CN103482572B - A kind of method and generator thereof of preparing thimerosal - Google Patents
A kind of method and generator thereof of preparing thimerosal Download PDFInfo
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- CN103482572B CN103482572B CN201310471599.2A CN201310471599A CN103482572B CN 103482572 B CN103482572 B CN 103482572B CN 201310471599 A CN201310471599 A CN 201310471599A CN 103482572 B CN103482572 B CN 103482572B
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Abstract
The invention discloses and a kind ofly prepare the method for thimerosal and realize the generator of the method, the method comprises the following steps: A, first by solution of chlorate, hydrochloric acid solution and catalyst placing response device, heating; In B, extraction step A, the reaction chlorine that is able to is main mist; C, step B gained mist is passed in water, aeration makes thimerosal. The present invention also provides a kind of generator of realizing the method. The invention has the beneficial effects as follows: energy consumption is little, cost is low, and its performance safety is reliable, and output is high, and conversion ratio is high, and technique is simple, is convenient to automation control, installation, easy to operate.
Description
Technical field
The present invention relates to a kind ofly prepare the method for thimerosal and realize the generator that the method is used.
Background technology
At present, China's water treatment market, still taking chlorine as main sterilization means, requires strictly but store the each side such as transport due to chlorine, uses danger larger, is badly in need of wanting a kind of in situ preparation, and the equipment of on-the-spot use improves safety in utilization and convenience.
In prior art, report many methods by preparation of hydrogen chloride chlorine, mainly contained electrolysis, inorganic oxidizer direct oxidation method and air or oxygen catalytic oxidation. But these methods all have limitation, the shortcoming of for example electrolysis is that energy consumption is too large, and cost is high. The shortcoming of five machine oxidant direct oxidation methods is comparison in equipment complexity, product separation difficulty, and power consumption is larger simultaneously. And Deacon process is under the condition of copper dioxide or copper oxide catalyst existence, reacted the process of preparing chlorine gas with oxygen by hydrogen chloride, because this reaction is reversible reaction, in product gas, comprise a small amount of inert gas that may contain in unreacted hydrogen chloride, oxygen, unstrpped gas, and product chlorine G&W, the hydrogen chloride conversion ratio of the method is less than 80% conventionally.
Although on market, have chlorine dioxide generator to provide produced on-site scene to add, part solution chlorine use in safety problem, the feature of chlorine dioxide ubiquity low conversion rate in the market, causes accessory substance chlorate to exceed standard; After disinfection by chlorine dioxide, be first converted into chlorite simultaneously, cause chlorine dioxide dosage to exceed standard, thereby cause chlorite to exceed standard, and most water factory dosage can not meet sterilization requirement far away.
Summary of the invention
In view of this, the present invention need to provide a kind of and simplely prepares the method for thimerosal and realize the generator of the method. For at least one in solving the problems of the technologies described above, object of the present invention is to provide a kind of method of preparing thimerosal.
Another object of the present invention is to provide a kind of generator of preparing thimerosal.
One aspect of the present invention has been to provide a kind of method of preparing thimerosal, and the method comprises the following steps:
A, first by solution of chlorate, hydrochloric acid solution and catalyst placing response device, heating;
In B, extraction step A, the reaction chlorine that is able to is main mist;
C, step B gained mist is passed in water, aeration makes thimerosal.
Wherein, in described steps A, solution of chlorate comprises the strong metal such as sodium chlorate solution, potassium chlorate solution solution of chlorate, and described solution of chlorate mass concentration is 20%-40%, hydrochloric acid solution mass concentration 25%-36%; Described heating comprises heating water bath, oil bath heating and directly heating, and mode of heating adopts corrosion-resistant heating tube, and described heating tube is provided with temperature detection and temperature control system.
Wherein, in described steps A, catalyst can be MnCl2、FeCl2、FeCl3、MnSO4、FeSO4、Fe2（SO4）2One or more, the amount of described catalyst is the 1%-3% of added solution of chlorate amount, is the 3%-5% of added hydrochloric acid solution amount, described catalyst does not reclaim; The described temperature that is heated to is 70-90 degree Celsius, and the reaction time is 10-60 minute.
Wherein in step B, in extraction step A, the reaction chlorine that is able to is that the negative pressure that main mist forms is-90--5KPa.
Wherein the input material volume ratio of the solution of chlorate in steps A and hydrochloric acid solution is 1.5-0.5, according to the difference that generates amount of chlorine, reaction volume is also different, and it is 1.0-1.7L that general every generation 1kg chlorine needs reactant solution total amount, and this reaction can generate 1kg/h chlorine continuously;
Wherein in step B and C, every generation 1-10kg/h chlorine passes in the water in water sprayer, and aeration absorbs the water yield 1-20m3/ h, forms concentration 200-1000mg/l thimerosal.
