CN1235913C - Production for stable chlorinedioxide solution - Google Patents
Production for stable chlorinedioxide solution Download PDFInfo
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- CN1235913C CN1235913C CN 03121405 CN03121405A CN1235913C CN 1235913 C CN1235913 C CN 1235913C CN 03121405 CN03121405 CN 03121405 CN 03121405 A CN03121405 A CN 03121405A CN 1235913 C CN1235913 C CN 1235913C
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- chlorine dioxide
- hydrogen peroxide
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Abstract
The present invention relates to a method for producing stable chlorine dioxide solution. Hydrogen peroxide is used as a reducing agent, alkali metal chlorate is reduced in sulfuric acid medium for generating chlorine dioxide, in the reaction, a composite catalyst which is proportionally composed of tetrasodium pyrophosphate, 2-hydroxyphosphonoacetic acid and urea is used, the composite reaction liquid which is proportionally composed of the composite catalyst, hydrogen peroxide and alkali metal chlorate reacts with sulfuric acid solution in a multi-step reactor, and high-purity chlorine dioxide gas is generated; then, the chlorine dioxide gas is led into a combined absorption tower to carry out stable absorption treatment together with a composite stable absorption liquid, and stable chlorine dioxide solution is generated. The production method has the advantages of high absorption rate obtainment, high chlorine dioxide solution stability, high productivity, great cost reduction, safe operation process, stable and reliable operation and continuous automatic production and is suitable for industrialization.
Description
Technical field
The present invention relates to a kind of production method of stable ClO 2 solution.
Background technology
ClO 2 solution is as a kind of efficient, wide spectrum, quick, nontoxic disinfection sanitizer, reodorant, mould inhibitor, food insurance agent, water quality and air purifying preparation and excellent association with pulp bleaching agent, obtain extensive studies in the world in recent years scope and use broad market prospect.Domestic leading technology now is Textone conversion method and methyl alcohol reduction method at present, the raw material of Textone conversion method and power consumption exceed external mean level (ML) more than 3 times, the methyl alcohol reduction method also exists problems such as methanol content easily exceeds standard in production equipment complexity, reflection temperature height, the final product, has restricted applying of stabilized chlorine chlorine solution.
Chinese patent CN1097716A discloses a kind of production method of stability chlorine dioxide, makes reductive agent with hydrogen peroxide, and the reduction sodium chlorate produces dioxide peroxide in sulfuric acid medium, imports to absorb in the sodium carbonate solution to make ClO 2 solution again.The shortcoming that aforementioned production method exists is, three kinds of raw material while dropwise reactions in the single-stage retort, produce local superheating, reaction insufficient, easily produce explosion phenomenon, the difficult accurately control of technological operation waits speed, specific absorption, the purity that all can cause chlorine dioxide reaction to descend, the difficult control of reaction process, be difficult to production high density, highly purified stable ClO 2 solution, chlorine dioxide content is 2.0～2.5% usually, and purity of chlorine dioxide is lower.
Summary of the invention
The object of the present invention is to provide a kind of production method of stable ClO 2 solution of new efficient, high-purity, high density.Utilize the ClO 2 solution of present method preparation that its cost is significantly descended, product concentration, purity obviously improve, and make production process safety and steady, easy to operate, efficient, environmental protection.
The present invention is achieved by following technical proposals:
A kind of production method of stable ClO 2 solution adopts hydrogen peroxide to make reductive agent, and dioxide peroxide takes place the reducine metal chlorate in sulfuric acid medium, and it may further comprise the steps:
1. form composite catalyst by trisodium phosphate, 2-HPAA, urea by proportioning, weight ratio is 1: 0.1～0.5: 0.5～1.
2. the alkaline metal chlorate is used the softening water stirring and dissolving in material-compound tank, add superoxol (30%) and composite catalyst by proportioning, continue down to stir to make to dissolve fully in normal temperature as complex reaction liquid, complex reaction liquid proportioning, promptly the weight proportion of alkaline metal chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.5～0.8: 0.4～1: 0.006～0.01.
3. complex reaction liquid and sulphuric acid soln 1: 1 by weight ratio～1.5, enter in many graduated responses device through volume pump and to react, produce chlorine dioxide, control is reflected under the temperature of the negative pressure of 0.02～0.05Mpa and 20～50 ℃ to be carried out, and wherein the concentration of sulphuric acid soln is 50～70%.
