CN107879319B - Preparation method and device of monochloramine - Google Patents
Preparation method and device of monochloramine Download PDFInfo
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- CN107879319B CN107879319B CN201710075590.8A CN201710075590A CN107879319B CN 107879319 B CN107879319 B CN 107879319B CN 201710075590 A CN201710075590 A CN 201710075590A CN 107879319 B CN107879319 B CN 107879319B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/088—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more halogen atoms
- C01B21/09—Halogeno-amines, e.g. chloramine
- C01B21/091—Chloramine, i.e. NH2Cl or dichloramine, i.e. NHCl2
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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Abstract
The invention discloses a preparation method and a device of monochloramine, wherein the preparation method comprises the following steps: (1) taking ammonium chloride and sodium hypochlorite as reaction raw materials, firstly dissolving the ammonium chloride in the reaction raw materials to obtain an ammonium chloride solution, and adding acid to adjust the pH value of the ammonium chloride solution to 1-3; the acid is phosphoric acid and/or hydrochloric acid; (2) adding sodium hypochlorite into the ammonium chloride solution and stirring to increase the pH value to 8-9; (3) respectively adding sodium hypochlorite and a solution containing phosphoric acid into the ammonium chloride solution and stirring to keep the pH value of the mixed solution at 8-9; and obtaining a monochloramine solution after sodium hypochlorite is added. The method has low product cost, and the product concentration reaches 1000 ppm; the stability is relatively good, the storage can be stably carried out for 30 minutes, and the decomposition rate is 1%; the test shows that the pH value of the product is stable and drops slowly.
Description
Technical Field
The invention relates to a preparation method and a device of monochloramine, in particular to a preparation method and a device of monochloramine for tap water disinfection, and relates to the technical field of drinking water disinfectants.
Background
Monochloramine, also known as monochloramine, has the chemical formula NH2Cl is a disinfectant newly added in the new national sanitary standard of drinking water. Since monochloramine is unstable, and particularly, the aqueous solution is easy to decompose, the use mode is selected for preparation at present.
Monochloramine disinfectants are being popularized and used in domestic waterworks. The monochloramine preparation can avoid direct use of chlorine gas and liquid ammonia, namely a process route which takes sodium hypochlorite and ammonium chloride as raw materials is selected. The use of monochloramine is not only free from urban public safety problems, but also free from sanitary safety problems. Monochloramine disinfectants do not risk producing the carcinogen trihalomethane. Compared with chlorine gas, the monochloramine has better disinfection durability and is more beneficial to controlling the propagation of harmful microorganisms in a pipe network, particularly in a dead water area at the tail end of the pipe network. Disinfection by monochloramine does not impart off-flavors to the water as does chlorine disinfection. The monochloramine disinfection is also less corrosive to the water supply network.
Since the chlorine and the liquid ammonia which are highly toxic dangerous goods are directly used as the tap water disinfectant and have potential threat to urban public safety, and the chlorine disinfection by-products also have threat to sanitary safety, people in all circles have reached consensus, and the direct use of the chlorine and the liquid ammonia as the drinking water disinfectant does not meet the requirement of urban development progress, and a more superior disinfectant should be selected for substitution.
Chinese patent application CN200780046526.1 discloses a method for preparing chloramine, which is dichloramine and is mainly used for killing insects. The existing patent methods for existing preparation have the characteristics that: some pay attention to the change of water temperature in different seasons, namely the change of the content of organic ammonia nitrogen in water, and the dosage proportion of the reaction medicament is automatically adjusted according to the change of the temperature to intermittently prepare the monochloramine. The common characteristics of the existing patent methods are high automation degree; compared with manual operation, the technical guarantee requirement for maintaining stable production operation is high, the equipment investment is relatively large, the plant area is relatively large, and the important reaction control condition pH value is not paid attention to or is hardly taken into consideration.
Monochloramine is less stable, is easily decomposed when the pH value exceeds an appropriate range, and is accelerated when the medium temperature is higher. The synthesis and decomposition of monochloramine have large reaction heat and difficult preparation concentration increase; the degradation of monochloramine is accompanied by a decrease in pH, with higher concentrations decreasing more rapidly, making it more difficult to increase the formulated concentration. Therefore, examples of higher concentrations such as 100ppm, i.e., 0.01% by mass, of monochloramine solutions are not common. In addition, main equipment for preparing the monochloramine is huge, and the common on-site preparation almost has no transfer time, so that the occupied area of a workshop is reduced, the process control difficulty is reduced, the yield and the stability of the product are improved (namely, the preparation process and the decomposition after the preparation are reduced), and the monochloramine preparation method has good practical significance for popularization of the application of the monochloramine.
