CN117069211B - Dibromohydantoin compound water treatment agent for black and odorous water treatment - Google Patents
Dibromohydantoin compound water treatment agent for black and odorous water treatment Download PDFInfo
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- CN117069211B CN117069211B CN202311331140.2A CN202311331140A CN117069211B CN 117069211 B CN117069211 B CN 117069211B CN 202311331140 A CN202311331140 A CN 202311331140A CN 117069211 B CN117069211 B CN 117069211B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 153
- -1 Dibromohydantoin compound Chemical class 0.000 title claims abstract description 68
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 59
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 101
- 238000004090 dissolution Methods 0.000 claims abstract description 61
- MENYRYNFSIBDQN-UHFFFAOYSA-N 5,5-dibromoimidazolidine-2,4-dione Chemical compound BrC1(Br)NC(=O)NC1=O MENYRYNFSIBDQN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000002156 mixing Methods 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000006184 cosolvent Substances 0.000 claims abstract description 33
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229920001983 poloxamer Polymers 0.000 claims abstract description 22
- 229960000502 poloxamer Drugs 0.000 claims abstract description 22
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000002699 waste material Substances 0.000 claims abstract description 14
- 238000005086 pumping Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 230000005484 gravity Effects 0.000 claims description 97
- 239000007788 liquid Substances 0.000 claims description 53
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 39
- 238000005406 washing Methods 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 34
- 239000003814 drug Substances 0.000 claims description 33
- 235000019441 ethanol Nutrition 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 21
- 239000000706 filtrate Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 17
- 239000000725 suspension Substances 0.000 claims description 17
- 239000002243 precursor Substances 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 11
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 claims description 10
- 238000010298 pulverizing process Methods 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N monoethanolamine hydrochloride Natural products NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 229920001993 poloxamer 188 Polymers 0.000 claims description 5
- 229940044519 poloxamer 188 Drugs 0.000 claims description 5
- 229920001992 poloxamer 407 Polymers 0.000 claims description 5
- 229940044476 poloxamer 407 Drugs 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012047 saturated solution Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000645 desinfectant Substances 0.000 description 2
- 230000002147 killing effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013535 sea water Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- XAEZQQVZRXSKKJ-UHFFFAOYSA-N 1,3-dibromoimidazolidine-2,4-dione Chemical compound BrN1CC(=O)N(Br)C1=O XAEZQQVZRXSKKJ-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- VRLDVERQJMEPIF-UHFFFAOYSA-N dbdmh Chemical compound CC1(C)N(Br)C(=O)N(Br)C1=O VRLDVERQJMEPIF-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a dibromohydantoin compound water treatment agent for black and odorous water treatment. The dibromohydantoin compound water treatment agent for treating black and odorous water body comprises the following preparation processes: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing; pumping a mixing agent to react to prepare a cosolvent; mixing and melting dibromohydantoin and mixed poloxamer; cooling, solidifying, crushing and grinding; ultrasonically dissolving and adding a cosolvent. According to the invention, the dibromohydantoin and the mixed poloxamer are mixed and dispersed, then heated, melted and mixed, cooled and solidified, then dissolved in ethanol, mixed with a cosolvent, and subjected to filter pressing and drying, so that the obtained dibromohydantoin compound water treatment agent has better water solubility and faster dissolution rate than that of dibromohydantoin, thereby improving the treatment efficiency of dibromohydantoin on black and odorous water bodies, reducing the waste of the dibromohydantoin water treatment agent and reducing the treatment cost.
Description
Technical Field
The invention relates to the technical field of bioengineering, in particular to a dibromohydantoin compound water treatment agent for black and odorous water treatment.
Background
Dibromohydantoin, 1, 3-dibromo-5, 5-dimethyl hydantoin or 1, 3-dibromo-2, 4-imidazoline dione, its molecular formula is C 5 H 6 Br 2 N 2 O 2 The disinfectant is usually white or light yellow solid, has stronger killing or inhibiting effect on most common microorganisms and viruses, has the functions of killing buds and holding, has wide sterilization range, high stability, is nontoxic and non-irritating to people, can be naturally decomposed after being sterilized, has no pollution to the environment, is an environment-friendly high-efficiency oxidation disinfectant, and can be used for treating polluted water.
At present, the existing dibromohydantoin water treatment medicament is divided into solid and liquid, wherein the solid dibromohydantoin water treatment medicament has low treatment efficiency on polluted water due to low water solubility and low dissolution speed, and the aim of treating sewage can be fulfilled only by consuming a large amount of dibromohydantoin water treatment medicament, so that the waste of the dibromohydantoin water treatment medicament is caused, and the treatment cost is greatly increased.
Therefore, the dibromohydantoin compound water treatment agent for treating black and odorous water body has good water solubility and high dissolution speed, so that the sewage treatment efficiency is improved, and the waste is reduced.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a dibromohydantoin compound water treatment agent for treating black and odorous water bodies.
