CN106518801A - Method for recovering insoluble saccharin from probenazole produced wastewater - Google Patents
Method for recovering insoluble saccharin from probenazole produced wastewater Download PDFInfo
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- CN106518801A CN106518801A CN201610873314.1A CN201610873314A CN106518801A CN 106518801 A CN106518801 A CN 106518801A CN 201610873314 A CN201610873314 A CN 201610873314A CN 106518801 A CN106518801 A CN 106518801A
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- opened
- suction filtration
- kettle
- waste water
- decolouring
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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
- C07D275/04—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems
- C07D275/06—Heterocyclic compounds containing 1,2-thiazole or hydrogenated 1,2-thiazole rings condensed with carbocyclic rings or ring systems with hetero atoms directly attached to the ring sulfur atom
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for recovering saccharin from probenazole wastewater, wherein the method comprises the steps: adding activated carbon to wastewater obtained after chlorination, dispersion, etherification, neutralization and suction filtration, and adsorbing for two times at the temperature of 20-60 DEG C; and then adding a hydrochloric acid solution, stirring, allowing to stand, after crystals are formed, filtering, extracting a filter cake to be dry, washing, and drying to obtain the insoluble saccharin. The preparation method is simple and feasible, and convenient to operate; the purity of the insoluble saccharin recovered from the wastewater can reach 95% or more, the insoluble saccharin can completely return to chlorination to be used as a raw material for continual use, the cost is reduced, and the environment is protected.
Description
Technical field
The invention belongs to chemical field, reclaims insoluble sugar in more particularly to a kind of production waste water from allyl benzene thiazole
The method of essence.
Background technology
Saccharin, scientific name saccharin, also known as saccharin insoluble (insoluble saccharin), are white
Odorless has the crystalline powder of sweet taste, is most ancient synthetic sweetener.Saccharin purposes is extremely wide, and which is mainly used as food
Additive, feed addictive, it is also possible to as multiple fields such as fertilizer agricultural chemicals.
The industrial preparative method of saccharin mainly has two kinds at present, and one kind is toluene method, and another kind is phthalic anhydride method.
Wherein it is most widely used with phthalic anhydride method.
Allyl benzene thiazole is external using a kind of relatively broad bactericide, and its production process is more complicated, thus its row
The production waste component for going out is complicated, and COD is also higher.After the processing method of existing allyl benzene thiazole waste water is mainly using concentration
The processing method burned again, so, not only results in the waste of beneficial resource so that waste sufficiently cannot be utilized, and
Increase energy consumption.The process of such waste water does not temporarily also have more good processing method at present.
The content of the invention
In view of the foregoing, the invention provides a kind of simple, easy to operate gives up from the production of allyl benzene thiazole
The method for reclaiming saccharin insoluble in water.
For reaching above-mentioned purpose, the technical solution adopted for the present invention to solve the technical problems is：
It is a kind of to produce the method for reclaiming saccharin insoluble in waste water from allyl benzene thiazole, it is characterised in that to comprise the following steps：
（1）Waste water Jing after chlorination, dispersion, etherificate, neutralization, suction filtration is squeezed in decolouring kettle；
（2）Watery hydrochloric acid is added in decolouring kettle, and the pH value for adjusting waste water is 5.0-5.5, while open steam heated, will
The temperature of waste water is raised to 40 DEG C；
（3）To in decolouring kettle, add activated carbon, weight to press activated carbon and waste water 0.005-0.05：The ratio of 1 (kg/L), continues to stir
Mix 0.5-2 hours；
（4）Decolouring bottom valve is opened, feed liquid is put into into suction filtration tank, vacuum system is opened, suction filtration operation is carried out；
（5）Transfering material pump is opened, filtrate is continued to be driven in decolouring kettle, the pH value for being added thereto to watery hydrochloric acid regulation feed liquid is
Feed temperature, while opening heating steam, is raised to 55 DEG C by 3.0-3.5；
（6）Activated carbon is continuously added, weight presses activated carbon and waste water 0.005：The ratio of 1 (kg/L), continues stirring 0.5-2 little
When；
（7）Decolouring bottom valve is opened, feed liquid is put into into suction filtration tank, vacuum system is opened, suction filtration operation is carried out；
（8）Transfering material pump is opened, filtrate is driven in acid out kettle, stirring is opened, be slowly added to watery hydrochloric acid, the PH for adjusting kettle liquid is
1.0, freezing is opened, kettle temperature is down to into 0 DEG C, continue stirring 2 hours；
（9）Acid out bottom valve blowing suction filtration is opened, during suction filtration and adds cold water to drain after washing twice；
（10）Filter cake is taken out, is dried in 120 DEG C or so in being sent to drier.
