A kind of chlorine dioxide preparation apparatus of integration and method
Technical field
The present invention relates to a kind of chlorine dioxide preparation apparatus and method of integration.
Background technology
Dioxide peroxide is a kind of sterilizing agent of generally acknowledged efficient, nontoxic, quick, broad-spectrum sterilization, becomes the substitute products of the chlorine system sterilizing agents such as liquid chlorine, clorox, chloramines in fields such as water sterilization, paper-making pulping, fabric bleachings.The preparation method of dioxide peroxide mainly contains chemical method and electrolytic process two kinds, electrolytic process due to one-time investment large, production energy consumption is high, so there is no be promoted; Chemical method is with sodium chlorate, Textone, clorox and hydrochloric acid, sulfuric acid etc. for raw material, prepares dioxide peroxide by reaction in chemical reactor.Because chemical reaction is of a great variety, distinct, therefore chemical reactor differs greatly on configuration and size, needs in design to consider the feature of chemical reaction process and chemical technology.
Prepared by dioxide peroxide, now widely used technique reactor is divided into the reaction chamber of more than 3, again with effuser by the collection and confinement of gases of output in each reaction chamber and deliver to use point (or absorption system), reactor adopts carbon steel liner lass lining to replace titanium material in material, and titanium material is the optimal material of chlorine dioxide reaction device, but due to expensive, on the multiplex reaction unit larger at production scale, for medium-sized chlorine dioxide preparation apparatus (daily output 3-6 ton), titanium material is replaced with carbon steel liner lass lining, although this reduces the one-time investment of equipment ton output, but also make the wearing quality of equipment have a greatly reduced quality, and due to lass lining frangible, the later maintenance cost of equipment is also higher.
Utility model patent " a kind of stable chlorine dioxide reactor " (number of patent application: 201320194842.6), disclose a kind of horizontal chlorine dioxide reaction device, inside reactor is by dividing plate subregion, be divided into 5-7 reaction chamber, but this reactor takes up an area large, consumptive material is many, be generally used for the operating mode of daily output dioxide peroxide 8 tons and above scale, be not suitable for the dioxide peroxide preparation carrying out medium-sized production scale, because this reactor extends the mother liquor residence time by adopting to arrange to cut off in large reaction compartment more and prevent the short stream of mother liquor, but the reactor of multi-chamber structure adds consumptive material, the chlorine dioxide preparation apparatus of medium-sized production scale is not suitable for from ton output one-time investment angle, the simple multi-cavity type geometries shrink by large-scale chlorine dioxide preparation facilities is used for the preparation of medium-sized dioxide peroxide in addition, enough heat interchanging areas and aeration area to be ensured simultaneously, then will there is limitation in device on internals are arranged and be fixing, is unfavorable for inspection and maintenance.
Summary of the invention
For the deficiency that above-mentioned medium-sized chlorine dioxide preparation apparatus exists, the object of the invention is the singularity according to reaction mass and dioxide peroxide medium, a kind of chlorine dioxide preparation apparatus of integration is provided, feature for medium-scale reaction designs, reaction efficiency is improve by composition optimizes, Whole Equipment uses titanium material to make, structure-integrated by the integration realization of reaction zone, a reactor-comparting is become two reaction chambers and a gas collection district, thus reduce weight of equipment, decrease cost, be specially adapted to the operating mode of medium-scale output.
Another object of the present invention is to provide a kind of preparation method of dioxide peroxide, and this kind of method raw material consumption is few, and reaction efficiency is high, and security is good, and effectively reduces the generation of harmful side product in reaction process.
