CN115872362A - Method for continuously preparing high-purity sodium hypochlorite - Google Patents
Method for continuously preparing high-purity sodium hypochlorite Download PDFInfo
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- CN115872362A CN115872362A CN202211599831.6A CN202211599831A CN115872362A CN 115872362 A CN115872362 A CN 115872362A CN 202211599831 A CN202211599831 A CN 202211599831A CN 115872362 A CN115872362 A CN 115872362A
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- sodium hypochlorite
- heat exchanger
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- reaction kettle
- sodium hydroxide
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- 239000005708 Sodium hypochlorite Substances 0.000 title claims abstract description 248
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 title claims abstract description 247
- 238000000034 method Methods 0.000 title claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 656
- 238000006243 chemical reaction Methods 0.000 claims abstract description 268
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 101
- 239000000460 chlorine Substances 0.000 claims abstract description 92
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 92
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000000498 cooling water Substances 0.000 claims abstract description 82
- 239000008367 deionised water Substances 0.000 claims abstract description 39
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 39
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 121
- 239000007789 gas Substances 0.000 claims description 94
- 239000011261 inert gas Substances 0.000 claims description 60
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 58
- 230000033116 oxidation-reduction process Effects 0.000 claims description 39
- 230000003068 static effect Effects 0.000 claims description 36
- 238000003860 storage Methods 0.000 claims description 32
- 239000007921 spray Substances 0.000 claims description 22
- 230000002093 peripheral effect Effects 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000889 atomisation Methods 0.000 claims description 10
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 9
- 238000012544 monitoring process Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000005660 chlorination reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052743 krypton Inorganic materials 0.000 claims description 6
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052754 neon Inorganic materials 0.000 claims description 6
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 23
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 243
- 235000011121 sodium hydroxide Nutrition 0.000 description 193
- 239000000047 product Substances 0.000 description 47
- 230000008901 benefit Effects 0.000 description 11
- 238000001514 detection method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000003113 dilution method Methods 0.000 description 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 239000004155 Chlorine dioxide Substances 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000003443 antiviral agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000019398 chlorine dioxide Nutrition 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention relates to the technical field of sodium hypochlorite production and preparation, and particularly discloses a method for continuously preparing high-purity sodium hypochlorite, which comprises the following steps of (a) preparing a sodium hydroxide concentrated solution; (a1) Adding a certain mass of concentrated alkali into a first reaction kettle with a first jacketed heat exchanger, and opening circulating cooling water; (a2) Adding a certain mass of deionized water into the first reaction kettle in the step (a 1), and starting a stirrer in the first stirring kettle; (a3) Adjusting the flow rate of circulating cooling water in the first jacketed heat exchanger outside the first reaction kettle in the step (a 1) through the reading of the first online thermometer, and controlling the temperature of the solution in the first reaction kettle; (a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer to control the concentration of the concentrated sodium hydroxide solution; and (b) preparing a dilute sodium hydroxide solution. The invention has the characteristics of reducing by-products, improving the effective rate content and reducing the waste of the raw material chlorine.
Description
Technical Field
The invention relates to the technical field of sodium hypochlorite production and preparation, in particular to a method for continuously preparing high-purity sodium hypochlorite.
Background
Sodium hypochlorite is a colorless or yellowish liquid, has a chlorine-like odor, has a melting point of-6 ℃ and a boiling point of 102.2 ℃, is easily dissolved in water to generate caustic soda and hypochlorous acid, and is decomposed to generate hydrogen chloride and nascent oxygen, and is a strong oxidant due to strong oxidizing capacity of the nascent oxygen. As a powerful sterilizing and virucidal agent with real high efficiency, broad spectrum and safety, the bactericidal composition has good affinity with water, can be mutually dissolved with water in any ratio, does not have the potential safety hazard of liquid chlorine, chlorine dioxide and other medicaments, has a disinfection effect which is known to be equivalent to chlorine, and is widely applied to the fields of disinfectants, paper pulp bleaching, medical industry and the like.
At present, the domestic sodium hypochlorite production process mainly comprises an electrolysis method and a sodium hydroxide absorption method. The electrolysis product has low available chlorine content and is mainly used for disinfection or algae removal in water treatment in occasions requiring a small amount of sodium hypochlorite. The sodium hydroxide absorption method is mainly used for pulp, textiles and chemical fibers as bleaching agents, water treatment as water purifying agents, bactericides or disinfectants, organic industry for manufacturing chloride mantles, dye industry for manufacturing indigo and medical industry for producing monochloramine or dicloroamine.
The sodium hydroxide absorption method mostly adopts an intermittent production process, the production process needs to continuously analyze the excessive alkali amount, personnel are needed to switch the absorption tower when the sodium hypochlorite solution is qualified, and the over-chlorine can be caused if the switching is not timely. Therefore, the production line needs to be monitored and operated all the time, the labor intensity of production personnel is high, the required control level is high, the production efficiency is inconvenient to improve, and a lot of troubles are brought to producers; meanwhile, the problems of difficult control of the content of the perchloride or the excessive alkali, unstable product quality and the like exist.
In view of the above problems, the prior patent literature discloses a method for producing sodium hypochlorite using a continuous process (CN 111732081A; CN111792625A; CN 107010599A). The continuous method for producing sodium hypochlorite has the advantages of high efficiency and good product quality, and can also carry out sustainable stable production. However, the techniques also have the defects that a sodium hypochlorite solution with accurate concentration cannot be obtained, the conditions such as temperature, pH, sodium hypochlorite concentration, system pressure and the like involved in the reaction process cannot be monitored in real time in the whole process, and a large amount of human resources are consumed for analysis and detection; in addition, the existing sodium hypochlorite preparation technology involves adding excessive chlorine gas into a reactor, and dissolving the chlorine gas into water under a pressurized state to perform chlorination reaction with sodium hydroxide. On one hand, the dissolved excessive chlorine gas can react with the product sodium hypochlorite, so that the by-products are increased, and the content of effective chlorine is reduced; in addition, the excess chlorine is often treated as tail gas, and multiple stages of absorption are usually required to meet the requirement of evacuation, which not only wastes the raw material chlorine, but also increases the investment cost and the environmental risk caused by chlorine leakage.
Therefore, the existing method for producing sodium hypochlorite has the problems that a sodium hypochlorite solution with accurate concentration cannot be obtained, the conditions such as temperature, pH, sodium hypochlorite concentration, system pressure and the like involved in the reaction process cannot be monitored in real time in the whole process, a large amount of human resources are consumed for analysis and detection, by-products caused by adding excessive chlorine gas are increased, raw material chlorine gas is wasted, investment cost is increased, and environmental risks caused by chlorine gas leakage exist.
Disclosure of Invention
The invention aims to solve the technical problems of the existing sodium hypochlorite production method and provides a method for continuously preparing high-purity sodium hypochlorite, which can reduce byproducts, improve the effective content and reduce the waste of raw material chlorine.
The first technical scheme of the invention is as follows: a method for continuously preparing high-purity sodium hypochlorite comprises the following steps,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle with a first jacketed heat exchanger, and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle in the step (a 1), and starting a stirrer in the first stirring kettle;
(a3) Adjusting the flow rate of circulating cooling water in the first jacketed heat exchanger outside the first reaction kettle in the step (a 1) through the reading of the first online thermometer, and controlling the temperature of the solution in the first reaction kettle;
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer to control the concentration of the concentrated sodium hydroxide solution;
(b) Preparing dilute solution of sodium hydroxide
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle with a second jacketed heat exchanger, and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle in the step (b 1), and starting a stirrer in the second reaction kettle;
(b3) Adjusting the flow rate of circulating cooling water of a second jacketed heat exchanger outside the second reaction kettle in the step (b 1) through the reading of a second online thermometer, and controlling the temperature of the solution in the second reaction kettle;
(b4) Adjusting the flow rate of the deionized water in the step (b 2) through the reading of the second online densitometer to control the concentration of the dilute sodium hydroxide solution;
(c) Conveying dilute sodium hydroxide solution
(c1) Sending the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution obtained in the step (c 1) into a static mixer for mixing;
(d) Chlorination reaction
(d1) Inputting the mixed sodium hydroxide dilute solution in the step (c 2) into a spray tower atomizer (30) at the top of a sodium hypochlorite reactor, and spraying and atomizing the sodium hydroxide dilute solution downwards from the top of the spray tower atomizer;
(d2) Conveying chlorine gas into a gas distributor, wherein the chlorine gas is distributed in a sodium hypochlorite reactor by the gas distributor;
(d3) Carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution;
(e) On-line monitoring
(e1) Online testing the pH of the sodium hypochlorite solution in the step (d 3) by a pH meter in the sodium hypochlorite reactor, and interlocking the opening size of a back pressure valve of the dilute sodium hydroxide solution online to keep the pH of the reaction system in a certain range;
(e2) A cooling water valve is interlocked on line through a third online thermometer in the sodium hypochlorite reactor, and the opening size of the cooling water valve is adjusted on line to adjust the flow of cooling water so as to control the reaction temperature on line;
(e3) The method comprises the following steps of interlocking an inert gas valve on line through an online pressure gauge in the sodium hypochlorite reactor, adjusting the opening of the inert gas valve on line, and adjusting the flow of inert gas, so as to keep the internal pressure of the sodium hypochlorite reactor constant;
(e4) The chlorine valve is interlocked on line by an on-line oxidation-reduction potential analyzer in the sodium hypochlorite reactor, and the chlorine flow is adjusted by adjusting the opening of the chlorine valve on line;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the readings of the online oxidation-reduction potential analyzer in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution obtained in the step (d 3) to a finished product tank; if not, continuing to stay the sodium hypochlorite solution in the sodium hypochlorite reactor, interlocking a corresponding chlorine valve on line through an on-line oxidation-reduction potential analyzer until the sodium hypochlorite solution reaches the standard, and conveying the sodium hypochlorite solution to a finished product tank.
According to the invention, a first reaction kettle and a second reaction kettle are arranged, sodium hydroxide solid and deionized water are firstly added into the first reaction kettle to prepare a sodium hydroxide concentrated solution, the sodium hydroxide concentrated solution is transferred into the second reaction kettle, the deionized water is added to dilute the sodium hydroxide to prepare a sodium hydroxide dilute solution, the opening size of a cooling water valve is adjusted on line through an on-line thermometer, the flow rate of cooling water is adjusted to realize the temperature control in the sodium hydroxide dissolving and diluting processes, the opening size of the deionized water valve is adjusted on line through an on-line densimeter, the flow rate of the deionized water is adjusted to realize the accurate control of the sodium hydroxide mass fraction, the temperature and concentration can be accurately controlled by adopting an on-line monitoring interlocking valve technology in the whole sodium hydroxide dissolving and diluting process, a good foundation is laid for the subsequent preparation of a sodium hypochlorite solution with stable mass concentration, and the quality of the final sodium hypochlorite solution is ensured;
the invention carries out real-time monitoring on the whole process of pH, temperature, pressure and oxidation-reduction potential involved in the reaction process and interlocks the corresponding valve opening; the pH of the reaction mixed solution is tested on line through a pH meter, the opening of a sodium hydroxide dilute solution valve is interlocked on line, the flow of the sodium hydroxide dilute solution is adjusted on line, and the pH of a reaction system is kept in a certain range; the cooling water flow is adjusted by adjusting the opening of the valve on line through an on-line thermometer and an on-line interlocking cooling water valve, so that the reaction temperature is controlled on line; the pressure of the reaction system is monitored on line through an online pressure gauge, the inert gas valve is interlocked on line, and the opening of the inert gas valve is adjusted on line to adjust the flow of the inert gas;
the method successfully realizes the continuous production of sodium hypochlorite products with stable quality concentration by online oxidation-reduction potential analyzer, online interlocking of the chlorine valve, online adjustment of the opening of the chlorine valve, adjustment of chlorine flow, and online instrument interlocking valve technology, so that the controllability of the reaction process can be ensured, and the cooperative control of reaction process parameters is integrated; the invention adopts inert gas to replace chlorine gas to pressurize the reaction system, and can perform online pressure compensation on the amount of the chlorine gas consumed by the reaction, thereby effectively avoiding the situations of increasing by-products and reducing the content of effective chlorine due to the reaction of the chlorine gas and the product sodium hypochlorite, realizing zero emission of the chlorine gas, completely avoiding tail gas treatment of the chlorine gas, avoiding waste of raw material chlorine gas, effectively avoiding investment cost brought by a tail gas treatment device and environmental risk brought by leakage of the chlorine gas, and having greater economic benefit and social benefit.
