CN106588810A - Method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone - Google Patents
Method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone Download PDFInfo
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- CN106588810A CN106588810A CN201611073461.7A CN201611073461A CN106588810A CN 106588810 A CN106588810 A CN 106588810A CN 201611073461 A CN201611073461 A CN 201611073461A CN 106588810 A CN106588810 A CN 106588810A
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- isothiazolone
- kettle
- residual
- octyl groups
- chlorine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D275/00—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings
- C07D275/02—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings not condensed with other rings
- C07D275/03—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention relates to the technical field of pretreatment of hazardous waste, in particular to a method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone. The technical scheme is characterized by comprising steps as follows: the cauldron bottom residues of 2-octyl-3(2H)-isothiazolone are transferred into an enamel reactor by a transfer pump, and the temperature of the enamel reactor is reduced to minus 20 DEG C- minus 22 DEG C by a freezing brine supply system; chlorine is introduced into the cooled enamel reactor at a rate of 1.9-2.1 kg/min and is stopped from being introduced when the molar ratio of the introduced chlorine to 2-octyl-3(2H)-isothiazolone is (0.5-0.7):1, and a deeply chlorinated product is obtained. According to the deep chlorination method, two chloride ions are added to the structure of 2-octyl-3(2H)-isothiazolone, and the residual 2-octyl-3(2H)-isothiazolone in the treated cauldron bottom residues is smaller than or equal to 0.5wt%.
Description
Technical field
The present invention relates to a kind of production and processing technology of antibacterial, especially produces to the chlorination during production, recrystallization
The processing procedure of raw mother solution, and in particular to the method for the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone, belongs to dangerous
Waste disposal preconditioning technique field.
Background technology
2- octyl groups -3 (2H)-isothiazolone is a kind of antibacterial, has the operating procedures such as chlorination, recrystallization in its production, its
Middle recrystallization process can produce substantial amounts of waste mother liquor, the active component containing 5wt% or so in mother solution.These active components
(i.e. 2- octyl groups -3 (2H)-isothiazolone) can not bring economic benefit, be the waste of resource, in addition, being also performed to go out during discharge
It is living to process, so not only waste resource but also pollute environment.And in currently available technology, processed both without residual to its kettle
The economic and means of environmental protection.
The content of the invention
To solve above-mentioned technical problem, the invention provides a kind of residual depth chlorine of the kettle of 2- octyl groups -3 (2H)-isothiazolone
The method of change, so as to reach the residual discharge of kettle is reduced, and increases the purpose of the utilization rate of intermediate products.
Technical scheme is as follows：A kind of method of the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone, bag
Include following steps：
(1) proceeded to the kettle of 2- octyl groups -3 (2H)-isothiazolone is residual in enamel still by transfering material pump, supplied by chilled brine
Enamel still kettle temperature is down to into -20 DEG C to -22 DEG C to system；The temperature of chilled brine is -30 DEG C；Chilled brine is the water of ethylene glycol
The mass percent concentration of solution, wherein ethylene glycol is 50%；
(2) to the kettle after cooling it is residual in chlorine is passed through with the speed of 1.9-2.1 kg/minutes, be passed through the molal quantity of chlorine
It is (0.5-0.7) with the mole ratio of 2- octyl groups -3 (2H)-isothiazolone:Stop when 1, obtain final product depth chlorizate；It is passed through chlorine
During gas, keep enamel temperature in the kettle at -15 DEG C to -20 DEG C, the exhaust emissions in chlorination process enters in absorption plant, inhales
Receiving apparatus include tertiary effluent absorption equipment and one-level Alkali absorption equipment；
(3) the depth chlorizate for obtaining step (2) is just pungent through being refining to obtain the chloro- 2- of final goal thing 4,5- bis-
Base-the ketone of isothiazoline -3.
Further, after the completion of described step (2), the residual of 2- octyl groups -3 (the 2H)-isothiazolone during kettle is residual≤
0.5wt%.
Further, the speed that is passed through of chlorine is 2.0 kg/minutes in described step (2).
Further, the molal quantity of described chlorine and the mole ratio of 2- octyl groups -3 (2H)-isothiazolone are 0.6:1.
Further, described 2- octyl groups -3 (2H)-content of the isothiazolone in kettle is residual is 5.0wt%.