4. chlorine dioxide is pumped to surge tank with negative pressure after the air dilution, imports built-up type absorption tower and stable composition absorption liquid then and carries out the stable absorption processing, produces stable ClO 2 solution; The stable composition absorption liquid is made up of yellow soda ash, sodium hydroxide, hydrogen peroxide, deionized water, and proportioning is a yellow soda ash 3.5～5%; Sodium hydroxide 0.5～5%; Hydrogen peroxide 4～17%; Deionized water 73～92%.
The said process reaction principle is:
Comprehensive (1) (2) (3) formula:
The production method of described stable ClO 2 solution, the optimum weight proportioning of the composite catalyst of being made up of trisodium phosphate, 2-HPAA, urea is 1: 0.35～0.45: 0.6～0.7; The optimum weight ratio of the complex reaction liquid of being made up of alkaline metal chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.65～0.75: 0.6～0.7: 0.007～0.008; Weight proportion the best 1: 1.15～1.25 of complex reaction liquid and sulphuric acid soln; Concentration the best of sulphuric acid soln is 60～70%.
The concrete technical process of ClO 2 solution production method provided by the invention is such, at first trisodium phosphate, the 2-HPAA, it is stand-by that urea is made into composite catalyst by weight 1: 0.1～0.5: 0.5～1, then the alkaline metal chlorate is used the softening water stirring and dissolving in material-compound tank, add superoxol (30%) and composite catalyst by proportioning, continue down to stir to make to dissolve fully in normal temperature as complex reaction liquid, the alkaline metal chlorate, hydrogen peroxide, the weight proportion of softening water and composite catalyst is 1: 0.5～0.8: 0.4～1: 0.006～0.01, the most handy sodium chlorate of alkaline metal chlorate; Then with complex reaction liquid and sulphuric acid soln 1: 1 by weight ratio～1.5, enter in many graduated responses device through volume pump and to react, produce chlorine dioxide, control is reflected under the temperature of the negative pressure of 0.02～0.05Mpa and 20～50 ℃ to be carried out, the high-purity chlorine dioxide gas that produces is after the air dilution, pump to cleaner with negative pressure, surge tank, enter then in the built-up type absorption tower, with by yellow soda ash, sodium hydroxide, hydrogen peroxide, the stable composition absorption liquid that deionized water is formed by proportioning carries out abundant gas-to-liquid contact, reach the purpose of efficient absorption, generate many specifications stable ClO 2 solution of chlorine dioxide content 2～8% concentration, weight proportion the best of stable composition absorption liquid is: sodium carbonate-3.5～5%; Sodium hydroxide 0.5～5%; Hydrogen peroxide 4～17%; Deionized water 73～92%, in operating process for avoiding the excessive and hydrogen peroxide decomposition loss under negative pressure condition of hydrogen peroxide, the method of utilization continuous monitoring midbody product content, temperature and pH value in the stable absorption process, continuous and quantitative is added superoxol, obtain high absorption yield and stable, successive operating process, absorbed yield more than 99%.Reduce cost more than 40% than SPC-D solution absorption technology, said process is finished in stable ClO 2 solution combinations produce device.
The raffinate that produces in reaction process is generally the sodium bisulfate about 15～25%, and activator or toilet as stabilizing chlorine dioxide after composite the processing clean byproduct sales such as reodorant; Reaction residue also can reclaim solid sodium sulfate and sell as byproduct after concentrated, crystallization, filtration, drying treatment, and acid filtrate returns reaction workshop section and applies mechanically, and production process does not have discharging of waste liquid, not only reduce production costs greatly, and environmental protection and economy.
The present invention compared with prior art, its significant advantage is: 1. compare with at present leading technology Textone conversion method, methyl alcohol reduction method, raw material and power consumption reduce by 3 times than Textone method, reduce by 20～30% than methyl alcohol method, thoroughly solved in methyl alcohol method production equipment complexity, the product methanol content problem that easily exceeds standard in addition, do not contain harmful organic solvent in the product, prevented environmental pollution yet.2. the employing of composite catalyst and chlorine dioxide generation technology, efficiently solve the unstable in the chlorine dioxide generating process, increased the operating restraint of process control parameter, the purity of chlorine dioxide of generation reaches more than 98%, overall yield of reaction reaches more than 80%, and production efficiency increases substantially.3. adopt special stable composition absorption liquid, the high absorption yield and the operating process of steady and continuous have been obtained, specific absorption reduces cost more than 40% than SPC-D solution absorption technology more than 99%, can make the stable ClO 2 solution product content reach 8%.4. whole process of production safely, operate steadily reliably, feedstock conversion is thorough, and can produce automatically continuously, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing.
