CN1611493A - Dibromo glucolycurea sterilizing and disinfecting algaecide preparing method - Google Patents
Dibromo glucolycurea sterilizing and disinfecting algaecide preparing method Download PDFInfo
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- CN1611493A CN1611493A CN 200310105376 CN200310105376A CN1611493A CN 1611493 A CN1611493 A CN 1611493A CN 200310105376 CN200310105376 CN 200310105376 CN 200310105376 A CN200310105376 A CN 200310105376A CN 1611493 A CN1611493 A CN 1611493A
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Abstract
The invention relates to a kind of manufacturing method of dibromine hydantoin disinfection algaecide. It uses 5,5-dimethyl hydantoin as main material; and then make it dissolve in water or in mother liquor; then add halogen this solution, at the same time, dropwise sodium hydroxide solution in order to proceed bromination reaction; after, make the product have water washing, filtration and drying treatment in order to get dibromine hydantoin. The features are as follows: the concentration of sodium hydroxide solution added in is 33-37%; use online measurement to control adding molar composition of material, so that it can proceed instant optimal controls all through the reaction. It has the remarkable effictiveness, such as simple operation, high product yield that can reach up to more than 96%, high product purity that can reach to more than 99%, low discharge capacity.
Description
One, technical field
The invention belongs to the hydantoin halides technology of preparing, be specifically related to a kind of preparation method of C5H6Br2N2O2 disinfection algicide.
Two, background technology
What hydantoin halides was used the earliest is two chlordantoins, and present two chlordantoins are used few, are replaced by bromochlorohydantoin and C5H6Br2N2O2.The end of the seventies, U.S. Biglake chemical Corp etc. are with bromochlorohydantoin industrialization and commercialization, this product is owing to be to be the integrated preparation of bromine chlorine of carrier with the organic substance, its mechanism is active to be the bromine preparation, so become state-of-the art green disinfectant, it has stable in properties, having overcome traditional chlorinated product (as chlorinated lime, high test bleaching powder, clorox etc.) chlorine easily loses, be difficult for shortcomings such as storage, it is active high, when being low to moderate 1ppm, just can kill various mushrooms in the water body, algae etc. effectively.Have killing livestock property of wide spectrum, slow-releasing, adapt to the pH wide ranges, adapt to water body scope wide (can adapt to the recirculating cooling water system that contains ammonia, nitrogen, H2S hydro carbons etc.), pungency is little, has no side effect after the degraded, discharges pollution-free.Therefore, be widely used in disinfection, the algae removal of industrial circulating water, oil-field flooding, swimming pool, hot spring; The sterilizing prevent disease that is applied to aquaculture is cured the disease; The sterilization of living environment at home; The sterilizing prevent disease in livestock culture place; Because C5H6Br2N2O2 is not chloride, be used widely having replaced bromochlorohydantoin aspect the sterilization of the washing one's hands of medical apparatus, medical berth articles for use, medical worker, hospital sewage in recent years.Since the excellent specific property of hydantoin halides, the speed increment in developed country with year 10-15%, China has the production of two chlordantoins the early 1990s in last century, and the end of the nineties, bromochlorohydantoin was also realized industrialization.Classify bromochlorohydantoin one of as water treatment agent in the State Economic and Trade Commission in July calendar year 2001 No. 5 " the saving product of water catalogue of current national institute encourage growth ", in April, 2003, the health ministry Center for Disease Control was classified C5H6Br2N2O2 as one of sterilized product of popularization.
The hydantoin halides production method of domestic and foreign literature report has following three kinds.The commercial run that first method just adopts the earliest, its method are to prepare hypohalite (clorox, sodium hypobromite) with alkali and halogen earlier, then as halogenating agent and dimethyl hydantion reaction, again with the hydrochloric acid neutralization, and obtain hydantoin halides; Second method then is that a kind of method of improvement promptly is raw material with the dimethyl hydantion, add bromide solution (as Sodium Bromide or Potassium Bromide) again and in the presence of alkali, feed chlorine then, bromide anion in the bromide is oxidized to bromine, carry out bromination, can obtain bromochlorohydantoin and C5H6Br2N2O2 according to different proportionings; The third method then is to be raw material with the dimethyl hydantion, and the logical chlorine of logical bromine obtains hydantoin halides in the presence of alkali.More than three kinds of methods have all that the production control difficulty is big, yield is low, cost is high, product purity is low, the shortcoming of product color difference.
Three, summary of the invention
It is simple to the purpose of this invention is to provide a kind of operation control, yield height, purity height, the preparation method of the C5H6Br2N2O2 disinfection algicide that wastewater displacement is few.
