CN102701157A - Method and device for producing sodium hypochlorite - Google Patents
Method and device for producing sodium hypochlorite Download PDFInfo
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- CN102701157A CN102701157A CN2012102067810A CN201210206781A CN102701157A CN 102701157 A CN102701157 A CN 102701157A CN 2012102067810 A CN2012102067810 A CN 2012102067810A CN 201210206781 A CN201210206781 A CN 201210206781A CN 102701157 A CN102701157 A CN 102701157A
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Abstract
The invention discloses a method and a device for producing sodium hypochlorite. The method comprises the steps as follows: adding a caustic soda solution into a reactor; adding chlorine, adjusting the chlorine adding speed of a chlorine adding device according to a temperature value, controlling the opening and closing of a cooling device to enable the temperature value of the reaction liquid to be not more than 45 DEG C, and adjusting the chlorine adding speed of the chlorine adding device according to the pH value to enable the pH value of the reaction liquid to be not less than 10; and the reaction is finished when the pH value of the reaction liquid is kept less than 12 within a first time interval. The device comprises the reactor, the chlorine adding device, a pH value detection device, a temperature detection device, the cooling device and a control device. According to the device and the method provided by the invention, accuracy control of the production process is realized, side reaction is suppressed, the reaction end point can be judged accurately, chlorination reaction is avoided, the utilization ratio of liquid chlorine reaches 99.68 to 99.95 percent, and the available chlorine content of the sodium hypochlorite is greater than or equal to 11.5 percent. According to the device provided by the invention, automatic control of the production process of the sodium hypochlorite is realized, manual labor and material resources are saved, and the production efficiency is improved.
Description
Technical field
The present invention relates to the Youxiaolin production field, relate in particular to a kind of working method and device of Youxiaolin.
Background technology
Youxiaolin and chlorine all have stronger oxidisability, can be as the desirable sterilizing agent of water treatment field.In existing water treatment field; Generally adopt chlorine as sterilizing agent; Along with the development of society and the construction in city, the applying unit of chlorine is surrounded by commercial zone, Residential areas gradually, but there is higher disclosure risk in chlorine in transportation and use; Therefore, safer, stable sterilizing agent certainly will will replace chlorine.The danger of Youxiaolin is very low, in transportation and use, all has higher security, will replace chlorine gradually in water treatment field, and market outlook are considerable.
The Youxiaolin product is more in the market; But mainly be the sub product of chlor-alkali industry; This kind Youxiaolin product has several quality problems such as available chlorine content is low, impurity big, free alkali exceeds standard; General as the manufacture raw material, seldom use because its sterilizing agent effect is low at sewage treatment area.External Youxiaolin is pushed out with regard to the U.S. in early days in nineteen seventies and is used for drinking water disinfection, and particularly Youxiaolin is applied in the U.S. as the substitute of chlorine especially in recent years.The more metropolitan water factories of China are also at the agent retrofit work that actively carries out disinfection at present, and the demand of Youxiaolin will be increasing.
The production technique of Youxiaolin mainly contains electrolytic process and chlorination.Electrolytic process mainly is to utilize sodium chloride solution under galvanic action, and anode produces chlorine (Cl
2), negative electrode produces hydrogen (H
2) and sodium hydroxide (NaOH), generate Youxiaolin between electrode.The aforesaid method production cost is high, and energy consumption is big, produces hydrogen, and is dangerous high, is not suitable for a large amount of industrial production and uses.Chlorination mainly is in sodium hydroxide solution, to feed chlorine (liquid chlorine), after sodium hydroxide and chlorine reaction are accomplished, through precipitate and separate sodium-chlor, produces the chlorine bleach liquor.Aforesaid method is accomplished scale production in industrial production easily.
But chlorination is produced in the process of Youxiaolin, and temperature and pH value are all had strict requirement.The too high Youxiaolin decomposition rate of temperature is accelerated, and following side reaction can take place.Simultaneously, reaction end is very important to Youxiaolin production, and the perchlorizing reaction can take place the overstep of end point line, and perchlorizing reacts even possibly cause Youxiaolin all to decompose.
High-efficient automatic Youxiaolin production technique is not seen report.Therefore, need a kind of can accurately control to above-mentioned side reaction, and the production technique and the device of the Youxiaolin of production high-quality efficiently.