Embodiment 1:
Production product specification concentration is defined as 2%.It is stand-by at first trisodium phosphate, 2-HPAA, urea to be made into composite catalyst by weight 1: 0.4: 0.7; By proportioning sodium chlorate is used the softening water stirring and dissolving in material-compound tank then, add superoxol (30%) and composite catalyst, continue down to stir to make to dissolve fully as complex reaction liquid in normal temperature, the weight proportion of sodium chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.7: 0.7: 0.008; Add the stable composition absorption liquid in the built-up type absorption tower, proportioning is a sodium carbonate 3.5%; Sodium hydroxide 0.5%; Hydrogen peroxide 5%; Deionized water 91%, the reaction and negative pressure of controlling many graduated responses device is at 0.04～0.42Mpa, temperature of reaction 32～35C.Move after 8 hours, discharge 1.15 tons of stability chlorine dioxide aqueous solution, calculating the raw material consumption cost is 342 yuan of/ton products, and total recovery 89.1% is 98.5% by purity of chlorine dioxide in the continuous iodometric determination product.Detect by the method for inspection shown in the national standard HG3669-2000, index is as follows:
| Project | HG/3669-2000 standard-required index | Test result |
| Chlorine dioxide content (ClO2) 〉= | 2％ | 2.14％ |
| Density (20 ℃) g/cm3 | 1.020～1.060 | 1.042 |
| PH value | 8.2～9.2 | 8.9 |
| Arsenic (AS) content≤ | 0.0002 | 0.0002 |
| Heavy metal (in Pb) content≤ | 0.001 | 0.001 |
| Methanol content g/100ml≤ | 0.04 | Do not detect |
| Outward appearance | Colourless or light yellow transparent liquid, no suspended substance | Colourless transparent liquid, no suspended substance |
Embodiment 2:
Product specification concentration is defined as 4%.Getting the see weight proportion of acyl acetic acid, urea of composite catalyst trisodium phosphate, 2-hydroxyl is 1: 0.4: 0.6; The weight proportion of sodium chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.65: 0.76 in the complex reaction liquid: 0.008; Add the stable composition absorption liquid in the built-up type absorption tower, proportioning is a sodium carbonate 4%; Sodium hydroxide 1%; Hydrogen peroxide 8%; Deionized water 87%, concentration of hydrogen peroxide 30%, adjusting the complex reaction flow quantity is 22L/h, and the sulphuric acid soln flow is 26L/h, and the reaction and negative pressure of controlling many graduated responses device is 32～35 ℃ of 0.04～0.42Mpa, temperature of reaction.Move after 15 hours, discharge 3.07 tons of stability chlorine dioxide aqueous solution, calculating the raw material consumption cost is 703 yuan of/ton products, and total recovery 88.2% is 98.3% by purity of chlorine dioxide in the continuous iodometric determination product.
Embodiment 3:
Product specification concentration is defined as 8%.Getting see acyl acetic acid, weight of urea proportioning of composite catalyst trisodium phosphate, 2-hydroxyl is 1: 0.5: 0.1; The weight proportion of sodium chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.65: 0.8 in the complex reaction liquid: 0.008; Add the stable composition absorption liquid in the built-up type absorption tower, proportioning is a sodium carbonate 5%; Sodium hydroxide 4.5%; Hydrogen peroxide 16%; Deionized water 74.5%, adjusting the complex reaction flow quantity is 27.5L/h, the sulphuric acid soln flow is 18.5L/h; Pure water flow: 14L/h; The reaction and negative pressure of controlling many graduated responses device is 32～35 ℃ of 0.04～0.42Mpa, temperature of reaction.Move after 8 hours, discharge 1.08 tons of stability chlorine dioxide aqueous solution, calculating the raw material consumption cost is 1448 yuan of/ton products, and total recovery 87.9% is 98.1% by purity of chlorine dioxide in the continuous iodometric determination product.
