CN102701157B - Method and device for producing sodium hypochlorite - Google Patents
Method and device for producing sodium hypochlorite Download PDFInfo
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- CN102701157B CN102701157B CN201210206781.0A CN201210206781A CN102701157B CN 102701157 B CN102701157 B CN 102701157B CN 201210206781 A CN201210206781 A CN 201210206781A CN 102701157 B CN102701157 B CN 102701157B
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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 clorox production field, relate in particular to a kind of production method and device of clorox.
Background technology
Clorox 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 social development 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 procedure, therefore, safer, stable sterilizing agent certainly will will replace chlorine.The danger of clorox is very low, in transportation and use procedure, all has higher security, in water treatment field, will replace gradually chlorine, and market outlook are considerable.
Clorox product is more in the market, but be mainly the byproduct of chlor-alkali industry, this kind of clorox product has the several quality problems such as available chlorine content is low, impurity large, free alkali exceeds standard, general as manufacture raw material, at sewage treatment area, because its sterilizing agent effect is low, seldom use.External clorox was pushed out for drinking water disinfection with regard to the U.S. in early days in nineteen seventies, and particularly clorox is widely 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 clorox will be increasing.
The production technique of clorox mainly contains electrolytic process and chlorination process.Electrolytic process is mainly to utilize sodium chloride solution under galvanic action, and anode produces chlorine (Cl
2), negative electrode produces hydrogen (H
2) and sodium hydroxide (NaOH), between electrode, generate clorox.Aforesaid method production cost is high, and energy consumption is large, produces hydrogen, dangerous high, is not suitable for a large amount of industrial production application.Chlorination process is mainly in sodium hydroxide solution, to pass into chlorine (liquid chlorine), after sodium hydroxide has reacted with chlorine, through precipitate and separate sodium-chlor, produces chlorine bleach liquor.Aforesaid method is easily accomplished scale production in industrial production.
But chlorination process is produced in the process of clorox, and temperature and pH value are had to strict requirement.Excess Temperature clorox decomposition rate is accelerated, and following side reaction can occur.Meanwhile, reaction end is produced very important to clorox, and superchlorination reaction can occur overstep of end point line, and superchlorination reaction even may cause clorox all to decompose.
High-efficient automatic production process of sodium hypochlorite is not seen report.Therefore, need a kind of can accurately control above-mentioned side reaction, and production technique and device that can efficiently production high-quality clorox.
Summary of the invention
One object of the present invention is to provide a kind of production method of clorox.Production method of the present invention detects in real time to the pH value of reaction solution, regulate chlorination speed, make 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 the accurate control to production process, suppressed the generation of side reaction.And based on production method of the present invention, can realize the accurate judgement to reaction end, avoid the generation of superchlorination reaction.The present invention has guaranteed the stable of product in production process, has improved the utilization ratio of raw material, 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 of the production method for clorox.Device of the present invention is provided with pH value detection device and chlorinating equipment in reactor, by chlorinating equipment, regulate chlorination speed, device of the present invention also comprises temperature-detecting device and refrigerating unit, by refrigerating unit, control the temperature of reaction solution, by chlorinating equipment, regulate chlorination speed, to regulate the degree of chlorination reaction, thereby reach the object to the control of the temperature of reaction solution, the working order of chlorination speed and refrigerating unit adapts, and the work of above-mentioned each device all controlled device is controlled.Device of the present invention has been realized the automatization of clorox production process has been controlled, and has saved manpower and materials, has improved production efficiency.
Technical scheme provided by the invention is:
A production method for clorox, comprises the following steps:
Step 1, in reactor, add sodium hydroxide solution;
Step 2, use chlorinating equipment to add chlorine in the sodium hydroxide solution in described reactor, in reaction process, by temperature-detecting device, detect the temperature value of described reaction solution, and regulate described chlorinating equipment to the chlorination speed in described reaction solution according to this temperature value, and according to this temperature value, control the open and close of refrigerating unit, so that the temperature value of described reaction solution is not more than 45 ℃, simultaneously, by pH value detection device, detect the pH value of described reaction solution, and regulate chlorinating equipment to the chlorination speed in reaction solution according to this pH value, so that the pH value of described reaction solution is not less than 10,
The judgement of step 3, reaction end: when the pH of reaction solution value keeps being less than 12 in very first time interval, reacted, described chlorinating equipment stops chlorination.
