CN1206171C - Industrial composite sulfur dioxide preparation method - Google Patents
Industrial composite sulfur dioxide preparation method Download PDFInfo
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- CN1206171C CN1206171C CN 03111901 CN03111901A CN1206171C CN 1206171 C CN1206171 C CN 1206171C CN 03111901 CN03111901 CN 03111901 CN 03111901 A CN03111901 A CN 03111901A CN 1206171 C CN1206171 C CN 1206171C
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Abstract
The present invention discloses a preparation method for industrial compound chlorine dioxide, which mainly comprises: sodium chlorate is taken as an oxidant; sodium chloride is taken as a reducing agent; a negative pressure aeration technology is adopted; continuous feeding to reactors is adopted; a reaction is carried out in a sulphuric acid medium; the liquid phase parts of the three reactors orderly flow in series in a lower overflow mode to generate compound chlorine dioxide gas which is carried out by a hydraulic ejector and sent to the water body to be treated. Compared with the technical skill of the same class, the present invention has the characteristics of high production capacity, simple operation, low production cost, high feed stock conversion, high security and stability, no pollution-carrying waste material, etc.; the product can be used for decolorization of industrial wastewater, sterilization of large-sized water works, sewage treatment plants and marine industry circulating water and other processes.
Description
Technical Field
The invention relates toAnd the technical field of inorganic chemical industry, in particular to an industrial preparation of composite chlorine dioxide (ClO)2And Cl2) The method of (1).
Background
Chlorine dioxide is a new generation of internationally recognized broad-spectrum strong sterilizing disinfectant, high-efficiency oxidant and high-quality bleaching agent, is listed as an AI-level high-efficiency safe disinfectant by the United nations World Health Organization (WHO), and can be widely applied to sterilization in various fields. The liquid chlorine not only has lower sterilizing effect than chlorine dioxide, but also is unsafe to use and inconvenient to manage, and the liquid chlorine is easy to generate a large amount of organic halide (such as trichloromethane) in water to cause secondary pollution of water, particularly drinking water, and potential harm is caused to the health of human bodies. Chlorine dioxide has gradually replaced liquid chlorine in these areas with its unique advantages. At present, chlorine dioxide is also widely used internationally for disinfection of large-scale water works and sterilization, decoloration and deodorization treatment of municipal sewage treatment plants. Experiments show that the chlorine and the chlorine dioxide have synergistic sterilization and decoloration effects, so that the effect is more ideal. Therefore, the composite chlorine dioxide is more suitable for the application in the fields. However, the existing preparation methods in China cannot meet the requirements of the fields.
The preparation method of the composite chlorine dioxide mainly comprises a chemical method and an electrolytic method. The main raw material used in the chemical process is sodium chlorate. The sodium chlorate method is classified into methods such as R2, R3, R3H, R5, R6, and R7 depending on the reducing agent. However, the main problem in the aspect of preparing composite chlorine dioxide in China at present is that the preparation capacity is small, and the process technology cannot reach the corresponding production scale, so that the use of the composite chlorine dioxide is influenced. Chinese patent ZL93111202.8 and Chinese patent ZL97233737.7 disclose a novel technology for producing a negative-pressure aeration chlorine dioxide generator, and the technology uses sodium chlorate as an oxidant and hydrochloric acid as a reducing agent to produce a composite disinfectant of chlorine dioxide and chlorine, but the preparation method belongs to small-sized composite chlorine dioxide generating equipment and a production process thereof, and is a binary production formula, and the preparation method has the main defects of small production scale and high cost, and is difficult to meet the requirement of enterprises with large treatment capacity on composite chlorine dioxide at present.
Disclosure of Invention
The invention aims to provide an industrial composite chlorine dioxide preparation method with high yield, high raw material conversion rate and low production cost aiming at the defects of the existing composite chlorine dioxide preparation method.
The technical scheme adopted for realizing the invention is as follows: sodium chlorate is used as oxidant, sodium chloride is used as reducer, and the reaction is carried out in sulfuric acid medium to generate composite chlorine dioxide (ClO)2And Cl2) The reaction process is as follows:
adopting a negative pressure aeration method, generating negative pressure by a hydraulic ejector, reacting in three reactors, continuously adding a mixed aqueous solution of sodium chlorate with the concentration of about 26.2 percent and sodium chloride with the concentration of about 14.2 percent and concentrated sulfuric acid into a first-stage reactor according to the proportion of 1: 0.50-0.55: 2.3-2.5, wherein the mass percent of sulfuric acid in a reaction medium is 38-40.5 percent, the temperature of the reactors is increased from 45 ℃ to 71 ℃, and the three reactors flow in series in a manner of overflowing below liquid phase parts in the three reactors in sequence; compressed air is introduced from an aeration disc at the lower part of reaction liquid of each reactor, and the air enters from the upper part of the primary reactor; composite chlorine dioxide gas (ClO) generated in three-reactor reaction liquid2And Cl2) The introduced compressed air and the upper air are diluted and then taken out, and the generated composite chlorine dioxide gas is brought into the water body to be treated by the hydraulic ejector; the molar ratio of the sodium chlorate to the sodium chloride in the mixed aqueous solution is 1: 0.93-1.0.
Compared with the prior art, the invention has the main advantages of large production capacity, continuous production, raw material conversion rate of over 90 percent, simple operation, stable operation, safety and reliability.