Claims (5)
1, a kind of production method of stable ClO 2 solution adopts hydrogen peroxide to make reductive agent, and dioxide peroxide takes place the reducine metal chlorate in sulfuric acid medium, it is characterized in that this production method may further comprise the steps:
1. form composite catalyst by trisodium phosphate, 2-HPAA, urea by proportioning, weight ratio is 1: 0.1～0.5: 0.5～1;
2. the alkaline metal chlorate is used the softening water stirring and dissolving in material-compound tank, superoxol and composite catalyst by proportioning adding 30%, continue down to stir to make to dissolve fully in normal temperature as complex reaction liquid, complex reaction liquid proportioning, promptly the weight proportion of alkaline metal chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.5～0.8: 0.4～1: 0.006～0.01;
3. complex reaction liquid and sulphuric acid soln 1: 1 by weight ratio～1.5, enter in many graduated responses device through volume pump and to react, produce chlorine dioxide, control is reflected under the temperature of the negative pressure of 0.02～0.05Mpa and 20～50 ℃ carries out sulphuric acid soln concentration 50～70%;
4. chlorine dioxide is pumped to surge tank with negative pressure after dilution, enters the built-up type absorption tower then, carries out stable absorption with the stable composition absorption liquid and handles, and produces stable ClO 2 solution; The stable composition absorption liquid is made up of yellow soda ash, sodium hydroxide, hydrogen peroxide, deionized water, and proportioning is a yellow soda ash 3.5～5%; Sodium hydroxide 0.5～5%; Hydrogen peroxide 4～17%; Deionized water 73～92%.
2, the production method of a kind of stable ClO 2 solution according to claim 1 is characterized in that the weight proportion of the composite catalyst be made up of trisodium phosphate, 2-HPAA, urea is 1: 0.35～0.45: 0.6～0.7.
3, the production method of a kind of stable ClO 2 solution according to claim 1 is characterized in that the weight ratio of the complex reaction liquid be made up of alkaline metal chlorate, hydrogen peroxide, softening water and composite catalyst is 1: 0.65～0.75: 0.6～0.7: 0.007～0.008.
4, the production method of a kind of stable ClO 2 solution according to claim 1, the weight proportion that it is characterized in that complex reaction liquid and sulphuric acid soln is 1: 1.15～1.25.
5, the production method of a kind of stable ClO 2 solution according to claim 1 is characterized in that the alkaline metal chlorate is a sodium chlorate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 03121405 CN1235913C (en) | 2003-03-28 | 2003-03-28 | Production for stable chlorinedioxide solution |
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|---|---|---|---|
| CN 03121405 CN1235913C (en) | 2003-03-28 | 2003-03-28 | Production for stable chlorinedioxide solution |
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| CN1235913C true CN1235913C (en) | 2006-01-11 |
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| CN 03121405 Expired - Fee Related CN1235913C (en) | 2003-03-28 | 2003-03-28 | Production for stable chlorinedioxide solution |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US8917169B2 (en) | 1993-02-26 | 2014-12-23 | Magna Electronics Inc. | Vehicular vision system |
| US8993951B2 (en) | 1996-03-25 | 2015-03-31 | Magna Electronics Inc. | Driver assistance system for a vehicle |
| US9008369B2 (en) | 2004-04-15 | 2015-04-14 | Magna Electronics Inc. | Vision system for vehicle |
| US9171217B2 (en) | 2002-05-03 | 2015-10-27 | Magna Electronics Inc. | Vision system for vehicle |
| US9193302B2 (en) | 1999-11-04 | 2015-11-24 | Magna Electronics Inc. | Vision system for a vehicle |
| US9233645B2 (en) | 1999-11-04 | 2016-01-12 | Magna Electronics Inc. | Accessory mounting system for a vehicle |
| US9266474B2 (en) | 2004-08-18 | 2016-02-23 | Magna Electronics Inc. | Accessory system for vehicle |
| US9436880B2 (en) | 1999-08-12 | 2016-09-06 | Magna Electronics Inc. | Vehicle vision system |