Preferably, in the production method of described clorox, in described step 2, by pH value detection device, detect the pH value of described reaction solution, and regulate chlorinating equipment to the chlorination speed in reaction solution according to this pH value, so that the pH value of described reaction solution is not less than 10, by following process implementation
When the pH of described reaction solution value is greater than 12, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the pH of described reaction solution value is reduced between 11 ~ 12 within second timed interval, the chlorination speed of described chlorinating equipment is down to 2 ~ 3kg/min, when the pH of described reaction solution value is reduced to while being less than or equal to 11 within second timed interval, described chlorinating equipment stops chlorination.
Preferably, in the production method of described clorox,
In described step 2, in reaction process, by pH value detection device, detect the pH value of described reaction solution, its Ё, described pH value detection device includes at least two pH value detection devices, described at least two pH detect and are arranged in described reactor, and the position in described reactor deposits gap in height, the pH value of described reaction solution serve as reasons described in minimum value in the pH value of the reaction solution that detects of at least two pH proofing units;
In described step 3, when the pH value of the reaction solution detecting when described at least two pH proofing units all keeps being less than 12 in described very first time interval, reaction completes, and described chlorinating equipment stops chlorination.
Preferably, in the production method of described clorox, in described step 2, in reaction process, open cold radiator cooler, so that the temperature value of described reaction solution is not more than 45 ℃, by following process implementation, when the temperature value of described reaction solution is less than 25 ℃, close refrigerating unit, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 25 ~ 30 ℃ within described second timed interval, open cold radiator cooler, the chlorination speed that simultaneously keeps described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 30 ~ 40 ℃ within described second timed interval, keep refrigerating unit in opened condition, regulate chlorination Speed Reduction to the 2 ~ 3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination.
Preferably, in the production method of described clorox, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, and described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, and described the second heat exchange component is arranged at the outside of described reactor
When the temperature value of described reaction solution is less than 25 ℃, close interior refrigerating unit and external cooling device, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of reaction solution rises between 25 ~ 30 ℃ within described second timed interval, refrigerating unit in opening, keep external cooling device in closing condition, the chlorination speed that simultaneously keeps described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 30 ~ 40 ℃ within described second timed interval, in keeping, refrigerating unit is in opened condition, open external cooling device, regulate chlorination Speed Reduction to the 2 ~ 3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination.
Preferably, in the production method of described clorox,
In described step 2, in reaction process, by temperature-detecting device, detect the temperature value of described reaction solution, wherein, described temperature-detecting device includes at least two temperature-detecting devices, described at least two temperature-detecting devices are arranged in described reactor, and the position in described reactor deposits gap in height, the temperature value of described reaction solution serve as reasons described in maximum value in the temperature value of the reaction solution that detects of at least two temperature-detecting devices.
Preferably, in the production method of described clorox, in described step 2, use chlorinating equipment to add liquid chlorine in the sodium hydroxide solution in described reactor, wherein, described chlorinating equipment includes the chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
For realizing a device for clorox production method, comprising:
Reactor;
Chlorinating equipment, it has chlorination outlet, and described chlorination outlet is arranged in described reactor;
PH value detection device, it is arranged in described reactor;
Temperature-detecting device, it is arranged in described reactor;
Refrigerating unit, its inside passes into refrigerant, carries out heat exchange with described reactor;
Control device, it is connected with described pH value detection device, described temperature-detecting device, described chlorinating equipment and described refrigerating unit, the temperature value signal that the pH value signal detecting according to described pH value detection device and described temperature-detecting device detect, regulates the chlorination speed of described chlorinating equipment and the open and close of controlling described refrigerating unit.
Preferably, in described device, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, spiral pipe extending longitudinally for described reactor, described the second heat exchange component is arranged at the outside of described reactor, for being coated on the cavity of described reactor outer wall.