Preferably, the method further comprises the step of,
(a5) And interlocking the first jacketed heat exchanger through the reading of the first online thermometer in the first reaction kettle to control the temperature of the concentrated sodium hydroxide solution in the first reaction kettle. Through the online linkage between the first online thermometer and the first jacketed heat exchanger, when the temperature of the sodium hydroxide concentrated solution in the first reaction kettle is lower than or higher than a set value, the water inlet speed of the first jacketed heat exchanger is controlled to increase or decrease the temperature of the sodium hydroxide concentrated solution, and the temperature of the sodium hydroxide concentrated solution in the first reaction kettle is ensured to be in a reasonable temperature range.
Preferably, the mass concentration of the concentrated sodium hydroxide solution in the step (a 4) is 20 to 50%, and more preferably, the mass concentration of the concentrated sodium hydroxide solution in the step (a 4) is 30 to 40%. The preparation method is ready for the subsequent rapid preparation of the sodium hydroxide dilute solution.
Preferably, the temperature of the concentrated sodium hydroxide solution in the first reaction kettle is 30-50 ℃, and more preferably, the temperature of the concentrated sodium hydroxide solution in the first reaction kettle is 35-45 ℃. The temperature of the concentrated sodium hydroxide solution in the first reaction kettle can be controlled to ensure that the preparation work of the concentrated sodium hydroxide solution is in a better state.
Preferably, the method further comprises the step of,
(b5) And interlocking the second jacketed heat exchanger through the reading of a second online thermometer in the second reaction kettle to control the temperature of the dilute sodium hydroxide solution in the second reaction kettle. When the temperature of the dilute sodium hydroxide solution in the second jacketed heat exchanger is lower than or higher than a set value, the water inlet speed of the second jacketed heat exchanger is controlled to increase or decrease the temperature of the concentrated sodium hydroxide solution, and the temperature of the concentrated sodium hydroxide solution in the second reaction kettle is ensured to be in a reasonable temperature range.
Preferably, the mass concentration of the dilute sodium hydroxide solution in the step (b 4) is 13 to 18 percent, and more preferably, the mass concentration of the dilute sodium hydroxide solution in the step (b 4) is 15 to 16 percent. Can prepare for follow-up preparation sodium hypochlorite solution process, guarantee that sodium hypochlorite solution can be produced better more accurately.
Preferably, the temperature of the dilute sodium hydroxide solution in the second reaction kettle is 20-40 ℃, and more preferably, the temperature of the dilute sodium hydroxide solution in the second reaction kettle is 25-35 ℃. The sodium hydroxide solution in the second reaction kettle can be ensured to be at a safe and proper temperature, and preparation is made for subsequent production reaction.
Preferably, the ratio of the length to the pipe diameter of the static mixer is 10 to 15, and more preferably, the ratio of the length to the pipe diameter of the static mixer is 12 to 14. The homogenizing effect of the dilute sodium hydroxide solution is ensured, so that the dilute sodium hydroxide solution can be put into the subsequent reaction process at any time.
Preferably, the pipe diameter of the static mixer is 0.05m to 0.2m, and more preferably, the pipe diameter of the static mixer is 0.1m to 0.15m. The volume of the solution in the static mixer can be controlled within a reasonable range, so that the effect of mixing homogeneity and subsequent reaction can be ensured to be smoothly carried out.
Preferably, the pressure applied to the spray tower atomizer is 0.2 to 0.5MPa, and more preferably, the pressure applied to the spray tower atomizer is 0.3 to 0.4MPa. The granularity of the atomized sodium hydroxide solution particles is ensured to be in a qualified range.
Preferably, the flow rate of the dilute sodium hydroxide solution in the step (d 1) is 20mL/min to 40mL/min, and more preferably, the flow rate of the dilute sodium hydroxide solution in the step (d 1) is 25mL/min to 35mL/min. The quantity of the sodium hydroxide solution which is atomized and sprayed can be matched with the quantity of the gas blown out by the gas uniform distributor at the bottom of the sodium hypochlorite reactor, and the sodium hydroxide solution and the gas can be fully and effectively contacted with each other and react, so that the stability and the reliability of the reaction are ensured.
Preferably, the size of the liquid drop after the atomization of the dilute sodium hydroxide solution in the step (d 1) is 5um to 50um, and more preferably, the size of the liquid drop after the atomization of the dilute sodium hydroxide solution in the step (d 1) is 10um to 45um. More preferably, the size of the liquid drop after the sodium hydroxide dilute solution is atomized in the step (d 1) is 15 um-40 um. More preferably, the size of the liquid drop after the sodium hydroxide dilute solution is atomized in the step (d 1) is 20 um-35 um. More preferably, the size of the liquid drop after the sodium hydroxide dilute solution is atomized in the step (d 1) is 25um to 30um. Can increase the contact area between the sodium hydroxide solution and the chlorine gas, thereby effectively improving the reaction speed between the sodium hydroxide solution and the chlorine gas and further improving the efficiency of the whole preparation process.
Preferably, the flow rate of chlorine gas in the step (d 2) is 5mL/min to 25mL/min, and more preferably, the flow rate of chlorine gas in the step (d 2) is 10mL/min to 20mL/min. Therefore, the flow speed of the chlorine can be flexibly adjusted according to the flow of the sprayed sodium hydroxide solution, and the full reaction between the chlorine and the sodium hydroxide solution can be ensured.
Preferably, the reaction system pH in the step (e 1) is maintained at 12 to 13. Ensures that the reaction can be carried out in a proper acid-base environment, and improves the reliability and quality of preparation work.
Preferably, the reaction temperature in the step (e 2) is maintained at 30-50 ℃, more preferably, the reaction temperature in the step (e 2) is maintained at 35-45 ℃, so that the reaction can be kept at a proper temperature, and the reliability and safety of the reaction are ensured.
Preferably, the reaction pressure in the step (e 3) is controlled to 0.09MPa to 0.11MPa, and more preferably, the reaction pressure in the step (e 3) is controlled to 0.095MPa to 0.105MPa. The reaction pressure can be controlled in a reasonable interval, thereby ensuring that the reaction is carried out efficiently and orderly.
Preferably, the indication number of the online oxidation-reduction potential analyzer in the step (e 4) is controlled to be 500 mv-600 mv, more preferably, the indication number of the online oxidation-reduction potential analyzer in the step (e 4) is controlled to be 520 mv-570 mv, the indication number range of the oxidation-reduction potential analyzer can be obtained by utilizing the linear relation between the indication number of the oxidation-reduction potential analyzer and the concentration of sodium hypochlorite, the indication number is larger than the upper limit value, the opening degree of a chlorine valve is reduced, the flow of chlorine gas is reduced, a back pressure valve of a synchronous interlocking finished product is opened, the product is input into a finished product tank through a ninth delivery pump, if the indication number is smaller than the lower limit value, the concentration of sodium hypochlorite in the product is low, the opening degree of the chlorine valve is increased through online interlocking, the flow of chlorine gas is increased, the back pressure valve of the synchronous interlocking product is closed, and the mixture continues to react until the indication number reaches the standard and is input into the finished product tank.
Preferably, the inert gas is at least one of nitrogen, helium, neon, argon, krypton, or xenon. Different kinds of inert gases can be selected according to specific production conditions, so that the flexibility of the method can be improved to the maximum extent, and the cost required by production can be reduced as far as possible.
Preferably, the product in the step (f) meets the standard that the mass fraction of the available chlorine is 6-15%, and the content of free alkali is less than 0.5% by mass concentration. The high effective chlorine content in the produced sodium hypochlorite solution is ensured, and the quality of the product is ensured.
The second technical scheme of the invention is as follows: the equipment for continuously preparing the high-purity sodium hypochlorite comprises a first reaction kettle, wherein a water inlet of the first reaction kettle is connected with a first water inlet pipeline, and a first delivery pump is arranged on the first water inlet pipeline; a first backpressure valve is arranged on a first water inlet pipeline between the first delivery pump and the first reaction kettle; a first jacketed heat exchanger is sleeved on the outer peripheral surface of the first reaction kettle, a first jacketed heat exchanger inlet and a first jacketed heat exchanger outlet are arranged on the first jacketed heat exchanger, the first jacketed heat exchanger inlet is connected with a water outlet of the first reaction kettle through a pipeline, the first jacketed heat exchanger inlet is connected with cooling water through a pipeline, and a second back pressure valve is arranged on the pipeline between the cooling water and the first jacketed heat exchanger inlet;
the liquid inlet of the second reaction kettle is connected with the liquid outlet of the first reaction kettle through a pipeline, and a second delivery pump and a third back pressure valve are sequentially arranged on the pipeline between the liquid outlet of the first reaction kettle and the liquid inlet of the second reaction kettle along the liquid flow direction; a water inlet of the second reaction kettle is connected with a second water inlet pipeline, a third delivery pump is arranged on the second water inlet pipeline, and a fifth backpressure valve is arranged on a pipeline between the third delivery pump and the second reaction kettle; a second jacketed heat exchanger is sleeved on the outer peripheral surface of the second reaction kettle, a second jacketed heat exchanger inlet and a second jacketed heat exchanger outlet are arranged on the second jacketed heat exchanger, the second jacketed heat exchanger inlet is connected with a water outlet of the second reaction kettle through a pipeline, the second jacketed heat exchanger inlet is connected with cooling water through a pipeline, and a fourth back pressure valve is arranged on the pipeline between the cooling water and the second jacketed heat exchanger inlet; the liquid outlet of the second reaction kettle is connected with a heat exchanger through a pipeline, a fourth conveying pump and a sixth backpressure valve are arranged on the pipeline between the heat exchanger and the liquid outlet of the second reaction kettle, and the sixth backpressure valve is close to the heat exchanger compared with the fourth conveying pump;
a liquid outlet of the heat exchanger is connected with a static mixer through a pipeline, a fifth delivery pump and a seventh backpressure valve are arranged on the pipeline between the static mixer and the heat exchanger, and the seventh backpressure valve is close to the static mixer compared with the fifth delivery pump;
the liquid outlet of the static mixer is connected with a sodium hypochlorite reactor through a pipeline, a sixth delivery pump and a sodium hydroxide dilute solution back pressure valve are arranged on the pipeline between the sodium hypochlorite reactor and the static mixer, and the sodium hydroxide dilute solution back pressure valve is close to the sodium hypochlorite reactor compared with the sixth delivery pump; an atomizer is arranged at the top in the sodium hypochlorite reactor;
the gas inlet of the gas distributor is connected with a gas buffer tank through a pipeline, an eighth back pressure valve is arranged on the pipeline between the gas buffer tank and the gas distributor, the gas inlet of the gas buffer tank is connected with the chlorine gas inlet through a pipeline, and a seventh conveying pump is arranged on the pipeline between the chlorine gas inlet and the gas buffer tank;
the bottom of the sodium hypochlorite reactor is connected with an inert gas inlet through a pipeline, an eighth delivery pump and an inert gas valve are arranged on the pipeline between the inert gas inlet and the sodium hypochlorite reactor, and the inert gas valve is closer to the sodium hypochlorite reactor than the eighth delivery pump;
a third jacketed heat exchanger is sleeved on the outer peripheral surface of the sodium hypochlorite reactor, a third jacketed heat exchanger inlet and a third jacketed heat exchanger outlet are arranged on the third jacketed heat exchanger, the third jacketed heat exchanger inlet is connected with a cooling water interface through a pipeline, and a cooling water valve is arranged on a pipeline between the cooling water interface and the third jacketed heat exchanger inlet;
and a liquid outlet of the sodium hypochlorite reactor is connected with a finished product tank through a pipeline, a ninth delivery pump and an eighth back pressure valve are arranged on the pipeline between the finished product tank and the sodium chlorate reactor, and the eighth back pressure valve is close to the sodium chlorate reactor compared with the ninth delivery pump.