Summary of the invention
One object of the present invention is to provide a kind of working method of Youxiaolin.Working method of the present invention detects the pH value of reaction solution in real time, regulates chlorination speed, makes the pH value of reaction solution be not less than 10; Also the temperature of reaction solution is detected in real time simultaneously; Regulate chlorination speed, and utilize refrigerating unit, make the temperature value of reaction solution be not more than 45 ℃; Thereby realize accurate control, suppressed the generation of side reaction production process.And can realize accurate judgement based on working method of the present invention, avoid the generation of perchlorizing reaction reaction end.The present invention has guaranteed the stable of product in the production process, has improved utilization ratio of raw materials, and the utilization ratio of liquid chlorine reaches 99.68%～99.95%, and the utilization ratio of sodium hydroxide reaches 99.10～99.90%.
Another object of the present invention is to provide a kind of device that is used for the working method of Youxiaolin.Device of the present invention is provided with pH value detection device and chlorinating equipment in reactor drum, regulate chlorination speed through chlorinating equipment, and device of the present invention also comprises temperature-detecting device and refrigerating unit; Temperature through refrigerating unit control reaction solution; Regulate chlorination speed through chlorinating equipment,, thereby reach purpose the temperature controlling of reaction solution with the degree of adjusting chlorination reaction; The working order of chlorination speed and refrigerating unit adapts, all controlled device control of the work of above-mentioned each device.Device of the present invention has been realized the robotization control to the Youxiaolin production process, has saved manpower and materials, has improved production efficiency.
Technical scheme provided by the invention is:
A kind of working method of Youxiaolin may further comprise the steps:
Step 1, in reactor drum, add sodium hydroxide solution;
Add chlorine in step 2, the sodium hydroxide solution of use chlorinating equipment in said reactor drum; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, and regulate the chlorination speed of said chlorinating equipment in said reaction solution according to this temperature value; And open and close according to this temperature value controlled chilling device; So that the temperature value of said reaction solution is not more than 45 ℃, simultaneously, detect the pH value of said reaction solution through the pH value detection device; And according to the chlorination speed of this pH value adjusting chlorinating equipment in reaction solution, so that the pH value of said reaction solution is not less than 10;
The judgement of step 3, reaction end: when the pH of reaction solution value keeps less than 12 in very first time interval, then react and accomplish, said chlorinating equipment stops chlorination.
Preferably; In the working method of described Youxiaolin, in the said step 2, detect the pH value of said reaction solution through the pH value detection device; And according to the chlorination speed of this pH value adjusting chlorinating equipment in reaction solution; So that the pH value of said reaction solution is not less than 10, realize through following process
When the pH of said reaction solution value greater than 12 the time; The chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the pH of said reaction solution value was reduced between 11 ~ 12 in second timed interval; The chlorination speed of said chlorinating equipment is reduced to 2 ~ 3kg/min, and when the pH of said reaction solution value is reduced in second timed interval smaller or equal to 11 the time, said chlorinating equipment stops chlorination.
Preferably, in the working method of described Youxiaolin,
In the said step 2; In reaction process, detect the pH value of said reaction solution, its Ё through the pH value detection device; Said pH value detection device includes at least two pH value detection devices; Said at least two pH detect and are arranged in the said reactor drum, and there is the gap on the height in the position in said reactor drum, and the pH value of said reaction solution is the minimum value in the pH value of the reaction solution that detected by said at least two pH proofing units;
In the said step 3, when the pH value of the reaction solution that said at least two pH proofing units are detected all keeps at interval less than 12 the time in the said very first time, the reaction completion, said chlorinating equipment stops chlorination.
Preferably, in the working method of described Youxiaolin, in the said step 2; In reaction process, the open cold radiator cooler is so that the temperature value of said reaction solution is not more than 45 ℃; Realize through following process,, close refrigerating unit when the temperature value of said reaction solution during less than 25 ℃; The chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min, when the temperature value of said reaction solution rises between 25 ~ 30 ℃ in said second timed interval, and the open cold radiator cooler; The chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min; When the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval, keep refrigerating unit to be in opened condition, the chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min; When the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
Preferably, in the working method of described Youxiaolin, said refrigerating unit includes internal cooling device and outer refrigerating unit; Wherein, said internal cooling device has first heat exchange component, and said outer refrigerating unit has second heat exchange component; And the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant; Said first heat exchange component is arranged in the said reactor drum, and said second heat exchange component is arranged at the outside of said reactor drum
When the temperature value of said reaction solution during less than 25 ℃, close internal cooling device and outer refrigerating unit, the chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the temperature value of reaction solution rises between 25 ~ 30 ℃ in said second timed interval; Open the internal cooling device, keep outer refrigerating unit to be in closing condition, the chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min; When the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval; Keep the internal cooling device to be in opened condition, open outer refrigerating unit, the chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min; When the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
Preferably, in the working method of described Youxiaolin,
In the said step 2; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, wherein; Said temperature-detecting device includes at least two temperature-detecting devices; Said at least two temperature-detecting devices are arranged in the said reactor drum, and there is the gap on the height in the position in said reactor drum, and the temperature value of said reaction solution is for by the peak in the temperature value of the reaction solution that said at least two temperature-detecting devices detected.
