CN1062715C - Method for preparing chlorine dioxide and its generation equipment - Google Patents
Method for preparing chlorine dioxide and its generation equipment Download PDFInfo
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- CN1062715C CN1062715C CN98101677A CN98101677A CN1062715C CN 1062715 C CN1062715 C CN 1062715C CN 98101677 A CN98101677 A CN 98101677A CN 98101677 A CN98101677 A CN 98101677A CN 1062715 C CN1062715 C CN 1062715C
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Abstract
The present invention discloses a method for preparing chlorine dioxide disinfectant and a generation device thereof. The preparing method of the present invention comprises the steps that sodium chlorate water solution (540 g/l) and 31% of hydrochloric acid in volume ratio of 1: 1 are added to a first negative pressure reactor and a second negative pressure reactor for reacting on each other while hot air is pumped into reaction liquid by air inlet pipes, and the temperature of the first reactor and the second reactor are respectively 40 DEG C and 70 DEG C. The device of the present invention comprises a feeding device, two-stage reaction chambers connected in series, an external heater, the air inlet pipes communicated with each reaction chamber, an air collecting chamber, a heater of the air collecting chamber, a water blaster and a safety device. The method of the present invention has the advantages of high conversion rate and safe operation of the device; the disinfectant is suitable for disinfecting drinking water, hospital sewage, swimming poll water and industrial waste water.
Description
The inventionrelates to a preparation method of chlorine oxide and generating equipment thereof, in particular to a preparation method of a chlorine dioxide disinfectant and generating equipment thereof.
Chlorine dioxide (ClO) is known2) Is an oxidant, a deodorizer, and a bleaching agent. At present, the environmental protection is increasingly valued, chlorine dioxide only has the oxidation effect and does not have the chlorination effect in water, and the characteristic not only leads the dioxygenChlorine dioxide is used as a disinfectant for hospital sewage, cyanide and paper-making wastewater, swimming pool water and the like, and also as a disinfectant for drinking water, particularly when drinking water is severely polluted by ammonia and phenol or chlorine disinfection is difficult, showing the unique feature of chlorine dioxide as a disinfectant.
Chlorine is also a bleaching, disinfecting agent. Can be used for sterilizing drinking water, but the chlorine can form chloralkane during the sterilization, and has carcinogenic effect, so the use of the chlorine as the disinfectant of the drinking water is influenced. However, in some cases, such as the disinfection of swimming pool water, chlorine may be used as the disinfectant.
Currently, there are two general types of methods for producing chlorine dioxide. One type is electrolytic. The method adopts sodium chloride as electrolyte, and puts the electrolyte into an electrolytic tank with a diaphragm for electrolysis to generate mixed gas of chlorine dioxide, chlorine, ozone and hydrogen peroxide, and byproducts are sodium hydroxide and hydrogen. The method has the disadvantages of large investment, large raw material consumption and high power consumption, and the diaphragm needs to be cleaned and replaced frequently. The proportion of chlorine dioxide is less than 30 percent, and the yield is limited. Another type of process is a chemical process. Chemical processes are divided into two cases, one of which is an industrial implementation process, which can be represented by US 3844456. The method disclosed by the patent has the advantages of high investment cost, large equipment volume and more accessory equipment, is only suitable for large-scale industrial application, and is not suitable for commercial and small-batch production. Another situation is that of commercial generators, which are currently in existence in the country. According to the introduction of CN1114632A, the method of the patent application adopts sodium chlorate as a raw material, sodium chloride as a reducing agent and sulfuric acid as an acidifying agent, and the reaction is carried out in a single-stage reaction chamber at normal temperature and high acidity, the reaction is not carried out completely, and the reaction residual liquid needs to be neutralized for use. In addition, the reaction is carried out by the negative pressure generated by the circulation pump, and if the circulation pump fails, explosion due to the excessively high concentration of chlorine dioxide is likely to occur. Although the charging pump is added to make up the facility to blow chlorine dioxide and chlorine out of the generator, the air is heavily filled with chlorine dioxide and chlorine, which also causes injury to personnel and corrosion of peripheral equipment.