Technical scheme of the present invention is achieved in that a kind of preparation method of C5H6Br2N2O2 disinfection algicide, is with 5, and the 5-dimethyl hydantion is a main raw material; A, dissolve in water by it, dropping sodium solution carries out bromination reaction when this solution drips bromine, afterwards to product wash, filtration and drying treatment make C5H6Br2N2O2; B or in the mother liquor that above-mentioned a reaction produces, dissolve by it, dropping sodium solution carries out chlorination reaction in the time of the logical chlorine of this solution, afterwards to product wash, filtration and drying treatment make C5H6Br2N2O2; Its process chemistry reaction formula is respectively:
It is characterized in that: the concentration of dropping sodium solution is 33～37%; Utilize the method for on-line metering to control the mole proportioning that material adds, carry out the moment optimal control of halogenating reaction whole process; The material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is dimethyl hydantion: water: bromine: sodium hydroxide=1: 900～1100: 2.0～2.1: 2.0～2.2, the bromination temperature is 5～12 ℃, and the concentration that the mother liquor that recovery is produced contains NaBr is 11.5～12.5%; The material mole proportioning that participates in the b reaction is dimethyl hydantion: NaBr: chlorine: sodium hydroxide=1: 2.0～2.2: 2.0～2.1: 2.0～2.1, chlorination temperature are 3～10 ℃.
Realize that a kind of best mode of the present invention is; The concentration of sodium hydroxide solution is 35%; The material mole proportioning (it is outer for restraining to dewater) that participates in a step reaction is dimethyl hydantion: water: bromine: sodium hydroxide=1: 1000: 2.06: 2.12, and the bromination temperature is 9 ℃; The concentration that the mother liquor that recovery is produced contains NaBr is 12%; The material proportion that participates in the b reaction is dimethyl hydantion: NaBr: chlorine: sodium hydroxide=1: 2.05: 2.08: 2.03, and chlorination temperature is 7 ℃.
Preparation method of the present invention adds the mole proportioning of material owing to adopted the method for on-line metering in the strict control halogenating reaction process, carry out the moment optimal control, has suppressed the generation of side reaction effectively; Again initial mother liquor is recycled again simultaneously.Compare with prior art that to have operation control simple, the product yield height reaches more than 96%, and the product purity height reaches more than 99%, the unusual effect that wastewater discharge is few.
Four, embodiment
Come technical scheme of the present invention is described further below in conjunction with specific embodiment.
Embodiment 1
In 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 152Kg, water 1180Kg, stirred at normal temperatures 15 minutes, controlled temperature drips 34.5% sodium hydroxide solution 290Kg simultaneously and drips bromine 390Kg by the on-line metering device at 5 ℃ then, when dripping sodium hydroxide solution, residue bromine 5Kg, and continue to drip, drip off bromine after, still under 5 ℃, continued stirring reaction 40 minutes, reaction finishes, and just reaction solution is sent from the scheming separation, use the 120Kg water washing again, get rid of clean, dry under 60-80 ℃, get white powder crystalline product C5H6Br2N2O2 330Kg, yield 96.9%, purity 99.2% reclaims mother liquor and the about 1200kg of washing lotion; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 100Kg, add above-mentioned recovery and prepare the Sodium Bromide mother liquor 1430Kg of 11.5% concentration, stirred at normal temperatures 15 minutes, controlled temperature is at 3 ℃ then, by the on-line metering device sodium hydroxide solution 181Kg of Dropwise 35 % in proportion simultaneously, logical chlorine 115Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 3 ℃, continued stirring reaction 40 minutes then, reaction finishes.Reaction solution is sent from scheming separates, and use the 80Kg water washing, dry under 60-80 ℃, get white powder crystallization C5H6Br2N2O2 216Kg, yield 96.5%, purity 99.3%.
Embodiment 2
In 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 152Kg, water 1180Kg, stirred at normal temperatures 15 minutes, controlled temperature is at 12 ℃, by on-line metering device while Dropwise 35 .5% sodium hydroxide solution 282Kg and dropping bromine 390Kg then, when dripping sodium hydroxide solution, residue bromine 5Kg, and continue to drip, drip off bromine after, still under 12 ℃, continued stirring reaction 40 minutes, reaction finishes, and reaction solution is sent from scheming separates, use the 120Kg water washing again, get rid of clean, dry under 60-80 ℃, get white powder crystalline product C5H6Br2N2O2 330Kg, yield 96.9%, purity 99.2% reclaims mother liquor and the about 1200Kg of washing lotion; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 100Kg, add above-mentioned recovery and prepare the Sodium Bromide mother liquor 1312Kg of 12.5% concentration, stirred at normal temperatures 15 minutes, controlled temperature is at 10 ℃ then, by the on-line metering device sodium hydroxide solution 181Kg of Dropwise 35 % in proportion simultaneously, logical chlorine 115Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 10 ℃, continued stirring reaction 40 minutes then, reaction finishes.Reaction solution is sent from scheming separates, and use the 80Kg water washing, dry under 60-80 ℃, get white powder crystallization C5H6Br2N2O2 216Kg, yield 96.5%, purity 99.3%.