| US9434314B2 (en) | 1998-04-08 | 2016-09-06 | Donnelly Corporation | Electronic accessory system for a vehicle |
| US9440535B2 (en) | 2006-08-11 | 2016-09-13 | Magna Electronics Inc. | Vision system for vehicle |
| US9527445B2 (en) | 1998-01-07 | 2016-12-27 | Magna Electronics Inc. | Accessory mounting system for mounting an accessory at a vehicle such that a camera views through the vehicle windshield |
| US9539956B2 (en) | 1999-08-25 | 2017-01-10 | Magna Electronics Inc. | Accessory system for a vehicle |
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| CN101538017B (en) * | 2008-03-21 | 2011-05-25 | 东莞市中加消毒科技有限公司 | Process for producing high-purity chlorine dioxide |
| CN101305734B (en) * | 2008-05-29 | 2011-06-08 | 龙泽云 | Manufacturing method of chlorine dioxide aqueous solution disinfectant with high stability |
| CN103101883B (en) * | 2013-03-01 | 2015-04-15 | 唐洪权 | Method for producing and activating food additive stabilized chlorine dioxide solution |
| CN106698353A (en) * | 2016-12-26 | 2017-05-24 | 四川齐力绿源水处理科技有限公司 | Method for preparing chlorine dioxide from composite chlorate |
| CN106835799B (en) * | 2017-03-13 | 2018-04-10 | 广西大学 | A kind of method for improving ClO 2 solution stability |
| CN113812403A (en) * | 2021-10-29 | 2021-12-21 | 石家庄北赫环保科技有限公司 | Chlorine dioxide solution and preparation method thereof |
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2003
- 2003-03-28 CN CN 03121405 patent/CN1235913C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US8917169B2 (en) | 1993-02-26 | 2014-12-23 | Magna Electronics Inc. | Vehicular vision system |
| US8993951B2 (en) | 1996-03-25 | 2015-03-31 | Magna Electronics Inc. | Driver assistance system for a vehicle |
| US9527445B2 (en) | 1998-01-07 | 2016-12-27 | Magna Electronics Inc. | Accessory mounting system for mounting an accessory at a vehicle such that a camera views through the vehicle windshield |
| US9434314B2 (en) | 1998-04-08 | 2016-09-06 | Donnelly Corporation | Electronic accessory system for a vehicle |
| US9436880B2 (en) | 1999-08-12 | 2016-09-06 | Magna Electronics Inc. | Vehicle vision system |
| US9446715B2 (en) | 1999-08-25 | 2016-09-20 | Magna Electronics Inc. | Vision system for a vehicle |
| US9539956B2 (en) | 1999-08-25 | 2017-01-10 | Magna Electronics Inc. | Accessory system for a vehicle |
| US9193302B2 (en) | 1999-11-04 | 2015-11-24 | Magna Electronics Inc. | Vision system for a vehicle |
| US9233645B2 (en) | 1999-11-04 | 2016-01-12 | Magna Electronics Inc. | Accessory mounting system for a vehicle |
| US9555803B2 (en) | 2002-05-03 | 2017-01-31 | Magna Electronics Inc. | Driver assistance system for vehicle |
| US9171217B2 (en) | 2002-05-03 | 2015-10-27 | Magna Electronics Inc. | Vision system for vehicle |
| US9191634B2 (en) | 2004-04-15 | 2015-11-17 | Magna Electronics Inc. | Vision system for vehicle |
| US9428192B2 (en) | 2004-04-15 | 2016-08-30 | Magna Electronics Inc. | Vision system for vehicle |
| US9008369B2 (en) | 2004-04-15 | 2015-04-14 | Magna Electronics Inc. | Vision system for vehicle |
| US9266474B2 (en) | 2004-08-18 | 2016-02-23 | Magna Electronics Inc. | Accessory system for vehicle |
| US9440535B2 (en) | 2006-08-11 | 2016-09-13 | Magna Electronics Inc. | Vision system for vehicle |
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Assignee: Fine Silicon Co., Ltd. Assignor: Hebei University of Science and Technology Contract fulfillment period: 2009.4.21 to 2014.4.20 contract change Contract record no.: 2009990000552 Denomination of invention: Production for stable chlorinedioxide solution Granted publication date: 20060111 License type: Exclusive license Record date: 2009.5.25 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.21 TO 2014.4.20; CHANGE OF CONTRACT Name of requester: 69 SILICON INDUSTRY CO., LTD. Effective date: 20090525 |
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Granted publication date: 20060111 Termination date: 20110328 |