Preferably, in described device, described chlorinating equipment includes the spirrillum chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
The present invention has following beneficial effect:
(1) device of the present invention has interior refrigerating unit and external cooling device, according to the temperature conditions of reaction solution, the work of control refrigerating unit, when temperature value is less than 25 ℃, open cold radiator cooler not, in temperature rises to the scope of 25 ~ 30 ℃ within second timed interval, refrigerating unit work in only opening, when temperature rises to 30 ~ 40 ℃ within second timed interval, refrigerating unit and external cooling device in opening simultaneously, the common work of interior refrigerating unit and external cooling device, the homogeneity of cooling and suitable cooling rate have been guaranteed, realized the accurate control of reacting liquid temperature, reaction is carried out all the time in low temperature environment, avoid 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 to monitor reaction, particularly, in reactor of the present invention, be provided with two temperature-detecting devices and two pH value detection devices, gap is in height deposited in two temperature-detecting devices position in reactor, two pH value detection devices also take same mode to arrange, thereby can monitor the reaction severe degree of the different piece in reactor, local side reaction or the generation of superchlorination reaction have been avoided, guarantee the accurate sensitive judgement to reaction end simultaneously.
(3) chlorinating equipment of the present invention has the spirrillum chlorination pipeline extending longitudinally along reactor, and during chlorination, first liquid chlorine vaporizes in chlorination pipeline, with the reaction solution heat exchange in reactor, has also reached the effect that reduces the temperature of reaction solution.
(4) in method of the present invention according to actual temperature or pH value situation, divide ladder to set chlorination speed, to realize the control to the severe degree of chlorination reaction under different situations, when controlling the temperature of reaction solution, also want open cold radiator cooler, said process has been realized the accurate control to the production process of clorox, improved production efficiency, greatly improved the utilization ratio of raw material, in the present invention, the utilization ratio of liquid chlorine reaches 99.68%～99.95%, the utilization ratio of sodium hydroxide reaches 99.10～99.90%, reduced the scrap rate of product, product clorox available chlorine content >=11.5%.
Accompanying drawing explanation
Fig. 1 is of the present invention for realizing the structural representation of device of the production method of clorox of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to specification sheets word.
As shown in Figure 1, the invention provides a kind of production method of clorox, comprise the following steps:
Step 1, in reactor, add sodium hydroxide solution;
Step 2, use chlorinating equipment to add chlorine in the sodium hydroxide solution in described reactor, in reaction process, by temperature-detecting device, detect the temperature value of described reaction solution, and regulate described chlorinating equipment to the chlorination speed in described reaction solution according to this temperature value, and according to this temperature value, control the open and close of refrigerating unit, so that the temperature value of described reaction solution is not more than 45 ℃, simultaneously, by pH value detection device, detect the pH value of described reaction solution, and regulate chlorinating equipment to the chlorination speed in reaction solution according to this pH value, so that the pH value of described reaction solution is not less than 10,
The judgement of step 3, reaction end: when the pH of reaction solution value keeps being less than 12 in very first time interval, reacted, described chlorinating equipment stops chlorination.
In the production method of described clorox, in described step 2, by pH value detection device, detect the pH value of described reaction solution, and regulate chlorinating equipment to the chlorination speed in reaction solution according to this pH value, so that the pH value of described reaction solution is not less than 10, by following process implementation, when the pH of described reaction solution value is greater than 12, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the pH of described reaction solution value is reduced between 11 ~ 12 within second timed interval, the chlorination speed of described chlorinating equipment is down to 2 ~ 3kg/min, when the pH of described reaction solution value is reduced to while being less than or equal to 11 within second timed interval, described chlorinating equipment stops chlorination.
In the production method of described clorox, in described step 2, in reaction process, by pH value detection device, detect the pH value of described reaction solution, wherein, described pH value detection device includes at least two pH value detection devices, and described at least two pH detect and are arranged in described reactor, and gap is in height deposited in the position in described reactor, the pH value of described reaction solution serve as reasons described in minimum value in the pH value of the reaction solution that detects of at least two pH proofing units; In described step 3, when the pH value of the reaction solution detecting when described at least two pH proofing units all keeps being less than 12 in described very first time interval, reaction completes, and described chlorinating equipment stops chlorination.