Due to the utilization of above-mentioned technical proposal, the present invention has following beneficial effect compared with prior art：
Preparation method of the present invention is simple, easy to operate, produces the saccharin insoluble reclaimed in waste water from allyl benzene thiazole
Purity is continuing with as raw material in may return to chlorination completely, reduces cost, protect environment up to more than 95%.
Specific embodiment
With reference to specific embodiment, present disclosure is described in further detail：
Embodiment（One）：
To in flask add 500ml in and suction filtration after probenazole waste water, plus watery hydrochloric acid adjust PH be 5.0, be warmed up to 40 DEG C,
After adding 2.5 grams of activated carbons to stir 2 hours, pour suction filtration in Buchner funnel into, filtrate returned in flask, it is 3.0 to adjust PH,
Continue to be warmed up to 55 DEG C, suction filtration after adding 2.5 grams of activated carbons to stir 2 hours, adjust PH to be 1.0 by the acid of filtrate salt adding continuous, and cold temperature
To 0 DEG C, filter cake is dried in 120 DEG C of baking ovens, obtains slightly yellow 95.5% saccharin insoluble by low rate mixing suction filtration after 2 hours
3.6 gram.
Embodiment（Two）：
To in flask add 1000ml in and suction filtration after probenazole waste water, plus watery hydrochloric acid adjust PH be 5.0, be warmed up to 40
DEG C, after adding 5 grams of activated carbons to stir 2 hours, pour suction filtration in Buchner funnel into, filtrate is returned in flask, adjusting PH is
2.5, continue to be warmed up to 55 DEG C, suction filtration after adding 5 grams of activated carbons to stir 2 hours, adjust PH to be 1.0 by the acid of filtrate salt adding continuous, and it is cold
Filter cake is dried in 120 DEG C of baking ovens, obtains slightly yellow 96.5% saccharin insoluble by temperature to 0 DEG C, low rate mixing suction filtration after 2 hours
7.5 gram.
Embodiment（Three）：
To in flask add 500ml in and suction filtration after probenazole waste water, plus watery hydrochloric acid adjust PH be 5.5, be warmed up to 40 DEG C,
After adding 2 grams of activated carbons to stir 2 hours, pour suction filtration in Buchner funnel into, filtrate is returned in flask, it is 3.0 to adjust PH, after
Continuous to be warmed up to 55 DEG C, suction filtration after adding 2.5 grams of activated carbons to stir 2 hours is adjusted PH to be 1.0 by the acid of filtrate salt adding continuous, and cold temperature is arrived
0 DEG C, filter cake is dried in 120 DEG C of baking ovens, obtains slightly yellow 95.1% saccharin insoluble 3.7 by low rate mixing suction filtration after 2 hours
Gram.
The main chemical reactions formula being related in embodiment is as follows：
Above-described embodiment technology design only to illustrate the invention and feature, its object is to allow person skilled in the art's energy
Solution present disclosure much of that is simultaneously carried out, and can not be limited the scope of the invention with this, all according to spirit of the invention
Equivalence changes or modification that essence is made, should all cover within the scope of the present invention.