The present invention is achieved by the following technical solutions:
A kind of chlorine dioxide preparation apparatus of integration, comprise vertical reactor body, described vertical reactor body upper part is provided with charging opening, bottom is provided with temperature measuring equipment interface and loop exit, top is provided with end socket, end socket is respectively equipped with shower, aeration valve door interface and pressure tester interface, described inner barrel is provided with dividing plate, vertical reactor body is divided into main reaction chamber and the second reaction chamber, main reaction chamber space is greater than the second reaction chamber, and main reaction chamber is communicated with the gas-phase space of the second reactor top, and gas-phase space top is provided with air outlet and pressure relief device; The bottom of described main reaction chamber to be provided with the dioxide peroxide blowout that generates to the aerating apparatus of gas-phase space, is provided with the heating unit controlling temperature of reaction and speed of reaction in main reaction chamber; The thrust-augmenting nozzle preventing the short stream of reaction solution is provided with in described dividing plate; Be provided with bottom described second reaction chamber and will remain the aerating apparatus of dioxide peroxide blowout to gas-phase space, be provided with in second reaction chamber and control the reaction solution residence time and the upflow tube avoiding the short stream of reaction solution, upflow tube is provided with opening at the sidewall of vertical reactor body, and communicates with raffinate recovery and processing system; Reactor body is connected with outside feeding device, described outside feeding device comprises forced circulation pump, feeder and injector, one end of described forced circulation pump is connected with loop exit, the other end is connected with feeder, injector one end is connected with feeder, the other end is connected with charging opening, forms the circulation path making reaction solution keep turbulence state.
Described vertical reactor body is fixedly connected with infrastructure device by anchor;
Described end socket is oval;
Described vertical reactor body bottom portion is flat;
Described aerating apparatus is aeration plate or aeration tube;
Described heating unit is heating coil;
Described reactor body adopts the full titanium material of integration.
A kind of dioxide peroxide preparation method, adopt sodium chlorate, the vitriol oil as raw material, methyl alcohol, as reductive agent, reacts in above-mentioned chlorine dioxide preparation apparatus, and generate dioxide peroxide, concrete steps are as follows:
(1) in feeder, the vitriol oil and sodium chlorate solution is added, mixing;
(2) mixing solutions that step (1) obtains enters in injector, with methanol mixed;
(3) mixing solutions that step (2) obtains provides power by injector, enters in the main reaction chamber of reactor, react in main reaction chamber from charging opening;
(4), in step (3), the Air blowing that the dioxide peroxide of generation is bloated by aeration plate is to gas-phase space, and reaction solution is flowed out by the loop exit of reactor, power is provided by forced circulation pump, circulating of realization response liquid, improves reaction efficiency, ensure that fully carrying out of reaction;
(5) abundant reacted reaction solution enters the second reaction chamber by thrust-augmenting nozzle, aeration tube is provided with in second reaction chamber, by remaining dioxide peroxide blowout to gas-phase space, the chlorine dioxide generated drains into absorption system (or using point) eventually through air outlet, and the reacted raffinate overflow of the second reaction chamber is to raffinate recovery and processing system.
Wherein in step (1) and (2), the mass concentration of reductive agent methyl alcohol used is 95-100%, and the mass concentration of sodium chlorate solution is 30-60%, and the ratio of the quality of material of the reaction of sodium chlorate solution, the vitriol oil, methyl alcohol is 20 ~ 25:10 ~ 14:1;
In step (3), temperature of reaction is 55-85 DEG C.