According to the invention, the first reaction kettle and the second reaction kettle are matched with each other, so that a concentrated sodium hydroxide solution can be prepared firstly, then the concentrated sodium hydroxide solution is diluted into a dilute sodium hydroxide solution, therefore, during preparation, a large amount of sodium hydroxide solids are poured into the first reaction kettle, a proper amount of deionized water is added to prepare the concentrated sodium hydroxide solution, then the concentrated sodium hydroxide solution is introduced into a plurality of second reaction kettles, and then the deionized water is added into the plurality of second reaction kettles to dilute the concentrated sodium hydroxide solution into the required dilute sodium hydroxide solution, so that the time and labor amount required for directly preparing the dilute sodium hydroxide solution by adding the concentrated sodium hydroxide solution into the plurality of different first reaction kettles can be effectively reduced, the preparation efficiency of the sodium hydroxide solution is greatly improved, and the labor intensity of workers is reduced;
according to the invention, the atomizer is matched with the gas uniform distributor, the atomizer can uniformly atomize and spray the dilute sodium hydroxide solution through the plurality of atomizing nozzles, and the gas is uniformly dispersed by matching with the plurality of gas nozzles in the gas uniform distributor, so that the sufficient contact reaction of the dilute sodium hydroxide solution and the chlorine can be ensured, the reaction speed and the reaction thoroughness are improved, and the production efficiency of the device is effectively improved;
according to the invention, through a pipeline between the bottom of the sodium hypochlorite reactor and the inert gas inlet, the pipeline is provided with the eighth delivery pump and the inert gas valve, and the pressure gauge on the sodium hypochlorite reactor is matched, so that after the chlorine gas is consumed, the pressure gauge detects that the pressure in the sodium hypochlorite reactor is reduced, at the moment, the pressure gauge opens the inert gas valve on line to send the inert gas into the sodium hypochlorite reactor to replace the chlorine gas so as to maintain the pressure in the sodium hypochlorite reactor, the reaction can be smoothly carried out, and the consumed chlorine gas is replaced by the inert gas, so that the conditions of increasing by-products and reducing the effective chlorine content caused by the reaction of the chlorine gas and the product sodium hypochlorite can be effectively avoided, zero emission of the chlorine gas can be realized, the tail gas treatment of the chlorine gas is completely avoided, the waste of the raw material chlorine gas is avoided, the investment cost brought by a tail gas treatment device and the environmental risk brought by the leakage of the chlorine gas are effectively avoided, and the economic benefit and the social benefit are greater;
according to the invention, the temperatures of the liquids in the first reaction kettle, the second reaction kettle and the sodium hypochlorite reactor can be monitored in real time by the first jacketed type heat exchanger, the second jacketed type heat exchanger and the third jacketed type heat exchanger in cooperation with the first online thermometer, the second online thermometer and the third online thermometer, and when the temperature is too low or too high, the amount of cooling water entering the jackets of the first jacketed type heat exchanger, the second jacketed type heat exchanger or the third jacketed type heat exchanger is reduced or increased, so that the temperature of the liquid in the first reaction kettle, the second reaction kettle or the sodium hypochlorite reactor is increased or reduced, the temperature of the liquid in the first reaction kettle, the second reaction kettle and the sodium hypochlorite reactor is maintained in a proper range, and the smooth operation of preparing the sodium hypochlorite solution is ensured.
Preferably, a first densimeter is arranged on the first reaction kettle and is linked with the first back pressure valve in an online mode. Can in time respond to and monitor the concentration of the inside concentrated solution of sodium hydroxide of first reation kettle through online linkage between first densimeter and the first back pressure valve to the concentration of the inside concentrated solution of sodium hydroxide of first reation kettle is adjusted through the flow that control deionized water got into first reation kettle.
Preferably, a first online thermometer is arranged on a pipeline between the water outlet of the first reaction kettle and the inlet of the first jacketed heat exchanger. Can the sodium hydroxide solution temperature in the real-time supervision first reation kettle through first online thermometer, and then guaranteed that the sodium hydroxide solution temperature is in a suitable temperature to cooperate first jacketed type heat exchanger to adjust the inflow of first jacketed type heat exchanger entry when the concentrated solution temperature of sodium hydroxide is in abnormal condition, and then adjust in the temperature of the concentrated solution of sodium hydroxide among the first reation kettle reachs suitable interval.
Preferably, a second densimeter is arranged on the second reaction kettle and is interlocked with a fifth back pressure valve in an online manner. The density of the dilute sodium hydroxide solution in the second reaction kettle is tested by the second densimeter, so that the concentration of the dilute sodium hydroxide solution is detected in time, the dilute sodium hydroxide solution can participate in subsequent reactions smoothly, and the smooth production and processing are guaranteed.
Preferably, a second online thermometer is arranged on a pipeline between the water outlet of the second reaction kettle and the inlet of the second jacketed heat exchanger. The temperature of the dilute solution of sodium hydroxide can be monitored in real time, and the temperature of the solution in the second reaction kettle can be adjusted in time by matching with the water inlet speed at the inlet of the second jacketed heat exchanger.
Preferably, a pH meter is connected to the sodium hypochlorite reactor. Can monitor sodium hypochlorite solution's pH value in the sodium hypochlorite reactor to this judges whether take place to react fully between dilute solution of sodium hydroxide and the chlorine, thereby can in time discover the problem and adjust the reaction in order to take measures.
Preferably, the bottom of the sodium hypochlorite reactor is connected with a pressure gauge, and the pressure gauge is in on-line linkage with an inert gas valve. Whether pressure in the sodium hypochlorite reactor is in the best reaction pressure scope can be detected through the pressure gauge, if too big or undersize of pressure, then can reduce or increase the speed that inert gas got into in the sodium hypochlorite reactor through the flow size of adjusting online chain inert gas valve to make the interior pressure of sodium hypochlorite reactor do not adjust to the best reaction pressure scope fast.
Preferably, a third online thermometer is connected to the water outlet of the sodium hypochlorite reactor, and the third online thermometer is in online linkage with a cooling water valve. Can monitor the temperature of sodium hypochlorite solution in the sodium hypochlorite reactor, when the high or low time of temperature, then can control the increase of online chain cooling water valve or reduce the cooling water yield that gets into in the third jacket type heat exchanger to reduce the inside temperature of sodium hypochlorite reactor or slow down and reduce the inside temperature of sodium hypochlorite reactor with higher speed, adjusted to suitable within range fast with the temperature of guaranteeing sodium hypochlorite solution in the sodium hypochlorite reactor.
Preferably, an oxidation-reduction potential analyzer is arranged on a pipeline between the ninth back pressure valve and the sodium chlorate reactor, and the oxidation-reduction potential analyzer is in online linkage with the chlorine valve. The chlorine valve can be interlocked on line, and the flow of the chlorine entering the sodium hypochlorite reactor is adjusted by adjusting the opening of the chlorine valve on line.
As preferred, the atomizer includes the feed liquor pipe, the feed liquor end of feed liquor pipe is connected with static mixer through the pipeline, the play liquid end of feed liquor pipe rotates and is connected with the feed liquor and violently manages, be equipped with many feed liquor branch pipes on the outer peripheral face that the feed liquor was violently managed, the top and the bottom of feed liquor branch pipe all are equipped with a plurality of atomizing nozzle, the last solenoid valve that is equipped with of atomizing nozzle. Can spray the dilute solution of sodium hydroxide through the even atomizing of a plurality of atomizing nozzles, guarantee that the dilute solution of sodium hydroxide can be abundant with chlorine contact reaction, improve the degree of fullness and the speed of reaction.
Still include driving motor, driving motor sets up on sodium hypochlorite reactor's outer wall, driving motor's drive end is equipped with the carousel, the carousel is located inside the sodium hypochlorite reactor, the carousel is connected with the one end that the feed liquor was violently managed. The driving motor can drive the feed liquor and violently manage and rotate one hundred eighty degrees to make the new atomizing nozzle that is located the upside replace originally to be located the atomizing nozzle that the downside has damaged and atomize and spray work, thereby can be under the prerequisite of guaranteeing that the reaction goes on smoothly, prolong atomizer's change maintenance cycle, effectively improved the device's practicality and reliability.
Preferably, the gas distributor includes the intake pipe, the inlet end of intake pipe passes through the pipeline and is connected with gaseous buffer tank, the end of giving vent to anger of intake pipe is connected with the violently pipe of admitting air, the violently pipe of admitting air is located sodium hypochlorite reactor's inside, it is equipped with many air intake branch pipes on the outer peripheral face of violently pipe to admit air, the top of air intake branch pipe all communicates there are a plurality of air nozzles. Can spray chlorine evenly into sodium hypochlorite reactor through a plurality of air nozzles to make the dilute solution of sodium hydroxide that the cooperation atomizing sprayed down, both can the at utmost abundant contact reaction, improved the efficiency of reaction.
Still include one-level reposition of redundant personnel subassembly, one-level reposition of redundant personnel subassembly is located the air nozzle upside, the upside of one-level reposition of redundant personnel subassembly is equipped with second grade reposition of redundant personnel subassembly. The chlorine can be better shunted, the area of the uniform distribution of the chlorine is increased, and the reaction efficiency is ensured.
Preferably, the one-level shunt assembly comprises a plurality of first shunts in an inverted cone shape, the first shunts correspond to the air nozzles, the first shunts are located above the corresponding air nozzles and connected through a first connecting rod between the adjacent first shunts, a first fixing ring is connected to the inner side wall of the sodium hypochlorite reactor, and the first shunts are close to the first fixing ring and connected with the first fixing ring through the first connecting rod. Chlorine can be further shunted, and the reaction efficiency is improved to the maximum extent.
Preferably, the secondary flow dividing assembly comprises a plurality of liquid storage boxes, the liquid storage boxes are located above the first flow divider, a water leakage hole is formed in the bottom of each liquid storage box, the top of each liquid storage box is connected with a plurality of second flow dividers through support rods, adjacent liquid storage boxes are connected through second connecting rods, a second fixing ring is connected to the inner side wall of the sodium hypochlorite reactor in a sliding mode, and the liquid storage boxes close to the second fixing ring are connected with the second fixing ring through the second connecting rods. When atomizing nozzle is corroded and damaged, the atomization effect worsens, because the distribution area diminishes this moment for hold the liquid box and can receive more dilute solution of sodium hydroxide in the same time, when receiving speed is greater than the hole that leaks weeping speed, the solution in holding the liquid box can be more and more, thereby produces bigger pulling force to the pull rod, when the pulling force that force sensor received was greater than the setting value, explains that atomizing nozzle has seriously damaged.
Preferably, the device also comprises an atomization state detection component; the atomization state detection assembly comprises a plurality of seal boxes, the seal boxes are arranged on the inner side wall of the sodium hypochlorite reactor, tension sensors are arranged in the seal boxes, straight rods are arranged on the tension sensors, the bottom ends of the straight rods penetrate through the bottom wall of the seal boxes and are connected with connecting plates, pull rods are arranged on the connecting plates, the bottom ends of the pull rods are connected with second fixing rings, and the tension sensors are in wired or wireless connection with a driving motor. Be connected with the solid fixed ring of second through the pull rod for tension sensor can monitor whole second grade reposition of redundant personnel subassembly's weight, and when holding the sodium hydroxide solution in the liquid box and increase, tension value that tension sensor received will increase, thereby can monitor atomizing nozzle atomization effect and judge whether the atomizing nozzle that needs to be renewed goes on in order to guarantee going on smoothly of reaction.
The invention has the following beneficial effects:
(1) Through the first reation kettle who sets up, add sodium hydroxide solid and deionized water in first reation kettle earlier, prepare the concentrated solution of sodium hydroxide, transfer the concentrated solution of sodium hydroxide to the second reation kettle, add the deionized water and dilute the dilute solution of preparation sodium hydroxide, adjust cooling water valve aperture size on line through online thermometer, adjust cooling water flow, realize the accuse temperature of sodium hydroxide dissolution and dilution process, adjust the valve aperture size of deionized water through online densimeter on line, adjust the deionized water flow, realize the accurate control of sodium hydroxide mass fraction, the whole sodium hydroxide dissolution and dilution process adopts the control that online control interlocking valve technique can accurate realization temperature and concentration, for the stable sodium hypochlorite solution of follow-up preparation mass concentration has laid good basis, the quality of final sodium hypochlorite solution has been guaranteed.
(2) The pH meter, the back pressure valve, the pressure gauge and the like are arranged, the whole process real-time monitoring can be carried out on the pH, the temperature, the pressure and the oxidation-reduction potential involved in the reaction process, the corresponding valve opening degree is interlocked, the pH of the reaction mixed liquid is tested on line through the pH meter, the opening degree of the sodium hydroxide dilute solution valve is interlocked on line, the flow of the sodium hydroxide dilute solution is adjusted on line, the pH of the reaction system is kept in a certain range, the cooling water valve is interlocked on line through the online thermometer, the cooling water flow is adjusted through the online adjusting valve opening degree, the reaction temperature is controlled on line, the pressure of the reaction system is monitored on line through the online pressure gauge, the chlorine valve is interlocked on line, the inert gas flow is adjusted through the online adjusting valve opening degree, the chlorine valve is interlocked on line through the online oxidation-reduction potential analyzer, the controllable sodium hypochlorite in the reaction process can be ensured through the online adjusting valve opening degree, the comprehensive reaction process parameter cooperative control can be ensured, and the continuous production of products with the quality concentration can be successfully realized.