Therefore, the present inventors have conducted a great deal of research and completed the invention of preparing a chlorine dioxide disinfectant by using sodium chloride as a raw material and hydrochloric acid as an acidifying agent to carry out a thorough reaction in a multi-stage reaction system in which the reaction temperature is raised step by step under negative pressure while blowing air into the reaction solution. The invention can overcome the defects in the prior art.
The invention aims to provide a preparation method of a chlorine dioxide disinfectant.
It is a further object of the present invention to provide an apparatus suitable for producing the chlorine dioxide disinfectant described above.
In order to complete the task of the invention, the following technical scheme is adopted.
A method of producing a chlorine dioxide disinfectant, the method comprising the steps of:
(1) preparing 540g/l aqueous solution of sodium chlorate;
(2) the sodium chlorate aqueous solution and 31 percent hydrochloric acid enter a first-stage reaction chamber and a second-stage reaction chamber with negative pressure and temperature of 40 ℃ and 70 ℃ respectively according to the volume ratio of 1: 1 for reaction;
(3) blowing air heated by a heating box into the reaction liquid in the two reaction chambers respectively;
(4) the generated chlorine dioxide, chlorine and reaction liquid enter a gas collection chamber at the temperature of 95 ℃; and
(5) and recovering the mixed gas and the reaction liquid which reacts completely through a water ejector to prepare the chlorine dioxide disinfectant.
The chlorine dioxide prepared by the invention is obtained by taking sodium chlorate as a raw material and hydrochloric acid as an acidifier through chemical reaction, and the two raw materials can start to react as expressed by the following reaction formula after being mixed in a reaction chamber:
in order to make the reaction proceed to the bottom as far as possible, the invention adopts a multi-stage reaction chamber system. Firstly, the material is sent into a first-stage reaction chamber and then enters a second-stage reaction chamber and a gas collecting chamber, and the temperature of each chamber is gradually increased, so that the reaction equilibrium moves towards the direction of forming reaction products. In addition, the reaction of sodium chlorate and hydrochloric acid tends to be more complete by blowing air into the reaction system so that the generated chlorine dioxide and chlorine gas rapidly leave the reaction system.
In order to better control the whole reaction, the temperature of each heating box is usually varied within + -2 deg.C.
The heating of the closed reaction chamber is carried out by means of a heating box placed outside the reaction chamber. The heating box can be made into a water bath, and is heated by a conventional controllable electric heating method to heat the reaction chamber and the reaction liquid in the reaction chamber to a preset temperature.
In order to ensure the temperature of each part of the reaction chamber is consistent, the invention firstly heats the reaction chamber from the outside through the heating box, and secondly heats the reaction solution in the reaction chamber to the air with the same temperature as the reaction chamber through the air inlet pipe arranged in the corresponding heating box. By doing so, the temperature of the reaction system can be ensured to be uniform, and the chlorine dioxide and the chlorine gas generated in the stripping reaction liquid can be simultaneously played.
The air inlet pipe can blow air with the same temperature as the reaction chamber into the reaction chamber because the air inlet pipe for introducing air is heated by the first-stage or the first-stage and the second-stage heating boxes. The number of heating stages depends on the reaction chamber into which the inlet pipe is intended to enter.
The mixed gas of chlorine dioxide and chlorine blown by air is collected by the air collecting chamber. The reaction liquid flows into the gas collecting chamber, reacts quickly and thoroughly at the high temperature of 95 ℃, is pumped out together with the mixed gas through the water ejector, and can be directly sent to a user to be used as a disinfectant.
The invention can control the ratio of the reaction materials accurately, so that the reactants can react under the condition that the pH value is 6-7.
The equipment for preparing chlorine dioxide disinfectant includes feeding device formed from two raw material proportioning tanks and two quantitative feeders, two-stage reaction chambers connected in series, heating tank and air inlet pipe, gas-collecting chamber and heating tank, water injector and safety device formed from pressure gauge, neutralization tank, electromagnetic valve and explosion-proof valve.
The quantitative feeder is used for controlling the adding amount of the two raw materials. Any device that can be used to quantitatively control the flow of a liquid can be used with the present invention. For example, a general-purpose metering pump, a titrator for counting the number of liquid drops in seconds, a flow meter, and the like.