Principle of work is: in reactor, first add water to that liquid level reaches height for reactor 1/2, start forced circulation pump, liquid in reactor is flowed out by loop exit, power is provided to enter feeder by forced circulation pump, reinforced and the pre-mixing of the vitriol oil and sodium chlorate solution's two kinds of raw materials is completed at this, flow through again injector complete methanol solution feed in raw material, then mixed material is added in the main reaction chamber of reactor by charging opening as propulsion source by injector, react in main reaction chamber, the Air blowing that the dioxide peroxide generated is bloated by aeration plate is to gas-phase space, the forced convection of external circulating system realization response liquid improves reaction efficiency, ensure fully carrying out of reaction, reaction solution enters the second reaction chamber further by thrust-augmenting nozzle.Second reaction chamber is provided with aeration tube by the blowout of the dioxide peroxide of remnants to gas-phase space, chlorine dioxide drains into absorption system (or using point) eventually through air outlet, the reaction residue overflow of the second reaction chamber is to raffinate recovery and processing system, and main reaction chamber is provided with heating unit and ensures temperature of reaction and speed of reaction; Be provided with aerating apparatus provide the uniform microbubble of enough tolerance by the dioxide peroxide stripping in reaction solution and air lift out, the disturbance simultaneously also strengthening reaction solution further increases reaction efficiency; Be provided with the generation that guiding device avoids the short stream of reaction solution; Be provided with loop exit make reaction solution keep circulation under turbulence state, be beneficial to the generation of reaction; Be provided with temperature and pressure-detecting device monitoring reaction solution state.This device also can be connected with DCS Controlling System, and under normal circumstances, DCS Controlling System can open and close tonifying Qi valve regulated reaction pressure by interlocking action, opens and closes the circulation of heating coil inner vapor and regulates temperature of reaction, ensure that reaction keeps perfect condition.Setting range is exceeded when causing temperature or pressure due to fault cause; DCS Controlling System also can be made according to fault urgency level and chainly stop the actions such as material, spraying cooling, Concatenate shut-down; especially fault superpressure also can cause pressure relief device to start pressure release, ensures equipment and production safety.Second reaction chamber is provided with the further stripping residual air of aeration tube, is provided with upflow tube, residence time of the reaction solution of guarantee the short stream of the reaction solution avoided.For improving security, reactor air outlet is provided with pressure relief device, ensures under the operational condition of tiny structure, the timely pressure release of energy when there is the situation causing pressure to raise due to dioxide peroxide detonation or other labile factors institute.
Beneficial effect of the present invention is:
(1) equipment adopts two chamber structures can realize conventional apparatus and adopts three chambers and the above reaction effect that can reach, Whole Equipment uses titanium material to make, structure-integrated by the integration realization of reaction zone, because reaction chamber only has two, cut off less in reaction chamber, therefore compared with the conventional apparatus of same volume, installation and repairing is convenient, and reduce weight of equipment, decrease cost, be specially adapted to the medium scale dioxide peroxide preparation of daily output 3 ~ 6 tons.
(2) the present invention ensures the residence time of mother liquor in reaction chamber mainly through external circulating system, and ensures the heat interchanging area that mother liquor is enough and aeration area, and the forced convection of realization response liquid improves reaction efficiency, ensures fully carrying out of reaction.
(3) on feed way, carry out adding raw material in external circulating system, according to reaction raw materials and reaction characteristics appropriate design feed way and feeding structure, carry out reaction raw materials pre-mixing, this just overcomes because short the caused reaction of the mother liquor residence time is insufficient, improves reaction efficiency and speed of reaction.
(4) preparation method of dioxide peroxide of the present invention, raw material consumption is few, and reaction efficiency is high, and security is good, and effectively reduces the generation of harmful side product in reaction process.
Accompanying drawing explanation
Fig. 1 is chlorine dioxide preparation apparatus structural representation of the present invention.
Description of reference numerals:
Wherein, 1 is aeration plate, and 2 is flat, and 3 is earth anchor, and 4 is cylindrical shell, 5 is charging opening, and 6 is shower, and 7 is air outlet, and 8 is pressure relief device, 9 is end socket, and 10 is upflow tube, and 11 is dividing plate, and 12 is heating coil, 13 is thrust-augmenting nozzle, and 14 is aeration tube, and 15 is loop exit, and 16 is forced circulation pump, 17 is temperature measuring equipment interface, and 18 is feeder, and 19 is injector, and 20 is aeration valve door interface, 21 is pressure tester interface, and 22 is gas-phase space, and 23 is main reaction chamber, and 24 is the second reaction chamber.Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.Structure, the principle of not detailed description are common practise.