A dibromohydantoin compound water treatment agent for black and odorous water treatment comprises the following preparation processes:
s1: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing
Adding deionized water, ethanol and triethylamine into a stirrer, adding cetyltrimethylammonium bromide, heating, stirring and mixing to obtain a premix;
s2: pumping the mixture to react and prepare the cosolvent
Pumping the mixture into the premix at a constant speed, stirring for reaction, filtering and washing, adding hydrochloric acid-methanol solution for soaking, filtering and drying to obtain a cosolvent;
s3: mixing and melting dibromohydantoin and mixed poloxamer
Mixing dibromohydantoin and mixed poloxamer together at high speed, stirring and heating to fully melt to obtain a mixed melt;
s4: cooling, solidifying and pulverizing
Turning off the heater, stopping heating, gradually naturally cooling and solidifying the mixed melt, cooling to room temperature, adding into a crushing grinder, and crushing and grinding to obtain dibromohydantoin mixed material;
s5: ultrasonic dissolving and adding cosolvent
Mixing the dibromohydantoin mixed material with ethanol, performing ultrasonic dissolution, adding the cosolvent, stirring, and performing filter pressing, drying and crushing to obtain the dibromohydantoin compound water treatment medicament.
Further, the step S1 of adding cetyl trimethyl ammonium bromide, heating, stirring and mixing comprises the following steps:
s1.1: adding deionized water, ethanol and triethylamine into a stirrer together according to the volume ratio of 300-400:50-60:1 until a liquid level sensor in the stirrer detects that the liquid level in the stirrer is not increased any more, and sending a signal to a controller by the liquid level sensor;
s1.2: after the controller receives the signal sent by the liquid level sensor, the feeding component is controlled to add hexadecyl trimethyl ammonium bromide into the stirrer according to the solid-to-liquid ratio of 1g to 150-200mL until a first gravity sensor in the stirrer detects that the gravity in the stirrer is not increased any more, and the first gravity sensor sends a signal to the controller;
s1.3: after the controller receives the signal sent by the first gravity sensor, the first heater in the stirrer is controlled to heat at the temperature of 70-80 ℃, and the stirrer is controlled to stir for 2-3 hours at the speed of 400-600r/min, so that the premix liquid is obtained.
Further, the step S2 of pumping the mixture for reaction to prepare the cosolvent specifically comprises the following steps:
s2.1: the controller controls the stirring speed of the stirrer to be 800-1000r/min, controls the hydraulic pump to pump the mixture into the premix prepared in the step S1.3 at a constant speed of 3-5mL/min, and carries out stirring reaction for 6-8h to obtain suspension;
s2.2: the controller controls a centrifugal filter device in the stirrer to start, centrifugally filters the suspension, and discharges filtrate to obtain filter residues;
s2.3: opening a washing component in the stirrer, introducing absolute ethyl alcohol into the stirrer through the washing component, washing the filter residues for 2-3 times, introducing deionized water into the stirrer, washing the filter residues washed by the absolute ethyl alcohol for 2-3 times again, and removing impurity reactants to obtain pure filter residues;
s2.4: adding hydrochloric acid-methanol solution containing 0.5-1% hydrochloric acid into a stirrer until the hydrochloric acid-methanol solution submerges the pure filter residues, soaking for 8-10h, filtering and drying to obtain the cosolvent.
Further, the step S3 of mixing and melting dibromohydantoin and mixed poloxamer specifically comprises the following steps:
s3.1: adding dibromohydantoin and mixed poloxamer into the high-speed dispersing machine together according to the mass ratio of 1:10-12 until a second gravity sensor in the high-speed dispersing machine detects that the gravity in the box is not increased any more, and sending a signal to a controller by the second gravity sensor;
s3.2: after the controller receives the signal sent by the second gravity sensor, the high-speed dispersing machine is controlled to disperse for 30-40min at the speed of 4000-5000r/min to obtain a mixed material;
s3.3: opening a discharge valve of the high-speed dispersing machine, and throwing the mixed materials into a melting tank until the second gravity sensor detects that the gravity in the high-speed dispersing machine is 0, and sending a signal to the controller again by the second gravity sensor;
s3.4: and after receiving the signal sent by the second gravity sensor again, the controller controls a second heater in the melting tank to heat the mixed material at 200-250 ℃ and controls the stirrer to stir at the speed of 300-500r/min until the mixed material is completely melted, so as to obtain a mixed melt.
Further, the ultrasonic dissolution in the step S5 and the addition of a cosolvent specifically comprise the following steps:
s5.1: adding the dibromohydantoin mixed material prepared in the step S4 and ethanol into an ultrasonic dissolution tank according to a solid-to-liquid ratio of 1g to 3-5mL until a third gravity sensor in the ultrasonic dissolution tank detects that the gravity in the ultrasonic dissolution tank is not increased any more, and sending a signal to a controller by the third gravity sensor;
s5.2: after the controller receives the signal sent by the third gravity sensor, controlling the ultrasonic dissolving box to assist dissolving for 20-30min at the frequency of 20-30kHz to obtain dissolving liquid;
s5.3: adding the cosolvent prepared in the step S2.4 into the dissolving liquid until the third gravity sensor detects that the gravity in the ultrasonic dissolving tank is not increased again, and sending a signal to the controller again by the third gravity sensor;
s5.4: after receiving the signal sent by the third gravity sensor again, the controller controls a second stirrer in the ultrasonic dissolving tank to stir for 18-24 hours at the speed of 100-200r/min, so as to obtain suspension;
s5.5: the controller controls a filter pressing assembly in the ultrasonic dissolution box to be opened, and the suspension is subjected to filter pressing through the filter pressing assembly to obtain a precursor medicament;
s5.6: and (3) placing the precursor medicament in an oven, drying at 80-90 ℃, adding into a pulverizer, and pulverizing to obtain the dibromohydantoin compound water treatment medicament.