The negative pressure in the apparatus of the invention is provided by pressurized water. If the pressure of the pressurized water becomes small or absent, the reaction will not proceed. A large amount of chlorine dioxide and chlorine gas exist in the reaction liquid, and if the chlorine dioxide and the chlorine gas are not treated in time, the chlorine dioxide and the chlorine gas are harmful. The known generating device blows gas to the reaction liquid through a gas pump in the case, and the method certainly blows chlorine dioxide and chlorine gas to the space, and because the chlorine dioxide generating device is generally placed in a room, a large amount of chlorine dioxide and chlorine gas in the air is inevitably generated, and operators and peripheral equipment in the field are harmed. Based on the consideration, the equipment of the invention is additionally provided with a pressure gauge with a sensor on the jet device, and simultaneously, the bottom parts of the first-stage reaction chamber and the second-stage reaction chamber are additionally provided with discharge pipes with electromagnetic valves, under the condition of low water pressure or no pressure, the pressure gauge drives the electromagnetic valves to be opened, the reaction liquid in the reaction chambers is rapidly discharged into a reaction liquid neutralization tank, and the sodium hydroxide in the tank is utilized to absorb chlorine dioxide and chlorine in the reaction liquid and simultaneously give an alarm. If the electromagnetic valve fails, the pressure in the reaction chamber can open the explosion-proof valve when reaching a certain pressure, so that the mixed gas is discharged to the outside. The explosion-proof valve is arranged on the mixed gas communicating pipe.
Compared with the prior art, the preparation method of the chlorine dioxide disinfectant and the generating equipment thereof have the following remarkable advantages:
1. the reaction is carried out by utilizing two stages of reaction chambers at gradually increased reaction temperature, so that the reaction has higher reaction speed, meanwhile, the temperature of the gas collection chamber is close to the boiling point, the reaction can be more complete, and the reaction conversion rate can be increased to more than 95%;
2. the raw materials and the acidifying agent are properly proportioned, so that the reaction product has a pH value between 6 and 7, the extraction of mixed gas and the reaction liquid complete in reaction are completed simultaneously, and the mixed gas can be directly sent to a user to be used as a disinfectant without further treatment:
3. only two raw materials are used, so that the cost is reduced and the operation procedure is simplified;
4. the water ejector directly uses tap water as a pressure source, so that the inconvenience caused by using a pump is avoided, and meanwhile, an explosion-proof valve and an electromagnetic valve are added, so that the equipment is operated within a safe range at any time.
5. The equipment for preparing the chlorine dioxide disinfectant has the advantages of simple structure, convenient operation, safe and reliable operation, less equipment investment and low operation cost, is suitable for commercial dispersed users, and can be used on the spot in small batches.
Fig. 1 is a schematic diagram of an apparatus for producing chlorine dioxide disinfectant in accordance with the present invention.
In the figure, the generating equipment comprises raw material proportioning boxes 1 and 2, a first-stage reaction chamber 3, a second-stage reaction chamber 4, a gas collecting chamber 5, a reaction liquid neutralizing tank 6, a water ejector 7, a heating box 8 of the first-stage reaction chamber 3, a heating box 9 of the second-stage reaction chamber 4, a heating box 10 of the gas collecting chamber 5, quantitative feeders 11 and 12, an air inlet pipe 13, a reaction liquid connecting pipe 14 between the first-stage reaction chamber 3 and the second-stage reaction chamber 4, a reaction liquid connecting pipe 15 between the second-stage reaction chamber 4 and the gas collecting chamber 5, a reaction chamber low-level discharge electromagnetic valve 16, a mixed disinfectant suction pipe 17, an explosion-proof valve 18, a pressure gauge 19 with a sensor, a mixed gas communicating pipe 20 between the first-stage reaction chamber 3 and the second-stage reaction chamber 4 and the gas collecting chamber 5, feed pipes 21 and 22, a water injection valve 23a and a drain valve 23b of the heating box 8 outside the first-stage reaction chamber 3, and water injection valves 24a and 24b, a water injection valve 25a and a water discharge valve 25b of the heating box 10 outside the gas collection chamber 5, and a reaction chamber low-level discharge manual valve 26.