A kind of chlorine dioxide preparation apparatus of integration, comprise reactor body, described reactor body is vertical cylinder 4, cylindrical shell 4 top is provided with charging opening 5, bottom is provided with temperature measuring equipment interface 17 and loop exit 15, top is provided with ellipsoidal head 9, end socket 9 is respectively equipped with shower 6, aeration valve door interface 20 and pressure tester interface 21, cylinder body bottom is flat 2, be fixedly connected with infrastructure device by earth anchor 3, described inner barrel is provided with dividing plate 11, cylindrical shell 4 is divided into main reaction chamber 23 and the second reaction chamber 24, main reaction chamber 23 space is greater than the second reaction chamber 24, main reaction chamber 23 is communicated with the gas-phase space 22 at the second reaction chamber 24 top, gas-phase space 22 top is provided with air outlet 7 and pressure relief device 8, the bottom of described main reaction chamber 23 to be provided with the dioxide peroxide blowout that generates to the aeration plate 1 of gas-phase space, is provided with the heating coil 12 controlling temperature of reaction and speed of reaction in main reaction chamber 23, the thrust-augmenting nozzle 13 preventing the short stream of reaction solution is provided with in described dividing plate 11, be provided with bottom described second reaction chamber 24 and will remain the aeration tube 14 of dioxide peroxide blowout to gas-phase space, be provided with in second reaction chamber 24 and control the reaction solution residence time and the upflow tube 10 avoiding the short stream of reaction solution, upflow tube 10 is provided with opening at the sidewall of cylindrical shell 4, and communicates with raffinate recovery and processing system, reactor body is connected with outside feeding device, described outside feeding device comprises forced circulation pump 16, feeder 18 and injector 19, one end of described forced circulation pump 16 is connected with loop exit 15, the other end is connected with feeder 18, injector 19 one end is connected with feeder 18, the other end is connected with charging opening 5, forms the circulation path making reaction solution keep turbulence state, and reactor body adopts the full titanium material of integration.
The chlorine dioxide preparation apparatus of integration of the present invention, principle of work is: in reactor, first add water to that liquid level reaches height for reactor 1/2, start forced circulation pump 16, liquid in reactor is flowed out by loop exit 15, power is provided to enter feeder 18 by forced circulation pump 16, reinforced and the pre-mixing of the vitriol oil and sodium chlorate solution's two kinds of raw materials is completed at this, flow through again injector 19 complete methanol solution feed in raw material, then mixed material is added in the main reaction chamber 23 of reactor by charging opening as propulsion source by injector 19, react in main reaction chamber 23, the Air blowing that the dioxide peroxide generated is bloated by aeration plate 1 is to gas-phase space 22.Reaction solution enters the second reaction chamber 24 further by thrust-augmenting nozzle 13.Second reaction chamber is provided with aeration tube 14 by the blowout of the dioxide peroxide of remnants to gas-phase space 22, and chlorine dioxide drains into absorption system (or using point) eventually through air outlet 7.The reaction residue overflow of the second reaction chamber 24 disables liquid recovery and processing system.Main reaction chamber is provided with heating coil 12 and ensures temperature of reaction and speed of reaction; Be provided with aeration plate 1 provide the uniform microbubble of enough tolerance by the dioxide peroxide stripping in reaction solution and air lift out, the disturbance simultaneously also strengthening reaction solution further increases reaction efficiency; Be provided with the generation that thrust-augmenting nozzle 13 avoids the short stream of reaction solution; Be provided with loop exit 15 make reaction solution keep circulation under turbulence state, be beneficial to the generation of reaction; Be connected with temperature and pressure-detecting device respectively with pressure tester interface 21 by temperature measuring equipment interface 17, monitor mother liquor state.Under normal circumstances, DCS Controlling System can open and close tonifying Qi valve regulated reaction pressure by interlocking action, opens and closes the circulation of heating coil inner vapor and regulates temperature of reaction, ensure that reaction keeps perfect condition.Setting range is exceeded when causing temperature or pressure due to fault cause; DCS Controlling System also can be made according to fault urgency level and chainly stop the actions such as material, spraying cooling, Concatenate shut-down; especially fault superpressure also can cause pressure relief device to start pressure release, ensures equipment and production safety.Second reaction chamber is provided with aeration tube 14 further stripping residual air, is provided with upflow tube 10, residence time of the mother liquor of guarantee the short stream of the mother liquor avoided.For improving security, reactor air outlet 7 is provided with pressure relief device Explosion-proof cap 8, ensures under the operational condition of tiny structure, the timely pressure release of energy when there is the situation causing pressure to raise due to dioxide peroxide detonation or other labile factors institute.