(3) Through the inert gas that sets up, can replace chlorine and pressurize the reaction system, can carry out online pressure compensation to the chlorine volume that the reaction consumed, thereby can effectively avoid chlorine and product sodium hypochlorite to take place the reaction, cause the accessory substance to increase and the condition that effective chlorine content reduces, can also accomplish the chlorine zero release, avoid carrying out tail gas treatment to chlorine completely, the waste of raw materials chlorine has been avoided, effectively avoided the investment cost that tail gas processing apparatus brought and the environmental risk that chlorine was revealed and is brought, great economic benefits and social have.
(4) Through mutually supporting at the first reation kettle and the second reation kettle that set up, can prepare the concentrated solution of sodium hydroxide earlier, then dilute the concentrated solution of sodium hydroxide into the dilute solution of sodium hydroxide, so can be when preparing, pour a large amount of sodium hydroxide solid into first reation kettle and add appropriate amount of deionized water in order to prepare the concentrated solution of sodium hydroxide earlier, then let in the concentrated solution of sodium hydroxide among a plurality of second reation kettle, then add deionized water in a plurality of second reation kettle in order to dilute the concentrated solution of sodium hydroxide into required dilute solution of sodium hydroxide, so can effectively reduce because of adding the time and the amount of labour that the dilute solution of sodium hydroxide needs in order directly to prepare the dilute solution of sodium hydroxide in a plurality of different first reation kettle with the solid of sodium hydroxide, greatly improved the efficiency that the sodium hydroxide solution was prepared, and reduced staff's intensity of labour.
(5) Through matching with the gaseous equipartition ware at the atomizer that sets up, the atomizer can be through a plurality of atomizing nozzle with the dilute solution of sodium hydroxide atomize the blowout uniformly, and a plurality of air nozzles in the gaseous equal portion ware of cooperation disperse chlorine uniformly, can guarantee the dilute solution of sodium hydroxide and the abundant contact reaction of chlorine, have improved the speed and the thoroughness of reaction, and then the effectual production efficiency who improves the device.
(6) Through the pipeline between sodium hypochlorite reactor bottom and the inert gas air inlet that sets up, be equipped with eighth delivery pump and inert gas valve on the pipeline, cooperate the pressure gauge on the sodium hypochlorite reactor again, can be after chlorine consumption, the pressure gauge detects sodium hypochlorite reactor internal pressure and reduces, the pressure gauge is opened the inert gas valve on line this moment and is sent inert gas into in the sodium hypochlorite reactor and replace chlorine in order to maintain the inside pressure of sodium hypochlorite reactor, guaranteed that the reaction can go on smoothly, and replace the chlorine of consumption through inert gas, can effectively avoid chlorine and product sodium hypochlorite to react, cause the condition that the accessory substance increases and effective chlorine content reduces, can also accomplish chlorine zero release, avoid carrying out tail gas treatment to chlorine completely, the waste of raw materials chlorine has been avoided, effectively avoided investment cost and the environmental risk that chlorine that the tail gas processing apparatus comes to reveal and bring, great economic benefits and social benefit have, the environment of the gas valve is revealed to the atmospheric pressure of the gas, the pressure of the gas valve is revealed to the effect of great economic benefits and social benefit
(7) Through the first jacketed type heat exchanger that sets up, second jacketed type heat exchanger and third jacketed type heat exchanger, and cooperate first online thermometer, online thermometer of second and the online thermometer of third, can real-time supervision first reation kettle, the temperature of the inside liquid of second reation kettle and sodium hypochlorite reactor, cross when the temperature crosses lowly or too high, this reduces or increases and gets into first jacketed type heat exchanger, the cooling water yield in second jacketed type heat exchanger or the third jacketed type heat exchanger jacket, thereby make first reation kettle, the temperature of the inside liquid of second reation kettle or sodium hypochlorite reactor risees or reduces, with this first reation kettle of maintaining, the temperature of the inside liquid of second reation kettle and sodium hypochlorite reactor is located suitable range, the smooth of work of preparing is prepared to the sodium hypochlorite solution has been guaranteed.
Drawings
FIG. 1 is a schematic flow diagram of a production facility according to the present invention;
FIG. 2 is a schematic flow diagram of a first part of the production apparatus of the present invention;
FIG. 3 is a schematic flow diagram of a second part of the production apparatus of the present invention;
FIG. 4 is a schematic diagram of the structure of a sodium hypochlorite reactor;
FIG. 5 is a schematic diagram of a partial structure of a hypochlorous acid reactor;
FIG. 6 is a front cross-sectional view of a hypochlorous acid reactor;
FIG. 7 is an enlarged schematic view at A in FIG. 6;
FIG. 8 is an enlarged schematic view at B of FIG. 6;
FIG. 9 is a bottom cross-sectional view of a hypochlorous acid reactor;
FIG. 10 is a schematic structural view of a primary flow splitting assembly;
FIG. 11 is a partial schematic view of a two-stage flow splitting assembly.
The labels in the figures are: 100-a first reaction kettle; 101-a first delivery pump; 102-a first back pressure valve; 103-a first densitometer; 104-a second back pressure valve; 105-a first online thermometer; 106 — first jacketed heat exchanger inlet; 107-a first jacketed heat exchanger; 108-first jacketed heat exchanger outlet; 200-a second reaction kettle; 201-a second delivery pump; 202-third backpressure valve; 203-a third delivery pump; 204-fourth backpressure valve; 205-a second densitometer; 206-a second jacketed heat exchanger inlet; 207-a second jacketed heat exchanger; 208-a second jacketed heat exchanger outlet; 209-a second online thermometer; 2010-fifth back pressure valve; 300-a heat exchanger; 301-a fourth delivery pump; 302-sixth backpressure valve; 400-a static mixer; 401-a fifth transfer pump; 402-seventh backpressure valve; 403-a sixth delivery pump; 404-sodium hydroxide dilute solution back pressure valve; 500-sodium hypochlorite reactor; 501-a pH meter; 502-an eighth delivery pump; 503-inert gas valve; 504-a pressure gauge; 505 — a third jacketed heat exchanger; 506-a third jacketed heat exchanger inlet; 507-outlet of the third jacketed heat exchanger; 508-cooling water valve; 509-third online thermometer; 600-a buffer tank; 601-a chlorine valve; 602-a seventh delivery pump; 34-a gas distributor; 702-eighth backpressure valve; 703-a ninth delivery pump; 704-oxidation reduction potential analyzer; 30-spray tower atomizer, 301-liquid inlet pipe, 302-liquid inlet horizontal pipe, 303-liquid inlet branch pipe, 304-atomizing nozzle, 305-driving motor, 306-rotary disc, 307-atomizing state detection component, 3071-sealing box, 3072-tension sensor, 3073-straight rod, 3074-connecting plate, 3075-pull rod, 341-air inlet pipe, 342-air inlet horizontal pipe, 343-air inlet branch pipe, 344-air nozzle, 345-primary flow distribution component, 3451-first flow distributor, 3452-first connecting rod, 3453-first fixing ring, 346-secondary flow distribution component, 3461-liquid storage box, 3462-water leakage hole, 3463-supporting rod, 3464-second flow distribution component, 3465-second connecting rod and 3466-second fixing ring.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
As shown in FIG. 1, a method for continuously preparing high-purity sodium hypochlorite comprises the following steps,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle 100 with a first jacketed heat exchanger 107, and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle (100) in the step (a 1), and starting a stirrer in the first stirring kettle (100);
(a3) Adjusting the flow rate of circulating cooling water in the first jacketed heat exchanger 107 outside the first reaction kettle 100 in the step (a 1) through the reading of the first online thermometer 105 to control the temperature of the solution in the first reaction kettle 100; the temperature of the sodium hydroxide concentrated solution in the first reaction kettle 100 is 30-50 ℃;
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer 103 to control the concentration of the concentrated sodium hydroxide solution; in the step (a 4), the mass concentration of the sodium hydroxide concentrated solution is 20-50%;
(a5) Interlocking the first jacketed heat exchanger 107 by reading of the first online thermometer 105 in the first reaction vessel 100 to control the temperature of the concentrated sodium hydroxide solution in the first reaction vessel 100;
(b) Preparing dilute solution of sodium hydroxide
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle 200 with a second jacketed heat exchanger 207, and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle 200 in the step (b 1), and starting a stirrer in the second reaction kettle 200;
(b3) Adjusting the flow rate of the circulating cooling water of the second jacketed heat exchanger 207 outside the second reaction kettle 200 in the step (b 1) through the reading of the second online thermometer 209, and controlling the temperature of the solution in the second reaction kettle 200; the temperature of the dilute sodium hydroxide solution in the second reaction kettle 200 is 20-40 ℃;
(b4) Adjusting the flow rate of the deionized water in step (b 2) by reading from the second online densitometer 205 to control the concentration of the dilute sodium hydroxide solution; the mass concentration of the dilute sodium hydroxide solution in the step (b 4) is 13-18 percent;
(b5) Interlocking the second jacketed heat exchanger 206 by reading of a second online thermometer 209 in the second reaction kettle 200, controlling the temperature of the dilute sodium hydroxide solution in the second reaction kettle 200;
(c) Conveying dilute sodium hydroxide solution
(c1) Feeding the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution of step (c 1) into a static mixer 400 for mixing; the ratio of the length to the pipe diameter of the static mixer 400 is 10-15; the pipe diameter of the static mixer 400 is 0.05 m-0.2 m;
(d) Chlorination reaction
(d1) Inputting the mixed dilute sodium hydroxide solution in the step (c 2) into a spray tower atomizer 30 at the top of a sodium hypochlorite reactor 500, and spraying and atomizing the dilute sodium hydroxide solution downwards from the top of the spray tower atomizer 30; the pressure applied on the atomizer 30 of the spray tower is 0.2MPa to 0.5MPa; in the step (d 1), the flow rate of the dilute sodium hydroxide solution is 20 mL/min-40 mL/min; in the step (d 1), the size of the liquid drop after the atomization of the dilute sodium hydroxide solution is 5-50 um;
(d2) Feeding chlorine gas into gas distributor 34, wherein the chlorine gas is distributed in sodium hypochlorite reactor 500 by gas distributor 34; the flow rate of the chlorine in the step (d 2) is 5mL/min to 25mL/min;
(d3) Carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution;
(e) On-line monitoring
(e1) Online testing the pH of the sodium hypochlorite solution in the step (d 3) by a pH meter 501 in the sodium hypochlorite reactor 500, and interlocking the opening size of a back pressure valve 404 of the dilute sodium hydroxide solution online to keep the pH of the reaction system in a certain range; in the step (e 1), the pH value of a reaction system is kept between 12 and 13;
(e2) The cooling water valve 508 is interlocked online through a third online thermometer 509 in the sodium hypochlorite reactor 500, and the flow of the cooling water is adjusted by adjusting the opening of the cooling water valve 508 online, so that the reaction temperature is controlled online; in the step (e 2), the reaction temperature is kept between 30 and 50 ℃;
(e3) An online pressure gauge 504 in the sodium hypochlorite reactor 500 is used for interlocking an inert gas valve 503 online, and the opening of the inert gas valve 503 is adjusted online to adjust the flow of the inert gas, so that the internal pressure of the sodium hypochlorite reactor 500 is kept constant; controlling the reaction pressure in the step (e 3) to be 0.09 MPa-0.11 MPa; the inert gas is at least one of nitrogen, helium, neon, argon, krypton or xenon;
(e4) The chlorine valve 601 is interlocked on line through an online oxidation-reduction potential analyzer 701 in the sodium hypochlorite reactor 500, and the chlorine flow is adjusted by adjusting the opening of the chlorine valve 601 on line; in the step (e 4), the reading number of the online oxidation-reduction potential analyzer 701 is controlled to be 500 mv-600 mv;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the readings of the online oxidation-reduction potential analyzer 701 in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution obtained in the step (d 3) to a finished product tank 700; if the sodium hypochlorite solution does not reach the standard, the sodium hypochlorite solution is continuously kept in the sodium hypochlorite reactor 500, and the corresponding chlorine valve 601 is interlocked on line through the online oxidation-reduction potential analyzer 701 until the sodium hypochlorite solution reaches the standard and is conveyed to the finished product tank 700; the product in the step (f) meets the standard that the mass fraction of the effective chlorine is 6-15%, and the free alkali content is less than 0.5% by mass concentration.
