 1 also improves the reaction efficiency, the hot gas flow that rises can also be taken the chlorine dioxide that reaction is generated out of along airway 17, the accident in order to avoid reactor 1 interior excessive concentration owing to chlorine dioxide meets accident.Reaction residue enters Drainage pipe 42 through the leakage fluid dram 21 of six layers of aeration board 12.
Breaking down or needing under the situation of emergency stop, the urgent tapping valve 29 on the urgent leakage fluid dram of offering on every layer of eddy flow plate and the aeration board 13 is the liquid starting material in the emptying reactor 1 at short notice, no longer produces chlorine dioxide.
The equipment of the preparation dioxide peroxide of realization high-conversion rate of the present invention, the purity of its preparation chlorine dioxide is 95%, the transformation efficiency that sodium chlorate is converted into chlorine dioxide is 95%.
Embodiment 1: the solid sodium chlorate of 99% concentration and the hydrogen peroxide of 50% concentration are formulated as the sodium chlorate mixed solution, are the dilute sulphuric acid of 75% concentration with the vitriol oil thin up of 98% concentration; By feedstock pump 32, it in this enforcement volume pump, sulfuric acid in molar ratio: sodium chlorate: the ratio of hydrogen peroxide=1.9: 1.9: 0.9 feeds intake to feeder 2 continuously, the water-bath warmer 30 that two kinds of solution enter before the feeder 2 by separately is heated to 56 ℃, also is heated to 56 ℃ by airheater 36 before the air admission feeder 2.Sulfuric acid, sodium chlorate mixed solution and warm air are mixed into vaporific gas-liquid mixture and begin reaction in Y type mixing filling tube 4, the reaction solution behind initial reaction enters reactor 1 through the multi-layer rotational flow aerated reaction.After tested, chlorine dioxide purity is 95%, and the transformation efficiency that sodium chlorate is converted into chlorine dioxide is 95%.
Embodiment 2: the solid sodium chlorate of 99% concentration and the hydrogen peroxide of 50% concentration are formulated as the sodium chlorate mixed solution, are the dilute sulphuric acid of 70% concentration with the vitriol oil thin up of 98% concentration; By feedstock pump 32, it in this enforcement volume pump, sulfuric acid in molar ratio: sodium chlorate: hydrogen peroxide=continuously to feeder 2 feed intake at 2: 2: 1, the water-bath warmer 30 that two kinds of solution enter before the feeder 2 by separately is heated to 60 ℃, also is heated to 60 ℃ by airheater 36 before the air admission feeder 2.Sulfuric acid, sodium chlorate mixed solution and warm air are mixed into vaporific gas-liquid mixture and begin reaction in Y type mixing filling tube 4, the reaction solution behind initial reaction enters reactor 1 through the multi-layer rotational flow aerated reaction.After tested, chlorine dioxide purity is 95%, and the transformation efficiency that sodium chlorate is converted into chlorine dioxide is 95%.
Embodiment 3: the solid sodium chlorate of 99% concentration and the hydrogen peroxide of 50% concentration are formulated as the sodium chlorate mixed solution, are the dilute sulphuric acid of 70% concentration with the vitriol oil thin up of 98% concentration; By feedstock pump 32, it in this enforcement volume pump, sulfuric acid in molar ratio: sodium chlorate: hydrogen peroxide=continuously to feeder 2 feed intake at 2.1: 2.1: 1.1, the water-bath warmer 30 that two kinds of solution enter before the feeder 2 by separately is heated to 64 ℃, also is heated to 64 ℃ by airheater 36 before the air admission feeder 2.Sulfuric acid, sodium chlorate mixed solution and warm air are mixed into vaporific gas-liquid mixture and begin reaction in Y type mixing filling tube 4, the reaction solution behind initial reaction enters reactor 1 through the multi-layer rotational flow aerated reaction.After tested, chlorine dioxide purity is 95%, and the transformation efficiency that sodium chlorate is converted into chlorine dioxide is 95%.
With the aqueous solution of the five step dioxide peroxide that make of iodometric determinations above embodiment, measure and testing data sees Table 1.Measuring method is five step iodimetry,iodometry in the 122nd page of 2.2.1.2.6 of " disinfection technology standard " version in 2002 " dioxide peroxide (ClO2) Determination on content " chapters and sections of issuing in November, 2002 according to Ministry of Health of the People's Republic of China.
In the iodine flask of 500ml, add 200ml distilled water, 1ml phosphate buffered saline buffer, draw 5ml ClO 2 solution sample in iodine flask, add the 10ml liquor kalii iodide again, and carry out uniform mixing.When faint yellow, add the 1ml starch solution with the Sulfothiorine titrating solution titration of 0.01mol/L, continue to drip just disappear to blueness till, the record reading is A.