Further, after centrifugal filtration in the step S2.2, discharging filtrate into a rectifying tower, discharging washing waste liquid discharged after washing absolute ethyl alcohol in the step S2.3 into the rectifying tower, mixing with the filtrate, heating the rectifying tower, condensing and recovering ethanol, and then in the production of a next batch of dibromohydantoin compound water treatment medicament, mixing the recovered ethanol with deionized water, triethylamine and cetyltrimethylammonium bromide to prepare a premix in the step S1.1.
Further, the mixture is prepared by mixing tetraethoxysilane and tetrasulfide according to a volume ratio of 2-3:1, and the volume ratio of the mixture to the premix is 1:90-100.
Further, the hydrochloric acid-methanol solution is a mixed solution of hydrochloric acid and methanol, wherein the content of hydrochloric acid is 0.5-1%.
Further, the mixed poloxamer is prepared by mixing poloxamer 188 and poloxamer 407 according to the mass ratio of 1-3:1.
Further, the solid-to-liquid ratio of the dibromohydantoin mixed material to the ethanol is 1g:3-5mL.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the dibromohydantoin and the mixed poloxamer are mixed and dispersed, then heated, melted and mixed, cooled and solidified, then dissolved in ethanol, mixed with a cosolvent, and subjected to filter pressing and drying, so that the obtained dibromohydantoin compound water treatment agent has better water solubility and faster dissolution rate than that of dibromohydantoin, thereby improving the treatment efficiency of dibromohydantoin on black and odorous water bodies, reducing the waste of the dibromohydantoin water treatment agent and reducing the treatment cost.
2. According to the invention, hexadecyl trimethyl ammonium bromide, ethanol, triethylamine and deionized water are premixed, and then tetraethoxysilane and tetrasulfide are added to prepare the mixture for reaction, so that the prepared cosolvent not only can improve the solubility of dibromohydantoin, but also has degradability, and the prepared dibromohydantoin compound water treatment agent can not cause secondary pollution to water after black and odorous water is treated, thereby achieving the effect of green and environment-friendly.
3. According to the invention, the ethanol in the filtrate and the washing waste liquid is recovered through condensation, and the recovered ethanol is used in the production of dibromohydantoin compound water treatment medicament in the next batch, so that the purpose of recycling is achieved, the resources are saved, and the waste is reduced.
Drawings
Fig. 1 is a flow chart of a preparation process of a dibromohydantoin compound water treatment agent for black and odorous water body treatment, which is adopted in the embodiment of the invention.
FIG. 2 is a summary of experimental test results for example 1, example 2 and example 3 of the present invention.
FIG. 3 is a summary of experimental test results of example 1 and comparative example 1 of the present invention.
FIG. 4 is a summary of experimental test results of inventive example 1 and comparative example 2.
FIG. 5 is a summary of experimental test results of example 1 and comparative example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The dibromohydantoin compound water treatment agent for black and odorous water treatment is shown in fig. 1 and 2, and comprises the following preparation processes:
s1: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing
Adding deionized water, ethanol and triethylamine into a stirrer together according to a volume ratio of 300:50:1 until a liquid level sensor in the stirrer detects that the liquid level in the stirrer is not increased any more, sending a signal to a controller by the liquid level sensor, controlling a feeding component to add cetyltrimethylammonium bromide into the stirrer according to a solid-to-liquid ratio of 1g:150mL after the controller receives the signal sent by the liquid level sensor, sending a signal to the controller by a first gravity sensor until the first gravity sensor in the stirrer detects that the gravity in the stirrer is not increased any more, and controlling a first heater in the stirrer to heat at 70 ℃ after receiving the signal sent by the first gravity sensor, and simultaneously controlling the stirrer to stir for 2 hours at a speed of 400r/min to obtain premixed liquid;
s2: pumping the mixture to react and prepare the cosolvent
The method comprises the steps that a controller controls the stirring speed of a stirrer to be 800r/min, controls a hydraulic pump to mix and prepare a mixture of ethyl orthosilicate and tetrasulfide according to a volume ratio of 2:1, pumps the mixture into the premix according to a volume ratio of 1:90 of the mixture to the premix, stirring and reacting for 6 hours to obtain a suspension, then controls a centrifugal filtering device in the stirrer to start, centrifugally filters the suspension, discharges filtrate to obtain filter residues, then opens a washing component in the stirrer, washes the filter residues for 2 times through the washing component, discharges the filtrate obtained by centrifugal filtration into a rectifying tower, discharges washing waste liquid discharged after washing the absolute ethanol into the rectifying tower, mixes the filtrate with the rectifying tower, condenses and recovers ethanol, and then mixes the recovered ethanol with deionized water, triethylamine and hexadecyl trimethyl ammonium bromide into the premix in the production of a next batch of the dibromo compound water treatment agent, then discharges filtrate into the stirrer, washes the filter residues for 2 times through the washing component, and then discharges the filter residues into the filter residues, and obtains pure hydrochloric acid solution after washing with the filter residues, and the filter residues are washed for 8 times, and the filter residues are washed again, and the pure hydrochloric acid solution is obtained after the filter residues are washed for 8 times, and the filter residues are washed, and the pure hydrochloric acid is washed and washed for 8 times;
