CN103482572A - Method for preparing disinfectant, and generator therefor - Google Patents

Method for preparing disinfectant, and generator therefor Download PDF

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Publication number
CN103482572A
CN103482572A CN201310471599.2A CN201310471599A CN103482572A CN 103482572 A CN103482572 A CN 103482572A CN 201310471599 A CN201310471599 A CN 201310471599A CN 103482572 A CN103482572 A CN 103482572A
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hydrochloric acid
solution
chlorate
heating
outlet
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CN103482572B (en
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尉婕
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New Day Electrical Equipment Co Ltd In Shandong
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New Day Electrical Equipment Co Ltd In Shandong
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Abstract

The invention discloses a method for preparing a disinfectant, and a generator for realizing the method. The method comprises the following steps: 1, putting a chlorate solution, a hydrochloric acid solution and a catalyst in a reactor, and heating; 2, extracting a chlorine-based mixed gas obtained in step 1; and 3, letting the mixed gas obtained in step 2 in water, and aerating to prepare the disinfectant. The invention also provides the generator for realizing the method. The method and the generator have the advantages of small energy consumption, low cost, safe and reliable performances, high output, high conversion rate, convenient automatic control, and convenient installation and operation.

Description

A kind of method and producer thereof for preparing thimerosal
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Technical field
The present invention relates to a kind ofly prepare the method for thimerosal and realize the producer that the method is used.
 
Background technology
At present, chlorine still be take as main sterilization means in China's water treatment market, but, because the each side such as chlorine storage transportation are strict, 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 accessibility.
Report many methods by preparation of hydrogen chloride chlorine in prior art, mainly contained electrolytic process, inorganic oxidizer direct oxidation method and air or oxygen catalytic oxidation.Yet these methods all have limitation, for example the shortcoming of electrolytic process is that energy consumption is too large, and cost is high.The shortcoming of five machine oxygenant direct oxidation methods is comparison in equipment complexity, the product separation difficulty, and power consumption is larger simultaneously.And the Deacon process is under the condition of copper dioxide or copper oxide catalyst existence, reacted the process of preparing chlorine gas with oxygen by hydrogenchloride, because this reaction is reversible reaction, comprise in unreacted hydrogenchloride, oxygen, unstripped gas a small amount of rare gas element that may contain in product gas, and product chlorine G&W, the hydrogenchloride transformation efficiency of the method is less than 80% usually.
Although on market, have chlorine dioxide generator to provide the situ production scene to add, the solution of part the safety problem of chlorine in using, the characteristics of dioxide peroxide ubiquity low conversion rate in the market, cause the by product oxymuriate to exceed standard; At first be converted into chlorite after disinfection by chlorine dioxide simultaneously, cause the dioxide peroxide dosage to exceed standard, thereby cause chlorite to exceed standard, and most water factory dosage can not meet the sterilization requirement far away.
 
