CN103214362A - Method for extracting trifluoroacetic acid from explosive waste water - Google Patents
Method for extracting trifluoroacetic acid from explosive waste water Download PDFInfo
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- CN103214362A CN103214362A CN2013101361515A CN201310136151A CN103214362A CN 103214362 A CN103214362 A CN 103214362A CN 2013101361515 A CN2013101361515 A CN 2013101361515A CN 201310136151 A CN201310136151 A CN 201310136151A CN 103214362 A CN103214362 A CN 103214362A
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Abstract
The invention discloses a method for extracting trifluoroacetic acid from explosive waste water. The method comprises the following steps of: distilling the explosive waste water produced by explosive synthesis, and obtaining a trifluoroacetic acid-water mixing solution by collection; distilling the trifluoroacetic acid-water mixing solution, and collecting fractions at the temperature of 105-106 DEG C to obtain a trifluoroacetic acid-water azeotrope; adding a solvent into the trifluoroacetic acid-water azeotrope, distilling the mixture, and collecting the fractions which are the trifluoroacetic acid; and distilling off the water from the mother solution obtained after distillation in the step 3 to obtain a recycled solvent. According to the method, fuming sulfuric acid or concentrated sulfuric acid is added into the trifluoroacetic acid-water azeotrope, so that during the distillation, only the trifluoroacetic acid is distilled off; the steps are simple, the conditions are mild, and the safety is high; the used solvent can be recycled and reused; the environment pollution is avoided, and the cost is saved; the concentration of the extracted trifluoroacetic acid can be up to over 96 percent; and the extracted trifluoroacetic acid can be used for preparing explosives, so that the production cost of the explosives can be obviously reduced.
Description
Technical field
The invention belongs to chemical field, relate to a kind of separation method of trifluoroacetic acid-water, be specifically related to a kind of method of extracting trifluoroacetic acid from explosive waste water, this method has application promise in clinical practice in the energetic material field.
Background technology
Trifluoroacetic acid (TFA) is a kind of colourless fuming liquid that the intense stimulus smell is arranged, and is one-level organic acidity corrosives.The TFA sedimentation and be accumulated in soil and water body in, be difficult to degrade by approach such as chemical reaction and microbiological deteriorations.When TFA concentration reaches 100-300 μ g/L, can suppress plant-growth in the water body, the regional ecosystem is impacted.The similar muriate trichoroacetic acid(TCA) of trifluoroacetic acid is known carcinogenic substance, and obviously, trifluoroacetic acid need think better of the influence of HUMAN HEALTH and environmental pollution.At present, trifluoroacetic acid does not still have known degraded to eliminate mechanism in environment.Trifluoroacetic acid and 20.6%(wt) water form binary azeotrope (azeotropic point is 105.5 ℃), can not separate trifluoroacetic acid and water with common rectificating method, and, owing to cost an arm and a leg, it is also inadvisable to handle trifluoroacetic acid with the method for acid-base neutralisation, therefore, trifluoroacetic acid-water is separated into a difficult problem that needs to be resolved hurrily in the Chemical Manufacture.
TFA is as reactant or catalyzer, prepares at explosive to have very wide application in the industry.As: 2,6-diamino-3, the nitrogen oxidation of 5-dinitrobenzene pyrazine-1-oxide compound, 3, the amino oxidation of 4-dinitrobenzene furazan base-furoxan, 3,6-diaminostilbene, 2,4,5-tetrazine-1, the nitrogen oxidation of 4-dioxide etc.The concentration of TFA can not directly recycle much larger than 100-300 μ g/L in the reacted explosive waste water, more can not discharge.Expensive TFA not only makes the manufacturing cost of explosive improve greatly, and there is harm greatly in the waste water that contains TFA to environment and human health, therefore, extracts trifluoroacetic acid from explosive waste water, has crucial economic benefit and environmental benefit.
At present, less about the report that from explosive waste water, extracts TFA, document [1] (Deng Mingzhe, Ye Zhihu etc., the recycling of trifluoroacetic acid during the LLM-105 explosive is synthetic, fire explosive journal, 2009,32 (4): 50-52) reported the recycling that the LLM-105 explosive synthesizes middle trifluoroacetic acid, document [2] (Zhou Xiaoqing, Cheng Bibo, Huang Jinglun etc., the recovery new technology of trifluoroacetic acid during the LLM-105 explosive is synthetic, energetic material, 2012,20(4): 501) reported the recovery new technology that the LLM-105 explosive synthesizes middle trifluoroacetic acid.Document [1] adopts the mode with salt rectifying, the spent acid treatment capacity of report only is 330mL, if reclaim a large amount of trifluoroacetic acid waste liquid of art breading with this, to face the recovery of salt, the conveying of solid materials, the problems such as the easy crystallization blocking pipe of salt of adding, and face that energy consumption is big, return period problem such as length, cost height, be unfavorable for amplifying and reclaim the trifluoroacetic acid waste liquid.Document [2] is though mention and will add a kind of strong absorptive solvent, and strong absorptive solvent content is very wide, specifically proposes in the document.