s3: mixing and melting dibromohydantoin and mixed poloxamer
Adding dibromohydantoin and mixed poloxamer prepared by mixing poloxamer 188 and poloxamer 407 according to the mass ratio of 1:1 into a high-speed dispersing machine together according to the mass ratio of 1:10, until a second gravity sensor in the high-speed dispersing machine detects that the gravity in a box is not increased any more, sending a signal to a controller by the second gravity sensor, after receiving the signal sent by the second gravity sensor, controlling the high-speed dispersing machine to disperse at the speed of 4000r/min for 30min to obtain a mixed material, then opening a discharge valve of the high-speed dispersing machine, throwing the mixed material into a melting tank until the second gravity sensor detects that the gravity in the high-speed dispersing machine is 0, sending a signal to the controller again, after receiving the signal sent by the second gravity sensor again by the controller, controlling a second heater in the melting tank to heat the mixed material at 200 ℃, and simultaneously controlling a stirrer to stir at the speed of 300r/min until the mixed material is completely melted to obtain a mixed melt;
s4: cooling, solidifying and pulverizing
Turning off the heater, stopping heating, gradually naturally cooling and solidifying the mixed melt, cooling to room temperature, adding into a crushing grinder, and crushing and grinding to obtain dibromohydantoin mixed material;
s5: ultrasonic dissolving and adding cosolvent
Adding the dibromohydantoin mixed material and ethanol into an ultrasonic dissolution tank together according to a solid-to-liquid ratio of 1g to 3mL, until a third gravity sensor in the ultrasonic dissolution tank detects that the gravity in the ultrasonic dissolution tank is no longer increased, sending a signal to a controller by the third gravity sensor, controlling the ultrasonic dissolution tank to carry out ultrasonic dissolution assistance for 20min at a frequency of 20kHz after receiving the signal sent by the third gravity sensor by the controller, obtaining dissolution liquid, adding the cosolvent prepared in the step S2 into the dissolution liquid until the third gravity sensor detects that the gravity in the ultrasonic dissolution tank is no longer increased again, sending the signal to the controller again by the third gravity sensor, controlling a second stirrer in the ultrasonic dissolution tank to stir for 18h at a speed of 100r/min after the controller receives the signal sent by the third gravity sensor again, obtaining a suspension, then controlling a filter pressing component in the ultrasonic dissolution tank to be opened by the controller, obtaining a precursor medicament through the filter pressing component, finally, placing the precursor medicament into an oven, drying at a temperature of 80 ℃ and adding the precursor medicament into a pulverizer, and pulverizing to obtain the dibromohydantoin compound seawater medicament.
Then, experimental tests are carried out on the prepared dibromohydantoin compound water treatment medicament:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then the prepared dibromohydantoin compound water treatment agent is added into the deionized water to be fully dissolved to prepare a saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 5.12g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 10.24% according to a solubility formula;
then, 5.12g of dibromohydantoin compound water treatment agent is weighed and added into 50mL of deionized water at 20 ℃, and the mixture is stirred by a magnetic stirrer at a speed of 100r/min until the mixture is completely dissolved, and the complete dissolution time is about 9.5s, namely the unit dissolution rate is about 0.5389g/s.
Example two
The dibromohydantoin compound water treatment agent for black and odorous water treatment is shown in fig. 1 and 2, and comprises the following preparation processes:
s1: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing
Adding deionized water, ethanol and triethylamine into a stirrer together according to a volume ratio of 350:55:1 until a liquid level sensor in the stirrer detects that the liquid level in the stirrer is not increased any more, sending a signal to a controller by the liquid level sensor, controlling a feeding component to add cetyltrimethylammonium bromide into the stirrer according to a solid-to-liquid ratio of 1g:175mL after the controller receives the signal sent by the liquid level sensor, sending a signal to the controller by a first gravity sensor until the first gravity sensor in the stirrer detects that the gravity in the stirrer is not increased any more, and controlling a first heater in the stirrer to heat at 75 ℃ after receiving the signal sent by the first gravity sensor, and simultaneously controlling the stirrer to stir for 2.5h at a speed of 500r/min to obtain premixed liquid;
s2: pumping the mixture to react and prepare the cosolvent