In the attached drawing, each stage of reaction chamber, the gas collection chamber, the air inlet pipe, the reaction liquid connecting pipe and the mixed gas communicating pipe are made of titanium. The corresponding heating boxes of the reaction chambers and the gas collecting chambers at all levels are made of temperature-resistant materials, such as organic glass, polytetrafluoroethylene and the like.
The present invention will be described in further detail with reference to the accompanying drawings.
540g/l of prepared sodium chlorate solution and 31 percent of hydrochloric acid are respectively added into the raw material proportioning boxes 1 and 2, meanwhile, a proper amount of clear water with the temperature of 40 ℃ is added into the first-stage reaction chamber 3, a proper amount of clear water with the temperature of 70 ℃ is added into the second-stage reaction chamber 4, the temperature of the first-stage reaction chamber heating box 8 is controlled to be 40 +/-2 ℃, the temperature of the second-stage reaction chamber heating box 9 is controlled to be 70 +/-2 ℃, and the temperature of the gas collection chamber heating box 10 is controlled to be more than 95 ℃. The pressure water is turned on to operate the water ejector 7, and the pressure gauge 19 is displayed above 0.2MPA, at which time the whole reaction apparatus exhibits a negative pressure condition. Under the condition of negative pressure, the quantitative feeders 11 and 12 start feeding the first-stage reaction chamber, the feeding volume ratio of 11 and 12 is adjusted to be 1: 1, and feeding is carried out according to the volume ratio of 3L/h. The air inlet pipe 13 is adjusted to maximize the air intake amount while ensuring normal feeding. At this time, the first-stage reaction is started, the produced chlorine dioxide and chlorine gas mixture is pumped into the gas collection chamber through the communicating pipe 20, meanwhile, the air inlet pipe 13a is communicated to the bottom of the first-stage reaction chamber, 40 ℃ air is blown into the reaction liquid, the chlorine dioxide and the chlorine gas in the reaction liquid are heated and blown out, and the gas mixture is also pumped into the gas collection chamber 5 through the communicating pipe 20. The reaction liquid enters the second-stage reaction chamber 4 through the connecting pipe 14, reacts rapidly at a high temperature of 70 ℃, the generated chlorine dioxide and chlorine are pumped into the gas collection chamber through the communicating pipe 20, meanwhile, the air inlet pipe 13b is communicated to the bottom of the second-stage reaction chamber, and 70 ℃ air is blown into the reaction liquid. The generated and bubbled chlorine dioxide and chlorine gas are pumped into the plenum 5 through the communicating tube 20. The reaction liquid enters the gas collection chamber 5 through the connecting pipe 15, because the temperature of the gas collection chamber is close to the boiling point, the reactant which is not completely reacted in the reaction liquid instantaneously reacts at the temperature, and at the moment, the mixed gas and the reaction liquid which completely reacts are pumped out together through the water injector to be directly sent to a user as a disinfectant. The chlorine dioxide content by sampling analysis was 1658mg/L, the chlorine content was 872mg/L, and the jet flow rate was 600L/h. The yieldof chlorine dioxide is 995g/h, the yield of chlorine is 523g/h, and the conversion rate of the chemical reaction is 97%.
Claims (3)
1. A method for preparing a chlorine dioxide disinfectant, characterized in that the method comprises the steps of:
(1) preparing 540g/l aqueous solution of sodium chlorate;
(2) the sodium chlorate aqueous solution and 31 percent hydrochloric acid enter a first-stage reaction chamber and a second-stage reaction chamber with negative pressure and temperature of 40 ℃ and 70 ℃ respectively according to the volume ratio of 1: 1 for reaction;
(3) blowing air heated by a heating box into the reaction liquid in the two reaction chambers respectively;
(4) the generated chlorine dioxide, chlorine and reaction liquid enter a gas collection chamber at the temperature of 95 ℃; and
(5) and recovering the mixed gas and the reaction liquid which reacts completely through a water ejector to prepare the chlorine dioxide disinfectant.
