CN1611492A - Bromochloro glucolylurea steribizing and disinfecting algae cide preparing method - Google Patents
Bromochloro glucolylurea steribizing and disinfecting algae cide preparing method Download PDFInfo
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- CN1611492A CN1611492A CN 200310105375 CN200310105375A CN1611492A CN 1611492 A CN1611492 A CN 1611492A CN 200310105375 CN200310105375 CN 200310105375 CN 200310105375 A CN200310105375 A CN 200310105375A CN 1611492 A CN1611492 A CN 1611492A
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Abstract
The invention relates to a kind of manufacturing method of bromine-chlorine hydantoin disinfection algaecide. It uses 5,5-dimethyl hydantoin as main material; and then make it dissolve in water or in mother liquor contained sodium bromide that generated in dibromine hydantoin production; uses bromine element and chlorine gas as halogenating agent, and meanwhile, dropwise sodium hydroxide solution in order to proceed bromination and chloridization reaction; after the halogenation product having centrifugation, water washing, and drying treatment, bromine-chlorine hydantoin can be get. 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 bromochlorohydantoin 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 the water body scope and extensively (can adapt to and contain ammonia, nitrogen, H
2The recirculating cooling water system of S hydro carbons etc.), pungency is little, has no side effect after the degraded, discharges pollution-free.Therefore, 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 ".
At present, the bromochlorohydantoin production method has following three kinds.The commercial run that first method just adopts the earliest, its method are to prepare clorox and sodium hypobromite with alkali and chlorine, bromine earlier, then as halogenating agent and dimethyl hydantion reaction, again with the hydrochloric acid neutralization, and obtain bromochlorohydantoin; Second method then is that a kind of method of improvement promptly is raw material with the dimethyl hydantion, adds bromide solution (as Sodium Bromide or Potassium Bromide) again and feeds chlorine then in the presence of alkali, and the bromide anion in the bromide is oxidized to bromine, carries out bromination, obtains bromochlorohydantoin; 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 bromochlorohydantoin disinfection algicide that wastewater displacement is few.
Technical scheme of the present invention is achieved in that a kind of preparation method of bromochlorohydantoin disinfection algicide, is with 5, and 5-diformazan glycolylurea glycolylurea is a main raw material; A, dissolve in water by it, as halogenating agent, dropping sodium solution carries out bromination and chlorination reaction simultaneously with bromine and chlorine, and halogenated products makes bromochlorohydantoin through centrifugation, washing, drying treatment; Dissolve in b or the mother liquor that contains Sodium Bromide that when producing C5H6Br2N2O2, produces with it, with chlorine as halogenating agent, dropping sodium solution carries out chlorination reaction simultaneously, chlorine is oxidized to bromine with the bromide anion of the bromide in the solution, carry out bromination and chlorination reaction, halogenated products makes bromochlorohydantoin through centrifugation, washing, drying treatment;
Its process chemistry reaction formula is respectively:
It is characterized in that: the concentration of dropping sodium solution is 33～37%, utilizes the method for on-line metering to control the mole proportioning that material adds, and reacts the moment optimal control of whole process; The material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is 5, and 5-dimethyl hydantion: water: bromine: chlorine: sodium hydroxide=1: 900～1100: 0.5～0.54: 1.50～1.55: 2.0～2.06, bromination temperature are 5～15 ℃; The material mole proportioning that participates in the b reaction is 5, and 5-dimethyl hydantion: Sodium Bromide: chlorine: sodium hydroxide=1: 1.0～1.10: 2.0～2.05: 2.0～2.05, chlorination temperature are 3～10 ℃, and the concentration of mother liquor sodium bromide solution is 11.5～12.5%.
Realize that best mode of the present invention is: the material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is 5, and 5-dimethyl hydantion: water: bromine: chlorine: sodium hydroxide=1: 1000: 0.52: 1.53: 2.04, the bromination temperature was 9 ℃; The material mole proportioning that participates in the b reaction is 5,5-dimethyl hydantion: Sodium Bromide: chlorine: sodium hydroxide=1: 1.07: 2.03: 2.03, and chlorination temperature is 7 ℃, and the concentration of sodium hydroxide solution is 35%, and the concentration of mother liquor sodium bromide solution is 12%.