The method comprises the steps of controlling the stirring speed of a stirrer to be 900r/min, controlling a hydraulic pump to mix tetrasulfide with ethyl orthosilicate at a volume ratio of 2.5:1, pumping a mixture prepared by mixing tetrasulfide with ethyl orthosilicate at a volume ratio of 1:95 into the premix, stirring for 7h to obtain a suspension, controlling a centrifugal filter device in the stirrer to start, centrifugally filtering the suspension, discharging filtrate to obtain filter residues, opening a washing component in the stirrer, introducing absolute ethyl alcohol into the stirrer through the washing component, washing the filter residues for 2 times, discharging the filtrate obtained by centrifugal filtration into a rectifying tower, discharging washing waste liquid discharged after washing the absolute ethyl alcohol into the rectifying tower, mixing the filtrate with the rectifying tower, heating the rectifying tower, condensing and recovering ethanol, then mixing the recovered ethanol with deionized water, triethylamine and cetyltrimethylammonium bromide in the production of a next batch of the dibromo compound water treatment medicament, stirring the premix, introducing absolute ethyl alcohol into the stirrer, washing the filter residues into the filter residues, washing solution, soaking the filter residues into the filter residues for 2 times, and obtaining hydrochloric acid solution after the filter residues are soaked in the solution, washing solution, and washing the solution is dried for 75 h, and filtering the filter residues after the solution is washed to obtain the solution, and the filter residues are washed and washed by the hydrochloric acid after the solution is washed and washed by the hydrochloric acid is washed by the pure solution and washed by the hydrochloric acid;
s3: mixing and melting dibromohydantoin and mixed poloxamer
Adding dibromohydantoin and mixed poloxamer prepared by mixing poloxamer 188 and poloxamer 407 according to the mass ratio of 2:1 into a high-speed dispersing machine together according to the mass ratio of 1:11, until a second gravity sensor in the high-speed dispersing machine detects that the gravity in a box is not increased any more, sending a signal to a controller by the second gravity sensor, after receiving the signal sent by the second gravity sensor, controlling the high-speed dispersing machine to disperse for 35min at the speed of 4500r/min to obtain a mixed material, then opening a discharge valve of the high-speed dispersing machine, adding the mixed material into a melting tank until the second gravity sensor detects that the gravity in the high-speed dispersing machine is 0, sending a signal to the controller again, after receiving the signal sent by the second gravity sensor again, controlling a second heater in the melting tank to heat the mixed material at 225 ℃, and simultaneously controlling a stirrer to stir at the speed of 400r/min until the mixed material is completely melted to obtain a mixed melt;
s4: cooling, solidifying and pulverizing
Turning off the heater, stopping heating, gradually naturally cooling and solidifying the mixed melt, cooling to room temperature, adding into a crushing grinder, and crushing and grinding to obtain dibromohydantoin mixed material;
s5: ultrasonic dissolving and adding cosolvent
Adding the dibromohydantoin mixed material and ethanol into an ultrasonic dissolution tank together according to a solid-to-liquid ratio of 1g to 4mL, until a third gravity sensor in the ultrasonic dissolution tank detects that the gravity in the ultrasonic dissolution tank is no longer increased, sending a signal to a controller by the third gravity sensor, controlling the ultrasonic dissolution tank to carry out ultrasonic dissolution assistance at a frequency of 25kHz for 25min after receiving the signal sent by the third gravity sensor by the controller, obtaining dissolution liquid, adding the cosolvent prepared in the step S2 into the dissolution liquid until the third gravity sensor detects that the gravity in the ultrasonic dissolution tank is no longer increased again, sending the signal to the controller again by the third gravity sensor, controlling a second stirrer in the ultrasonic dissolution tank to stir at a speed of 150r/min for 20h after the controller receives the signal sent by the third gravity sensor again, obtaining a suspension, then controlling a filter pressing component in the ultrasonic dissolution tank to be opened, obtaining a precursor medicament through the filter pressing component, finally, placing the precursor medicament into an oven, drying at a temperature of 85 ℃ and adding the precursor medicament into a pulverizer, and pulverizing to obtain the dibromohydantoin compound seawater medicament.
Then, experimental tests are carried out on the prepared dibromohydantoin compound water treatment medicament:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then the prepared dibromohydantoin compound water treatment agent is added into the deionized water to be fully dissolved to prepare a saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 5.2g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 10.4 percent according to a solubility formula;
then, 5.4g of dibromohydantoin compound water treatment agent is weighed and added into 50mL of deionized water at 20 ℃, and the mixture is stirred by a magnetic stirrer at a speed of 100r/min until the mixture is completely dissolved, and the complete dissolution time is about 9.6s, namely the unit dissolution rate is about 0.5625g/s.