Beneficial effects of the present invention are as follows：
(1) three waste discharge is reduced：The present invention using generate technique in as the residual process of kettle waste material through depth chlorination again
Process, useful product is transformed into again, per batch the residual discharge about 90kg of kettle can be reduced, calculate by 2 batches/day, whole year can be reduced
Residual 54 tons of the discharge of kettle (by annual 300 days production calculations)；
(2) product yield is improved：4 are obtained through depth chloridized by the kettle of 2- octyl groups -3 (2H)-isothiazolone is residual,
The product of the chloro- 2- n-octyls-ketone of isothiazoline -3 of 5- bis-, per batch product yield about 60kg can be increased, and calculated according to 2 batches/day,
Whole year can increase by 36 tons of product yield, increase about 6,000,000 yuan of economic benefit；
(3) method of the depth chlorination provided according to the present invention, i.e., increase in the structure of 2- octyl groups -3 (2H)-isothiazolone
Plus 2 chloride ion, the residual≤0.5wt% of residual middle 2- octyl groups -3 (the 2H)-isothiazolone of the kettle after process, if residual>
0.5wt%, then explanation reaction need to continue depth chlorination without complete.
(4) difficult point of present invention process is to control the intake of chlorine and be passed through speed, if be passed through in the unit interval
Another product is generated if chlorine is too fast, chlorine is passed through into rate controlled in 1.9-2.1 kg/minutes in the present invention,
Can be very good the yield and purity for controlling final goal product.
Specific embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not with any shape
Formula is limited to embodiment content.Test method described in embodiment if no special instructions, is conventional method；Such as without special theory
Bright, the reagent material is commercially obtained.
Embodiment 1
Proceed to about 6000 kilograms of kettle is residual in enamel still, kettle temperature be reduced to into -20 DEG C using -30 DEG C of chilled brine,
Then chlorine is passed through with the speed of 2 kg/minutes, is passed through chlorine total amount residual up to logical chlorine, 6000 kilograms of kettles are stopped when 100 kilograms
In effective active matter content be about 5wt%, quality is about 300kg, molal quantity about 1.4kmol, is with the mol ratio of chlorine
0.7:1, lead to the chilled brine during chlorine using -30 DEG C and lower the temperature to enamel still, make enamel still remain at -15 DEG C, obtain
To containing the chloro- 2- n-octyls-ketone of isothiazoline -3 of 4,5- bis- chlorizate, sample analysis, 2- octyl groups -3 (2H)-isothiazolone
Residue is 0.3wt%, by chloride through the refined sterling that the chloro- 2- n-octyls-ketone of isothiazoline -3 of 4,5- bis- is obtained.
Embodiment 2
Proceed to about 6000 kilograms of kettle is residual in enamel still, kettle temperature be reduced to into -22 DEG C using -30 DEG C of chilled brine,
Then chlorine is passed through with the speed of 1.9 kg/minutes, when the molal quantity and 2- octyl groups -3 (2H)-isothiazolone that are passed through chlorine
Mole ratio is 0.5:Stop logical chlorine when 1, the chilled brine during this using -30 DEG C is lowered the temperature to reactor, makes reactor
- 20 DEG C are remained at, the chlorizate containing the chloro- 2- n-octyls-ketone of isothiazoline -3 of 4,5- bis- is obtained, sample analysis, 2- is pungent
The residue of base -3 (2H)-isothiazolone is 0.5wt%, by chloride through it is refined be obtained the chloro- 2- n-octyls of 4,5- bis- -
The sterling of the ketone of isothiazoline -3.
Embodiment 3
Proceed to about 6000 kilograms of kettle is residual in enamel still, kettle temperature be reduced to into -22 DEG C using -30 DEG C of chilled brine,
Then chlorine is passed through with the speed of 2.1 kg/minutes, when the molal quantity and 2- octyl groups -3 (2H)-isothiazolone that are passed through chlorine
Mole ratio is 0.6:Stop logical chlorine when 1, the chilled brine during this using -30 DEG C is lowered the temperature to reactor, makes reactor
Temperature remain at -18 DEG C, obtain the chlorizate containing the chloro- 2- n-octyls-ketone of isothiazoline -3 of 4,5- bis-, sampling point
Analysis, the residue of 2- octyl groups -3 (2H)-isothiazolone is 0.4wt%, and chloride is obtained into the chloro- 2- of 4,5- bis- through refined
The sterling of n-octyl-ketone of isothiazoline -3.
It should be appreciated that above-described embodiment technology design only to illustrate the invention and feature, its object is to allow and are familiar with this
The personage of item technology will appreciate that present disclosure and be carried out, can not be limited the scope of the invention with this, all
The equivalence changes made according to spirit of the invention or modification, all should cover within the scope of the present invention.