Disclosure of Invention
The invention mainly solves the technical problem that monochloramine with better stability and higher concentration is synthesized by a method with low cost and easy operation and implementation of process control, and can be prevented from being rapidly decomposed, thereby improving the technical effect.
The technical scheme of the invention is to provide a preparation method of monochloramine, which comprises the following steps:
(1) taking ammonium chloride and sodium hypochlorite as reaction raw materials, firstly dissolving the ammonium chloride in the reaction raw materials to obtain an ammonium chloride solution, and adding acid to adjust the pH value of the ammonium chloride solution to 1-3; the acid is phosphoric acid and/or hydrochloric acid;
(2) adding sodium hypochlorite into the ammonium chloride solution and stirring to increase the pH value to 8-9;
(3) respectively adding sodium hypochlorite and a solution containing phosphoric acid into the ammonium chloride solution and stirring to keep the pH value of the mixed solution at 8-9; and obtaining a monochloramine solution after sodium hypochlorite is added.
The invention is greatly different from the prior art in that: the reaction process is controlled by controlling the pH value of the solution, and the stability of the product in the aqueous solution is improved. Wherein, the step (2) is preferably quick feeding, so that the feeding and reaction time is reduced; and (3) balanced feeding is adopted, namely feeding is carried out under the condition of strictly controlling the fluctuation range of the pH value, so that the generated monochloramine is prevented from decomposing.
The monochloramine solution obtained by the preparation method is mainly used for disinfecting tap water, and various indexes of the tap water need to be strictly controlled. Dichloramine and trichloroamine are not suitable for disinfection of tap water due to their properties. Other methods of synthesizing monochloramine in the industry may not be suitable for disinfecting tap water.
Preferably, in the step (3), the pH value of the mixed solution is maintained at 8.6-8.9. Experiments prove that the generated monochloramine is stable under the condition of the pH value.
Preferably, in the step (3), the solution containing phosphoric acid is a phosphoric acid solution or a mixed solution of phosphoric acid and hydrochloric acid.
Preferably, in the step (3), the concentration of phosphoric acid in the phosphoric acid-containing solution is 5% or less. The percentage is a mass percentage, and unless otherwise specified, the concentration of the solution referred to in the present invention is expressed by a mass fraction.
Preferably, the molar ratio of ammonium chloride to sodium hypochlorite in the reaction raw materials is less than or equal to 1.
Preferably, in the step (2), the mass of the added sodium hypochlorite accounts for more than 50% of the total mass of the sodium hypochlorite in the reaction raw materials, and more preferably 50-60%. In the step (3), the mass of the added sodium hypochlorite accounts for less than 50% of the total mass of the sodium hypochlorite in the reaction raw materials, and is more preferably 40-50%.
Preferably, in the step (1), the pH value of the ammonium chloride solution is adjusted to be 1.6-3.
Preferably, in the step (1), the acid is a mixed acid of phosphoric acid and hydrochloric acid; wherein the mass ratio of the phosphoric acid to the hydrochloric acid is 1:2-2: 1. In order to save cost and avoid introducing excessive phosphorus element into tap water, it is preferable to use mixed acid for acidification, and the pH value can be controlled by using the mixed acid in the step (3).
Preferably, in the step (1), the concentration of the ammonium chloride solution is 3% or less.
Preferably, in the step (2) and the step (3), sodium hypochlorite is added in the form of a sodium hypochlorite solution.
Preferably, the concentration of the sodium hypochlorite solution is 3% or less.
Preferably, the preparation method utilizes a device which comprises a reactor, wherein the reactor is respectively connected with a sodium hypochlorite solution feeding metering tank, a hydrochloric acid solution feeding metering tank, a phosphoric acid solution feeding metering tank and a water pipe, and a flowmeter is arranged between the sodium hypochlorite solution feeding metering tank and the reactor. The preparation method comprises the following steps: adding ammonium chloride into a reactor, adding water to dissolve the ammonium chloride, adding acid to adjust the pH value to a corresponding value, quickly adding a sodium hypochlorite solution into the reactor until the pH value is close to 9, slowly adding the sodium hypochlorite solution, simultaneously adding a phosphoric acid solution, controlling the flow rate to enable the pH value to be 8-9, preferably 8.6-8.9, and adding the chemicals according to the formula to obtain the monochloramine solution.