Example III
The dibromohydantoin compound water treatment agent for black and odorous water treatment is shown in fig. 1 and 2, and comprises the following preparation processes:
s1: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing
Adding deionized water, ethanol and triethylamine into a stirrer together according to a volume ratio of 400:60:1 until a liquid level sensor in the stirrer detects that the liquid level in the stirrer is not increased any more, sending a signal to a controller by the liquid level sensor, controlling a feeding component to add cetyltrimethylammonium bromide into the stirrer according to a solid-to-liquid ratio of 1g:200mL after the controller receives the signal sent by the liquid level sensor, sending a signal to the controller by a first gravity sensor until the first gravity sensor in the stirrer detects that the gravity in the stirrer is not increased any more, and controlling a first heater in the stirrer to heat at 80 ℃ after receiving the signal sent by the first gravity sensor, and simultaneously controlling the stirrer to stir for 3h at a speed of 600r/min to obtain premixed liquid;
s2: pumping the mixture to react and prepare the cosolvent
The controller controls the stirring speed of the stirrer to be 1000r/min, controls the hydraulic pump to pump a mixture prepared by mixing tetraethoxysilane and tetrasulfide according to the volume ratio of 3:1 into the premix according to the volume ratio of 1:100 of the mixture to the premix at a constant speed, stirring and reacting for 8 hours to obtain a suspension, then controls a centrifugal filter device in the stirrer to start, centrifugally filters the suspension, discharges filtrate to obtain filter residues, then opens a washing component in the stirrer, washes the filter residues for 3 times by introducing absolute ethyl alcohol into the stirrer through the washing component, discharges the filtrate obtained by centrifugal filtration into a rectifying tower, and the washing waste liquid discharged after washing the absolute ethyl alcohol is discharged into a rectifying tower and is mixed with filtrate, the rectifying tower is heated, the ethanol is condensed and recovered, then in the production of dibromohydantoin compound water treatment medicament of the next batch, the recovered ethanol is used in the step S1 and is mixed with deionized water, triethylamine and cetyltrimethylammonium bromide to prepare a premix, deionized water is then introduced into a stirrer, the filter residue after washing the absolute ethyl alcohol is washed for 3 times again to remove impurity reactants, pure filter residue is obtained, hydrochloric acid-methanol solution containing 1% hydrochloric acid is added into the stirrer until the hydrochloric acid-methanol solution submerges the pure filter residue, and after soaking for 10 hours, the cosolvent is obtained through filtration and drying;
s3: mixing and melting dibromohydantoin and mixed poloxamer
Adding dibromohydantoin and mixed poloxamer prepared by mixing poloxamer 188 and poloxamer 407 according to the mass ratio of 3:1 into a high-speed dispersing machine together according to the mass ratio of 1:12, until a second gravity sensor in the high-speed dispersing machine detects that the gravity in a box is not increased any more, sending a signal to a controller by the second gravity sensor, after receiving the signal sent by the second gravity sensor, controlling the high-speed dispersing machine to disperse for 40min at the speed of 5000r/min to obtain a mixed material, then opening a discharge valve of the high-speed dispersing machine, adding the mixed material into a melting tank, until the second gravity sensor detects that the gravity in the high-speed dispersing machine is 0, sending a signal to the controller again, after receiving the signal sent by the second gravity sensor again, controlling a second heater in the melting tank to heat the mixed material at 250 ℃, and simultaneously controlling a stirrer to stir at the speed of 500r/min until the mixed material is completely melted to obtain a mixed melt;
s4: cooling, solidifying and pulverizing
Turning off the heater, stopping heating, gradually naturally cooling and solidifying the mixed melt, cooling to room temperature, adding into a crushing grinder, and crushing and grinding to obtain dibromohydantoin mixed material;
s5: ultrasonic dissolving and adding cosolvent
Adding the dibromohydantoin mixed material and ethanol into an ultrasonic dissolution tank together according to a solid-to-liquid ratio of 1g to 5mL, until a third gravity sensor in the ultrasonic dissolution tank detects that the gravity in the ultrasonic dissolution tank is not increased any more, sending a signal to a controller by the third gravity sensor, controlling the ultrasonic dissolution tank to carry out ultrasonic dissolution assistance for 30min at a frequency of 30kHz after receiving the signal sent by the third gravity sensor by the controller, obtaining dissolution liquid, adding the cosolvent prepared in the step S2 into the dissolution liquid until the third gravity sensor detects that the gravity in the ultrasonic dissolution tank is not increased any more again, sending the signal to the controller again by the third gravity sensor, controlling a second stirrer in the ultrasonic dissolution tank to stir at a speed of 200r/min for 24h after the controller receives the signal sent by the third gravity sensor again, obtaining a suspension, then controlling a filter pressing component in the ultrasonic dissolution tank to be opened by the controller, obtaining a precursor medicament through the filter pressing component, finally, placing the precursor medicament into a drying oven at a temperature of 90 ℃ and adding the precursor medicament into a pulverizer, and pulverizing to obtain the dibromohydantoin compound water treatment medicament.
Then, experimental tests are carried out on the prepared dibromohydantoin compound water treatment medicament:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then the prepared dibromohydantoin compound water treatment agent is added into the deionized water to be fully dissolved to prepare a saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 5.06g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 10.12% according to a solubility formula;
then, 5.06g of dibromohydantoin compound water treatment agent is weighed and added into 50mL of deionized water at 20 ℃, and the mixture is stirred by a magnetic stirrer at a speed of 100r/min until the mixture is completely dissolved, and the complete dissolution time is about 9.2s, namely the unit dissolution rate is about 0.5500g/s.
Comparative example one
Experimental tests were performed on dibromohydantoin:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then dibromohydantoin is added into the deionized water to be fully dissolved to prepare saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 0.1g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 0.2% according to a solubility formula;
then, 0.1g of dibromohydantoin was weighed and added to 50mL of deionized water at 20℃and stirred with a magnetic stirrer at a rate of 100r/min until completely dissolved, and the time period for complete dissolution was measured to be about 15.4s, i.e., the unit dissolution rate was about 0.0065g/s.
As shown in fig. 3, comparing the performance test results of the above example 1, it is known that the dibromohydantoin compound water treatment agent obtained by mixing and dispersing dibromohydantoin and mixed poloxamer, then heating, melting and mixing, cooling and solidifying, then dissolving in ethanol, mixing with a cosolvent, and press-filtering and drying has better water solubility and faster dissolution rate than dibromohydantoin, thereby improving the treatment efficiency of dibromohydantoin on black and odorous water, reducing the waste of dibromohydantoin water treatment agent, and reducing the treatment cost.
Comparative example two
Referring to the preparation process of example 1, other conditions are unchanged, and only steps S1, S2 and S5 are removed.