In the production method of described clorox, in described step 2, in reaction process, open cold radiator cooler, so that the temperature value of described reaction solution is not more than 45 ℃, by following process implementation, when the temperature value of described reaction solution is less than 25 ℃, close refrigerating unit, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 25 ~ 30 ℃ within described second timed interval, open cold radiator cooler, the chlorination speed that simultaneously keeps described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 30 ~ 40 ℃ within described second timed interval, keep refrigerating unit in opened condition, regulate chlorination Speed Reduction to the 2 ~ 3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination.
In the production method of described clorox, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, described the second heat exchange component is arranged at the outside of described reactor, when the temperature value of described reaction solution is less than 25 ℃, close interior refrigerating unit and external cooling device, the chlorination speed setting of described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of reaction solution rises between 25 ~ 30 ℃ within described second timed interval, refrigerating unit in opening, keep external cooling device in closing condition, the chlorination speed that simultaneously keeps described chlorinating equipment is 5 ~ 8kg/min, when the temperature value of described reaction solution rises between 30 ~ 40 ℃ within described second timed interval, in keeping, refrigerating unit is in opened condition, open external cooling device, regulate chlorination Speed Reduction to the 2 ~ 3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination.
In the production method of described clorox, in described step 2, in reaction process, by temperature-detecting device, detect the temperature value of described reaction solution, wherein, described temperature-detecting device includes at least two temperature-detecting devices, described at least two temperature-detecting devices are arranged in described reactor, and gap is in height deposited in the position in described reactor, the temperature value of described reaction solution serve as reasons described in maximum value in the temperature value of the reaction solution that detects of at least two temperature-detecting devices.
In the production method of described clorox, in described step 2, use chlorinating equipment to add liquid chlorine in the sodium hydroxide solution in described reactor, wherein, described chlorinating equipment includes the chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
For realizing a device for clorox production method, comprising: reactor; Chlorinating equipment, it has chlorination outlet, and described chlorination outlet is arranged in described reactor; PH value detection device, it is arranged in described reactor; Temperature-detecting device, it is arranged in described reactor; Refrigerating unit, its inside passes into refrigerant, carries out heat exchange with described reactor; Control device, it is connected with described pH value detection device, described temperature-detecting device, described chlorinating equipment and described refrigerating unit, the temperature value signal that the pH value signal detecting according to described pH value detection device and described temperature-detecting device detect, regulates the chlorination speed of described chlorinating equipment and the open and close of controlling described refrigerating unit.
In described device, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, spiral pipe extending longitudinally for described reactor, described the second heat exchange component is arranged at the outside of described reactor, for being coated on the cavity of described reactor outer wall.
In described device, described chlorinating equipment includes the spirrillum chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
At least two temperature-detecting devices can be monitored the reaction severe degree of different zones in reactor, guarantee accuracy and the reliability of monitoring.Particularly, in the present invention, at reactor, two temperature-detecting devices are set, be respectively and urge a temperature-detecting device and low level temperature-detecting device, wherein, high-order temperature-detecting device is arranged at the position near the top of reactor, and low level temperature-detecting device is arranged on the position near the bottom of reactor.The number of temperature-detecting device and the position of setting are not limited to embodiments of the invention, take to realize that evenly to obtain reaction solution temperature value be everywhere object.In production method of the present invention, need to guarantee temperature value T relatively large in the temperature value of two detected reaction solutions of temperature-detecting device
maxmeet temperature requirement.
Based on above-mentioned same reason, pH proofing unit is arranged.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, and low level pH proofing unit is arranged on the position near the bottom of reactor.The number of pH value detection device and the position of setting are not limited to embodiments of the invention, take to realize that evenly to obtain reaction solution pH value be everywhere object.
Control device of the present invention is DCS (Distributed Control System, distribution type control system) Controlling System, based on above-mentioned DCS Controlling System, has realized production method of the present invention.