The invention further provides a device for obtaining monochloramine by using the preparation method, which comprises a reactor, wherein the reactor is respectively connected with the sodium hypochlorite solution feeding metering tank, the hydrochloric acid solution feeding metering tank, the phosphoric acid solution feeding metering tank and the water pipe, and a flowmeter is arranged between the sodium hypochlorite solution feeding metering tank and the reactor. Preferably, a flow meter is also provided between the phosphoric acid solution feed metering tank and the reactor.
The present invention aims to simplify the manual method from the source of technological principle, raise the competitive power of the method and make it suitable for use in small and medium water works.
The invention is a method for artificially preparing monochloramine in situ; the invention overcomes or relieves the defects of the manual method as much as possible, and simultaneously exerts and expands the advantages of the manual method as much as possible; the invention has strong market competitiveness in small and medium-sized waterworks.
The technical solution adopted by the present invention is further described below. The invention adopts an intermittent production mode, the raw materials adopt ammonium chloride and sodium hypochlorite, and the process comprises six steps:
a. preparing materials: pre-preparing sodium hypochlorite, diluting the raw material sodium hypochlorite with water to obtain sodium hypochlorite with the concentration of 0.5-1%; pre-preparing an acid material, and diluting the raw material phosphoric acid with water to obtain a concentration of about 5%. The starting hydrochloric acid was diluted to 5% with water.
b. Dissolving ammonium chloride. Ammonium chloride and water are directly fed into the reactor to dissolve the ammonium chloride, and the concentration is 1-2%.
c. And acidifying the ammonium chloride solution. A small amount of acid is metered in to bring the pH of the ammonium chloride solution down to below 3, preferably from 1.6 to 3, more preferably from 1.6 to 2.0.
d. And feeding in the early stage of reaction. More than half of the amount of sodium hypochlorite is added rapidly within 3 minutes to raise the pH of the reaction solution from 3 or below to approximately 9, and then the water required by the formula is added.
e. And (4) carrying out later-stage reaction feeding, namely acid-base balance feeding. The flow is controlled to be about 15 minutes, the rest sodium hypochlorite, namely about half of the dosage of the formula is added, and a proper amount of about 5 percent phosphoric acid is added under the condition of controlling the pH value to be 8.6-8.9. The feeding molar ratio of the ammonium chloride to the sodium hypochlorite of the whole formula is less than or equal to 1.
f. And (5) diluting the semi-finished product. Inverse directionDiluting the semi-finished product with water to obtain a finished product after the feeding is finished; or diluted according to relevant national standards and then immediately output for tap water application. Finished product NH of the invention2The Cl concentration can reach about 1000ppm (mass fraction is 0.1 percent).
In the preparation method, the sodium hypochlorite is fed in two steps (step d and step e), and the feeding time and the feeding speed of the sodium hypochlorite meet the control requirements. The early feeding is controlled within 3 minutes, and the late feeding is controlled within 12-18 minutes or about 15 minutes.
The preparation method of the present invention has the following advantages.
One of the advantages is that the ammonium chloride raw material is directly used for dissolving in the reactor, the ammonium chloride solution storage tank and the auxiliary equipment thereof are saved, and meanwhile, the dissolution heat absorption of the ammonium chloride is reasonably utilized, which is beneficial to the control of the reaction temperature.
The second advantage is that sodium hypochlorite is added after all ammonium chloride is fed, and the excess of ammonium chloride in the reaction process can be ensured under the operating condition, so that the generation of side reaction products of dichloramine and trichloroamine can be controlled.
Third of the advantage, acidify ammonium chloride solution in advance, for the quick reinforced condition of having created in earlier stage of sodium hypochlorite, be favorable to shortening production cycle, acidify in advance just can guarantee to add more sodium hypochlorite material and be unlikely to make the pH value of mixing material higher than usual once, can avoid generating the decomposition of monochloramine.
Fourthly, the acid-base equilibrium feeding is implemented by using phosphoric acid as an acid material and an alkaline material sodium hypochlorite at the later stage, and more than one dose of the phosphoric acid can be fully embodied: phosphoric acid is both an acid material and an inhibitor of harmful heavy metal ions, and is also a pH buffer. The phosphoric acid neutralization product is a phosphate. The disodium hydrogen phosphate salt has a pH of 9, and the rate of pH drop of the product can be retarded around pH = 9. The decrease in pH is extremely detrimental to the stability of the product, the monochloramine product rapidly decomposes, and the decomposed product further contributes to the decrease in pH. In addition, according to some literature reports, the pH at which the stability of monochloramine products is optimal may be in the range of 8.3 to 8.5.