Then, experimental tests are carried out on the prepared dibromohydantoin compound water treatment medicament:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then the prepared dibromohydantoin compound water treatment agent is added into the deionized water to be fully dissolved to prepare a saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 2.8g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 5.6% according to a solubility formula;
then, 2.8g of dibromohydantoin compound water treatment agent is weighed and added into 50mL of deionized water at 20 ℃, and the mixture is stirred by a magnetic stirrer at a speed of 100r/min until the mixture is completely dissolved, and the complete dissolution time is about 12.5s, namely the unit dissolution rate is about 0.2240g/s.
As shown in fig. 4, comparing the performance test results of the above example 1, it is known that the dibromohydantoin compound water treatment agent obtained by mixing the cosolvent, press-filtering and drying has better water solubility and faster dissolution rate than the dibromohydantoin, thereby improving the treatment efficiency of the dibromohydantoin on the black and odorous water body, reducing the waste of the dibromohydantoin water treatment agent and reducing the treatment cost.
Comparative example three
Referring to the preparation process of example 1, other conditions are unchanged, and only the mixed poloxamer in step S3 is replaced by the same amount of dibromohydantoin.
Then, experimental tests are carried out on the prepared dibromohydantoin compound water treatment medicament:
firstly, 50mL of deionized water is taken and stored in an incubator at 20 ℃, then the prepared dibromohydantoin compound water treatment agent is added into the deionized water to be fully dissolved to prepare a saturated solution, at the moment, the consumption of the dibromohydantoin compound water treatment agent is about 3.2g, and the solubility of the dibromohydantoin compound water treatment agent in water is about 6.4 percent according to a solubility formula;
then, 3.2g of dibromohydantoin compound water treatment agent is weighed and added into 50mL of deionized water at 20 ℃, and the mixture is stirred by a magnetic stirrer at a speed of 100r/min until the mixture is completely dissolved, and the complete dissolution time is about 11.9s, namely the unit dissolution rate is about 0.2689g/s.
As shown in fig. 5, comparing the performance test results of the above example 1, it is known that the dibromohydantoin compound water treatment agent prepared by mixing and dispersing dibromohydantoin and mixed poloxamer and then heating and melting and mixing has better water solubility and faster dissolution rate than dibromohydantoin, so that the treatment efficiency of dibromohydantoin on black and odorous water can be improved, the waste of dibromohydantoin water treatment agent can be reduced, and the treatment cost can be reduced.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The dibromohydantoin compound water treatment agent for treating black and odorous water is characterized by comprising the following preparation processes:
s1: adding cetyl trimethyl ammonium bromide, heating, stirring and mixing
Adding deionized water, ethanol and triethylamine into a stirrer, adding cetyltrimethylammonium bromide, heating, stirring and mixing to obtain a premix;
s2: pumping the mixture to react and prepare the cosolvent
Pumping a mixture prepared by mixing tetraethoxysilane and tetrasulfide according to a volume ratio of 2-3:1 into the premix at a constant speed, stirring for reaction, filtering and washing, adding hydrochloric acid-methanol solution for soaking, filtering and drying to obtain a cosolvent;
s3: mixing and melting dibromohydantoin and mixed poloxamer
Mixing dibromohydantoin and mixed poloxamer together at high speed, stirring and heating to fully melt to obtain a mixed melt;
s4: cooling, solidifying and pulverizing
Turning off the heater, stopping heating, gradually naturally cooling and solidifying the mixed melt, cooling to room temperature, adding into a crushing grinder, and crushing and grinding to obtain dibromohydantoin mixed material;
s5: ultrasonic dissolving and adding cosolvent
Mixing the dibromohydantoin mixed material with ethanol, performing ultrasonic dissolution, adding the cosolvent, stirring, and performing filter pressing, drying and crushing to obtain the dibromohydantoin compound water treatment medicament.
2. The preparation process of the dibromohydantoin compound water treatment agent for black and odorous water body treatment according to claim 1, wherein the preparation process is characterized in that cetyl trimethyl ammonium bromide is added in the step S1 and is heated and stirred for mixing, and the preparation process specifically comprises the following steps:
s1.1: adding deionized water, ethanol and triethylamine into a stirrer together according to the volume ratio of 300-400:50-60:1 until a liquid level sensor in the stirrer detects that the liquid level in the stirrer is not increased any more, and sending a signal to a controller by the liquid level sensor;
s1.2: after the controller receives the signal sent by the liquid level sensor, the feeding component is controlled to add hexadecyl trimethyl ammonium bromide into the stirrer according to the solid-to-liquid ratio of 1g to 150-200mL until a first gravity sensor in the stirrer detects that the gravity in the stirrer is not increased any more, and the first gravity sensor sends a signal to the controller;
s1.3: after the controller receives the signal sent by the first gravity sensor, the first heater in the stirrer is controlled to heat at the temperature of 70-80 ℃, and the stirrer is controlled to stir for 2-3 hours at the speed of 400-600r/min, so that the premix liquid is obtained.