As shown in fig. 2 and fig. 3, an apparatus for continuously preparing high-purity sodium hypochlorite comprises a first reaction kettle 100, wherein a water inlet of the first reaction kettle 100 is connected with a first water inlet pipeline, and a first delivery pump 101 is arranged on the first water inlet pipeline; a first backpressure valve 102 is arranged on a first water inlet pipeline between the first conveying pump 101 and the first reaction kettle 100; a first jacketed heat exchanger 107 is sleeved on the outer peripheral surface of the first reaction kettle 100, a first jacketed heat exchanger inlet 106 and a first jacketed heat exchanger outlet 108 are arranged on the first jacketed heat exchanger 107, the first jacketed heat exchanger inlet 106 is connected with a water outlet of the first reaction kettle 100 through a pipeline, the first jacketed heat exchanger inlet 106 is connected with cooling water through a pipeline, and a second back pressure valve 104 is arranged on the pipeline between the cooling water and the first jacketed heat exchanger inlet 106;
the device also comprises a second reaction kettle 200, wherein a liquid inlet of the second reaction kettle 200 is connected with a liquid outlet of the first reaction kettle 100 through a pipeline, and a second delivery pump 201 and a third backpressure valve 202 are sequentially arranged on the pipeline between the liquid outlet of the first reaction kettle 100 and the liquid inlet of the second reaction kettle 200 along the liquid flow direction; a second water inlet pipeline is connected to a water inlet of the second reaction kettle 200, a third delivery pump 203 is arranged on the second water inlet pipeline, and a fifth backpressure valve 2010 is arranged on a pipeline between the third delivery pump 203 and the second reaction kettle 200; a second jacketed heat exchanger 207 is sleeved on the outer peripheral surface of the second reaction kettle 200, a second jacketed heat exchanger inlet 206 and a second jacketed heat exchanger outlet 208 are arranged on the second jacketed heat exchanger 207, the second jacketed heat exchanger inlet 206 is connected with a water outlet of the second reaction kettle 200 through a pipeline, the second jacketed heat exchanger inlet 206 is connected with cooling water through a pipeline, and a fourth back pressure valve 204 is arranged on the pipeline between the cooling water and the second jacketed heat exchanger inlet 206; a liquid outlet of the second reaction kettle 200 is connected with a heat exchanger 300 through a pipeline, a fourth delivery pump 301 and a sixth backpressure valve 302 are arranged on the pipeline between the heat exchanger 300 and the liquid outlet of the second reaction kettle 200, and the sixth backpressure valve 302 is close to the heat exchanger 300 compared with the fourth delivery pump 301;
a liquid outlet of the heat exchanger 300 is connected with a static mixer 400 through a pipeline, a fifth delivery pump 401 and a seventh backpressure valve 402 are arranged on the pipeline between the static mixer 400 and the heat exchanger 300, and the seventh backpressure valve 402 is close to the static mixer 400 compared with the fifth delivery pump 401;
as shown in fig. 4 and 6, the liquid outlet of the static mixer 400 is connected to a sodium hypochlorite reactor 500 through a pipeline, a sixth delivery pump 403 and a back pressure valve 404 for sodium hydroxide dilute solution are arranged on the pipeline between the sodium hypochlorite reactor 500 and the static mixer 400, and the back pressure valve 404 for sodium hydroxide dilute solution is closer to the sodium hypochlorite reactor 500 than the sixth delivery pump 403; the atomizer 30 is arranged at the top in the sodium hypochlorite reactor 500; the bottom in the sodium hypochlorite reactor 500 is provided with a gas distributor 34;
as shown in fig. 5, the gas inlet of the gas distributor 34 is connected to a gas buffer tank 600 through a pipeline, a chlorine valve 601 is arranged on the pipeline between the gas buffer tank 600 and the gas distributor 34, the gas inlet of the gas buffer tank 600 is connected to a chlorine gas inlet through a pipeline, and a seventh delivery pump 602 is arranged on the pipeline between the chlorine gas inlet and the gas buffer tank 600;
the bottom of the sodium hypochlorite reactor 500 is connected with an inert gas inlet through a pipeline, an eighth delivery pump 502 and an inert gas valve 503 are arranged on the pipeline between the inert gas inlet and the sodium hypochlorite reactor 500, and the inert gas valve 503 is close to the sodium hypochlorite reactor 500 compared with the eighth delivery pump 502;
a third jacketed heat exchanger 505 is sleeved on the outer peripheral surface of the sodium hypochlorite reactor 500, a third jacketed heat exchanger inlet 506 and a third jacketed heat exchanger outlet 507 are arranged on the third jacketed heat exchanger 505, the third jacketed heat exchanger inlet 506 is connected with a cooling water interface through a pipeline, and a cooling water valve 508 is arranged on the pipeline between the cooling water interface and the third jacketed heat exchanger inlet 506;
a finished product tank 700 is connected to the liquid outlet of the sodium hypochlorite reactor 500 through a pipeline, a ninth delivery pump 703 and an eighth back pressure valve 702 are provided on the pipeline between the finished product tank 700 and the sodium chlorate reactor 500, and the eighth back pressure valve 702 is closer to the sodium chlorate reactor 500 than the ninth delivery pump 703.
The first reaction kettle 100 is provided with a first densimeter 103, and the first densimeter 103 is interlocked with a first back pressure valve 102 on line. A first online thermometer 105 is arranged on a pipeline between the water outlet of the first reaction kettle 100 and the inlet 106 of the first jacketed heat exchanger. A second densimeter 205 is arranged on the second reaction kettle 200, and the second densimeter 205 is interlocked with a fifth back pressure valve 2010 on line. A second online thermometer 209 is arranged on a pipeline between the water outlet of the second reaction kettle 200 and the inlet 206 of the second jacketed heat exchanger. A PH meter 501 is connected to sodium hypochlorite reactor 500. The bottom of sodium hypochlorite reactor 500 is connected with a pressure gauge 504, and the pressure gauge 504 is linked with an inert gas valve 503 on line. The water outlet of the sodium hypochlorite reactor 500 is connected with a third online thermometer 509, and the third online thermometer 509 is linked with a cooling water valve 508 in an online manner. An oxidation-reduction potential analyzer 701 is arranged on a pipeline between the ninth backpressure valve 702 and the sodium chlorate reactor 500, and the oxidation-reduction potential analyzer 701 is in online linkage with the chlorine valve 601.
As shown in fig. 9, the atomizer 30 includes a liquid inlet pipe 301, a liquid inlet end of the liquid inlet pipe 301 is connected to the static mixer 400 through a pipeline, a liquid outlet end of the liquid inlet pipe 301 is rotatably connected to a liquid inlet horizontal pipe 302, a plurality of liquid inlet branch pipes 303 are arranged on an outer circumferential surface of the liquid inlet horizontal pipe 302, a plurality of atomizing nozzles 304 are arranged at top and bottom of the liquid inlet branch pipes 303, and electromagnetic valves are arranged on the atomizing nozzles 304; still include driving motor 305, driving motor 305 sets up on sodium hypochlorite reactor 500's outer wall surface, and driving motor 305's drive end is equipped with carousel 306, and carousel 306 is located inside sodium hypochlorite reactor 500, and carousel 306 is connected with the one end of horizontal pipe 302 of feed liquor.
As shown in fig. 7, 8, 10 and 11, the gas distributor 34 includes a gas inlet pipe 341, a gas inlet end of the gas inlet pipe 341 is connected to the gas buffer tank 600 through a pipeline, a gas outlet end of the gas inlet pipe 341 is connected to a gas inlet horizontal pipe 342, the gas inlet horizontal pipe 342 is located inside the sodium hypochlorite reactor 500, a plurality of gas inlet branch pipes 343 are arranged on an outer circumferential surface of the gas inlet horizontal pipe 342, and a plurality of gas nozzles 344 are communicated with tops of the gas inlet branch pipes 343; the jet nozzle further comprises a primary flow splitting assembly 345, wherein the primary flow splitting assembly 345 is positioned on the upper side of the jet nozzle 344, and a secondary flow splitting assembly 346 is arranged on the upper side of the primary flow splitting assembly 345. The primary flow divider assembly 345 includes a plurality of first flow dividers 3451 having an inverted cone shape, the first flow dividers 3451 correspond to the air nozzles 344, the first flow dividers 3451 are located above the corresponding air nozzles 344, adjacent first flow dividers 3451 are connected by a first connecting rod 3452, the inner sidewall of the sodium hypochlorite reactor 500 is connected with a first fixing ring 3453, and the first flow dividers 3451 close to the first fixing ring 3453 are connected with the first fixing ring 3453 by a first connecting rod 3452. The secondary flow dividing assembly 346 includes a plurality of liquid storage boxes 3461, the liquid storage boxes 3461 are located above the first flow divider 3451, a water leakage hole 3462 is formed at the bottom of the liquid storage boxes 3461, the top of the liquid storage boxes 3461 is connected with a plurality of second flow dividers 3464 through a support rod 3463, the adjacent liquid storage boxes 3461 are connected through a second connecting rod 3465, a second fixing ring 3466 is slidably connected to the inner side wall of the sodium hypochlorite reactor 500, and the liquid storage boxes 3461 close to the second fixing ring 3466 are connected with the second fixing ring 3466 through the second connecting rod 3465. Also included is an atomization status detection component 307; the atomization state detection assembly 307 comprises a plurality of seal boxes 3071, the seal boxes 3071 are arranged on the inner side wall of the sodium hypochlorite reactor 500, tension sensors 3072 are arranged in the seal boxes 3071, straight rods 3073 are arranged on the tension sensors 3072, the bottom ends of the straight rods 3073 penetrate through the bottom wall of the seal boxes 3071 and are connected with connecting plates 3074, pull rods 3075 are arranged on the connecting plates 3074, the bottom ends of the pull rods 3075 are connected with second fixing rings 3466, and the tension sensors 3072 are in wired or wireless connection with the driving motor 305.
Example 1:
as shown in FIG. 1, a method for continuously preparing high-purity sodium hypochlorite comprises the following steps,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle 100 with a first jacketed heat exchanger 107, and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle 100 in the step (a 1), and starting a stirrer in the first stirring kettle 100;
(a3) Adjusting the flow rate of the circulating cooling water in the first jacketed heat exchanger 107 outside the first reaction kettle 100 in the step (a 1) through the reading of the first online thermometer 105, and controlling the temperature of the solution in the first reaction kettle 100 to be 30 ℃;
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer 103 to control the concentration of the concentrated sodium hydroxide solution to be 20%;
(a5) Interlocking the first jacketed heat exchanger 107 by reading the first online thermometer 105 in the first reaction kettle 100 to control the temperature of the concentrated sodium hydroxide solution in the first reaction kettle 100;
(b) Preparing dilute solution of sodium hydroxide
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle 200 with a second jacketed heat exchanger 207, and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle 200 in the step (b 1), and starting a stirrer in the second reaction kettle 200;
(b3) Adjusting the flow rate of circulating cooling water of the second jacketed heat exchanger 207 outside the second reaction kettle 200 in the step (b 1) through the reading of the second online thermometer 209, and controlling the temperature of the solution in the second reaction kettle 200 to be 20 ℃;
(b4) Adjusting the flow rate of the deionized water in the step (b 2) by reading of the second online densitometer 205 to control the concentration of the dilute sodium hydroxide solution to 13%;
further comprising the step (b 5) of interlocking the second jacketed heat exchanger 207 by reading a second online thermometer 209 in the second reaction vessel 200 to control the temperature of the dilute sodium hydroxide solution in the second reaction vessel 200;
(c) Conveying dilute sodium hydroxide solution
(c1) Sending the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution of step (c 1) into a static mixer 400 for mixing;
(d) Chlorination reaction
(d1) Inputting the mixed dilute sodium hydroxide solution in the step (c 2) into a spray tower atomizer 30 at the top of a sodium hypochlorite reactor 500 at a flow rate of 20mL/min, spraying and atomizing the dilute sodium hydroxide solution downwards from the top of the spray tower atomizer 30, wherein the size of liquid drops of the atomized dilute sodium hydroxide solution in the step (d 1) is 5um;
(d2) Conveying chlorine gas into a gas distributor 34 at a flow rate of 5mL/min, wherein the chlorine gas is distributed in a sodium hypochlorite reactor 500 by the gas distributor 34;
(d3) Carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution;
(e) On-line monitoring
(e1) Online testing the pH value of the sodium hypochlorite solution in the step (d 3) by a pH meter in the sodium hypochlorite reactor 500, and interlocking the opening size of the back pressure valve 404 of the dilute sodium hydroxide solution online to keep the pH value of the reaction system at 12;
(e2) The reaction temperature is controlled to be kept at 30 ℃ on line by a third online thermometer 509 in the sodium hypochlorite reactor 500, interlocking the cooling water valve 508 on line, and adjusting the opening of the cooling water valve 508 on line to adjust the flow of cooling water;
(e3) The method comprises the steps of interlocking an inert gas valve 503 on line through an online pressure gauge 504 in the sodium hypochlorite reactor 500, adjusting the flow of the inert gas by adjusting the opening of the inert gas valve 503 on line, wherein the inert gas is at least one of nitrogen, helium, neon, argon, krypton or xenon, so that the internal pressure of the sodium hypochlorite reactor 500 is kept constant and controlled at 0.09MPa;
(e4) The chlorine gas flow is adjusted by interlocking the chlorine gas valve 601 on line through the online oxidation-reduction potential analyzer 701 in the sodium hypochlorite reactor 500 and adjusting the opening of the chlorine gas valve 601 on line, and the reading of the online oxidation-reduction potential analyzer 701 in the step (e 4) is controlled at 500mv;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the readings of the online oxidation-reduction potential analyzer 701 in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution in the step (d 3) to a finished product tank 700; if the sodium hypochlorite solution does not reach the standard, the sodium hypochlorite solution is continuously kept in a sodium hypochlorite reactor 500, a corresponding chlorine valve 601 is interlocked on line through an online oxidation-reduction potential analyzer 701 until the sodium hypochlorite solution reaches the standard, and the sodium hypochlorite solution is conveyed into a finished product tank 700, wherein the standard of the product in the step (f) is required to reach the standard, the mass fraction of the effective chlorine is 6%, and the content of the free alkali is less than 0.5% of the mass concentration.
