CN1156457C - Prepn of bromochloro-fulminuric acid bactericide - Google Patents
Prepn of bromochloro-fulminuric acid bactericide Download PDFInfo
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- CN1156457C CN1156457C CNB011308893A CN01130889A CN1156457C CN 1156457 C CN1156457 C CN 1156457C CN B011308893 A CNB011308893 A CN B011308893A CN 01130889 A CN01130889 A CN 01130889A CN 1156457 C CN1156457 C CN 1156457C
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- bromochloro
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- fulminuric acid
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Abstract
The present invention discloses a preparation method of bromochloro fulminuric acid bactericide. The method uses isocyanuric acid as main raw material; through alkali adding dissolution operation, chlorination operation, bromination operation, chlorination operation, filtering operation and drying operation, bromochloro fulminuric acid is prepared. The present invention is characterized in that the isocyanuric acid is dissolved in water solution or emulsion of alkali; the temperature is from 5 to 15 DEG C, chlorine gas is respectively supplied for the solution or the emulsion, bromine liquid is dropped, and finally, chlorine gas is supplied for chlorination reaction; the final pH value of the reaction is controlled to be from 2.5 to 4, a product whose total active chlorine is from 54 to 58% is obtained, and the content of active bromine of the product is from 46 to 49%. The process of the preparation method is simple, conditions are easily controlled, and the product has the rapid sterilization effect in water.
Description
Technical field
The present invention relates to a kind of preparation method of bromochloro-fulminuric acid bactericide.The technology of preparing that belongs to the halo tricarbimide.
Background technology
Hydantoin halides class, halo tricarbimide class and halo glycoluril compounds are the relatively more typical efficient water treatment biocides of several classes.Especially bromine Chlorodimethyl glycolylurea, it have active high (under being lower than 1ppm concentration, just can very effectively kill bacterium in the water, algae etc.), killing livestock property of wide spectrum, lasting period long, use the pH scope extensively, to water in characteristics such as nitrogenous compound is insensitive.Be widely used in the algae removal of killing livestock of cooling water system, the sterilizing and purifying of swimming-pool water, the sterilizing disease-preventing of culture fishery etc.Bromine Chlorodimethyl glycolylurea is realized commercialization in the seventies in the U.S., and China also has many families to produce, and overall throughput has surpassed kiloton.Its consumption rises year by year.But bromine Chlorodimethyl glycolylurea solubleness in water is low, can not discharge the positive monovalence active halogen ion of high density at short notice, therefore is not suitable for the rapid sterilization of the aquaculture water of occurrence of large-area disease.Therefore, exploitation is a kind of can dissolve rapidly in water body that to discharge high density active halogen ionic antiseptic sterilization agent imperative.Though monobromo one chloroisocyan urate and monobromo DICHLOROISOCYANURIC ACID had report in five sixties, all be to add the way preparation of leading to chlorine behind the bromine earlier.Because earlier a bromo-derivative solubleness that generates is little, generate the fine particle precipitation rapidly, cause that follow-up chlorination is incomplete, product granularity is too small, filtration difficulty and never realize industrialization.The present invention just is being based on the problems referred to above, invented a kind of in the middle of the preparation method of bromination, the products obtained therefrom particle is big, be convenient to filter, the consumption of reaction solvent water is few, and total available chlorine content height.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of bromochloro-fulminuric acid bactericide.This procedure is simple.Prepared bromine symclosene dissolution rate in water body is fast, the positive monovalence active halogen ionic concentration height that discharges at short notice, the quick sterilization of particularly suitable aquaculture water.
The bromine symclosene is shown below:
X=Cl or M
+Or 1/2M
2+M=Na or K or Mg or Ca
Bromine symclosene of the present invention means the mixture that is made of monobromo DICHLOROISOCYANURIC ACID and monobromo one chloroisocyan urate.The present invention is realized by the following technical programs: be main raw material with the tricarbimide, by adding the method that alkali dissolution, chlorination, bromination, chlorination again, filtration, dry key step prepare the bromine symclosene.It is characterized in that: tricarbimide is dissolved in the aqueous solution or emulsion of alkali, then in solution or emulsion, feed respectively between 0～25 ℃ chlorine, then the dropping liquid bromine, feed chlorine at last and carry out chlorination reaction, and the final pH value of reaction is controlled between 2～7, obtain total available chlorine and be 54～58%, effectively bromine content is 46～49% product.
The alkali that above-mentioned reaction is adopted is sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, calcium oxide, magnesium oxide, calcium hydroxide, lime carbonate.
When adopting sodium hydroxide to be alkali, the weight ratio of above-mentioned reaction mass is: tricarbimide: sodium hydroxide: chlorine: the liquid bromine: water=129: 115～132: 140～180: 80: 600～3000; Optimum weight ratio is: tricarbimide: sodium hydroxide: chlorine: the liquid bromine: water=129: 120～128: 170～178: 80: 1000～1600.
The optimum temps of above-mentioned chlorate bromination reaction is 5-15 ℃.
Above-mentioned reaction fs chlorating pH value is 4～9, and the best is 4.5～5.5; At the end optimal ph is 2.5～4.