3. The preparation process of the dibromohydantoin compound water treatment agent for black and odorous water body treatment according to claim 2, wherein the step S2 of pumping the mixture for reaction to prepare the cosolvent specifically comprises the following steps:
s2.1: the controller controls the stirring speed of the stirrer to be 800-1000r/min, controls the hydraulic pump to pump the mixture prepared by mixing tetraethoxysilane and tetrasulfide according to the volume ratio of 2-3:1 into the premix prepared in the step S1.3 at a constant speed at the speed of 3-5mL/min, and carries out stirring reaction for 6-8h to obtain a suspension;
s2.2: the controller controls a centrifugal filter device in the stirrer to start, centrifugally filters the suspension, and discharges filtrate to obtain filter residues;
s2.3: opening a washing component in the stirrer, introducing absolute ethyl alcohol into the stirrer through the washing component, washing the filter residues for 2-3 times, introducing deionized water into the stirrer, washing the filter residues washed by the absolute ethyl alcohol for 2-3 times again, and removing impurity reactants to obtain pure filter residues;
s2.4: adding hydrochloric acid-methanol solution into a stirrer until the hydrochloric acid-methanol solution submerges the pure filter residues, soaking for 8-10h, filtering and drying to obtain the cosolvent.
4. The preparation process of the dibromohydantoin compound water treatment agent for black and odorous water body treatment according to claim 1, wherein the mixing and melting of the dibromohydantoin and the mixed poloxamer in the step S3 specifically comprises the following steps:
s3.1: adding dibromohydantoin and mixed poloxamer into the high-speed dispersing machine together according to the mass ratio of 1:10-12 until a second gravity sensor in the high-speed dispersing machine detects that the gravity in the box is not increased any more, and sending a signal to a controller by the second gravity sensor;
s3.2: after the controller receives the signal sent by the second gravity sensor, the high-speed dispersing machine is controlled to disperse for 30-40min at the speed of 4000-5000r/min to obtain a mixed material;
s3.3: opening a discharge valve of the high-speed dispersing machine, and throwing the mixed materials into a melting tank until the second gravity sensor detects that the gravity in the high-speed dispersing machine is 0, and sending a signal to the controller again by the second gravity sensor;
s3.4: and after receiving the signal sent by the second gravity sensor again, the controller controls a second heater in the melting tank to heat the mixed material at 200-250 ℃ and controls the stirrer to stir at the speed of 300-500r/min until the mixed material is completely melted, so as to obtain a mixed melt.
5. The process for preparing the dibromohydantoin compound water treatment agent for treating black and odorous water bodies according to claim 3, wherein the ultrasonic dissolution of the step S5 and the addition of a cosolvent comprise the following steps:
s5.1: adding the dibromo hydantoin mixed material prepared in the step S4 and ethanol into an ultrasonic dissolution tank until a third gravity sensor in the ultrasonic dissolution tank detects that the gravity in the ultrasonic dissolution tank is not increased any more, and sending a signal to a controller by the third gravity sensor;
s5.2: after the controller receives the signal sent by the third gravity sensor, controlling the ultrasonic dissolving box to assist dissolving for 20-30min at the frequency of 20-30kHz to obtain dissolving liquid;
s5.3: adding the cosolvent prepared in the step S2.4 into the dissolving liquid until the third gravity sensor detects that the gravity in the ultrasonic dissolving tank is not increased again, and sending a signal to the controller again by the third gravity sensor;
s5.4: after receiving the signal sent by the third gravity sensor again, the controller controls a second stirrer in the ultrasonic dissolving tank to stir for 18-24 hours at the speed of 100-200r/min, so as to obtain suspension;
s5.5: the controller controls a filter pressing assembly in the ultrasonic dissolution box to be opened, and the suspension is subjected to filter pressing through the filter pressing assembly to obtain a precursor medicament;
s5.6: and (3) placing the precursor medicament in an oven, drying at 80-90 ℃, adding into a pulverizer, and pulverizing to obtain the dibromohydantoin compound water treatment medicament.
6. The process for preparing a dibromohydantoin compound water treatment agent for black and odorous water body treatment according to claim 3, wherein after centrifugal filtration in the step S2.2, filtrate is discharged into a rectifying tower, washing waste liquid discharged after washing absolute ethyl alcohol in the step S2.3 is discharged into the rectifying tower, mixed with the filtrate, the rectifying tower is heated, condensed and recovered ethanol, and then in the production of the next batch of dibromohydantoin compound water treatment agent, the recovered ethanol is used in the step S1.1 and mixed with deionized water, triethylamine and cetyltrimethylammonium bromide to prepare a premix.
7. The process for preparing the dibromohydantoin compound water treatment agent for treating black and odorous water body according to claim 3, wherein the volume ratio of the mixing agent to the premix is 1:90-100.
8. The process for preparing the dibromohydantoin compound water treatment agent for treating black and odorous water body according to claim 3, wherein the hydrochloric acid-methanol solution is a mixed solution of hydrochloric acid and methanol, and the content of hydrochloric acid is 0.5-1%.
9. The preparation process of the dibromohydantoin compound water treatment agent for treating black and odorous water body according to claim 4, wherein the mixed poloxamer is prepared by mixing poloxamer 188 and poloxamer 407 according to the mass ratio of 1-3:1.
10. The process for preparing the dibromohydantoin compound water treatment agent for treating black and odorous water body according to claim 5, wherein the solid-liquid ratio of the dibromohydantoin mixed material to the ethanol is 1g:3-5mL.
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