Summary of the invention
In view of this, the present invention need to provide a kind of simple producer for preparing the method for thimerosal and realize the method.For at least one in solving the problems of the technologies described above, purpose of the present invention is to provide a kind of method for preparing thimerosal.
Another object of the present invention is to provide a kind of producer for preparing thimerosal.
One aspect of the present invention has been to provide a kind of method for preparing thimerosal, and the method comprises the following steps:
A, first by solution of chlorate, hydrochloric acid soln and catalyzer placing response device, the heating;
In B, extraction step A, the reaction chlorine that is able to is main mixed gas;
C, step B gained mixed gas is passed in water, aeration makes thimerosal.
Wherein, in described steps A, solution of chlorate comprises the strong metal solution of chlorate such as sodium chlorate solution, potassium chlorate solution, and described solution of chlorate mass concentration is 20%-40%, hydrochloric acid soln mass concentration 25%-36%; Described heating comprises heating in water bath, oil bath heating and direct heating, and type of heating adopts corrosion-resistant heating tube, and described heating tube is provided with temperature detection and temperature controlling system.
Wherein, in described steps A, catalyzer can be MnCl 2, FeCl 2, FeCl 3, MnSO 4, FeSO 4, Fe 2(SO 4) 2one or more, the amount of described catalyzer is the 1%-3% of added solution of chlorate amount, is the 3%-5% of added hydrochloric acid soln amount, described catalyzer does not reclaim; The described temperature that is heated to is 70-90 degree centigrade, and the reaction times is 10-60 minute.
The negative pressure that wherein in step B, in extraction step A, the reaction chlorine that is able to is main mixed gas formation is-90--5KPa.
Wherein the input material volume ratio of the solution of chlorate in steps A and hydrochloric acid soln 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 the 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 1-20m 3/ h, form concentration 200-1000mg/l thimerosal.
In order to realize the foregoing invention purpose, the present invention also provides the producer that completes above-mentioned thimerosal preparation method, and described producer comprises: the solution of chlorate storage tank, hydrochloric acid tank, the hydrochloric acid volume pump, the hydrochloric acid Traffic Monitor, controller, the solution of chlorate import, the hydrochloric acid import, the air inlet snubber, venting, air outlet, water sprayer, liquid level detector, reactor, heating jacket, the reactor sewage draining exit, temperature sensor, the heating jacket sewage draining exit, heating tube, the heating jacket liquid adding hole, oxymuriate volume pump and oxymuriate 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 hydrochloric acid volume pump with the import of oxymuriate volume pump respectively, described oxymuriate metering pump outlet, hydrochloric acid metering pump outlet is connected with the import of hydrochloric acid Traffic Monitor with the import of oxymuriate Traffic Monitor respectively, with the solution of chlorate import, with hydrochloric acid, import is connected respectively in the outlet of the outlet of described oxymuriate Traffic Monitor and hydrochloric acid Traffic Monitor, described solution of chlorate outlet, hydrochloric acid outlet is connected with the import of reactor respectively, the outlet of described reactor is connected with an end of air inlet snubber, venting, reactor sewage draining exit and air outlet respectively, and the other end of described air outlet is connected with water sprayer.
Described reactor head is provided with venting, bottom is provided with sewage draining exit, air inlet snubber entrance is connected with atmosphere, the outlet of air inlet snubber is connected with the reactor bottom inlet mouth, the reactor outer setting has the 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 liquid adding hole, its bottom is provided with sewage draining exit.
Described director port is connected respectively the liquid level for automatically controlling reacting by heating thing, the temperature that shows reactant, detecting reactant and controls reactant injection rate and work output with hydrochloric acid volume pump, hydrochloric acid Traffic Monitor, liquid level detector, temperature sensor port.
Described reactor material is the titanium material, is provided with venting, reactor sewage draining exit on it, and aeration enters reactor by air by the air inlet snubber and carries out aeration, and described reactor outer setting heating jacket, heated reactor by heating jacket.
Described reactor is provided with controller, described controller is connected with oxymuriate volume pump, hydrochloric acid volume pump, oxymuriate Traffic Monitor, hydrochloric acid Traffic Monitor, heating tube, temperature sensor, liquid level detector by electric wire, realizes automatically controlling the amount of reactant, the temperature of reactant, liquid level and the injection rate of reactant and the work output of resultant of detecting reactant.
Introduce in detail below in conjunction with above-mentioned producer the process that the present invention prepares chlorine:
Solution of chlorate in described solution of chlorate storage tank enters in the oxymuriate volume pump from its outlet, secondly at first measure pump outlet by oxymuriate and enter into the oxymuriate Traffic Monitor, enter into reactor in outlet and the solution of chlorate outlet by the oxymuriate Traffic Monitor successively; Secondly hydrochloric acid in described hydrochloric acid tank enters into the hydrochloric acid volume pump from its outlet, at first by hydrochloric acid, measures pump outlet and enters into the hydrochloric acid Traffic Monitor, enters into reactor at outlet and the hydrochloric acid outlet by the hydrochloric acid Traffic Monitor successively; By catalyzer MnCl 2, FeCl 2, FeCl 3, MnSO 4, FeSO 4, Fe 2(SO 4) 2one or more together with above-mentioned reactant in the placing response device, described reactor is heated to 70-95 degree centigrade by heating jacket to reactant, 10-60 minute is carried out in reaction, resultant be take chlorine as main, and, with a small amount of dioxide peroxide, the gas of generation is extracted by water sprayer through air outlet, aeration, form thimerosal, be transported to water body by pipeline and carry out disinfection; In addition, reactor, under the water sprayer decimate action, forms the negative pressure of-90-5KPa, enters reactor bottom by the air inlet snubber and carries out aeration, is conducive to reaction and carries out and gas overflowing.
By experiment, the invention has the beneficial effects as follows: energy consumption is little, and cost is low, and performance safety is reliable, and output is high, and transformation efficiency is high, and technique is simple, is convenient to automatization and controls, installation, easy to operate.
 