Preparation method of the present invention compares to have to operate with prior art and controls simply owing to adopted the method control halogenating reaction process of on-line metering, and 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 tools example 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 140Kg, water 1080Kg, stirred at normal temperatures 15 minutes, controlled temperature is at 5 ℃ then, drip simultaneously 34.5% sodium hydroxide solution 134Kg in proportion by the on-line metering device, drip bromine 90Kg, after sodium hydroxide and bromine have led to, still under 5 ℃, continued stirring reaction 30 minutes, controlled temperature is 3 ℃ then, drips 34.5% sodium hydroxide 122Kg simultaneously in proportion by the on-line metering device, logical chlorine 117Kg, when dripping off sodium hydroxide, residual nitrogen 5Kg, and continue to drip off is then still 3 ℃ of following stirring reactions 40 minutes, reaction mass being sent from scheming separates again, use the 110Kg water washing again, get rid of only, dry under 60-80 ℃, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.2%; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 140Kg, adding is mixed with the sodium bromide solution 1030Kg of 11.5% concentration by the mother liquor that contains Sodium Bromide that produces when producing C5H6Br2N2O2, stirred at normal temperatures 15 minutes, controlled temperature is at 3 ℃ then, drip simultaneously 34.5% sodium hydroxide solution 254Kg in proportion by the on-line metering device, logical chlorine 156Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 3 ℃, continued stirring reaction 1 hour then, reaction finishes.Reaction solution is sent from scheming separates, and use the 100Kg water washing, dry under 60-80 ℃, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.1%.
Embodiment 2:
In 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 140Kg, water 1080Kg, stirred at normal temperatures 15 minutes, controlled temperature is at 12 ℃ then, by on-line metering device Dropwise 35 .5% sodium hydroxide solution 130Kg in proportion simultaneously, drip bromine 90Kg, after alkali and bromine have led to, still under 12 ℃, continued stirring reaction 30 minutes, controlled temperature is 10 ℃ then, by the on-line metering device simultaneously in another ratio Dropwise 35 .5% sodium hydroxide 118Kg, logical chlorine 117Kg, when dripping off alkali, residual nitrogen 5Kg, and continue to have led to, still 10 ℃ of following stirring reactions 40 minutes, reaction finishes then.Reaction mass is sent from scheming separates, again with the 110Kg water washing, get rid of clean, 60-80 ℃ dry down, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.2%; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 140Kg, be added in the sodium bromide solution 950Kg that the mother liquor that contains Sodium Bromide that produces when producing C5H6Br2N2O2 is mixed with 12.5% concentration, stirred at normal temperatures 15 minutes, controlled temperature is at 10 ℃ then, drip simultaneously 34.5% sodium hydroxide solution 254Kg in proportion by the on-line metering device, logical chlorine 156Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 10 ℃, continued stirring reaction 1 hour then, reaction finishes.Reaction solution is sent from scheming separates, and use the 100Kg water washing, dry under 60-80 ℃, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.1%.
Embodiment 3:
In 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 140Kg, water 1080Kg, stirred at normal temperatures 15 minutes, controlled temperature is at 9 ℃ then, by on-line metering device Dropwise 35 % sodium hydroxide solution 132Kg in proportion simultaneously, drip bromine 90Kg, after alkali and bromine have led to, still under 9 ℃, continued stirring reaction 30 minutes, controlled temperature 3-10 ℃ then, by the on-line metering device simultaneously in another ratio Dropwise 35 % sodium hydroxide 120Kg, logical chlorine 117Kg, when dripping off alkali, residual nitrogen 5Kg, and continue to have led to, still 9 ℃ of following stirring reactions 40 minutes, reaction finishes then.Reaction mass is sent from scheming separates, again with the 110Kg water washing, get rid of clean, 60-80 ℃ dry down, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.2%; In another 2000 liters of glassed steel reaction vessels, add dimethyl hydantion 140Kg, be added in the sodium bromide solution 990Kg that the mother liquor that contains Sodium Bromide that produces when producing C5H6Br2N2O2 is mixed with 12% concentration, stirred at normal temperatures 15 minutes, controlled temperature is at 7 ℃ then, drip simultaneously 34.5% sodium hydroxide solution 250Kg in proportion by the on-line metering device, logical chlorine 156Kg, when dripping sodium hydroxide solution, residue chlorine 5kg, and continue to have led to, still under 7 ℃, continued stirring reaction 1 hour then, reaction finishes.Reaction solution is sent from scheming separates, and use the 100Kg water washing, dry under 60-80 ℃, get white powder crystallization bromochlorohydantoin 253Kg, yield 96.2%, purity 99.1%.