Embodiment 3
In 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 152Kg, water 1180Kg, stirred at normal temperatures 15 minutes, controlled temperature is at 9 ℃, by on-line metering device while Dropwise 35 % sodium hydroxide solution 286Kg and dropping bromine 390Kg then, when dripping sodium hydroxide solution, residue bromine 5Kg, and continue to drip, drip off bromine after, still under 9 ℃, continued stirring reaction 40 minutes, reaction finishes, and just reaction solution is sent from the scheming separation, use the 120Kg water washing again, get rid of clean, dry under 60-80 ℃, get white powder crystalline product C5H6Br2N2O2 330Kg, yield 96.9%, purity 99.2% reclaims mother liquor and the about 1200Kg of washing lotion; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 100Kg, add above-mentioned recovery and prepare the Sodium Bromide mother liquor 1370Kg of 12% concentration, stirred at normal temperatures 15 minutes, controlled temperature is at 7 ℃ then, by the on-line metering device sodium hydroxide solution 181Kg of Dropwise 35 % in proportion simultaneously, logical chlorine 115Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 7 ℃, continued stirring reaction 40 minutes then, reaction finishes.Reaction solution is sent from scheming separates, and use the 80Kg water washing, dry under 60-80 ℃, get white powder crystallization C5H6Br2N2O2 216Kg, yield 96.5%, purity 99.3%.
Claims (2)
1, a kind of preparation method of C5H6Br2N2O2 disinfection algicide is with 5, and the 5-dimethyl hydantion is a main raw material; A, dissolve in water by it, dropping sodium solution carries out bromination reaction when this solution drips bromine, afterwards to product wash, filtration and drying treatment make C5H6Br2N2O2; B or in the mother liquor that above-mentioned a reaction produces, dissolve by it, dropping sodium solution carries out chlorination reaction in the time of the logical chlorine of this solution, afterwards to product wash, filtration and drying treatment make C5H6Br2N2O2; Its process chemistry reaction formula is respectively:
It is characterized in that: the concentration of dropping sodium solution is 33～37%; Utilize the method for on-line metering to control the mole proportioning that material adds, carry out the moment optimal control of halogenating reaction whole process; The material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is dimethyl hydantion: water: bromine: sodium hydroxide=1: 900～1100: 2.0～2.1: 2.0～2.2, the bromination temperature is 5～12 ℃, and reclaiming mother liquor that a reaction produces, to make the concentration that contains NaBr be 11.5～12.5% solution; The material mole proportioning that participates in the b reaction is dimethyl hydantion: NaBr: chlorine: sodium hydroxide=1: 2.0～2.2: 2.0～2.1: 2.0～2.1, chlorination temperature are 3～10 ℃.
2, according to the preparation method of the described a kind of C5H6Br2N2O2 disinfection algicide of claim 1, it is characterized in that: the material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is dimethyl hydantion: water: bromine: sodium hydroxide=1: 1000: 2.06: 2.12, and the bromination temperature is 9 ℃; Reclaiming mother liquor that a reaction produces, to make the concentration that contains NaBr be 12% solution; The material mole proportioning that participates in the b reaction is dimethyl hydantion: NaBr: chlorine: sodium hydroxide=1: 2.05: 2.08: 2.03, and chlorination temperature is 7 ℃; The concentration of sodium hydroxide solution is 35%.
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| CN 200310105376 CN1611493A (en) | 2003-10-29 | 2003-10-29 | Dibromo glucolycurea sterilizing and disinfecting algaecide preparing method |
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| CN 200310105376 CN1611493A (en) | 2003-10-29 | 2003-10-29 | Dibromo glucolycurea sterilizing and disinfecting algaecide preparing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105379719A (en) * | 2015-10-08 | 2016-03-09 | 山东大明消毒科技有限公司 | Preparation method of high-stability dibromohydantoin disinfection solution |
| CN108299306A (en) * | 2018-03-30 | 2018-07-20 | 河北鑫淘源环保科技有限公司 | A kind of tail gas treatment process in bromochloroin building-up process |
| CN108586349A (en) * | 2017-12-30 | 2018-09-28 | 仙桃市信达化工有限责任公司 | A kind of novel water treatment scale fungicide and preparation method thereof |
| CN114805213A (en) * | 2022-04-09 | 2022-07-29 | 河北利仕化学科技有限公司 | Clean synthesis method of dibromohydantoin |
-
2003
- 2003-10-29 CN CN 200310105376 patent/CN1611493A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105379719A (en) * | 2015-10-08 | 2016-03-09 | 山东大明消毒科技有限公司 | Preparation method of high-stability dibromohydantoin disinfection solution |
| CN105379719B (en) * | 2015-10-08 | 2018-03-27 | 山东大明消毒科技有限公司 | A kind of preparation method of high stable 1,3-dibromo-5,5-dimedisinfectantn disinfectantn |
| CN108586349A (en) * | 2017-12-30 | 2018-09-28 | 仙桃市信达化工有限责任公司 | A kind of novel water treatment scale fungicide and preparation method thereof |
| CN108299306A (en) * | 2018-03-30 | 2018-07-20 | 河北鑫淘源环保科技有限公司 | A kind of tail gas treatment process in bromochloroin building-up process |
| CN114805213A (en) * | 2022-04-09 | 2022-07-29 | 河北利仕化学科技有限公司 | Clean synthesis method of dibromohydantoin |
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