Embodiment 1:
Adopt mass concentration be 50% sodium chlorate solution, mass concentration be that the vitriol oil of 98% is as raw material, feed intake in feeder, mixing, the mixing solutions obtained enters in injector, be the methanol mixed of 95% with mass concentration, wherein, the mass ratio that feeds intake of sodium chlorate solution, the vitriol oil, methyl alcohol is 20:10:1, then power is provided by injector, mixed reaction mass is entered in the main reaction chamber of reactor from charging opening, react in main reaction chamber, main reaction chamber is provided with heating unit and temperature measuring equipment, ensures that reaction is carried out at 70 DEG C; The Air blowing that the dioxide peroxide generated in main reaction chamber is bloated by aeration plate is to gas-phase space, reaction solution is exported by reactor cycles and flows out, and provides power, circulating of realization response liquid by forced circulation pump, improve reaction efficiency, ensure that fully carrying out of reaction; Abundant reacted reaction solution enters the second reaction chamber by thrust-augmenting nozzle, aeration tube is provided with in second reaction chamber, by remaining dioxide peroxide blowout to gas-phase space, the chlorine dioxide generated drains into absorption system (or using point) eventually through air outlet, and the reacted raffinate overflow of the second reaction chamber is to raffinate recovery and processing system.
Embodiment 2:
Adopt mass concentration be 30% sodium chlorate solution, mass concentration be that the vitriol oil of 98% is as raw material, feed intake in feeder, mixing, the mixing solutions obtained enters in injector, be the methanol mixed of 100% with mass concentration, wherein, the mass ratio that feeds intake of sodium chlorate solution, the vitriol oil, methyl alcohol is 25:14:1, then power is provided by injector, mixed reaction mass is entered in the main reaction chamber of reactor from charging opening, react in main reaction chamber, main reaction chamber is provided with heating unit and temperature measuring equipment, ensures that reaction is carried out at 55 DEG C; The Air blowing that the dioxide peroxide generated in main reaction chamber is bloated by aeration plate is to gas-phase space, reaction solution is exported by reactor cycles and flows out, and provides power, circulating of realization response liquid by forced circulation pump, improve reaction efficiency, ensure that fully carrying out of reaction; Abundant reacted reaction solution enters the second reaction chamber by thrust-augmenting nozzle, aeration tube is provided with in second reaction chamber, by remaining dioxide peroxide blowout to gas-phase space, the chlorine dioxide generated drains into absorption system (or using point) eventually through air outlet, and the reacted raffinate overflow of the second reaction chamber is to raffinate recovery and processing system.
Embodiment 3:
Adopt mass concentration be 60% sodium chlorate solution, mass concentration be that the vitriol oil of 98% is as raw material, feed intake in feeder, mixing, the mixing solutions obtained enters in injector, be the methanol mixed of 95% with mass concentration, wherein, the mass ratio that feeds intake of sodium chlorate solution, the vitriol oil, methyl alcohol is 23:12:1, then power is provided by injector, mixed reaction mass is entered in the main reaction chamber of reactor from charging opening, react in main reaction chamber, main reaction chamber is provided with heating unit and temperature measuring equipment, ensures that reaction is carried out at 85 DEG C; The Air blowing that the dioxide peroxide generated in main reaction chamber is bloated by aeration plate is to gas-phase space, reaction solution is exported by reactor cycles and flows out, and provides power, circulating of realization response liquid by forced circulation pump, improve reaction efficiency, ensure that fully carrying out of reaction; Abundant reacted reaction solution enters the second reaction chamber by thrust-augmenting nozzle, aeration tube is provided with in second reaction chamber, by remaining dioxide peroxide blowout to gas-phase space, the chlorine dioxide generated drains into absorption system (or using point) eventually through air outlet, and the reacted raffinate overflow of the second reaction chamber is to raffinate recovery and processing system.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.