Fifth, the reactant is after mixing, the time to finish reaction is 7 minutes, in the key moment after the monochloramine products produce and produce, namely the later stage of technological process of the invention, pay attention to the control of the condition of pH value extremely, it is worthy of recommending, it is scientific. The pH value is controlled before the mixing operation of the reaction materials is finished, and compared with the pH value controlled after the mixing operation is finished, the pH value control method is a better technical improvement and has better technical effect.
The method has the advantages that the conventional process flow of discharging finished products from the reactor is changed into the process flow of discharging the finished products from the transfer storage tank, so that the labor production efficiency of the main equipment reactor is improved, or the volume of the reactor is reduced.
Specifically, the method of the invention has the advantages that the use of the additive is more scientific, and the reaction control is more scientific in sections; the production period is short, the conversion rate of the monochloramine is high, and the equipment investment and the equipment floor area are small; the operation is simple, the control condition is easy to realize, and the requirements on the quality of operators are not high. In a 5-thousand-ton monthly water plant, the preparation system is only required to be equipped with a 500-liter reactor and a 1000-liter transfer tank and its particularly small equipment container.
The method has low product cost, and the product concentration reaches 1000 ppm; the stability is relatively good, the storage can be stably carried out for 30 minutes, and the decomposition rate is 1%; the test shows that the pH value of the product is stable and drops slowly.
Drawings
FIG. 1 shows an apparatus for producing monochloramine used in an embodiment of the present invention;
in the drawings, 1-a transfer tank; 2-a reactor; 3-sodium hypochlorite solution feeding metering tank; 4-hydrochloric acid solution feeding metering tank; a metering tank for feeding 5-phosphoric acid solution; 6-sodium hydroxide solution feed tank; 7-flow meter.
Detailed Description
The invention is further illustrated by the following figures and examples.
Example 1
17 kg of sodium hypochlorite is measured, sodium hypochlorite solution is added into a metering tank 3 (hereinafter referred to as metering tank 3), and the sodium hypochlorite solution is metered by a metering pump240 kg of raw material water is input into a metering tank 3; the sodium hypochlorite concentration in the measuring tank 3 is 0.7 percent by NaClO, and the total amount of the solution is 257 kilograms. 1.3 kg of powder ammonium chloride is measured and put into a reactor 2; simultaneously, 85 kilograms of raw material water is metered by a metering pump and is input into the reactor 2; simultaneously, 2 kilograms of 5 percent HCl is measured by a liquid level measuring method and is input into the reactor 2 from the hydrochloric acid solution feeding measuring tank 4; in the reactor 2, the concentration of ammonium chloride was 1.465%, the total amount of the solution was 88.3 kg, and the pH was 2.2. 147 kg of 0.7% NaClO were added rapidly to the reactor 2 over 2 minutes to raise the pH of the reaction solution to 8.9, after which 150 kg of feed water were metered into the reactor 2 by means of a pump. Starting a slow speed to continuously dropwise add 0.7% NaClO to the reactor 2, and intermittently dropwise adding 5% H to the reactor 2 through a phosphoric acid solution feeding metering tank 53PO4The flow rate was controlled by a flow meter 7 so that the fluctuation of the pH of the reaction solution was controlled within a range of 8.6 to 8.9. In the case of acid-base equilibrium addition, the 0.7% NaClO was added at a rate of 0.18 kg per second, and 5% H was added to reactor 23PO4Is 3 kg. 498 kg of semifinished product are discharged from the reactor 2 into a transfer tank 1, and 500 kg of feed water are metered into the transfer tank 1 by means of a metering pump. The finished monochloramine, NH, is output from the transfer tank 12Cl content 0.11%. Wherein if NH exists in the transfer storage tank 12The pH reduction caused by the decomposition of Cl can be controlled up by the sodium hydroxide solution feed tank 6.
Example 2
Measuring 17 kg of raw material sodium hypochlorite and putting into a measuring tank 3, and measuring 240 kg of raw material water by a measuring pump and inputting into the measuring tank 3; the sodium hypochlorite concentration in the measuring tank 3 is 0.7 percent by NaClO, and the total amount of the solution is 257 kilograms. 1.3 kg of powder ammonium chloride is measured and put into a reactor 2; simultaneously, 88 kg of raw material water is metered by a metering pump and is input into the reactor 2; simultaneously, 2.5 kilograms of 5 percent HCl is measured by a liquid level measuring method and is input into the reactor 2 from the hydrochloric acid solution feeding measuring tank 4; in the reactor 2, the concentration of ammonium chloride was 1.41%, the total amount of the solution was 91.8 kg, and the pH was 1.64. 206 kg of 0.7% NaClO were rapidly added to the reactor 2 over 2 minutes to raise the pH of the reaction solution to 8.9, and 150 kg of feed water were then metered into the reactor 2 by means of a pump. 0.7 percent of NaClO is continuously dripped into the reactor 2 at a slow speed, and simultaneously, the reactor is intermittently fed with phosphoric acid solution through a feeding metering groove 52 dropwise addition of 5% H3PO4The pH value fluctuation of the reaction solution was controlled within the range of 8.6 to 8.9. In the case of acid-base equilibrium addition, the 0.7% NaClO was added at a rate of 0.1 kg per second to 5% H in reactor 23PO4Is 1 kg. 499.5 kg of the semifinished product were discharged from the reactor 2 into the transfer tank 1, and 500 kg of the raw material water was metered into the transfer tank 1 by a metering pump. The finished monochloramine, NH, is output from the transfer tank 12Cl content 0.11%, pH 8.86.