In order to realize foregoing invention object, the present invention also provides the generator that completes above-mentioned thimerosal preparation method, and described generator comprises: solution of chlorate storage tank, hydrochloric acid tank, hydrochloric acid measuring pump, hydrochloric acid Traffic Monitor, controller, solution of chlorate import, hydrochloric acid import, air inlet buffer, venting, gas outlet, water sprayer, liquid level detector, reactor, heating jacket, reactor sewage draining exit, temperature sensor, heating jacket sewage draining exit, heating tube, heating jacket filling opening, chlorate measuring pump and chlorate Traffic Monitor, is characterized in that, the outlet of described solution of chlorate storage tank, the outlet of hydrochloric acid tank is connected with the import of chlorate measuring pump and the import of hydrochloric acid measuring pump respectively, described chlorate metering delivery side of pump, hydrochloric acid metering delivery side of pump is connected with the import of chlorate Traffic Monitor and the import of hydrochloric acid Traffic Monitor respectively, the outlet of the outlet of described chlorate Traffic Monitor and hydrochloric acid Traffic Monitor is connected with solution of chlorate import and hydrochloric acid import respectively, described solution of chlorate outlet, hydrochloric acid outlet is connected with the import of reactor respectively, the outlet of described reactor is connected with one end of air inlet buffer, venting, reactor sewage draining exit and gas outlet respectively, and the other end of described gas outlet is connected with water sprayer.
Described reactor head is provided with venting, bottom is provided with sewage draining exit, air inlet buffer entrance is connected with atmosphere, the outlet of air inlet buffer is connected with reactor bottom air inlet, reactor outer setting has immersion heating jacket, by heating jacket, the reactant in reactor is heated, heating tube, temperature sensor, liquid level detector, heating jacket are installed on described heating jacket and are provided with filling opening, its bottom is provided with sewage draining exit.
Described director port is connected respectively the liquid level for automatically controlling heating reactant, the temperature that shows reactant, detecting reactant and controls injection rate and the output quantity of reactant with hydrochloric acid measuring pump, hydrochloric acid Traffic Monitor, liquid level detector, temperature sensor port.
Described reactor material is titanium material, is provided with venting, reactor sewage draining exit on it, and aeration enters reactor by air by air inlet buffer and carries out aeration, and described reactor outer setting heating jacket, heats reactor by heating jacket.
Described reactor is provided with controller, described controller is connected with chlorate measuring pump, hydrochloric acid measuring pump, chlorate Traffic Monitor, hydrochloric acid Traffic Monitor, heating tube, temperature sensor, liquid level detector by electric wire, the output quantity of the amount of the automatic control of realization reactant, temperature, the liquid level of detecting reactant and the injection rate of reactant and the product of reactant.
Introduce in detail below in conjunction with above-mentioned generator the process that the present invention prepares chlorine:
Solution of chlorate in described solution of chlorate storage tank enters in chlorate measuring pump from its outlet, secondly first measure delivery side of pump by chlorate and enter into chlorate Traffic Monitor, enter into reactor in outlet and the solution of chlorate outlet by chlorate Traffic Monitor successively; Secondly hydrochloric acid in described hydrochloric acid tank enters into hydrochloric acid measuring pump from its outlet, first measures delivery side of pump by hydrochloric acid and enters into hydrochloric acid Traffic Monitor, enters into reactor at outlet and the hydrochloric acid outlet by hydrochloric acid Traffic Monitor successively; By catalyst MnCl2、FeCl2、FeCl3、MnSO4、FeSO4、Fe2（SO4）2One or more together with above-mentioned reactant in placing response device, described reactor is heated to 70-95 degree Celsius by heating jacket to reactant, 10-60 minute is carried out in reaction, product is taking chlorine as main, and with a small amount of chlorine dioxide, the gas of generation is extracted by water sprayer through gas outlet, aeration, form thimerosal, be transported to water body by pipeline and carry out disinfection; In addition, reactor, under water sprayer decimate action, forms the negative pressure of-90-5KPa, enters reactor bottom carry out aeration by air inlet buffer, is conducive to reaction and carries out and gas overflowing.
By experiment, the invention has the beneficial effects as follows: energy consumption is little, cost is low, and performance safety is reliable, and output is high, and conversion ratio is high, and technique is simple, is convenient to automation control, installation, easy to operate.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention prepares the generator of thimerosal.
Wherein, Reference numeral is: 1, solution of chlorate storage tank; 2, hydrochloric acid tank; 3, hydrochloric acid measuring pump; 4, hydrochloric acid Traffic Monitor; 5, controller; 6, solution of chlorate import; 7, hydrochloric acid import; 8, air inlet buffer; 9, venting; 10, gas outlet; 11, water sprayer; 12, liquid level detector; 13, reactor; 14, heating jacket; 15, reactor sewage draining exit; 16, temperature sensor; 17, heating jacket sewage draining exit; 18, heating tube; 19, heating jacket filling opening; 20, chlorate measuring pump; 21, chlorate Traffic Monitor.