Example 2:
as shown in FIG. 1, a method for continuously preparing high-purity sodium hypochlorite comprises the following steps,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle 100 with a first jacketed heat exchanger 107, and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle 100 in the step (a 1), and starting a stirrer in the first stirring kettle 100;
(a3) Adjusting the flow rate of circulating cooling water in the first jacketed heat exchanger 107 outside the first reaction kettle 100 in the step (a 1) through the reading of the first online thermometer 105, and controlling the temperature of the solution in the first reaction kettle 100 to be 50 ℃;
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer 103 to control the concentration of the concentrated sodium hydroxide solution to 50%;
(a5) Interlocking the first jacketed heat exchanger 107 by reading of the first online thermometer 105 in the first reaction vessel 100 to control the temperature of the concentrated sodium hydroxide solution in the first reaction vessel 100;
(b) Preparing a sodium hydroxide dilute solution.
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle 200 with a second jacketed heat exchanger 207, and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle 200 in the step (b 1), and starting a stirrer in the second reaction kettle 200;
(b3) Adjusting the flow rate of circulating cooling water of the second jacketed heat exchanger 207 outside the second reaction kettle 200 in the step (b 1) through the reading of the second online thermometer 209, and controlling the temperature of the solution in the second reaction kettle 200 to be 40 ℃;
(b4) Adjusting the flow rate of the deionized water in the step (b 2) by reading of the second online densitometer 205 to control the concentration of the dilute sodium hydroxide solution to 18%;
(b5) Interlocking the second jacketed heat exchanger 207 through the reading of the second online thermometer 209 in the second reaction kettle 200, controlling the temperature of the dilute sodium hydroxide solution in the second reaction kettle 200;
(c) Conveying dilute sodium hydroxide solution
(c1) Sending the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution of step (c 1) into a static mixer 400 for mixing;
(d) Chlorination reaction
(d1) Inputting the mixed dilute sodium hydroxide solution in the step (c 2) into a spray tower atomizer 30 at the top of a sodium hypochlorite reactor 500 at the flow rate of 40mL/min, spraying and atomizing the dilute sodium hydroxide solution downwards from the top of the spray tower atomizer 30, wherein the size of liquid drops of the atomized dilute sodium hydroxide solution in the step (d 1) is 50um;
(d2) Conveying chlorine gas into a gas distributor 34 at a flow rate of 25mL/min, wherein the chlorine gas is distributed in a sodium hypochlorite reactor 500 by the gas distributor 34;
(d3) And (d 1) carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution.
(e) On-line monitoring
(e1) Online testing the pH of the sodium hypochlorite solution in the step (d 3) by a pH meter in the sodium hypochlorite reactor 500, and interlocking the opening size of the back pressure valve 404 of the dilute sodium hydroxide solution online to keep the pH of the reaction system at 13;
(e2) The reaction temperature is controlled to be kept at 50 ℃ on line by a third online thermometer 509 in the sodium hypochlorite reactor 500, interlocking the cooling water valve 508 on line and adjusting the flow of the cooling water by adjusting the opening of the cooling water valve 508 on line;
(e3) The online pressure gauge 504 and the online interlocking inert gas valve 503 in the sodium hypochlorite reactor 500 are used for online adjusting the opening of the inert gas valve 503 to adjust the flow of the inert gas, wherein the inert gas is at least one of nitrogen, helium, neon, argon, krypton or xenon, so that the internal pressure of the sodium hypochlorite reactor 500 is constantly controlled to be 0.11MPa;
(e4) The chlorine gas flow is adjusted by interlocking the chlorine gas valve 601 on line through the online oxidation-reduction potential analyzer 701 in the sodium hypochlorite reactor 500 and adjusting the opening of the chlorine gas valve 601 on line, and the reading of the online oxidation-reduction potential analyzer 701 in the step (e 4) is controlled at 600mv;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the readings of the online oxidation-reduction potential analyzer 701 in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution in the step (d 3) to a finished product tank 700; if the sodium hypochlorite solution does not reach the standard, the sodium hypochlorite solution is continuously kept in the sodium hypochlorite reactor 500, the corresponding chlorine valve 601 is interlocked on line through the online oxidation-reduction potential analyzer 701 until the sodium hypochlorite solution reaches the standard, and the sodium hypochlorite solution is conveyed to the finished product tank 700, wherein the product in the step (f) meets the standard, the mass fraction of the effective chlorine is 15%, and the content of the free alkali is less than 0.5% of the mass concentration.
Example 3:
as shown in FIG. 1, a method for continuously preparing high-purity sodium hypochlorite comprises the following steps,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle 100 with a first jacketed heat exchanger 107, and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle 100 in the step (a 1), and starting a stirrer in the first stirring kettle 100;
(a3) Adjusting the flow rate of circulating cooling water in the first jacketed heat exchanger 107 outside the first reaction kettle 100 in the step (a 1) through the reading of the first online thermometer 105, and controlling the temperature of the solution in the first reaction kettle 100 to be 35 ℃;
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer 103 to control the concentration of the concentrated sodium hydroxide solution to be 30%;
(a5) Interlocking the first jacketed heat exchanger 107 by reading the first online thermometer 105 in the first reaction kettle 100 to control the temperature of the concentrated sodium hydroxide solution in the first reaction kettle 100;
(b) Preparing dilute solution of sodium hydroxide
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle 200 with a second jacketed heat exchanger 207, and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle 200 in the step (b 1), and starting a stirrer in the second reaction kettle 200;
(b3) Adjusting the flow rate of circulating cooling water of the second jacketed heat exchanger 207 outside the second reaction kettle 200 in the step (b 1) through the reading of the second online thermometer 209, and controlling the temperature of the solution in the second reaction kettle 200 to be 30 ℃;
(b4) Adjusting the flow rate of the deionized water in the step (b 2) by reading of the second online densitometer 205 to control the concentration of the dilute sodium hydroxide solution to 15%;
(b5) Interlocking the second jacketed heat exchanger 207 through the reading of the second online thermometer 209 in the second reaction kettle 200, controlling the temperature of the dilute sodium hydroxide solution in the second reaction kettle 200;
(c) Conveying dilute sodium hydroxide solution
(c1) Feeding the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution of step (c 1) into a static mixer 400 for mixing;
(d) Chlorination reaction
(d1) Inputting the mixed dilute sodium hydroxide solution in the step (c 2) into a spray tower atomizer 30 at the top of a sodium hypochlorite reactor 500 at a flow rate of 30L/min, spraying and atomizing the dilute sodium hydroxide solution downwards from the top of the spray tower atomizer 30, wherein the size of liquid drops of the atomized dilute sodium hydroxide solution in the step (d 1) is 35um;
(d2) Conveying chlorine gas into a gas distributor 34 at a flow rate of 15mL/min, wherein the chlorine gas is distributed in a sodium hypochlorite reactor 500 by the gas distributor 34;
(d3) Carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution;
(e) On-line monitoring
(e1) Online testing the pH of the sodium hypochlorite solution in the step (d 3) by a pH meter in the sodium hypochlorite reactor 500, and interlocking the opening size of the back pressure valve 404 of the dilute sodium hydroxide solution online to keep the pH of the reaction system at 12.5;
(e2) The reaction temperature is controlled to be kept at 40 ℃ on line by a third online thermometer 509 in the sodium hypochlorite reactor 500, interlocking the cooling water valve 508 on line and adjusting the flow of the cooling water by adjusting the opening of the cooling water valve 508 on line;
(e3) The method comprises the steps of online interlocking an inert gas valve 503 through an online pressure gauge 504 in the sodium hypochlorite reactor 500, and adjusting the flow of inert gas through online adjusting the opening of the inert gas valve 503, so as to keep the internal pressure of the sodium hypochlorite reactor 500 constant and control the internal pressure to be 0.1MPa, wherein the inert gas is at least one of nitrogen, helium, neon, argon, krypton or xenon;
(e4) The chlorine gas flow is adjusted by on-line interlocking of the chlorine gas valve 601 through the on-line oxidation-reduction potential analyzer 701 in the sodium hypochlorite reactor 500 and on-line adjustment of the opening degree of the chlorine gas valve 601, and the reading of the on-line oxidation-reduction potential analyzer 701 in the step (e 4) is controlled at 550mv;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the readings of the online oxidation-reduction potential analyzer 701 in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution obtained in the step (d 3) to a finished product tank 700; if the sodium hypochlorite solution does not reach the standard, the sodium hypochlorite solution is continuously kept in the sodium hypochlorite reactor 500, the corresponding chlorine valve 601 is interlocked on line through the online oxidation-reduction potential analyzer 701 until the sodium hypochlorite solution reaches the standard, and the sodium hypochlorite solution is conveyed to the finished product tank 700, wherein the product in the step (f) meets the standard, the mass fraction of the effective chlorine is 12%, and the content of the free alkali is less than 0.5% of the mass concentration.