Example 3
Measuring 17 kg of raw material sodium hypochlorite and putting into a measuring tank 3, and measuring 240 kg of raw material water by a measuring pump and inputting into the measuring tank 3; the sodium hypochlorite concentration in the measuring tank 3 is 0.7 percent by NaClO, and the total amount of the solution is 257 kilograms. 1.3 kg of powder ammonium chloride is measured and put into a reactor 2; simultaneously, 88 kg of raw material water is metered by a metering pump and is input into the reactor 2; at the same time, 4 kg of 5% mixed acid, which is 5% HCl and 5% H, is metered by a liquid level metering method and fed into the reactor 23PO4Mixing according to the weight ratio of 1: 1; in reactor 2, the concentration of ammonium chloride was 1.39%, the total amount of the solution was 93.3 kg, and the pH was 2.16. 188 kg of 0.7% NaClO were rapidly added to the reactor 2 over 2 minutes to raise the pH of the reaction solution to 8.9, and 150 kg of feed water were subsequently metered into the reactor 2 by means of a pump. Starting a slow speed to continuously dropwise add 0.7% NaClO to the reactor 2, and intermittently dropwise adding 5% mixed acid to the reactor 2 to control the fluctuation of the pH value of the reaction liquid within the range of 8.6-8.9. In the acid-base equilibrium, the 0.7% NaClO was added at a rate of 0.12 kg per second and the 5% mixed acid added to the reactor 2 was 1.6 kg. 501.5 kg of the semifinished product are discharged from the reactor 2 into the transfer tank 1, and 500 kg of the raw material water are metered by a metering pump into the transfer tank 1. The finished monochloramine, NH, is output from the transfer tank 12Cl content 0.11%.
Claims (9)
1. The preparation method of monochloramine is characterized by comprising the following steps:
(1) taking ammonium chloride and sodium hypochlorite as reaction raw materials, firstly dissolving the ammonium chloride in the reaction raw materials to obtain an ammonium chloride solution, and adding acid to adjust the pH value of the ammonium chloride solution to 1-3; the acid is phosphoric acid and/or hydrochloric acid;
(2) adding sodium hypochlorite into the ammonium chloride solution and stirring to increase the pH value to 8-9;
(3) respectively adding sodium hypochlorite and a solution containing phosphoric acid into the ammonium chloride solution, and stirring to keep the pH value of the mixed solution at 8-9; and obtaining a monochloramine solution after sodium hypochlorite is added.
2. The method according to claim 1, wherein in the step (3), the pH of the mixed solution is maintained at 8.6 to 8.9.
3. The method according to claim 1, wherein in the step (3), the concentration of phosphoric acid in the phosphoric acid-containing solution is 5% or less.
4. The method according to claim 1, wherein in the step (1), the pH of the ammonium chloride solution is adjusted to 1.6 to 3.
5. The method according to claim 1, wherein in the step (1), the acid is a mixed acid of phosphoric acid and hydrochloric acid; wherein the mass ratio of the phosphoric acid to the hydrochloric acid is 1:2-2: 1.
6. The method according to claim 1, wherein in the step (1), the concentration of the ammonium chloride solution is 3% or less.
7. The method according to claim 1, wherein in the steps (2) and (3), sodium hypochlorite is added in the form of a sodium hypochlorite solution.
8. The method according to claim 7, wherein the concentration of the sodium hypochlorite solution is 3% or less.
9. The method according to claim 1, wherein the method utilizes an apparatus comprising a reactor connected to a sodium hypochlorite solution feeding metering tank, a hydrochloric acid solution feeding metering tank, a phosphoric acid solution feeding metering tank and a water pipe, respectively, and a flow meter is provided between the sodium hypochlorite solution feeding metering tank and the reactor.
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