Preferably; In the working method of described Youxiaolin; In the said step 2, use in the sodium hydroxide solution of chlorinating equipment in said reactor drum to add liquid chlorine, wherein; Said chlorinating equipment includes along the chlorination pipeline of the longitudinal extension of said reactor drum, has the chlorination outlet in the end of said chlorination pipeline.
A kind of device that is used to realize the Youxiaolin working method comprises:
Reactor drum;
Chlorinating equipment, it has the chlorination outlet, and said chlorination outlet is arranged in the said reactor drum;
The pH value detection device, it is arranged in the said reactor drum;
Temperature-detecting device, it is arranged in the said reactor drum;
Refrigerating unit, its inner refrigerant that feeds carries out heat exchange with said reactor drum;
Gear; It is connected with said pH value detection device, said temperature-detecting device, said chlorinating equipment and said refrigerating unit; The temperature value signal that pH value signal and the said temperature-detecting device that is detected according to said pH value detection device detected is regulated the chlorination speed of said chlorinating equipment and the open and close of controlling said refrigerating unit.
Preferably, in the described device, said refrigerating unit includes internal cooling device and outer refrigerating unit; Wherein, Said internal cooling device has first heat exchange component, and said outer refrigerating unit has second heat exchange component, and the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant; Said first heat exchange component is arranged in the said reactor drum; Be the spiral pipe of the longitudinal extension of said reactor drum, said second heat exchange component is arranged at the outside of said reactor drum, for being coated on the cavity of said reactor drum outer wall.
Preferably, in the described device, said chlorinating equipment includes along the spirrillum chlorination pipeline of the longitudinal extension of said reactor drum, has the chlorination outlet in the end of said chlorination pipeline.
The present invention has following beneficial effect:
(1) device of the present invention has internal cooling device and outer refrigerating unit, according to the temperature conditions of reaction solution, and the work of controlled chilling device; When temperature value during less than 25 ℃, open cold radiator cooler not rises in second timed interval when temperature in 25 ~ 30 ℃ the scope; Only open the work of internal cooling device, when temperature rises to 30 ~ 40 ℃ in second timed interval, then open internal cooling device and outer refrigerating unit simultaneously; The co-operation of internal cooling device and outer refrigerating unit has guaranteed the homogeneity of cooling and suitable cooling rate, has realized the accurate control of reacting liquid temperature; Feasible reaction is carried out in low temperature environment all the time, avoids the generation of side reaction.
(2) method of the present invention adopts at least two temperature-detecting devices and at least two pH value detection devices that reaction is monitored; Particularly; In reactor drum of the present invention, be provided with two temperature-detecting devices and two pH value detection devices; There is the gap on the height in two positions of temperature-detecting device in reactor drum, and two pH value detection devices also take same mode to be provided with, thereby can monitor the reaction severe of the different piece in the reactor drum; Avoided the generation of partial side reaction or perchlorizing reaction, guaranteed simultaneously the accurate sensitive of reaction end is judged.
(3) chlorinating equipment of the present invention has along the spirrillum chlorination pipeline of the longitudinal extension of reactor drum, and liquid chlorine is at first vaporized in the chlorination pipeline during chlorination, with the reaction solution heat exchange in the reactor drum, has also reached the effect that reduces the temperature of reaction solution.
(4) in the method for the present invention according to the temperature or the pH value situation of reality, divide ladder to set chlorination speed, to realize under the different situations control to the severe of chlorination reaction; When the temperature of control reaction solution, also want the open cold radiator cooler, said process has been realized the accurate control to the production process of Youxiaolin; Improved production efficiency; Greatly improved utilization ratio of raw materials, the utilization ratio of liquid chlorine reaches 99.68%～99.95% among the present invention, and the utilization ratio of sodium hydroxide reaches 99.10～99.90%; Reduced the scrap rate of product, product Youxiaolin available chlorine content >=11.5%.
Description of drawings
Fig. 1 is the structural representation of the device of the working method that is used to realize Youxiaolin of the present invention of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is done further detailed description, can implement according to this with reference to the specification sheets literal to make those skilled in the art.