Detailed description of the invention
For the problem of above-mentioned existence, below in conjunction with drawings and the specific embodiments, the present invention is described in detail.
Embodiment 1
Described solution of chlorate is sodium chlorate solution, get 500ml concentration and be 20% sodium chlorate solution, quantitatively be transported to reactor 13 by chlorate measuring pump 20, the hydrochloric acid that is 25% by 750ml concentration again, quantitatively be transported to reactor 13 by hydrochloric acid measuring pump 3, by add that sodium chlorate solution measures 1% and add 3% of hydrochloric acid solution amount and add catalyst MnCl2、FeCl2、FeCl3，Enter into reactor 13 together with above-mentioned reactant, described reactor 13 is heated to 70 degrees Celsius by heating jacket 14, and the reaction time is 60min, reaction pressure-90KPa, being able to chlorine is main mist, described mist is extracted by water sprayer 11 through gas outlet 10, mixes with the interior water of water sprayer 11, forms thimerosal, thimerosal to water sprayer 11 exits detects, detect that chlorine output reaches 1kg/h, chlorine ratio 60%, conversion ratio 90%.
Embodiment 2
Described solution of chlorate adopts sodium chlorate solution, getting 800ml concentration is 25% sodium chlorate solution, quantitatively be transported to reactor 13 by chlorate measuring pump 20, getting 400ml concentration is 31% hydrochloric acid solution, quantitatively be transported to reactor 13 by hydrochloric acid measuring pump 3, by add that sodium chlorate solution measures 3% and add 5% of hydrochloric acid solution amount and add catalyst MnSO4、FeSO4、Fe2（SO4）2Enter into reactor 13 together with above-mentioned reactant, 50 degrees Celsius of reaction temperatures, reaction time 40min, reaction pressure-50KPa, being able to chlorine is main mist, described mist is extracted by water sprayer 11 through gas outlet 10, mixes with the interior water of water sprayer 11, forms thimerosal, water sprayer 11 exit thimerosals are detected, detect that chlorine output reaches 5kg/h, chlorine ratio 65%, conversion ratio 93%.
Embodiment 3
Described solution of chlorate adopts sodium chlorate solution, get 1200ml concentration and be 33% sodium chlorate solution, quantitatively be transported to reactor 13 by chlorate measuring pump 20, getting 1200ml concentration is 31% hydrochloric acid again, quantitatively be transported to reactor 13 by chlorate measuring pump 20, by add that sodium chlorate solution measures 2.5% and add 4% of hydrochloric acid solution amount and add catalyst Fe Cl3Enter into reactor 13 together with above-mentioned reactant, 45 degrees Celsius of reaction temperatures, reaction time 30min, reaction pressure-10KPa, being able to chlorine is main mist, described mist is extracted by water sprayer 11 through gas outlet 10, mixes with the interior water of water sprayer 11, forms thimerosal, thimerosal to water sprayer 11 exits detects, detect that chlorine output reaches 10kg/h, chlorine ratio 80%, conversion ratio 97%.
Embodiment 4
Described solution of chlorate adopts sodium chlorate solution, get 650ml concentration and be 40% sodium chlorate solution, quantitatively be transported to reactor 13 by chlorate measuring pump 20,780ml concentration is 36% hydrochloric acid solution, quantitatively be transported to reactor 13 by chlorate measuring pump 20, by add that sodium chlorate solution measures 1.8% and add 2.5% of hydrochloric acid solution amount and add catalyst Fe2（SO4）2Enter into reactor 13 together with above-mentioned reactant, reaction temperature 90 is spent, reaction time 25min, reaction pressure-5KPa, being able to chlorine is main mist, described mist is extracted out by water sprayer 11 through gas outlet 10, mixes with the interior water of water sprayer 11, forms thimerosal, thimerosal to water sprayer 11 exits detects, detect that chlorine output reaches 20kg/h, chlorine ratio 72%, conversion ratio 95%.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (1)
1. chemical method is prepared a method for thimerosal, said method comprising the steps of:
A, first by solution of chlorate, hydrochloric acid solution and catalyst placing response device, heating;
In B, extraction step A, the reaction chlorine that is able to is main mist;
C, step B gained mist is passed in water, aeration makes thimerosal;
Wherein, in steps A, the reaction chlorine that is able to is that negative pressure that main mist forms is-90 to-5Kpa;
Wherein, in step B and C, every generation 1-10kg/h chlorine passes in the water in water sprayer, and aeration absorbs water yield 1-20m3/ h, forms concentration 200-1000mg/l thimerosal;