The accompanying drawing explanation
Fig. 1 is the structural representation that the present invention prepares the producer of thimerosal.
Wherein, Reference numeral is: 1, solution of chlorate storage tank; 2, hydrochloric acid tank; 3, hydrochloric acid volume pump; 4, hydrochloric acid Traffic Monitor; 5, controller; 6, solution of chlorate import; 7, hydrochloric acid import; 8, air inlet snubber; 9, venting; 10, air 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 liquid adding hole; 20, oxymuriate volume pump; 21, oxymuriate Traffic Monitor.
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Embodiment
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 the sodium chlorate solution, get the sodium chlorate solution that 500ml concentration is 20%, quantitatively be transported to reactor 13 by oxymuriate volume pump 20, the hydrochloric acid that is 25% by 750ml concentration again, quantitatively be transported to reactor 13 by hydrochloric acid volume pump 3, by add the sodium chlorate solution to measure 1% and add 3% of hydrochloric acid soln amount and add catalyzer MnCl 2,feCl 2, FeCl 3,enter into reactor 13 together with above-mentioned reactant, described reactor 13 is heated to 70 degrees centigrade by heating jacket 14, and the reaction times is 60min, reaction pressure-90KPa, being able to chlorine is main mixed gas, described mixed gas is extracted by water sprayer 11 through air outlet 10, with the interior water of water sprayer 11, mixes, and forms thimerosal, thimerosal to water sprayer 11 exits is detected, chlorine output detected and reach 1 kg/h, chlorine ratio 60%, transformation efficiency 90%.
Embodiment 2
Described solution of chlorate adopts the sodium chlorate solution, getting 800ml concentration is 25% sodium chlorate solution, quantitatively be transported to reactor 13 by oxymuriate volume pump 20, getting 400ml concentration is 31% hydrochloric acid soln, quantitatively be transported to reactor 13 by hydrochloric acid volume pump 3, by add the sodium chlorate solution to measure 3% and add 5% of hydrochloric acid soln amount and add catalyzer MnSO 4, FeSO 4, Fe 2(SO 4) 2enter into reactor 13 together with above-mentioned reactant, 50 degrees centigrade of temperature of reaction, reaction times 40min, reaction pressure-50KPa, being able to chlorine is main mixed gas, described mixed gas is extracted by water sprayer 11 through air outlet 10, with the interior water of water sprayer 11, mixes, and forms thimerosal, water sprayer 11 exit thimerosals are detected, chlorine output detected and reach 5 kg/h, chlorine ratio 65%, transformation efficiency 93%.
Embodiment 3
Described solution of chlorate adopts the sodium chlorate solution, get the sodium chlorate solution that 1200ml concentration is 33%, quantitatively be transported to reactor 13 by oxymuriate volume pump 20, getting 1200ml concentration is 31% hydrochloric acid again, quantitatively be transported to reactor 13 by oxymuriate volume pump 20, by add the sodium chlorate solution to measure 2.5% and add 4% of hydrochloric acid soln amount and add catalyst Fe Cl 3enter into reactor 13 together with above-mentioned reactant, 45 degrees centigrade of temperature of reaction, reaction times 30min, reaction pressure-10KPa, being able to chlorine is main mixed gas, described mixed gas is extracted by water sprayer 11 through air outlet 10, with the interior water of water sprayer 11, mixes, and forms thimerosal, thimerosal to water sprayer 11 exits is detected, chlorine output detected and reach 10 kg/h, chlorine ratio 80%, transformation efficiency 97%.
Embodiment 4
Described solution of chlorate adopts the sodium chlorate solution, get the sodium chlorate solution that 650ml concentration is 40%, quantitatively be transported to reactor 13 by oxymuriate volume pump 20,780ml concentration is 36% hydrochloric acid soln, quantitatively be transported to reactor 13 by oxymuriate volume pump 20, by add the sodium chlorate solution to measure 1.8% and add 2.5% of hydrochloric acid soln amount and add catalyst Fe 2(SO 4) 2enter into reactor 13 together with above-mentioned reactant, temperature of reaction 90 degree, reaction times 25min, reaction pressure-5KPa, being able to chlorine is main mixed gas, described mixed gas is extracted out by water sprayer 11 through air outlet 10, with the interior water of water sprayer 11, mixes, and forms thimerosal, thimerosal to water sprayer 11 exits is detected, chlorine output detected and reach 20 kg/h, chlorine ratio 72%, transformation efficiency 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 modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (9)