As shown in Figure 1, the present invention provides a kind of working method of Youxiaolin, may further comprise the steps:
Step 1, in reactor drum, add sodium hydroxide solution;
Add chlorine in step 2, the sodium hydroxide solution of use chlorinating equipment in said reactor drum; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, and regulate the chlorination speed of said chlorinating equipment in said reaction solution according to this temperature value; And open and close according to this temperature value controlled chilling device; So that the temperature value of said reaction solution is not more than 45 ℃, simultaneously, detect the pH value of said reaction solution through the pH value detection device; And according to the chlorination speed of this pH value adjusting chlorinating equipment in reaction solution, so that the pH value of said reaction solution is not less than 10;
The judgement of step 3, reaction end: when the pH of reaction solution value keeps less than 12 in very first time interval, then react and accomplish, said chlorinating equipment stops chlorination.
In the working method of described Youxiaolin; In the said step 2, detect the pH value of said reaction solution, and regulate the chlorination speed of chlorinating equipment in reaction solution according to this pH value through the pH value detection device; So that the pH value of said reaction solution is not less than 10; Realize through following process, when the pH of said reaction solution value greater than 12 the time, the chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the pH of said reaction solution value was reduced between 11 ~ 12 in second timed interval; The chlorination speed of said chlorinating equipment is reduced to 2 ~ 3kg/min, and when the pH of said reaction solution value is reduced in second timed interval smaller or equal to 11 the time, said chlorinating equipment stops chlorination.
In the working method of described Youxiaolin, in the said step 2, in reaction process; Detect the pH value of said reaction solution through the pH value detection device; Wherein, said pH value detection device includes at least two pH value detection devices, and said at least two pH detect and are arranged in the said reactor drum; And there is the gap on the height in the position in said reactor drum, and the pH value of said reaction solution is the minimum value in the pH value of the reaction solution that detected by said at least two pH proofing units; In the said step 3, when the pH value of the reaction solution that said at least two pH proofing units are detected all keeps at interval less than 12 the time in the said very first time, the reaction completion, said chlorinating equipment stops chlorination.
In the working method of described Youxiaolin, in the said step 2, in reaction process; The open cold radiator cooler so that the temperature value of said reaction solution is not more than 45 ℃, is realized through following process; When the temperature value of said reaction solution during less than 25 ℃, close refrigerating unit, the chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the temperature value of said reaction solution rises between 25 ~ 30 ℃ in said second timed interval; The open cold radiator cooler, the chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min, when the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval; Keep refrigerating unit to be in opened condition; The chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min, and when the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
In the working method of described Youxiaolin, said refrigerating unit includes internal cooling device and outer refrigerating unit, wherein; Said internal cooling device has first heat exchange component, and said outer refrigerating unit has second heat exchange component, and the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant; Said first heat exchange component is arranged in the said reactor drum, and said second heat exchange component is arranged at the outside of said reactor drum, when the temperature value of said reaction solution during less than 25 ℃; Close internal cooling device and outer refrigerating unit; The chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min, when the temperature value of reaction solution rises between 25 ~ 30 ℃ in said second timed interval, opens the internal cooling device; Keep outer refrigerating unit to be in closing condition; The chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min, when the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval, keeps the internal cooling device to be in opened condition; Open outer refrigerating unit; The chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min, and when the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
In the working method of described Youxiaolin; In the said step 2; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, wherein; Said temperature-detecting device includes at least two temperature-detecting devices; Said at least two temperature-detecting devices are arranged in the said reactor drum, and there is the gap on the height in the position in said reactor drum, and the temperature value of said reaction solution is for by the peak in the temperature value of the reaction solution that said at least two temperature-detecting devices detected.
In the working method of described Youxiaolin; In the said step 2; Use in the sodium hydroxide solution of chlorinating equipment in said reactor drum and add liquid chlorine; Wherein, said chlorinating equipment includes along the chlorination pipeline of the longitudinal extension of said reactor drum, has the chlorination outlet in the end of said chlorination pipeline.
A kind of device that is used to realize the Youxiaolin working method comprises: reactor drum; Chlorinating equipment, it has the chlorination outlet, and said chlorination outlet is arranged in the said reactor drum; The pH value detection device, it is arranged in the said reactor drum; Temperature-detecting device, it is arranged in the said reactor drum; Refrigerating unit, its inner refrigerant that feeds carries out heat exchange with said reactor drum; Gear; It is connected with said pH value detection device, said temperature-detecting device, said chlorinating equipment and said refrigerating unit; The temperature value signal that pH value signal and the said temperature-detecting device that is detected according to said pH value detection device detected is regulated the chlorination speed of said chlorinating equipment and the open and close of controlling said refrigerating unit.