In going out the solution of A value, above-mentioned titration adds 2.5mol/L hydrochloric acid soln 2.5ml again, and the 5min that opens in dark place.Disappear to blue with the titration of 0.01mol/L Sulfothiorine titrating solution, the record reading is B.
In the 500ml iodine flask, add 200ml distilled water, 1ml phosphate buffered saline buffer, drawing 1.0ml～10.0ml ClO 2 solution or diluent is added in the iodine flask, feeding high pure nitrogen then blows to yellow-green colour and disappears, add the 10ml liquor kalii iodide again, with the titration of Sulfothiorine titrating solution when faint yellow, add the 1ml starch solution, continue to drip just disappear to blueness till, the record reading is C.
In going out the solution of C value, above-mentioned titration adds 2.5mol/L hydrochloric acid soln 2.5ml again, and the 5min that opens in dark place.Disappear to blue with the titration of 0.01mol/L Sulfothiorine titrating solution, the record reading is D.
Add 1ml potassium bromide solution and 10ml concentrated hydrochloric acid in the 50ml iodine flask, mixing also adds 1.0ml～10.0ml ClO 2 solution again, clogs bottle stopper and mixing immediately.Place dark place reaction 20min, add the 10ml liquor kalii iodide then, concuss 5s is transferred in the 500ml iodine flask that the saturated disodium phosphate soln of 25ml is housed immediately, clean the 50ml iodine flask and washing lotion is transferred in the 500ml iodine flask, make the last volume of solution at 200ml～300ml.When faint yellow, add the 1ml starch solution with the titration of 0.01mol/L Sulfothiorine titrating solution, continue to drip just disappear to blueness till.Make blank with distilled water simultaneously.Getting reading is E=sample reading-blank reading.
Table 1
| |
|
|
|
| Reading A | 3.58ml | 3.60ml | 3.60ml |
| Reading B | 14.85ml | 14.85ml | 14.95ml |
| Reading C | 0.30ml | 0.35ml | 0.30ml |
| Reading D | 0.70ml | 0.65ml | 0.70ml |
| Reading E | 18.48ml | 18.49ml | 18.60ml |
| ClO 2 | 501.08mg/L | 502.85mg/L | 504.62mg/L |
| ClO 2 - | 24.79mg/L | 23.02mg/L | 24.79mg/L |
| ClO 3 - | 1.46mg/L | 1.17mg/L | 1.46mg/L |
| Cl 2 | 2.98mg/L | 3.72mg/L | 2.83mg/L |
More than disclosed only be a specific embodiment of the present invention, still, the present invention is not limited thereto, any those skilled in the art can think variation all should fall into protection scope of the present invention.
Claims (10)
1. a method for preparing dioxide peroxide comprises batch mixing step, main reaction step and goes out finished product output step, it is characterized in that:
In the described batch mixing step, two kinds of stock liquids are fed in the feeder via the two-way carrier pipe respectively, described feeder is installed on the reactor top and connects as one structure with reactor, comprise a Y type mixing filling tube in the described feeder, described Y type mixing filling tube one side has two arms that are communicated with described two-way carrier pipe respectively, its opposite side is communicated with described reactor, described two-way stock liquid carries out initial action after being pumped in the described Y type mixing filling tube, and the described initial reaction mixed solution of formation enters in the described reactor;
In the described main reaction step, described initial reaction mixed solution falls on the eddy flow plate of described reactor and forms eddy flow, after carrying out uniform mixing and reaction through multi-layer rotational flow plate and the multilayer aeration board that is positioned at described eddy flow plate below successively, form chlorine dioxide and reaction residue.
2. preparation method according to claim 1 is characterized in that:
In the described batch mixing step, described feeder also comprises the warm air input tube, and the warm air input tube is positioned at the corresponding position of Y type mixing filling tube, is used to keep the initial action desired reaction temperature and derives the chlorine dioxide that initial reaction forms;
In the described main reaction step, the airway that has connection described eddy flow plate of each layer and described aeration board in the described reactor, described airway is communicated with gas output tube on the described reactor, and the dioxide peroxide that generates on described each layer eddy flow plate and the described aeration board enters described gas output tube by described airway;
In the finished product output step, the chlorine dioxide of described generation is exported through the gas output tube on described reactor top by the hot gas that described aeration board provides, and described reaction residue is discharged through the Drainage pipe of described reactor bottom.
3. preparation method according to claim 2 is characterized in that:
In the described batch mixing step, described Y type mixing filling tube comprises expansion section, contraction section and synthesis stage, and at expansion section and contraction section place, liquid starting material atomizes under pressure and forms the gas-liquid mixed state; Described two arms combine the formation synthesis stage in contraction section bottom separately, and the liquid starting material after the atomizing is in described synthesis stage mixing and carry out initial action, and forms the initial reaction mixed solution;
In the described main reaction step, described every layer of eddy flow plate comprises the eddy flow groove that passed through the connection of liquid mouth each other, initial reaction mixed solution formed eddy flow direction in the adjacent eddy flow groove of every layer of eddy flow plate opposite each other and flow into by eddy flow plate tremie pipe under on one deck eddy flow plate, the initial reaction mixed solution on last one deck eddy flow plate flows on the superiors' aeration board.