Drawings
The process flow of the invention is explained in detail below with reference to the drawings and examples:
FIG. 1 is a schematic process flow diagram of the preparation method of the present invention.
In the figure, 1, composite chlorine dioxide gas, 2, a sulfuric acid feeding pipe, 3, a mixed liquid feeding pipe, 4, a compressed air inlet pipe, 5, an upper air inlet, 6, a first-stage reactor, 7, a second-stage reactor, 8, a third-stage reactor, 9, a hydraulic ejector, 10, a water treatment body, 11, a centrifugal pump and 12, and reaction residual liquid.
Example 1: preparing 42.1kg/h composite chlorine dioxide
A negative pressure aeration method is adopted, a hydraulic ejector 9 generates negative pressure, the primary reactor 6, the secondary reactor 7 and the tertiary reactor 8 all run under the condition of negative pressure, and the system pressure is 752 mmHg. The method comprises the steps of adding a mixed solution of sodium chlorate and sodium chloride mixed according to a molar ratio of 1: 0.988 into a primary reactor 6 through a mixed solution feeding pipe 3, simultaneously adding a concentrated sulfuric acid solution into the primary reactor 6 through a sulfuric acid feeding pipe 2, adding the concentrated sulfuric acid solution and the concentrated sulfuric acid solution into the primary reactor 6 respectively according to feeding amounts of 178l/h and 85.0l/h, wherein the mass percent of sulfuric acid in a reaction medium is 39.8%, the reaction temperature of the reactors is increased from 46 ℃ to 71 ℃, compressed air is introduced from an aeration disc at the lower part of reaction liquid of each reactor through a compressed air inlet pipe 4, air is introduced from an upper air inlet 5 at the upper part of the primary reactor, liquid phase parts of the reactors sequentially flow in series in the form of overflow, and composite chlorine dioxide gas 1 generated in the reactors is mixed with a treatment water body 10 output by. The reaction raffinate 12 overflows from the bottom of the three-stage reactor.
Example 2: preparing 42.0kg/h composite chlorine dioxide
The negative pressure aeration method is adopted, and the system pressure is 753 mmHg. The mixed solution of sodium chlorate and sodium chloride mixed according to the molar ratio of 1: 0.97 is added into a first-stage reactor 6, simultaneously concentrated sulfuric acid solution is also added into the first-stage reactor, the sodium chlorate and the sodium chloride are respectively added according to the feeding amount of 178l/h and 84.5l/h, the mass percent of sulfuric acid in a reaction medium is 38.5 percent, the reaction temperature of the reactor is increased from 45 ℃ to 70 ℃, and the liquid phase parts of the reactors flow in series in the following overflow mode. The composite chlorine dioxide gas generated in the reactor is mixed with the water body to be treated in the hydraulic ejector. And overflowing the reaction residual liquid from the bottom of the three-stage reactor.
Example 3: preparing 42.0kg/h composite chlorine dioxide
The negative pressure aeration method is adopted, and the system pressure is 753 mmHg. The mixed solution of sodium chlorate and sodium chloride mixed according to the molar ratio of 1: 0.98 is added into a first-stage reactor, simultaneously concentrated sulfuric acid solution is also added into the first-stage reactor, the sodium chlorate and the sodium chloride are respectively added according to the feeding amount of 178l/h and 85.0l/h, the mass percent of sulfuric acid in a reaction medium is 39.4 percent, the reaction temperature of the reactor is increased from 44.5 ℃ to 70 ℃, the liquid phase part of the reactor flows in series in sequence in the following overflowmode, and the composite chlorine dioxide gas generated in the reactor is mixed with a water body to be treated in a hydraulic ejector. And overflowing the reaction residual liquid from the bottom of the three-stage reactor.
Claims (1)
1. The industrial composite chlorine dioxide preparing process with sodium chlorate as oxidant and sodium chloride as reductant and through reaction in sulfuric acid medium features that: adopting a negative pressure aeration method, reacting in three reactors (6, 7 and 8) under the condition of 740-; compressed air (4) is introduced from an aeration disc at the lower part of reaction liquid in each reactor, and air (5) enters from the upper part of a primary reactor (6); the composite chlorine dioxide gas generated in the reaction liquid of the three reactors (6, 7, 8) is diluted by the introduced compressed air (4) and the upper intake air (5) and then is taken out, and the generated composite chlorine dioxide gas (1) is taken into the water body to be treated by a hydraulic ejector (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03111901 CN1206171C (en) | 2003-02-25 | 2003-02-25 | Industrial composite sulfur dioxide preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03111901 CN1206171C (en) | 2003-02-25 | 2003-02-25 | Industrial composite sulfur dioxide preparation method |
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| Publication Number | Publication Date |
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| CN1438183A CN1438183A (en) | 2003-08-27 |
| CN1206171C true CN1206171C (en) | 2005-06-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 03111901 Expired - Fee Related CN1206171C (en) | 2003-02-25 | 2003-02-25 | Industrial composite sulfur dioxide preparation method |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754827B (en) * | 2014-01-13 | 2015-09-16 | 深圳欧泰华工程设备有限公司 | A kind of preparation method and specific equipment thereof mixing dioxide peroxide |
| CN115010093A (en) * | 2022-07-18 | 2022-09-06 | 宁夏艾克坚机械设备有限公司 | Gaseous chlorine dioxide continuous production system and production method |
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