In the described device; Said refrigerating unit includes internal cooling device and outer refrigerating unit, and wherein, said internal cooling device has first heat exchange component; Said outer refrigerating unit has second heat exchange component; And the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant, and said first heat exchange component is arranged in the said reactor drum, is the spiral pipe of the longitudinal extension of said reactor drum; Said second heat exchange component is arranged at the outside of said reactor drum, for being coated on the cavity of said reactor drum outer wall.
In the described device, said chlorinating equipment includes along the spirrillum chlorination pipeline of the longitudinal extension of said reactor drum, has the chlorination outlet in the end of said chlorination pipeline.
At least two temperature-detecting devices can be monitored the reaction severe of different zones in the reactor drum, guarantee monitoring accuracy and safety.Particularly; In the present invention; At reactor drum two temperature-detecting devices are set, are respectively and urge megadyne temperature degree proofing unit and low level temperature-detecting device, wherein; High-order temperature-detecting device is arranged at the position near the top of reactor drum, and the low level temperature-detecting device is arranged on the position near the bottom of reactor drum.The number of temperature-detecting device and the position of setting are not limited to embodiments of the invention, to realize that evenly obtaining reaction solution temperature value everywhere is purpose.In working method of the present invention, relatively large temperature value T in the temperature value of two detected reaction solutions of temperature-detecting device of needs assurance
MaxMeet temperature requirement.
Based on above-mentioned same reason, the pH proofing unit is provided with.The present invention is provided with high-order pH proofing unit and low level pH proofing unit, and wherein, high-order pH proofing unit is arranged at the position near the top of reactor drum, and low level pH proofing unit is arranged on the position near the bottom of reactor drum.The number of pH value detection device and the position of setting are not limited to embodiments of the invention, to realize that evenly obtaining reaction solution pH value everywhere is purpose.
Gear of the present invention is DCS (Distributed Control System, a distribution type control system) system, based on above-mentioned DCS system, has realized working method of the present invention.
As shown in Figure 1, the inventive system comprises following structure: gear 17, internal cooling device, outer refrigerating unit, high-order pH value detection device, low level pH value detection device, high-order temperature-detecting device, low level temperature-detecting device and chlorinating equipment.Gear 17 also has display interface.The internal cooling device includes the inside that first heat exchange component 9 and first unit, 2, the first heat exchange components 9 are arranged on reactor drum 18, is spiral helicine pipeline, its inner refrigerant that feeds, and first unit 2 is arranged at the refrigerant ingress of first heat exchange component.Outer refrigerating unit includes second heat exchange component 7 and second unit 13; Second heat exchange component 7 is for being coated on the cavity of reactor drum outer wall; Its inner refrigerant that feeds; Second unit 13 is arranged at the refrigerant ingress of second heat exchange component, above the cavity of second heat exchange component, is provided with refrigerant exit 6.Chlorinating equipment also has chlorination pipeline 10 and chlorination unit 3, and wherein, chlorination pipeline 10 is positioned at reactor drum 18, is spiral pipe, and chlorination outlet 12 is positioned at the end of chlorination pipeline 10, is positioned at the position of the bottom of reactor drum.Chlorination unit 3 sends module 5 through chlorination adjusting action command and is connected to gear; First unit sends module 14 through the order of internal cooling device action and is connected to gear; Second unit sends module 16 through outer refrigerating unit action command and is connected to gear, and the control command of difference receiving control device.High-order pH value detection device 1, low level pH value detection device 4, high-order temperature-detecting device 8 and low level temperature-detecting device 11 all signal transfer connector and the information parameter collection transport module 15 through separately are connected with gear, to the gear transmission signal.
Among the present invention, chlorination is in cold sodium hydroxide solution, to feed chlorine (liquid chlorine), controlled temperature≤45 ℃, and pH＞10 when free alkali content is 0.1%-1%, stop to feed chlorine through precipitate and separate sodium-chlor, produce the chlorine bleach liquor.
But chlorination is produced in the process of Youxiaolin, and the too high Youxiaolin decomposition rate of temperature is accelerated, and following side reaction can take place:
2NaClO+2H
2O=2NaOH+2HClO
2HClO+NaClO=NaClO
3+2HCl
2HCl+2NaOH=2NaCl+2H
2O
3NaClO=NaClO
3+2NaCl
Above-mentioned side reaction is acutely being carried out more than 40 ℃ and pH value significantly descends; For preventing this side reaction; In the reaction process, the pH value remains greater than 10, and drops to smaller or equal to 11 o'clock in very first time interval in the pH value; Just stop chlorination, make the pH value can return to state as early as possible greater than 11.When temperature when the very first time rises to greater than 40 ℃ at interval, also stop chlorination, the internal cooling device is worked with outer refrigerating unit simultaneously simultaneously, so that the temperature of reaction solution drops to below 40 ℃ (promptly smaller or equal to 40 ℃ state) as early as possible.