Example 4:
the equipment for continuously preparing the high-purity sodium hypochlorite comprises a first reaction kettle 100, wherein a water inlet of the first reaction kettle 100 is connected with a first water inlet pipeline, a first conveying pump 101 is arranged on the first water inlet pipeline, a first back pressure valve 102 is arranged on the first water inlet pipeline between the first conveying pump 101 and the first reaction kettle 100, a first densimeter 103 is arranged on the first reaction kettle 100, the first densimeter 103 is in online linkage with the first back pressure valve 102, a first jacketed heat exchanger 107 is sleeved on the outer peripheral surface of the first reaction kettle 100, a first jacketed heat exchanger inlet 106 and a first jacketed heat exchanger outlet 108 are arranged on the first jacketed heat exchanger 107, the first jacketed heat exchanger inlet 106 is connected with a water outlet of the first reaction kettle 100 through a pipeline, a first online thermometer 105 is arranged on the pipeline, a pipeline is communicated with the first jacketed heat exchanger inlet 106, and a second back pressure valve 104 is arranged on the pipeline;
the system also comprises a second reaction kettle 200, a liquid discharge port of the first reaction kettle 100 is communicated with a liquid inlet of the second reaction kettle 200 through a pipeline, a second conveying pump 201 and a third back pressure valve 202 are sequentially arranged on the pipeline along the liquid flow direction, a water inlet of the second reaction kettle 200 is connected with a second water inlet pipeline, a third conveying pump 203 and a fifth back pressure valve 2010 are arranged on the second water inlet pipeline, a second densimeter 205 is arranged on the second reaction kettle 200, the second densimeter 205 and the fifth back pressure valve 2010 are in online linkage, a second jacketed heat exchanger 207 is sleeved on the outer peripheral surface of the second reaction kettle 200, a second jacketed heat exchanger inlet 206 and a second jacketed heat exchanger outlet 208 are arranged on the second jacketed heat exchanger 207, the second jacketed heat exchanger inlet 206 is communicated with a water outlet of the second reaction kettle 200 through a pipeline, a second online thermometer 209 is arranged on the pipeline, another liquid inlet pipeline of the second jacketed heat exchanger 206 is communicated with a fourth back pressure valve 204, the liquid discharge port of the second reaction kettle 200 is communicated with the heat exchanger 300 through a pipeline, and a fourth conveying pump 301 and a sixth back pressure valve 302 are arranged on the pipeline;
a liquid discharge port of the heat exchanger 300 is communicated with a liquid inlet of the static mixer 400 through a pipeline, the pipeline is provided with a fifth delivery pump 401 and a seventh backpressure valve 402, the liquid discharge port of the static mixer 400 is communicated with a liquid inlet of the sodium hypochlorite reactor 500 through a pipeline, the pipeline is provided with a 403 and a sodium hydroxide dilute solution backpressure valve 404, the sodium hypochlorite reactor 500 is provided with a PH meter 501, the top inside the sodium hypochlorite reactor 500 is provided with an atomizer 30, and the bottom inside the sodium hypochlorite reactor 500 is provided with a gas distributor 34;
the gas inlet of the gas distributor 34 is communicated with the gas outlet of the buffer tank 600 through a gas inlet pipeline, a chlorine valve 601 is arranged on the gas inlet pipeline, the chlorine inlet on the buffer tank 600 is communicated with a pipeline, a seventh delivery pump 602 is arranged on the pipeline, a pipeline is arranged on the inert gas inlet at the bottom of the sodium hypochlorite reactor 500, an eighth delivery pump 502 and an inert gas valve 503 are arranged on the pipeline, a pressure gauge 504 is arranged at the bottom of the sodium hypochlorite reactor 500, and the pressure gauge 504 is in online linkage with the inert gas valve 503;
a third jacketed heat exchanger 505 is sleeved on the outer peripheral surface of the sodium hypochlorite reactor 500, a third jacketed heat exchanger inlet 506 and a third jacketed heat exchanger outlet 507 are arranged on the third jacketed heat exchanger 505, a water outlet of the sodium hypochlorite reactor 500 is communicated with the third jacketed heat exchanger inlet 506 through a water inlet pipeline, and a cooling water valve 508 and a third online thermometer 509 are arranged on the water inlet pipeline;
the liquid outlet of the sodium hypochlorite reactor 500 is communicated with the finished product tank 700 through a pipeline, the pipeline is provided with an oxidation-reduction potential analyzer 701, a ninth backpressure valve 702 and a ninth delivery pump 703, and the oxidation-reduction potential analyzer 701 is linked with the chlorine valve 601 on line.
Wherein, atomizer 30 includes feed liquor pipe 301, feed liquor pipe 301 one end runs through sodium hypochlorite reactor 500 and swivelling joint has the horizontal pipe 302 of feed liquor, feed liquor pipe 301 is linked together with horizontal pipe 302 of feed liquor, the symmetry is equipped with two sets of feed liquor branch pipes 303 on the outer peripheral face of horizontal pipe 302 of feed liquor, the top and the bottom of two sets of feed liquor branch pipes 303 all communicate and have a plurality of atomizing nozzle 304, be equipped with the solenoid valve on atomizing nozzle 304, atomizer 30 includes driving motor 305 and carousel 306, carousel 306 is located inside the sodium hypochlorite reactor 500 and violently manages 302 end connection with the feed liquor, driving motor 305 is located the outside of sodium hypochlorite reactor 500 and is connected with carousel 306, atomizer 30 still includes atomizing state detection subassembly 307.
Wherein, gas distributor 34 includes intake pipe 341, intake pipe 341 one end runs through sodium hypochlorite reactor 500 and communicates and has intake violently pipe 342, intake violently pipe 342 on the outer peripheral face of 342 symmetry intercommunication have two sets of branch pipes 343 that admit air, the top of two sets of branch pipes 343 that admit air all communicates with a plurality of air nozzles 344, gas distributor 34 still includes one-level reposition of redundant personnel subassembly 345 and second grade reposition of redundant personnel subassembly 346, one-level reposition of redundant personnel subassembly 345 is located air nozzles 344 upside, second grade reposition of redundant personnel subassembly 346 is located one-level reposition of redundant personnel subassembly 345 upside.
The first-stage flow splitting assembly 345 includes a plurality of first flow splitters 3451 in an inverted cone shape, the number of the first flow splitters 3451 is equal to the number of the air nozzles 344, the plurality of first flow splitters 3451 are respectively located right above the plurality of air nozzles 344, two adjacent first flow splitters 3451 are connected by a first connecting rod 3452, a first fixing ring 3453 is connected to the inner side wall of the sodium hypochlorite reactor 500, and the first flow splitters 3451 adjacent to the first fixing ring 3453 are connected to the first fixing ring 3453 by the first connecting rod 3452.
The secondary flow dividing assembly 346 includes a plurality of liquid storage boxes 3461, the number of the plurality of liquid storage boxes 3461 is equal to the number of the plurality of first flow dividers 3451, the plurality of liquid storage boxes 3461 are respectively located above the plurality of first flow dividers 3451, the bottom of the liquid storage boxes 3461 is provided with water leakage holes 3462, the top of the liquid storage boxes 3461 is connected to a plurality of second flow dividers 3464 in a ring shape through a support bar 3463, two adjacent liquid storage boxes 3461 are connected by a second connecting bar 3465, the inner side wall of the sodium hypochlorite reactor 500 is connected to a second fixing ring 3466 in a sliding manner, and the liquid storage boxes 3461 close to the second fixing ring 3466 are connected to the second fixing ring 3466 through the second connecting bar 3465 and the second fixing ring 3466.
The distance between the bottom ends of the second shunts 3464 on the liquid storage box 3461 and the axial line of the liquid storage box 3461 is greater than the radius of the top surface of the first shunt 3451 located right below the liquid storage box 3461.
Wherein, atomizing state detection subassembly 307 is including being a plurality of seal box 3071 of annular connection on sodium hypochlorite reactor 500 inside wall, be equipped with force sensor 3072 in the seal box 3071, the last straight-bar 3073 that is equipped with of force sensor 3072, the straight-bar 3073 bottom is run through the seal box 3071 diapire and is connected with connecting plate 3074, be equipped with pull rod 3075 on the connecting plate 3074, the pull rod 3075 bottom is connected with the solid fixed ring 3466 of second, force sensor 3072 is connected with driving motor 305 through wired or wireless mode.
The working principle of the invention is as follows:
after the power-on, upwards spout chlorine into sodium hypochlorite reactor 500 inside through intake pipe 341, air inlet horizontal pipe 342, air inlet branch pipe 343 and air nozzle 344, then chlorine spouts from air nozzle 344 to the first current divider 3451 directly over by preliminary dispersion, and then the chlorine that is by preliminary dispersion continues the upflow and collides and is dispersed here with a plurality of second current dividers 3464, and chlorine fully equipartition is inside sodium hypochlorite reactor 500 at this moment.
And simultaneously, the sodium hydroxide solution is atomized and sprayed to hypochlorous acid according to the lower part of the reactor 500 until the hypochlorous acid reacts with the chlorine which is thoroughly dispersed and uniformly distributed at the joint of the hypochlorous acid to generate mixed solution through a liquid inlet pipe 301, a liquid inlet horizontal pipe 302, a liquid inlet branch pipe 303 and an atomizing nozzle 304.
Along with the increase of the working time of the atomizing nozzle 304, the atomizing nozzle 304 can be corroded and damaged by sodium hydroxide solution, the atomizing effect of the atomizing nozzle 304 is deteriorated, the sodium hydroxide solution is difficult to be evenly atomized and distributed in the sodium hypochlorite reactor 500, so that the sodium hydroxide solution sprayed downwards is more concentrated, the sodium hydroxide solution falling in the liquid storage box 3461 in the same time is increased, when the speed of the sodium hydroxide solution entering the liquid storage box 3461 is greater than the speed of the sodium hydroxide solution discharged from the liquid leakage hole 3462, the sodium hydroxide solution in the liquid storage box 3461 can be continuously increased, the pulling force borne by the pull rod 3075 and the pull sensor 3072 is increased, after the pulling force reaches a set value, the driving motor 305 is started to drive the air inlet transverse pipe 342 to rotate for one hundred eighty degrees through the rotary disc 306 and the liquid inlet pipe 301, the original brand-new atomizing nozzle 304 positioned on the upper side is put into work, the damaged atomizing nozzle 304 rotates to the upper side and closes the electromagnetic valve on the damaged atomizing nozzle 304 to stop working, and the replacement cycle of the atomizing nozzle 304 can be prolonged on the premise that the atomizing spray effect is not affected, and the reliability of the atomizing tower 30 and the practicality and the atomizing tower are effectively improved.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. A method for continuously preparing high-purity sodium hypochlorite is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(a) Preparing concentrated solution of sodium hydroxide
(a1) Adding a certain mass of concentrated alkali into a first reaction kettle (100) with a first jacketed heat exchanger (107), and opening circulating cooling water;
(a2) Adding a certain mass of deionized water into the first reaction kettle (100) in the step (a 1), and starting a stirrer in the first stirring kettle (100);
(a3) Adjusting the flow rate of circulating cooling water in a first jacketed heat exchanger (107) outside the first reaction kettle (100) in the step (a 1) through the reading of a first online thermometer (105), and controlling the temperature of the solution in the first reaction kettle (100);
(a4) Adjusting the flow rate of the deionized water in the step (a 2) through the reading of the first online densitometer (103) to control the concentration of the concentrated sodium hydroxide solution;
(b) Preparing dilute solution of sodium hydroxide
(b1) Adding the concentrated sodium hydroxide solution prepared in the step (a 4) into a second reaction kettle (200) with a second jacketed heat exchanger (207), and opening circulating cooling water;
(b2) Inputting a certain mass of deionized water into the second reaction kettle (200) in the step (b 1), and starting a stirrer in the second reaction kettle (200);
(b3) Adjusting the flow rate of circulating cooling water of a second jacketed heat exchanger (207) outside the second reaction kettle (200) in the step (b 1) through the reading of a second online thermometer (209), and controlling the temperature of the solution in the second reaction kettle (200);
(b4) Adjusting the flow rate of the deionized water in the step (b 2) by reading of a second online densitometer (205) to control the concentration of the dilute sodium hydroxide solution;
(c) Conveying dilute sodium hydroxide solution
(c1) Sending the dilute sodium hydroxide solution prepared in the step (b 4) into a liquid storage tank for later use;
(c2) Feeding the dilute sodium hydroxide solution obtained in the step (c 1) into a static mixer (400) for mixing;
(d) Chlorination reaction
(d1) Inputting the mixed dilute sodium hydroxide solution in the step (c 2) into a spray tower atomizer (30) at the top of a sodium hypochlorite reactor (500), and spraying and atomizing the dilute sodium hydroxide solution downwards from the top of the spray tower atomizer (30);
(d2) Conveying chlorine gas into a gas distributor (34), wherein the chlorine gas is distributed in a sodium hypochlorite reactor (500) by the gas distributor (34);
(d3) Carrying out countercurrent contact reaction on the atomized sodium hydroxide dilute solution obtained in the step (d 1) and the chlorine dispersed in the step (d 2) to generate a sodium hypochlorite solution;
(e) On-line monitoring
(e1) Online testing the pH of the sodium hypochlorite solution in the step (d 3) by a pH meter in the sodium hypochlorite reactor (500), and interlocking the opening size of a back pressure valve (404) of the dilute sodium hydroxide solution online to keep the pH of the reaction system in a certain range;
(e2) Through a third online thermometer (509) in the sodium hypochlorite reactor (500), a cooling water valve (508) is interlocked online, and the opening of the cooling water valve (508) is adjusted online to adjust the flow of cooling water, so that the reaction temperature is controlled online;
(e3) An online pressure gauge (504) in the sodium hypochlorite reactor (500) is used for interlocking an inert gas valve (503) online, and the opening of the inert gas valve (503) is adjusted online to adjust the flow of the inert gas, so that the internal pressure of the sodium hypochlorite reactor (500) is kept constant;
(e4) The chlorine gas flow is adjusted by interlocking the chlorine gas valve (601) on line through an online oxidation-reduction potential analyzer (701) in the sodium hypochlorite reactor (500) and adjusting the opening of the chlorine gas valve (601) on line;
(f) Collecting the product
Judging whether the product reaches the standard or not by observing the reading of the online oxidation-reduction potential analyzer (701) in the step (e 4); if the sodium hypochlorite solution reaches the standard, sending the sodium hypochlorite solution in the step (d 3) to a finished product tank (700); if the sodium hypochlorite solution does not reach the standard, the sodium hypochlorite solution is continuously stopped in a sodium hypochlorite reactor (500), and a corresponding chlorine valve (601) is interlocked on line through an online oxidation-reduction potential analyzer (701) until the sodium hypochlorite solution reaches the standard and is conveyed into a finished product tank (700).