2. An apparatus for producing a chlorine dioxide disinfectant as set forth in claim 1, characterized in that the apparatus comprises:
the device comprises a feeding device consisting of two raw material proportioning tanks and two quantitative feeders, two stages of reaction chambers connected in series, a corresponding heating tank and an air inlet pipe thereof, an air collection chamber and a heating tank thereof, a water ejector and a safety device consisting of a pressure gauge, a neutralization tank, an electromagnetic valve and an explosion-proof valve, wherein the air inlet pipe enters the liquid level in the corresponding reaction chamber after being heated by the corresponding heating tank, the air collection chamber is connected with the reaction chambers at all stages through a mixed gas communicating pipe, the second stage of reaction chamber is connected with the air collection chamber through a reaction liquid connecting pipe, and the air collection chamber is connected with the water ejector through a mixed disinfectant suction pipe.
3. The apparatus of claim 2, wherein the reaction chamber, the gas collection chamber, the air inlet pipe, the reaction liquid connection pipe, and the mixed gas connection pipe are made of titanium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101677A CN1062715C (en) | 1998-04-30 | 1998-04-30 | Method for preparing chlorine dioxide and its generation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98101677A CN1062715C (en) | 1998-04-30 | 1998-04-30 | Method for preparing chlorine dioxide and its generation equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1212839A CN1212839A (en) | 1999-04-07 |
| CN1062715C true CN1062715C (en) | 2001-03-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN98101677A Expired - Fee Related CN1062715C (en) | 1998-04-30 | 1998-04-30 | Method for preparing chlorine dioxide and its generation equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100350843C (en) * | 2004-10-26 | 2007-11-28 | 淄博华润科贸有限责任公司 | Device for preparing pure chlorine dioxide disinfection liquid |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429162C (en) * | 2004-05-24 | 2008-10-29 | 大连雅希科技有限公司 | Physical and biological and chemical treatment system for water cycle in swimming pool or natatorium |
| CN101891153A (en) * | 2010-07-16 | 2010-11-24 | 山东大学 | Chlorine dioxide compound disinfectant generator and use method thereof |
| CN109205563A (en) * | 2017-07-05 | 2019-01-15 | 冠亚腾达（北京）科技有限公司 | A kind of chlorine dioxide generator with reaction of high order and raffinate separator |
| CN107617412A (en) * | 2017-08-31 | 2018-01-23 | 四川齐力绿源水处理科技有限公司 | A kind of chlorine dioxide preparation apparatus and preparation method |
| CN109607482A (en) * | 2018-12-24 | 2019-04-12 | 鲍立锋 | A kind of easily-controllable plural serial stage gas generating unit and chlorine dioxide generating device |
| CN112741109A (en) * | 2021-02-22 | 2021-05-04 | 卫溯源(北京)生物医药科技有限公司 | Preparation method of chlorine dioxide sterilizing gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5637203A (en) * | 1979-08-28 | 1981-04-10 | Erco Ind Ltd | Continuous chlorine dioxide manufacture |
| EP0095199A1 (en) * | 1982-05-18 | 1983-11-30 | Metallgesellschaft Ag | Reactor for preparing chlorine dioxide |
| CN1040182A (en) * | 1988-08-10 | 1990-03-07 | 田纳科加拿大分公司 | The preparation of dioxide peroxide |
-
1998
- 1998-04-30 CN CN98101677A patent/CN1062715C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5637203A (en) * | 1979-08-28 | 1981-04-10 | Erco Ind Ltd | Continuous chlorine dioxide manufacture |
| EP0095199A1 (en) * | 1982-05-18 | 1983-11-30 | Metallgesellschaft Ag | Reactor for preparing chlorine dioxide |
| CN1040182A (en) * | 1988-08-10 | 1990-03-07 | 田纳科加拿大分公司 | The preparation of dioxide peroxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100350843C (en) * | 2004-10-26 | 2007-11-28 | 淄博华润科贸有限责任公司 | Device for preparing pure chlorine dioxide disinfection liquid |
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| Publication number | Publication date |
|---|---|
| CN1212839A (en) | 1999-04-07 |
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Owner name: BEIJING CITY BANGDA NEW TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: SIJIA ENVIRONMENTAL EGINEERING CO., LTD., BEIJING Effective date: 20060825 |
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Effective date of registration: 20060825 Address after: 100091 Beijing city Haidian District Guajiatun Department of education No. 40 Patentee after: Bangda New Technology Co., Beijing Address before: 100011, No. 18, Delhi North Street, Beijing, Dongcheng District Patentee before: Sijia Environmental Egineering Co., Ltd., Beijing |
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