Reaction end is very important to Youxiaolin production, the reaction of overstep of end point line generation perchlorizing, and reaction process is following:
NaClO+Cl
2+ H
2O=NaCl ten 2HClO
NaClO+2HClO=NaClO
3+2HCl
NaClO+2HCl=NaCl+H
2O+Cl
2
3NaClO=NaClO
3+2NaCl
The present invention is 12 to be reaction end with the pH value, reaches for second pitch time when the pH of reaction solution value keeps the state less than 12, then thinks sodium hydroxide in the reaction solution by total overall reaction, and this moment, reaction reached terminal point, stopped chlorination.The present invention can fully suppress side reaction and perchlorizing reaction, at utmost utilizes raw material, realizes the High-efficient Production of Youxiaolin.
The present invention adopts water as refrigerant.
Embodiment one
In following embodiment, the very first time is set at 10min at interval, and second timed interval was set at 3min, and wherein, second timed interval was that gear judges that accurately the variation of pH value and temperature value provides foundation.
Working method of the present invention includes two stages---initiation section and production control section.
(1) initiation section
In reactor drum, add the sodium hydroxide solution of 8000kg15%, before production started, the initial temperature through temperature-detecting device monitoring sodium hydroxide solution determined whether the open cold radiator cooler according to this initial temperature.Relatively large that temperature value T in detected two initial temperature value of high-order temperature-detecting device of the present invention and low level temperature-detecting device
MaxMeet T
MaxIn the time of＞25 ℃, then open the internal cooling device; Work as T
MaxIn the time of≤25 ℃, start chlorinating equipment, begin in sodium hydroxide solution, to add liquid chlorine, this moment the chlorination speed control at 5 ~ 8kg/min, and get into the production control section.
(2) production control section
In the production control section, mainly need control, with the generation of effective inhibition side reaction to pH value and temperature in the production process.
The while is by the temperature of high-order temperature-detecting device and low level temperature-detecting device detection reaction liquid among the present invention.When the temperature value of reaction solution rises between 25 ~ 30 ℃ in 3min, open the internal cooling device, keep outer refrigerating unit to be in closing condition, the chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min; When temperature value in 3min rises to T rapidly
MaxBetween 30 ~ 40 ℃, then control the internal cooling device and work simultaneously with outer refrigerating unit, at this moment, chlorination speed is reduced to 2 ~ 3kg/min; Continue the temperature information collection, if temperature value rises to T in the 3min
MaxGreater than 40 ℃, then chlorinating equipment is closed, and stops chlorination, because this moment, the internal cooling device was all in running order with outer refrigerating unit, therefore, has only the TSD chlorinating equipment, to relax the severe of chlorination reaction, helps to reduce the temperature of reaction solution.
In reaction process, if temperature value satisfies T
MaxBetween 30 ~ 35 ℃, then keep the internal cooling device and open simultaneously with outer refrigerating unit; If temperature value is reduced to T rapidly in 3min
MaxBetween 25 ~ 30 ℃, then only to keep the internal cooling device and open, outer refrigerating unit is closed, and slowly increases to big flow chlorination, and chlorination speed slowly returns to 5 ~ 8kg/min; Continue the temperature information collection, if temperature value is reduced to T rapidly in 3min
MaxSmaller or equal to 25 ℃, then internal cooling device and outer refrigerating unit are all closed, keep big flow chlorination, chlorination speed is 5 ~ 8kg/min.The cycle control of said process formation temperature realizes the high-efficient automatic production control.
Real-time monitoring to the pH value of reaction solution relies on two pH value detection devices to realize.PH hereinafter
MinRefer to that the less relatively value in two pH values of the reaction solution that two pH proofing units are detected.If the pH value satisfies pH rapidly in 3min
MinBetween 11 ~ 12, then reduce chlorination speed---2 ~ 3kg/min; Continue the pH information acquisition, if the pH value is decreased to pH rapidly in 3min
MinSmaller or equal to 11, then close chlorinating equipment, stop chlorination.Continue the pH information acquisition, when the pH value satisfies pH
Min＞12 o'clock, open chlorinating equipment again, chlorination speed is 5 ~ 8kg/min.Said process has formed the cycle control of pH.
(3) judgement of reaction end
Two pH values that detected when high-order pH value detection device and low level pH value detection device continue 10min all less than 12, then close chlorinating equipment, and gear provides the reaction end report information, starts the blowing program, accomplish a collection of production.