Present method preparation process is simple, and condition is easily controlled, and product available chlorine content height has rapid sterilization effect in water body.
Embodiment
Embodiment 1: add the 240mL tap water in the 500mL four-hole bottle, stir adding 25.2g NaOH down.Be cooled to 10 ℃.Stir and slowly to add the 25.8g tricarbimide down, continue to stir and dissolved substantially to material in 5-10 minute.Under quick stirring and 10 ℃ of conditions of control reaction temperature, feed Cl
2, behind pH=4.8, drip 16g Br
2, and then feed Cl
2Till pH=2.5.Gained white solid suction filtration, the solid seasoning.Weigh 64.8 grams.Total available chlorine: 57.9%; Effective bromine: 47.7%.
Embodiment 2: add the 240mL tap water in the 500mL four-hole bottle, stir adding 23g Na down
2C0
3Be cooled to 10 ℃.Stir and slowly to add the 25.8g tricarbimide down, continue to stir and dissolved substantially to material in 5-10 minute.Under quick stirring and 10 ℃ of conditions of control reaction temperature, feed Cl
2, behind pH=4.8, drip 16g Br
2, feed Cl then
2, till pH=2.5.Gained white solid suction filtration, the solid seasoning.Weigh 63.4 grams.Total available chlorine: 55.7%; Effective bromine: 46.8%.
Embodiment 3: add the 240mL tap water in the 500mL four-hole bottle, stir the Powdered CaO of adding 17.5g down.Be cooled to 10 ℃.Stir and slowly to add the 25.8g tricarbimide down, continue to stir and became the even diploma to material in 5-10 minute.Under quick stirring and 10 ℃ of conditions of control reaction temperature, feed Cl
2, behind pH=4.8, drip 16g Br
2, feed Cl then
2, till pH=2.5.Gained white solid suction filtration, the solid seasoning.Heavily about 64.9 grams.Total available chlorine: 56.4%; Effective bromine: 47.3%.
Claims (7)
1. the preparation method of a bromochloro-fulminuric acid bactericide, this method is main raw material with the tricarbimide, by adding alkali dissolution, chlorination, bromination, chlorination again, filter, dry key step prepares the method for bromine symclosene, it is characterized in that: tricarbimide is dissolved in the aqueous solution or emulsion of alkali, in solution or emulsion, feeding chlorine respectively between 0～25 ℃ then, dropping liquid bromine then, feed chlorine at last and carry out chlorination reaction, and the reaction a final pH value be controlled between 2～7, obtaining total available chlorine is 54～58%, effectively bromine content is 46～49% product.
2. according to the preparation method of the described bromochloro-fulminuric acid bactericide of claim 1, it is characterized in that: the alkali that reaction is adopted is sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, calcium oxide, magnesium oxide, calcium hydroxide, lime carbonate.
3. according to the preparation method of claim 1 and 2 described bromochloro-fulminuric acid bactericides, it is characterized in that: when adopting sodium hydroxide to be alkali, the weight ratio of above-mentioned reaction mass is: tricarbimide: sodium hydroxide: chlorine: the liquid bromine: water=129: 115～132: 140～180: 80: 600～3000.
4. according to the preparation method of claim 1 and 2 described bromochloro-fulminuric acid bactericides, it is characterized in that: when adopting sodium hydroxide to be alkali, the weight ratio of above-mentioned reaction mass is: tricarbimide: sodium hydroxide: chlorine: the liquid bromine: water=129: 120～128: 170～178: 80: 1000～1600.
5. according to the preparation method of the described bromochloro-fulminuric acid bactericide of claim 1, it is characterized in that: the temperature of chlorate bromination reaction is 5-15 ℃.
6. according to the preparation method of the described bromochloro-fulminuric acid bactericide of claim 1, it is characterized in that: reaction fs chlorating pH value is 4～9, and at the end the pH value is 2.5～4.
7. according to the preparation method of the described bromochloro-fulminuric acid bactericide of claim 1, it is characterized in that: reaction fs chlorating pH value is 4.5～5.5, and at the end the pH value is 2.5～4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011308893A CN1156457C (en) | 2001-08-31 | 2001-08-31 | Prepn of bromochloro-fulminuric acid bactericide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011308893A CN1156457C (en) | 2001-08-31 | 2001-08-31 | Prepn of bromochloro-fulminuric acid bactericide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1337396A CN1337396A (en) | 2002-02-27 |
| CN1156457C true CN1156457C (en) | 2004-07-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011308893A Expired - Fee Related CN1156457C (en) | 2001-08-31 | 2001-08-31 | Prepn of bromochloro-fulminuric acid bactericide |
Country Status (1)
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| CN (1) | CN1156457C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104803930B (en) * | 2015-05-07 | 2017-10-27 | 河南银田精细化工有限公司 | A kind of production method of chlorobromide isocyanuric acid |
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2001
- 2001-08-31 CN CNB011308893A patent/CN1156457C/en not_active Expired - Fee Related
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| CN1337396A (en) | 2002-02-27 |
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Granted publication date: 20040707 Termination date: 20090930 |