Claims (1)
1. it is a kind of to produce the method for reclaiming saccharin insoluble in waste water from allyl benzene thiazole, it is characterised in that including following step
Suddenly：
（1）Waste water Jing after chlorination, dispersion, etherificate, neutralization, suction filtration is squeezed in decolouring kettle；
（2）Watery hydrochloric acid is added in decolouring kettle, and the pH value for adjusting waste water is 5.0-5.5, while open steam heated, will be useless
The temperature of water is raised to 40 DEG C；
（3）To in decolouring kettle, add activated carbon, weight to press activated carbon and waste water 0.005-0.05：The ratio of 1 (kg/L), continues to stir
Mix 0.5-2 hours；
（4）Decolouring bottom valve is opened, feed liquid is put into into suction filtration tank, vacuum system is opened, suction filtration operation is carried out；
（5）Transfering material pump is opened, filtrate is continued to be driven in decolouring kettle, the pH value for being added thereto to watery hydrochloric acid regulation feed liquid is
Feed temperature, while opening heating steam, is raised to 55 DEG C by 3.0-3.5；
（6）Activated carbon is continuously added, weight presses activated carbon and waste water 0.005：The ratio of 1 (kg/L), continues stirring 0.5-2 little
When；
（7）Decolouring bottom valve is opened, feed liquid is put into into suction filtration tank, vacuum system is opened, suction filtration operation is carried out；
（8）Transfering material pump is opened, filtrate is driven in acid out kettle, stirring is opened, be slowly added to watery hydrochloric acid, the PH for adjusting kettle liquid is
1.0, freezing is opened, kettle temperature is down to into 0 DEG C, continue stirring 2 hours；
（9）Acid out bottom valve blowing suction filtration is opened, during suction filtration and adds cold water to drain after washing twice；
（10）Filter cake is taken out, is dried in 120 DEG C or so in being sent to drier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610873314.1A CN106518801A (en) | 2016-10-08 | 2016-10-08 | Method for recovering insoluble saccharin from probenazole produced wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610873314.1A CN106518801A (en) | 2016-10-08 | 2016-10-08 | Method for recovering insoluble saccharin from probenazole produced wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106518801A true CN106518801A (en) | 2017-03-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610873314.1A Pending CN106518801A (en) | 2016-10-08 | 2016-10-08 | Method for recovering insoluble saccharin from probenazole produced wastewater |
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| Country | Link |
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| CN (1) | CN106518801A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698424A (en) * | 2019-11-05 | 2020-01-17 | 天津北方食品有限公司 | Preparation method of probenazole |
| CN110759872A (en) * | 2019-10-16 | 2020-02-07 | 天津北方食品有限公司 | Method for removing saccharin in probenazole |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786998A (en) * | 2010-04-08 | 2010-07-28 | 天津市鑫卫化工有限责任公司 | Preparation method of high-purity o-sulfonylbenzoylimine |
| CN101891699A (en) * | 2010-07-08 | 2010-11-24 | 平煤集团开封兴化精细化工厂 | Method for recovery of insoluble saccharin in acidic wastewater by resin adsorption method |
| CN103420935A (en) * | 2012-05-15 | 2013-12-04 | 张卫民 | Method of processing sodium saccharin crystallized mother liquid |
| CN103508974A (en) * | 2012-06-28 | 2014-01-15 | 张卫民 | Method for treating methyl 2-(aminosulfonyl)benzoate crystallization mother solution |
-
2016
- 2016-10-08 CN CN201610873314.1A patent/CN106518801A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786998A (en) * | 2010-04-08 | 2010-07-28 | 天津市鑫卫化工有限责任公司 | Preparation method of high-purity o-sulfonylbenzoylimine |
| CN101891699A (en) * | 2010-07-08 | 2010-11-24 | 平煤集团开封兴化精细化工厂 | Method for recovery of insoluble saccharin in acidic wastewater by resin adsorption method |
| CN103420935A (en) * | 2012-05-15 | 2013-12-04 | 张卫民 | Method of processing sodium saccharin crystallized mother liquid |
| CN103508974A (en) * | 2012-06-28 | 2014-01-15 | 张卫民 | Method for treating methyl 2-(aminosulfonyl)benzoate crystallization mother solution |
Non-Patent Citations (1)
| Title |
|---|
| 崔玉民，等: "从糖精废液中回收糖精的研究", 《天津化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759872A (en) * | 2019-10-16 | 2020-02-07 | 天津北方食品有限公司 | Method for removing saccharin in probenazole |
| CN110698424A (en) * | 2019-11-05 | 2020-01-17 | 天津北方食品有限公司 | Preparation method of probenazole |
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Application publication date: 20170322 |
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