Embodiment two ~ embodiment ten
Following examples two ~ embodiment ten all adopts the method same with embodiment one, and sodium hydroxide concentration remains unchanged, and each step parameter all is consistent in the implementation process.The result of each embodiment sees table 1.
Table 1
The utilization ratio of liquid chlorine reaches 99.68%～99.95% among the present invention, and the utilization ratio of sodium hydroxide reaches 99.10～99.90%, has reduced the scrap rate of product, product Youxiaolin available chlorine content >=11.5%.
Although embodiment of the present invention are open as above; But it is not restricted to listed utilization in specification sheets and the embodiment; It can be applied to various suitable the field of the invention fully, for being familiar with those skilled in the art, can easily realize other modification; Therefore under the universal that does not deviate from claim and equivalency range and limited, the legend that the present invention is not limited to specific details and illustrates here and describe.
Claims (10)
1. the working method of a Youxiaolin is characterized in that, may further comprise the steps:
Step 1, in reactor drum, add sodium hydroxide solution;
Add chlorine in step 2, the sodium hydroxide solution of use chlorinating equipment in said reactor drum; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, and regulate the chlorination speed of said chlorinating equipment in said reaction solution according to this temperature value; And open and close according to this temperature value controlled chilling device; So that the temperature value of said reaction solution is not more than 45 ℃, simultaneously, detect the pH value of said reaction solution through the pH value detection device; And according to the chlorination speed of this pH value adjusting chlorinating equipment in reaction solution, so that the pH value of said reaction solution is not less than 10;
The judgement of step 3, reaction end: when the pH of reaction solution value keeps less than 12 in very first time interval, then react and accomplish, said chlorinating equipment stops chlorination.
2. the working method of Youxiaolin as claimed in claim 1; It is characterized in that, in the said step 2, detect the pH value of said reaction solution through the pH value detection device; And according to the chlorination speed of this pH value adjusting chlorinating equipment in reaction solution; So that the pH value of said reaction solution is not less than 10, realize through following process
When the pH of said reaction solution value greater than 12 the time; The chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the pH of said reaction solution value was reduced between 11 ~ 12 in second timed interval; The chlorination speed of said chlorinating equipment is reduced to 2 ~ 3kg/min, and when the pH of said reaction solution value is reduced in second timed interval smaller or equal to 11 the time, said chlorinating equipment stops chlorination.
3. according to claim 1 or claim 2 the working method of Youxiaolin is characterized in that,
In the said step 2; In reaction process, detect the pH value of said reaction solution through the pH value detection device, wherein; Said pH value detection device includes at least two pH value detection devices; Said at least two pH detect and are arranged in the said reactor drum, and there is the gap on the height in the position in said reactor drum, and the pH value of said reaction solution is the minimum value in the pH value of the reaction solution that detected by said at least two pH proofing units;
In the said step 3, when the pH value of the reaction solution that said at least two pH proofing units are detected all keeps at interval less than 12 the time in the said very first time, the reaction completion, said chlorinating equipment stops chlorination.
4. the working method of Youxiaolin as claimed in claim 2 is characterized in that, in the said step 2; In reaction process, the open cold radiator cooler is so that the temperature value of said reaction solution is not more than 45 ℃; Realize through following process,, close refrigerating unit when the temperature value of said reaction solution during less than 25 ℃; The chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min, when the temperature value of said reaction solution rises between 25 ~ 30 ℃ in said second timed interval, and the open cold radiator cooler; The chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min; When the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval, keep refrigerating unit to be in opened condition, the chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min; When the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
5. the working method of Youxiaolin as claimed in claim 4 is characterized in that, said refrigerating unit includes internal cooling device and outer refrigerating unit; Wherein, said internal cooling device has first heat exchange component, and said outer refrigerating unit has second heat exchange component; And the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant; Said first heat exchange component is arranged in the said reactor drum, and said second heat exchange component is arranged at the outside of said reactor drum
When the temperature value of said reaction solution during less than 25 ℃, close internal cooling device and outer refrigerating unit, the chlorination speed setting of said chlorinating equipment is 5 ~ 8kg/min; When the temperature value of reaction solution rises between 25 ~ 30 ℃ in said second timed interval; Open the internal cooling device, keep outer refrigerating unit to be in closing condition, the chlorination speed that keeps said chlorinating equipment simultaneously is 5 ~ 8kg/min; When the temperature value of said reaction solution rose between 30 ~ 40 ℃ in said second timed interval; Keep the internal cooling device to be in opened condition, open outer refrigerating unit, the chlorination speed of regulating said chlorinating equipment simultaneously is reduced to 2 ~ 3kg/min; When the temperature value of said reaction solution rose to greater than 40 ℃ in said second timed interval, said chlorinating equipment stopped chlorination.