2. The method of claim 1, wherein the method comprises the following steps: further comprising the steps of (a 5) interlocking the first jacketed heat exchanger (107) by reading of a first on-line thermometer (105) in the first reaction vessel (100) to control the temperature of the concentrated sodium hydroxide solution in the first reaction vessel (100);
further comprising the step of (b 5) controlling the temperature of the dilute sodium hydroxide solution in the second reaction vessel (200) by interlocking the second jacketed heat exchanger (207) with the reading of a second online thermometer (209) in the second reaction vessel (200).
3. The method of claim 1, wherein the method comprises the following steps: the mass concentration of the sodium hydroxide concentrated solution in the step (a 4) is 20-50%; the temperature of the concentrated sodium hydroxide solution in the first reaction kettle (100) is 30-50 ℃; the mass concentration of the dilute sodium hydroxide solution in the step (b 4) is 13-18%; the temperature of the dilute sodium hydroxide solution in the second reaction kettle (200) is 20-40 ℃; the ratio of the length to the pipe diameter of the static mixer (400) is 10-15; the pipe diameter of the static mixer (400) is 0.05-0.2 m; the pressure applied on the spray tower atomizer (30) is 0.2 MPa-0.5 MPa.
4. The process according to claim 1 for the continuous preparation of sodium hypochlorite of high purity, characterized in that: the flow rate of the dilute sodium hydroxide solution in the step (d 1) is 20mL/min to 40mL/min; in the step (d 1), the size of the liquid drop after the atomization of the dilute sodium hydroxide solution is 5-50 um; (ii) a The flow rate of the chlorine in the step (d 2) is 5mL/min to 25mL/min; the pH value of the reaction system in the step (e 1) is kept between 12 and 13; the reaction temperature in the step (e 2) is kept between 30 and 50 ℃; the reaction pressure in the step (e 3) is controlled to be 0.09MPa to 0.11MPa; in the step (e 4), the number of the on-line oxidation-reduction potential analyzer (701) is controlled to be 500 mv-600 mv.
5. The process according to claim 1 for the continuous preparation of sodium hypochlorite of high purity, characterized in that: the inert gas is at least one of nitrogen, helium, neon, argon, krypton or xenon.
6. The method of claim 1, wherein the method comprises the following steps: the product in the step (f) meets the standard that the mass fraction of the effective chlorine is 6-15%, and the free alkali content is less than 0.5% by mass concentration.
7. The utility model provides an equipment of continuous preparation high-purity sodium hypochlorite which characterized in that: the device comprises a first reaction kettle (100), wherein a water inlet of the first reaction kettle (100) is connected with a first water inlet pipeline, and a first delivery pump (101) is arranged on the first water inlet pipeline; a first backpressure valve (102) is arranged on a first water inlet pipeline between the first conveying pump (101) and the first reaction kettle (100); a first jacketed heat exchanger (107) is sleeved on the outer peripheral surface of the first reaction kettle (100), a first jacketed heat exchanger inlet (106) and a first jacketed heat exchanger outlet (108) are arranged on the first jacketed heat exchanger (107), the first jacketed heat exchanger inlet (106) is connected with a water outlet of the first reaction kettle (100) through a pipeline, the first jacketed heat exchanger inlet (106) is connected with cooling water through a pipeline, and a second back pressure valve (104) is arranged on the pipeline between the cooling water and the first jacketed heat exchanger inlet (106);
the device is characterized by further comprising a second reaction kettle (200), wherein a liquid inlet of the second reaction kettle (200) is connected with a liquid outlet of the first reaction kettle (100) through a pipeline, and a second conveying pump (201) and a third backpressure valve (203) are sequentially arranged on the pipeline between the liquid outlet of the first reaction kettle (100) and the liquid inlet of the second reaction kettle (200) along the liquid flow direction; a water inlet of the second reaction kettle (200) is connected with a second water inlet pipeline, a third conveying pump (203) is arranged on the second water inlet pipeline, and a fifth backpressure valve (2010) is arranged on a pipeline between the third conveying pump (203) and the second reaction kettle (200); a second jacketed heat exchanger (207) is sleeved on the outer peripheral surface of the second reaction kettle (200), a second jacketed heat exchanger inlet (206) and a second jacketed heat exchanger outlet (208) are arranged on the second jacketed heat exchanger (207), the second jacketed heat exchanger inlet (207) is connected with a water outlet of the second reaction kettle (200) through a pipeline, the second jacketed heat exchanger inlet (206) is connected with cooling water through a pipeline, and a fourth back pressure valve (204) is arranged on a pipeline between the cooling water and the second jacketed heat exchanger inlet (206); a liquid outlet of the second reaction kettle (200) is connected with a heat exchanger (300) through a pipeline, a fourth conveying pump (301) and a sixth backpressure valve (302) are arranged on the pipeline between the heat exchanger (300) and the liquid outlet of the second reaction kettle (200), and the sixth backpressure valve (302) is close to the heat exchanger (300) compared with the fourth conveying pump (301);
a liquid outlet of the heat exchanger (300) is connected with a static mixer (400) through a pipeline, a fifth delivery pump (401) and a seventh backpressure valve (402) are arranged on the pipeline between the static mixer (400) and the heat exchanger (300), and the seventh backpressure valve (402) is close to the static mixer (400) compared with the fifth delivery pump (401);
a liquid outlet of the static mixer (400) is connected with a sodium hypochlorite reactor (500) through a pipeline, a sixth delivery pump (403) and a sodium hydroxide dilute solution back pressure valve (404) are arranged on the pipeline between the sodium hypochlorite reactor (500) and the static mixer (400), and the sodium hydroxide dilute solution back pressure valve (404) is close to the sodium hypochlorite reactor (500) compared with the sixth delivery pump (403); an atomizer (30) is arranged at the top in the sodium hypochlorite reactor (500); a gas distributor (34) is arranged at the bottom in the sodium hypochlorite reactor (500);
the gas distributor is characterized in that a gas inlet of the gas distributor (34) is connected with a gas buffer tank (600) through a pipeline, a chlorine valve (601) is arranged on the pipeline between the gas buffer tank (600) and the gas distributor (34), the gas inlet of the gas buffer tank (600) is connected with a chlorine gas inlet through a pipeline, and a seventh delivery pump (602) is arranged on the pipeline between the chlorine gas inlet and the gas buffer tank (600);
the bottom of the sodium hypochlorite reactor (500) is connected with an inert gas inlet through a pipeline, an eighth delivery pump (502) and a chlorine valve (601) are arranged on the pipeline between the inert gas inlet and the sodium hypochlorite reactor (500), and the chlorine valve (601) is close to the sodium hypochlorite reactor (500) compared with the eighth delivery pump (502);
a third jacketed heat exchanger (505) is sleeved on the outer peripheral surface of the sodium hypochlorite reactor (500), a third jacketed heat exchanger inlet (506) and a third jacketed heat exchanger outlet (507) are arranged on the third jacketed heat exchanger (505), the third jacketed heat exchanger inlet (506) is connected with a cooling water interface through a pipeline, and a cooling water valve (508) is arranged on the pipeline between the cooling water interface and the third jacketed heat exchanger inlet (506);
the liquid outlet of the sodium hypochlorite reactor (500) is connected with a finished product tank (700) through a pipeline, a ninth delivery pump (703) and an eighth backpressure valve (702) are arranged on the pipeline between the finished product tank (700) and the sodium chlorate reactor (500), and the eighth backpressure valve (702) is close to the sodium chlorate reactor (500) compared with the ninth delivery pump (703).
8. The apparatus according to claim 7, wherein the apparatus comprises: a first densimeter (103) is arranged on the first reaction kettle (100), and the first densimeter (103) is linked with a first back pressure valve (102) on line; a first online thermometer (105) is arranged on a pipeline between the water outlet of the first reaction kettle (100) and the inlet (106) of the first jacketed heat exchanger; a second densimeter (205) is arranged on the second reaction kettle (200), and the second densimeter (205) is interlocked with a fifth back pressure valve (2010) in an online manner; a second online thermometer (209) is arranged on a pipeline between the water outlet of the second reaction kettle (200) and the inlet (206) of the second jacketed heat exchanger.
9. The apparatus according to claim 7, wherein the apparatus comprises: a PH meter (501) is connected to the sodium hypochlorite reactor (500); the bottom of the sodium hypochlorite reactor (500) is connected with a pressure gauge (504), and the pressure gauge (504) is linked with an inert gas valve (503) in an online manner; a third online thermometer (509) is connected to a water outlet of the sodium hypochlorite reactor (500), and the third online thermometer (509) is linked with a cooling water valve (508) in an online manner; an oxidation-reduction potential analyzer (701) is arranged on a pipeline between the ninth backpressure valve (702) and the sodium chlorate reactor (500), and the oxidation-reduction potential analyzer (701) is linked with the chlorine valve (601) in an online mode.
10. The apparatus according to claim 7, wherein the apparatus comprises: the atomizer (30) comprises a liquid inlet pipe (301), the liquid inlet end of the liquid inlet pipe (301) is connected with the static mixer (400) through a pipeline, the liquid outlet end of the liquid inlet pipe (301) is rotatably connected with a horizontal liquid inlet pipe (302), a plurality of liquid inlet branch pipes (303) are arranged on the peripheral surface of the horizontal liquid inlet pipe (302), a plurality of atomizing nozzles (304) are arranged at the top and the bottom of each liquid inlet branch pipe (303), and electromagnetic valves are arranged on the atomizing nozzles (304);
the sodium hypochlorite reactor is characterized by further comprising a driving motor (305), wherein the driving motor (305) is arranged on the outer wall surface of the sodium hypochlorite reactor (500), a rotary disc (306) is arranged at the driving end of the driving motor (305), the rotary disc (306) is positioned inside the sodium hypochlorite reactor (500), and the rotary disc (306) is connected with one end of the liquid inlet transverse pipe (302);
the gas distributor (34) comprises a gas inlet pipe (341), the gas inlet end of the gas inlet pipe (341) is connected with a gas buffer tank (600) through a pipeline, the gas outlet end of the gas inlet pipe (341) is connected with a transverse gas inlet pipe (342), the transverse gas inlet pipe (342) is positioned inside a sodium hypochlorite reactor (500), a plurality of gas inlet branch pipes (343) are arranged on the outer peripheral surface of the transverse gas inlet pipe (342), and the tops of the gas inlet branch pipes (343) are communicated with a plurality of gas nozzles (344);
still include one-level reposition of redundant personnel subassembly (345), one-level reposition of redundant personnel subassembly (345) are located air nozzle (344) upside, the upside of one-level reposition of redundant personnel subassembly (345) is equipped with second grade reposition of redundant personnel subassembly (346).
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| CN202211599831.6A CN115872362B (en) | 2022-12-12 | 2022-12-12 | Method for continuously preparing high-purity sodium hypochlorite |
| CN202311360335.XA CN117658076A (en) | 2022-12-12 | 2022-12-12 | Equipment for continuously preparing high-purity sodium hypochlorite |
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| CN117742278A (en) * | 2024-02-07 | 2024-03-22 | 四川飞洁科技发展有限公司 | Intelligent monitoring and management method and system for sodium hypochlorite production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104743513A (en) * | 2013-12-26 | 2015-07-01 | 昭和电工株式会社 | Production process of aqueous sodium hypochlorite solution |
| CN216837139U (en) * | 2022-03-10 | 2022-06-28 | 广西德陆科技有限公司 | High-efficient continuous controllable sodium hypochlorite apparatus for producing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104743513A (en) * | 2013-12-26 | 2015-07-01 | 昭和电工株式会社 | Production process of aqueous sodium hypochlorite solution |
| CN216837139U (en) * | 2022-03-10 | 2022-06-28 | 广西德陆科技有限公司 | High-efficient continuous controllable sodium hypochlorite apparatus for producing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117742278A (en) * | 2024-02-07 | 2024-03-22 | 四川飞洁科技发展有限公司 | Intelligent monitoring and management method and system for sodium hypochlorite production process |
| CN117742278B (en) * | 2024-02-07 | 2024-04-30 | 四川飞洁科技发展有限公司 | Intelligent monitoring and management method and system for sodium hypochlorite production process |
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| CN117658076A (en) | 2024-03-08 |
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