As shown in Figure 1, the inventive system comprises following structure: control device 17, interior refrigerating unit, external cooling device, 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.Control device 17 also has display interface.Interior refrigerating unit includes the inside that the first heat exchange component 9 and the first controller 2, the first heat exchange components 9 are arranged on reactor 18, is spiral helicine pipeline, and its inside passes into refrigerant, and the first controller 2 is arranged at the refrigerant ingress of the first heat exchange component.External cooling device includes the second heat exchange component 7 and second controller 13, the second heat exchange component 7 is for being coated on the cavity of reactor outer wall, its inside passes into refrigerant, second controller 13 is arranged at the refrigerant ingress of the second heat exchange component, above the cavity of the second heat exchange component, is provided with refrigerant exit 6.Chlorinating equipment also has chlorination pipeline 10 and chlorine dosing control device 3, and wherein, chlorination pipeline 10 is positioned at reactor 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.Chlorine dosing control device 3 regulates action command to send module 5 by chlorination and is connected to control device, the first controller sends module 14 by interior refrigerating unit action command and is connected to control device, second controller sends module 16 by external cooling device action command and is connected to control device, 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 the signal transfer connector by separately and information parameter gather transport module 15 and are connected with control device, to control device transmission signal.
In the present invention, chlorination process is in cold sodium hydroxide solution, to pass into chlorine (liquid chlorine), controls temperature≤45 ℃, pH > 10, when free alkali content is 0.1%-1%, stop passing into chlorine through precipitate and separate sodium-chlor, produce chlorine bleach liquor.
But chlorination process is produced in the process of clorox, and excess Temperature clorox decomposition rate is accelerated, and following side reaction can occur:
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 carried out and pH value significantly declines above at 40 ℃, for preventing this side reaction, in reaction process, pH value remains and is greater than 10, and drop to and be less than or equal at 11 o'clock in very first time interval in pH value, just stop chlorination, make pH value can return to as early as possible the state that is greater than 11.When temperature rises to while being greater than 40 ℃ in very first time interval, also stop chlorination, simultaneously in refrigerating unit and external cooling device work simultaneously so that the temperature of reaction solution drops to 40 ℃ following (being less than or equal to the state of 40 ℃) as early as possible.
Reaction end is produced very important to clorox, the reaction of overstep of end point line generation superchlorination, and reaction process is as follows:
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 be take pH value as 12 being reaction end, keeps being less than 12 state reached for the second interval time when the pH of reaction solution value, thinks that sodium hydroxide in reaction solution is by total overall reaction, and now reaction reaches terminal, stops chlorination.The present invention can fully suppress side reaction and superchlorination reaction, at utmost utilizes raw material, realizes the High-efficient Production of clorox.
The present invention adopts water as refrigerant.
Embodiment mono-
In following embodiment, very first time interval is set as 10min, and second timed interval was set as 3min, and wherein, second timed interval was accurately judged the variation of pH value and temperature value for control device provides foundation.
Production method of the present invention includes two stages---start section and production control section.
(1) start section
To the sodium hydroxide solution that adds 8000kg15% in reactor, before producing and starting, by temperature-detecting device, monitor the initial temperature of sodium hydroxide solution, according to this initial temperature, determine whether open cold radiator cooler.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
maxduring 25 ℃ of >, refrigerating unit in opening; Work as T
maxin the time of≤25 ℃, start chlorinating equipment, start to add liquid chlorine in sodium hydroxide solution, now chlorination speed control is at 5 ~ 8kg/min, and enters production control section.
(2) production control section
In production control section, mainly need to control pH value and temperature in production process, effectively to suppress the generation of side reaction.
In the present invention, the while is by the temperature of high-order temperature-detecting device and low level temperature-detecting device detection reaction liquid.When the temperature value of reaction solution rises between 25 ~ 30 ℃ in 3min, refrigerating unit in opening, keeps external cooling device in closing condition, and the chlorination speed that simultaneously keeps described chlorinating equipment is 5 ~ 8kg/min; When temperature value in 3min rises to rapidly T
maxbetween 30 ~ 40 ℃, in controlling, refrigerating unit and external cooling device are worked simultaneously, and now, chlorination speed is down to 2 ~ 3kg/min; Continue temperature information collection, if temperature value rises to T in 3min
maxbe greater than 40 ℃, chlorinating equipment is closed, and stops chlorination, because now interior refrigerating unit and external cooling device are all in running order, therefore, only has temporary close chlorinating equipment, to relax the severe degree of chlorination reaction, helps to reduce the temperature of reaction solution.