6. like the working method of claim 4 or 5 described Youxiaolin, it is characterized in that,
In the said step 2; In reaction process, detect the temperature value of said reaction solution through temperature-detecting device, wherein; Said temperature-detecting device includes at least two temperature-detecting devices; Said at least two temperature-detecting devices are arranged in the said reactor drum, and there is the gap on the height in the position in said reactor drum, and the temperature value of said reaction solution is for by the peak in the temperature value of the reaction solution that said at least two temperature-detecting devices detected.
7. like the working method of claim 4 or 5 described Youxiaolin; It is characterized in that; In the said step 2, use in the sodium hydroxide solution of chlorinating equipment in said reactor drum to add liquid chlorine, wherein; Said chlorinating equipment includes along the chlorination pipeline of the longitudinal extension of said reactor drum, has the chlorination outlet in the end of said chlorination pipeline.
8. a device that is used to realize Youxiaolin working method as claimed in claim 1 is characterized in that, comprising:
Reactor drum;
Chlorinating equipment, it has the chlorination outlet, and said chlorination outlet is arranged in the said reactor drum;
The pH value detection device, it is arranged in the said reactor drum;
Temperature-detecting device, it is arranged in the said reactor drum;
Refrigerating unit, its inner refrigerant that feeds carries out heat exchange with said reactor drum;
Gear; It is connected with said pH value detection device, said temperature-detecting device, said chlorinating equipment and said refrigerating unit; The temperature value signal that pH value signal and the said temperature-detecting device that is detected according to said pH value detection device detected is regulated the chlorination speed of said chlorinating equipment and the open and close of controlling said refrigerating unit.
9. device as claimed in claim 8 is characterized in that, said refrigerating unit includes internal cooling device and outer refrigerating unit; Wherein, Said internal cooling device has first heat exchange component, and said outer refrigerating unit has second heat exchange component, and the inside of said first heat exchange component and said second heat exchange component all feeds refrigerant; Said first heat exchange component is arranged in the said reactor drum; Be the spiral pipe of the longitudinal extension of said reactor drum, said second heat exchange component is arranged at the outside of said reactor drum, for being coated on the cavity of said reactor drum outer wall.
10. like claim 8 or 9 described devices, it is characterized in that said chlorinating equipment includes along the spirrillum chlorination pipeline of the longitudinal extension of said reactor drum, have the chlorination outlet in the end of said chlorination pipeline.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103677025A (en) * | 2013-12-19 | 2014-03-26 | 芜湖融汇化工有限公司 | On-line monitoring and controlling system used for sodium hypochlorite production |
| CN104338427A (en) * | 2013-08-09 | 2015-02-11 | 攀钢集团钛业有限责任公司 | Method for treating magnesium electrolysis chlorine-containing waste gas |
| CN109133010A (en) * | 2018-11-09 | 2019-01-04 | 杭州电化集团有限公司 | A kind of production method for sodium hypochlorite of paddling |
| CN111066812A (en) * | 2019-11-07 | 2020-04-28 | 天津绿涛环保科技有限公司 | Sodium hypochlorite disinfectant for drinking water and preparation method thereof |
| CN111732081A (en) * | 2020-05-19 | 2020-10-02 | 湖北宜化化工股份有限公司 | Device and method for industrially and continuously producing sodium hypochlorite |
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2012
- 2012-06-19 CN CN201210206781.0A patent/CN102701157B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104338427A (en) * | 2013-08-09 | 2015-02-11 | 攀钢集团钛业有限责任公司 | Method for treating magnesium electrolysis chlorine-containing waste gas |
| CN103677025A (en) * | 2013-12-19 | 2014-03-26 | 芜湖融汇化工有限公司 | On-line monitoring and controlling system used for sodium hypochlorite production |
| CN109133010A (en) * | 2018-11-09 | 2019-01-04 | 杭州电化集团有限公司 | A kind of production method for sodium hypochlorite of paddling |
| CN111066812A (en) * | 2019-11-07 | 2020-04-28 | 天津绿涛环保科技有限公司 | Sodium hypochlorite disinfectant for drinking water and preparation method thereof |
| CN111732081A (en) * | 2020-05-19 | 2020-10-02 | 湖北宜化化工股份有限公司 | Device and method for industrially and continuously producing sodium hypochlorite |
| CN111732081B (en) * | 2020-05-19 | 2023-07-14 | 湖北宜化化工股份有限公司 | Device and method for industrially and continuously producing sodium hypochlorite |
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| CN102701157B (en) | 2014-11-05 |
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