Claims (5)
1. the method for the residual depth chlorination of kettle of a kind of 2- octyl groups -3 (2H)-isothiazolone, it is characterised in that comprise the steps：
(1) proceeded to the kettle for containing 2- octyl groups -3 (2H)-isothiazolone is residual in enamel still by transfering material pump, supplied by chilled brine
Enamel still kettle temperature is down to -20 DEG C to -22 DEG C by system；The temperature of chilled brine is -30 DEG C；
(2) to the kettle after cooling it is residual in chlorine is passed through with the speed of 1.9-2.1 kg/minutes, be passed through the molal quantity and 2- of chlorine
The mole ratio of octyl group -3 (2H)-isothiazolone is (0.5-0.7):Stop when 1, obtain final product depth chlorizate；It is passed through chlorine
During, keep enamel temperature in the kettle at -15 DEG C to -20 DEG C, the exhaust emissions in chlorination process enters in absorption plant, absorbs dress
Put including tertiary effluent absorption equipment and one-level Alkali absorption equipment；
(3) the depth chlorizate that obtains step (2) is through being refining to obtain chloro- 2- n-octyls of final goal thing 4,5- bis--different
The ketone of thiazoline -3.
2. a kind of method of the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone as claimed in claim 1, its feature exists
In, after the completion of described step (2), the residual≤0.5wt% of 2- octyl groups -3 (the 2H)-isothiazolone during kettle is residual.
3. a kind of method of the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone as claimed in claim 1, its feature exists
In chlorine is passed through speed for 2.0 kg/minutes in described step (2).
4. a kind of method of the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone as claimed in claim 1, its feature exists
In the described molal quantity of chlorine and the mole ratio of 2- octyl groups -3 (2H)-isothiazolone is 0.6:1.
5. a kind of method of the residual depth chlorination of kettle of 2- octyl groups -3 (2H)-isothiazolone as claimed in claim 1, its feature exists
In described 2- octyl groups -3 (2H)-content of the isothiazolone in kettle is residual is 5.0wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611073461.7A CN106588810A (en) | 2016-11-29 | 2016-11-29 | Method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611073461.7A CN106588810A (en) | 2016-11-29 | 2016-11-29 | Method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone |
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| CN106588810A true CN106588810A (en) | 2017-04-26 |
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| CN201611073461.7A Pending CN106588810A (en) | 2016-11-29 | 2016-11-29 | Method for deeply chlorinating cauldron bottom residues of 2-octyl-3(2H)-isothiazolone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112159365A (en) * | 2020-10-13 | 2021-01-01 | 大连百傲化学股份有限公司 | Method for co-producing OIT and DCOIT |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080227986A1 (en) * | 2006-04-03 | 2008-09-18 | Beijing Tianqing Chemicals Co. Ltd. | Preparation of N-Substituted Isothiazolinone Derivatives |
| CN101412698A (en) * | 2008-11-04 | 2009-04-22 | 东华大学 | Preparation of reactive isothiazolone antibacterial finishing agent |
| CN104072440A (en) * | 2014-07-17 | 2014-10-01 | 上海化学试剂研究所有限公司 | Preparation method of 4,5-dichloro-N-n-octyl isothiazolinone |
-
2016
- 2016-11-29 CN CN201611073461.7A patent/CN106588810A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080227986A1 (en) * | 2006-04-03 | 2008-09-18 | Beijing Tianqing Chemicals Co. Ltd. | Preparation of N-Substituted Isothiazolinone Derivatives |
| CN101412698A (en) * | 2008-11-04 | 2009-04-22 | 东华大学 | Preparation of reactive isothiazolone antibacterial finishing agent |
| CN104072440A (en) * | 2014-07-17 | 2014-10-01 | 上海化学试剂研究所有限公司 | Preparation method of 4,5-dichloro-N-n-octyl isothiazolinone |
Non-Patent Citations (1)
| Title |
|---|
| WEILER, ERNEST D. ET AL: "Isothiazoles. IX. Halogenation of 2-substituted-4-isothiazolin-3-ones", 《JOURNAL OF HETEROCYCLIC CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112159365A (en) * | 2020-10-13 | 2021-01-01 | 大连百傲化学股份有限公司 | Method for co-producing OIT and DCOIT |
| CN112159365B (en) * | 2020-10-13 | 2022-05-20 | 大连百傲化学股份有限公司 | Method for co-producing OIT and DCOIT |
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Application publication date: 20170426 |
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