In reaction process, if temperature value meets T
maxbetween 30 ~ 35 ℃, maintain interior refrigerating unit and external cooling device and open simultaneously; If temperature value is reduced to rapidly T in 3min
maxbetween 25 ~ 30 ℃, only maintain interior refrigerating unit and open, external cooling device is closed, and slowly increases to large flow chlorination, and chlorination speed slowly returns to 5 ~ 8kg/min; Continue temperature information collection, if temperature value is reduced to rapidly T in 3min
maxbe less than or equal to 25 ℃, interior refrigerating unit and external cooling device all closed, keep large flow chlorination, chlorination speed is 5 ~ 8kg/min.The cycle control of said process formation temperature, realizes high-efficient automatic production control.
To the Real-Time Monitoring of the pH value of reaction solution, rely on two pH value detection devices to realize.PH hereinafter
minrefer to that the relatively little value in two pH values of the reaction solution that two pH proofing units detect.If pH value meets rapidly pH in 3min
minbetween 11 ~ 12, reduce chlorination speed---2 ~ 3kg/min; Continue pH information acquisition, if pH value is decreased to rapidly pH in 3min
minbe less than or equal to 11, close chlorinating equipment, stop chlorination.Continue pH information acquisition, when pH value meets pH
minduring > 12, reopen chlorinating equipment, chlorination speed is 5 ~ 8kg/min.Said process has formed the cycle control of pH.
(3) judgement of reaction end
Two pH values that detect when high-order pH value detection device and low level pH value detection device continue 10min and are all less than 12, close chlorinating equipment, and control device provides reaction end report information, starts blowing program, completes a collection of time and produces.
Embodiment bis-~ embodiment ten
Following examples two ~ embodiment ten all adopts the method same with embodiment mono-, and sodium hydroxide concentration remains unchanged, and in implementation process, each step parameter is all consistent.Each embodiment the results are shown in Table 1.
Table 1
In the present invention, the utilization ratio of liquid chlorine reaches 99.68%～99.95%, and the utilization ratio of sodium hydroxide reaches 99.10～99.90%, has reduced the scrap rate of product, product clorox 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 embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend of describing.
Claims (8)
1. a production method for clorox, is characterized in that, comprises the following steps:
Step 1, in reactor, add sodium hydroxide solution;
Step 2, use chlorinating equipment to add chlorine in the sodium hydroxide solution in described reactor, in reaction process,
By temperature-detecting device, detect the temperature value of described reaction solution, and regulate described chlorinating equipment to the chlorination speed in described reaction solution according to this temperature value, and according to this temperature value, control the open and close of refrigerating unit, so that the temperature value of described reaction solution is not more than 45 ℃, detailed process is: when the temperature value of described reaction solution is less than 25 ℃, close refrigerating unit, the chlorination speed setting of described chlorinating equipment is 5～8kg/min, when the temperature value of described reaction solution rises between 25～30 ℃ within second timed interval, open cold radiator cooler, the chlorination speed that simultaneously keeps described chlorinating equipment is 5～8kg/min, when the temperature value of described reaction solution rises between 30～40 ℃ within described second timed interval, keep refrigerating unit in opened condition, regulate chlorination Speed Reduction to the 2～3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination,
Simultaneously, by pH value detection device, detect the pH value of described reaction solution, and regulate chlorinating equipment to the chlorination speed in reaction solution according to this pH value, so that the pH value of described reaction solution is not less than 10, detailed process is: when the pH of described reaction solution value is greater than 12, the chlorination speed setting of described chlorinating equipment is 5～8kg/min, when the pH of described reaction solution value is reduced between 11～12 within described second timed interval, the chlorination speed of described chlorinating equipment is down to 2～3kg/min, when the pH of described reaction solution value is reduced to while being less than or equal to 11 within second timed interval, described chlorinating equipment stops chlorination,
The judgement of step 3, reaction end: when the pH of reaction solution value keeps being less than 12 in very first time interval, reacted, described chlorinating equipment stops chlorination.