4. according to any described preparation method of claim 1 to 3, it is characterized in that:
In two kinds of stock liquids, a kind of is aqueous sulfuric acid, and a kind of is the sodium chlorate and the hydrogen peroxide mixture aqueous solution, and the mol ratio that adds sulfuric acid, sodium chlorate and hydrogen peroxide in the described stock liquid is (1.9～2.1): (1.9～2.1): (0.9～1.1);
Described initial reaction mixed solution keeps the time of eddy flow state more than or equal to 2 hours in described reactor.
5. according to any described preparation method of claim 1 to 3, it is characterized in that: described two carrier pipes are coated with liquid working media outward respectively so that it is heated, accordingly, shape is twined at described two carrier pipes heating zone place of being coated with liquid working media twist.
6. according to any described preparation method of claim 1 to 3; it is characterized in that: described reactor is provided with urgent tapping valve; be used for breaking down or needing under the situation of emergency stop, the liquid emptying with in the reactor no longer produces chlorine dioxide.
7. an equipment for preparing dioxide peroxide comprises the feeder and the reactor that are communicated with in turn, it is characterized in that:
Described feeder is installed on the reactor top, and connects as one structure with reactor, comprises a Y type mixing filling tube in the described feeder, and described Y type mixing filling tube one side has two arms, is communicated with the carrier pipe that two-way is used to import stock liquid respectively; Its opposite side is communicated with described reactor;
From top to bottom be provided with the aeration board that is used to provide rising hot gas that multilayer is used to form the eddy flow plate of eddy flow and is positioned at described eddy flow plate below in the described reactor successively.
8. equipment according to claim 7 is characterized in that:
Have in the described reactor one be communicated with described eddy flow plate of each layer and described aeration board deriving the airway of chlorine dioxide, described airway is communicated with gas output tube on the described reactor, the reactor bottom is provided with the Drainage pipe of discharge reaction residue.
9. equipment according to claim 8 is characterized in that:
Described every layer of eddy flow plate comprises eddy flow plate base plate, is positioned at the eddy flow plate outer wall at outer rim place, described eddy flow plate base plate upper surface, and the gas port that is positioned at the described airway of formation at described base plate middle part, described plate upper surface is provided with eddy flow plate baffle plate and multiple tracks begins from inside to outside the eddy flow cell wall of setting in turn from the gas port periphery, and described eddy flow plate baffle plate radially extends to eddy flow plate outer wall place by the most inboard eddy flow cell wall; Form the eddy flow groove between the adjacent eddy flow cell wall and between outermost eddy flow cell wall and eddy flow plate outer wall; Offered the liquid mouth on the eddy flow cell wall between adjacent eddy flow groove, the described liquid mouth of crossing alternately is divided into the eddy flow baffle plate both sides, so that the formed eddy flow direction of adjacent eddy flow groove is opposite, the base plate of described eddy flow groove correspondence is provided with the tremie pipe of downward one deck eddy flow plate or aeration board extension, and the base plate of the eddy flow groove correspondence on last one deck eddy flow plate is provided with the tremie pipe that extends to the superiors' aeration board.
10. equipment according to claim 9 is characterized in that: in the described reactor, the eddy flow plate structure of alternate setting is identical, and the described tremie pipe on two eddy flow plates of adjacent setting is arranged at the eddy flow groove place of different positions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010103162XA CN102134059A (en) | 2010-01-27 | 2010-01-27 | Method and device for preparing chlorine dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010103162XA CN102134059A (en) | 2010-01-27 | 2010-01-27 | Method and device for preparing chlorine dioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583251A (en) * | 2012-03-30 | 2012-07-18 | 云南玉溪滇豫化工科技有限公司 | Chlorine dioxide reaction device |
| CN105056847A (en) * | 2015-09-17 | 2015-11-18 | 天津滨海新区东一科技发展有限公司 | Solvent hydrocyclone reaction vessel device |
-
2010
- 2010-01-27 CN CN201010103162XA patent/CN102134059A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583251A (en) * | 2012-03-30 | 2012-07-18 | 云南玉溪滇豫化工科技有限公司 | Chlorine dioxide reaction device |
| CN102583251B (en) * | 2012-03-30 | 2013-08-21 | 云南玉溪滇豫化工科技有限公司 | Chlorine dioxide reaction device |
| CN105056847A (en) * | 2015-09-17 | 2015-11-18 | 天津滨海新区东一科技发展有限公司 | Solvent hydrocyclone reaction vessel device |
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Application publication date: 20110727 |