Wherein in steps A, solution of chlorate comprises sodium chlorate solution or potassium chlorate solution, and described solution of chlorate mass concentration is 20%-40%, hydrochloric acid solution mass concentration 25%-36%; Described heating comprises heating water bath, oil bath heating and directly heating, and mode of heating adopts corrosion-resistant heating tube, and described heating tube is provided with temperature detection and temperature control system;
Wherein in steps A, catalyst is MnCl2、FeCl2、FeCl3、MnSO4、FeSO4、Fe2（SO4）3One or more, the amount of described catalyst is the 1%-3% of added solution of chlorate amount, is the 3%-5% of added hydrochloric acid solution amount, described catalyst does not reclaim; The described temperature that is heated to is 70-90 degree Celsius, and the reaction time is 10-60 minute;
The generator of described method comprises: solution of chlorate storage tank (1), hydrochloric acid tank (2), hydrochloric acid measuring pump (3), hydrochloric acid Traffic Monitor (4), controller (5), solution of chlorate import (6), hydrochloric acid import (7), air inlet buffer (8), venting (9), gas outlet (10), water sprayer (11), liquid level detector (12), reactor (13), heating jacket (14), reactor sewage draining exit (15), temperature sensor (16), heating jacket sewage draining exit (17), heating tube (18), heating jacket filling opening (19), chlorate measuring pump (20) and chlorate Traffic Monitor (21), the outlet of described solution of chlorate storage tank (1), the outlet of hydrochloric acid tank (2) is connected with the import of chlorate measuring pump (20) and the import of hydrochloric acid measuring pump (3) respectively, the outlet of described chlorate measuring pump (20), the outlet of hydrochloric acid measuring pump (3) is connected with the import of chlorate Traffic Monitor (21) and the import of hydrochloric acid Traffic Monitor (4) respectively, the outlet of the outlet of described chlorate Traffic Monitor (21) and hydrochloric acid Traffic Monitor (4) is connected with solution of chlorate import (6) and hydrochloric acid import (7) respectively, described solution of chlorate outlet (6), hydrochloric acid outlet (7) is connected with the import of reactor (13) respectively, the outlet of described reactor (13) is connected with one end of air inlet buffer (8), venting (9), reactor sewage draining exit (15) and gas outlet (10) respectively, and the other end of described gas outlet (10) is connected with water sprayer (11),
Described controller (5) port respectively with hydrochloric acid measuring pump (3), hydrochloric acid Traffic Monitor (4), liquid level detector (12), temperature sensor (16); Heating jacket sewage draining exit (17), heating tube (18), chlorate measuring pump (20) and chlorate Traffic Monitor (21) port are connected, for the output quantity of temperature, the liquid level of detecting reactant and the injection rate of reactant and the product of automatic generator reactant;
(13) at least 2 grades of described reactors, it is provided with venting (9), air inlet buffer (8) and reactor sewage draining exit (15);
Described heating jacket (14) arranges heating tube (18), heating jacket filling opening (19), for heating reactant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310471599.2A CN103482572B (en) | 2013-10-11 | 2013-10-11 | A kind of method and generator thereof of preparing thimerosal |
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| CN201310471599.2A CN103482572B (en) | 2013-10-11 | 2013-10-11 | A kind of method and generator thereof of preparing thimerosal |
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| CN103482572B true CN103482572B (en) | 2016-05-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105129733B (en) * | 2015-09-21 | 2018-06-22 | 宁波镇洋化工发展有限公司 | A kind of production technology of chlorine |
| CN110921888A (en) * | 2019-11-12 | 2020-03-27 | 江苏乾宝生物科技有限公司 | Efficient antibacterial disinfectant fluid preparation device and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2343152Y (en) * | 1998-08-18 | 1999-10-13 | 朱明永 | Chlorine dioxide disinfectant generator |
| CN203498077U (en) * | 2013-10-11 | 2014-03-26 | 山东新日电器设备有限公司 | Generator for preparing disinfectant |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201325874Y (en) * | 2009-03-24 | 2009-10-14 | 河北瑞特电力科技有限公司 | Negative pressure reactor for producing chlorine dioxide |
| CN201647989U (en) * | 2009-09-07 | 2010-11-24 | 北京联合大学生物化学工程学院 | Chlorine dioxide generating device |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2343152Y (en) * | 1998-08-18 | 1999-10-13 | 朱明永 | Chlorine dioxide disinfectant generator |
| CN203498077U (en) * | 2013-10-11 | 2014-03-26 | 山东新日电器设备有限公司 | Generator for preparing disinfectant |
Non-Patent Citations (1)
| Title |
|---|
| 全盐酸法生产C1O2消毒剂反应条件研究;张吉库等;《沈阳建筑大学学报(自然科学版)》;20090731;第25卷(第4期);第741-746页 * |
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