2. the production method of clorox as claimed in claim 1, is characterized in that,
In described step 2, in reaction process, by pH value detection device, detect the pH value of described reaction solution, wherein, described pH value detection device includes at least two pH value detection devices, described at least two pH detect and are arranged in described reactor, and the position in described reactor deposits gap in height, the pH value of described reaction solution serve as reasons described in minimum value in the pH value of the reaction solution that detects of at least two pH proofing units;
In described step 3, when the pH value of the reaction solution detecting when described at least two pH proofing units all keeps being less than 12 in described very first time interval, reaction completes, and described chlorinating equipment stops chlorination.
3. the production method of clorox as claimed in claim 1 or 2, it is characterized in that, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, and described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, and described the second heat exchange component is arranged at the outside of described reactor
When the temperature value of described reaction solution is less than 25 ℃, close interior refrigerating unit and external cooling device, the chlorination speed setting of described chlorinating equipment is 5～8kg/min, when the temperature value of reaction solution rises between 25～30 ℃ within described second timed interval, refrigerating unit in opening, keep external cooling device in closing condition, the chlorination speed that simultaneously keeps described chlorinating equipment is 5～8kg/min, when the temperature value of described reaction solution rises between 30～40 ℃ within described second timed interval, in keeping, refrigerating unit is in opened condition, open external cooling device, regulate chlorination Speed Reduction to the 2～3kg/min of described chlorinating equipment simultaneously, when the temperature value of described reaction solution rises to while being greater than 40 ℃ within described second timed interval, described chlorinating equipment stops chlorination.
4. the production method of clorox as claimed in claim 3, is characterized in that,
In described step 2, in reaction process, by temperature-detecting device, detect the temperature value of described reaction solution, wherein, described temperature-detecting device includes at least two temperature-detecting devices, described at least two temperature-detecting devices are arranged in described reactor, and the position in described reactor deposits gap in height, the temperature value of described reaction solution serve as reasons described in maximum value in the temperature value of the reaction solution that detects of at least two temperature-detecting devices.
5. the production method of clorox as claimed in claim 1 or 2, it is characterized in that, in described step 2, use chlorinating equipment to add liquid chlorine in the sodium hydroxide solution in described reactor, wherein, described chlorinating equipment includes the chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
6. for realizing a device for clorox production method as claimed in claim 1, it is characterized in that, comprising:
Reactor:
Chlorinating equipment, it has chlorination outlet, and described chlorination outlet is arranged in described reactor;
PH value detection device, it is arranged in described reactor;
Temperature-detecting device, it is arranged in described reactor;
Refrigerating unit, its inside passes into refrigerant, carries out heat exchange with described reactor;
Control device, it is connected with described pH value detection device, described temperature-detecting device, described chlorinating equipment and described refrigerating unit, the temperature value signal that the pH value signal detecting according to described pH value detection device and described temperature-detecting device detect, regulates the chlorination speed of described chlorinating equipment and the open and close of controlling described refrigerating unit.
7. device as claimed in claim 6, it is characterized in that, described refrigerating unit includes interior refrigerating unit and external cooling device, wherein, described interior refrigerating unit has the first heat exchange component, described external cooling device has the second heat exchange component, and the inside of described the first heat exchange component and described the second heat exchange component all passes into refrigerant, described the first heat exchange component is arranged in described reactor, spiral pipe extending longitudinally for described reactor, described the second heat exchange component is arranged at the outside of described reactor, for being coated on the cavity of described reactor outer wall.
8. the device as described in claim 6 or 7, is characterized in that, described chlorinating equipment includes the spirrillum chlorination pipeline extending longitudinally along described reactor, has chlorination outlet in the end of described chlorination pipeline.
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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 |
| 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 |
| 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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