Claims (2)
1, a kind of preparation method of bromochlorohydantoin disinfection algicide is with 5, and the 5-dimethyl hydantion is a main raw material; A, dissolve in water by it, as halogenating agent, dropping sodium solution carries out bromination and chlorination reaction simultaneously with bromine and chlorine, and halogenated products makes bromochlorohydantoin through centrifugation, washing, drying treatment; Dissolve in b or the mother liquor that contains Sodium Bromide that when producing C5H6Br2N2O2, produces with it, with chlorine as halogenating agent, dropping sodium solution carries out chlorination reaction simultaneously, chlorine is oxidized to bromine with the bromide anion of the bromide in the solution, carry out bromination and chlorination reaction, halogenated products makes bromochlorohydantoin through centrifugation, washing, drying treatment; Its process chemistry reaction formula is respectively:
It is characterized in that: the concentration of dropping sodium solution is 33～37%, utilizes the method for on-line metering to control the mole proportioning that material adds, and reacts the moment optimal control of whole process; The material mole proportioning (it is outer for restraining to dewater) that participates in a reaction is 5, and 5-dimethyl hydantion: water: bromine: chlorine: sodium hydroxide=1: 900～1100: 0.5～0.54: 1.50～1.55: 2.0～2.06, bromination temperature are 5～15 ℃; The material mole proportioning that participates in the b reaction is 5, and 5-dimethyl hydantion: Sodium Bromide: chlorine: sodium hydroxide=1: 1.0～1.10: 2.0～2.05: 2.0～2.05, chlorination temperature are 3～10 ℃, and the concentration of mother liquor sodium bromide solution is 11.5～12.5%.
2, press the preparation method of the described a kind of bromochlorohydantoin 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 5,5-dimethyl hydantion: water: bromine: chlorine: sodium hydroxide=1: 1000: 0.52: 1.53: 2.04, the bromination temperature was 9 ℃; The material mole proportioning that participates in the b reaction is 5,5-dimethyl hydantion: Sodium Bromide: chlorine: sodium hydroxide=1: 1.07: 2.03: 2.03, and chlorination temperature is 7 ℃, and the concentration of sodium hydroxide solution is 35%, and the concentration of mother liquor sodium bromide solution is 12%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363539A (en) * | 2011-06-30 | 2012-02-29 | 上海明诺环境科技有限公司 | Method for controlling growth of pipeline biological film by utilizing bromine chlorine hydantoin liposome |
| 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 |
| CN109644997A (en) * | 2019-01-25 | 2019-04-19 | 龙口科达化工有限公司 | A kind of environment-friendly type slurry emulsus bromochloroin and its no three wastes clean preparation method |
| CN110305065A (en) * | 2019-07-26 | 2019-10-08 | 河北利仕化学科技有限公司 | Bromochloroin continuous production equipment and production method |
| CN111961003A (en) * | 2020-08-24 | 2020-11-20 | 河北利仕化学科技有限公司 | Synthesis method of low-chroma 1, 3-diiodo-5, 5-dimethyl hydantoin |
-
2003
- 2003-10-29 CN CN 200310105375 patent/CN1611492A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102363539A (en) * | 2011-06-30 | 2012-02-29 | 上海明诺环境科技有限公司 | Method for controlling growth of pipeline biological film by utilizing bromine chlorine hydantoin liposome |
| 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 |
| 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 |
| CN109644997A (en) * | 2019-01-25 | 2019-04-19 | 龙口科达化工有限公司 | A kind of environment-friendly type slurry emulsus bromochloroin and its no three wastes clean preparation method |
| CN110305065A (en) * | 2019-07-26 | 2019-10-08 | 河北利仕化学科技有限公司 | Bromochloroin continuous production equipment and production method |
| CN110305065B (en) * | 2019-07-26 | 2022-05-17 | 河北利仕化学科技有限公司 | Continuous production equipment and production method of bromochlorohydantoin |
| CN111961003A (en) * | 2020-08-24 | 2020-11-20 | 河北利仕化学科技有限公司 | Synthesis method of low-chroma 1, 3-diiodo-5, 5-dimethyl hydantoin |
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