1. a chemical method prepares the method for thimerosal, said method comprising the steps of:
A, first by solution of chlorate, hydrochloric acid soln and catalyzer placing response device, the heating;
In B, extraction step A, the reaction chlorine that is able to is main mixed gas;
C, step B gained mixed gas is passed in water, aeration makes thimerosal.
2. method according to claim 1, wherein in steps A, solution of chlorate comprises the strong metal solution of chlorate such as sodium chlorate solution, potassium chlorate solution, described solution of chlorate mass concentration is 20%-40%, hydrochloric acid soln mass concentration 25%-36%; Described heating comprises heating in water bath, oil bath heating and direct heating, and type of heating adopts corrosion-resistant heating tube, and described heating tube is provided with temperature detection and temperature controlling system.
3. method according to claim 1, wherein in steps A, catalyzer can be MnCl 2, FeCl 2, FeCl 3, MnSO 4, FeSO 4, Fe 2(SO 4) 2one or more, the amount of described catalyzer is the 1%-3% of added solution of chlorate amount, is the 3%-5% of added hydrochloric acid soln amount, described catalyzer does not reclaim; The described temperature that is heated to is 70-90 degree centigrade, and the reaction times is 10-60 minute.
4. method according to claim 1, the negative pressure that wherein in step B, in extraction step A, the reaction chlorine that is able to is main mixed gas formation is-90--5KPa.
5. method according to claim 1, wherein the input material volume ratio of the solution of chlorate in steps A and hydrochloric acid soln is 1.5-0.5, according to the difference that generates amount of chlorine, reaction volume is also different, it is 1.0-1.7L that general every generation 1kg chlorine needs the 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 1-20m 3/ h, form concentration 200-1000mg/l thimerosal.
6. one kind for realizing the producer of the described method of claim 1-8 any one, and described producer comprises: solution of chlorate storage tank (1), hydrochloric acid tank (2), hydrochloric acid volume pump (3), hydrochloric acid Traffic Monitor (4), controller (5), solution of chlorate import (6), hydrochloric acid import (7), air inlet snubber (8), venting (9), air 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 liquid adding hole (19), oxymuriate volume pump (20) and oxymuriate Traffic Monitor (21), is characterized in that, the outlet of described solution of chlorate storage tank (1), the outlet of hydrochloric acid tank (2) is connected with the import of hydrochloric acid volume pump (3) with the import of oxymuriate volume pump (20) respectively, the outlet of described oxymuriate volume pump (20), the outlet of hydrochloric acid volume pump (3) is connected with the import of hydrochloric acid Traffic Monitor (4) with the import of oxymuriate Traffic Monitor (21) respectively, the outlet of the outlet of described oxymuriate Traffic Monitor (21) and hydrochloric acid Traffic Monitor (4) is connected with hydrochloric acid import (7) with solution of chlorate import (6) 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 air inlet snubber (8), venting (9), reactor sewage draining exit (15) and an end of air outlet (10) respectively, and the other end of described air outlet (10) is connected with water sprayer (11).
7. producer according to claim 6, is characterized in that, (13) at least 2 grades of described reactors, and it is provided with venting (9), air inlet snubber (8) and reactor sewage draining exit (15).
8. producer according to claim 6, is characterized in that, described controller (5) port respectively with hydrochloric acid volume pump (3), hydrochloric acid Traffic Monitor (4), liquid level detector (12), temperature sensor (16); Heating jacket sewage draining exit (17), heating tube (18), oxymuriate volume pump (20) and oxymuriate Traffic Monitor (21) port are connected, for the temperature of automatic generator reactant, liquid level and the injection rate of reactant and the work output of resultant of detecting reactant.
9. producer according to claim 6, described heating jacket (14) arranges heating tube (18), heating jacket liquid adding hole (19), for reacting by heating thing and injection rate and the work output of controlling reactant.
CN201310471599.2A 2013-10-11 2013-10-11 A kind of method and generator thereof of preparing thimerosal Active CN103482572B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105129733A (en) * 2015-09-21 2015-12-09 宁波镇洋化工发展有限公司 Chlorine gas production technology
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 (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2343152Y (en) * 1998-08-18 1999-10-13 朱明永 Chlorine dioxide disinfectant generator
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
CN203498077U (en) * 2013-10-11 2014-03-26 山东新日电器设备有限公司 Generator for preparing disinfectant

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2343152Y (en) * 1998-08-18 1999-10-13 朱明永 Chlorine dioxide disinfectant generator
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
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)

* Cited by examiner, † Cited by third party
Title
张吉库等: "全盐酸法生产C1O2消毒剂反应条件研究", 《沈阳建筑大学学报(自然科学版)》, vol. 25, no. 4, 31 July 2009 (2009-07-31), pages 741 - 746 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105129733A (en) * 2015-09-21 2015-12-09 宁波镇洋化工发展有限公司 Chlorine gas production technology
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

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