Summary of the invention
In order to solve in the prior art problem such as from trifluoroacetic acid-water mixed liquid, extract trifluoroacetic acid technology cost height, return period is long, treatment capacity is little, the invention provides a kind of method of extracting trifluoroacetic acid from explosive waste water, the extraction step of this method is simple, the trifluoroacetic acid concentration of mild condition, extraction can reach more than 96%.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
A kind of method of extracting trifluoroacetic acid from explosive waste water may further comprise the steps:
Step 1: the explosive waste water that explosive is produced in synthetic distills, collect trifluoroacetic acid-water mixed solution;
Step 2: trifluoroacetic acid-water mixed solution is distilled, collect 105～106 ℃ cut, obtain trifluoroacetic acid-water azeotrope;
Step 3: add solvent in trifluoroacetic acid-water azeotrope, distillation is collected cut and is trifluoroacetic acid;
Above-mentioned method is further comprising the steps of: the mother liquor distillation with after the step 3 distillation, the moisture in the mother liquor is distilled out, and obtain reclaiming solvent, reclaim solvent and can be recycled.
In above-mentioned method, described solvent is not for all to form azeotrope with water and trifluoroacetic acid; As the preferred embodiments of the present invention, preferably: described solvent is a kind of in the oleum and the vitriol oil.
In above-mentioned method, can separate fully in order to make the trifluoroacetic acid in trifluoroacetic acid-water mixed liquid, the consumption of described solvent is that every gram trifluoroacetic acid-water azeotrope adds 1～1.6g solvent.
In above-mentioned method, the described distillation of step 1 is air distillation or underpressure distillation.
In above-mentioned method, obtain the high trifluoroacetic acid of concentration in order to distill, the described distillation of step 3 is air distillation or rectifying.
The present invention compared with prior art has following beneficial effect:
(1) extracting method of the present invention adopts the oleum or the vitriol oil to join trifluoroacetic acid-water azeotrope, utilize the oleum or the vitriol oil to have stronger water-retaining capacity, thereby distillation the time only distills out trifluoroacetic acid, method steps is simple, mild condition, security is good.
(2) the used recyclable utilization again of solvent of the present invention not only can not cause environmental pollution, has also saved cost.
(3) the trifluoroacetic acid concentration that adopts present method to extract can reach more than 96%, and the trifluoroacetic acid of extraction can be used for the preparation of explosive, can reduce the cost of explosive production significantly.
Embodiment
The invention will be further elaborated and explanation below in conjunction with embodiments of the invention.
Embodiment 1
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 700ml, heat up then, solution distills behind the backflow 0.5h 72 ℃ of-75 ℃ of boilings, collects cut, obtains trifluoroacetic acid (310ml, purity 96%).
Embodiment 2
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 900ml, heat up then, solution distills behind the backflow 1.0h 72 ℃ of-75 ℃ of boilings, collects cut, obtains trifluoroacetic acid (320ml, purity 96%).
Embodiment 3
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 1050ml, heat up then, solution distills behind the backflow 1.0h 72 ℃ of-75 ℃ of boilings, collects cut, obtains trifluoroacetic acid (340ml, purity 96%).
Embodiment 4
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 900ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 900ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, and behind the backflow 0.5h, cut is collected in rectifying, obtains trifluoroacetic acid (400ml, purity 98%).
Embodiment 5
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 800ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, and behind the backflow 1.0h, cut is collected in rectifying, obtains trifluoroacetic acid (330ml, purity 99%).
Embodiment 6
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 800ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add oleum 1200ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, behind the backflow 1.0h, and rectifying, collect cut, obtain trifluoroacetic acid (350ml, purity 99%).
Embodiment 7
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 700ml, heat up then, solution distills behind the backflow 0.5h 72 ℃ of-75 ℃ of boilings, collect cut, obtain trifluoroacetic acid (280ml, purity 96%).
Embodiment 8
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 900ml, heat up then, solution distills behind the backflow 1.0h 72 ℃ of-75 ℃ of boilings, collect cut, obtain trifluoroacetic acid (300ml, purity 96%).
Embodiment 9
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 1120ml, heat up then, solution distills behind the backflow 1.0h 72 ℃ of-75 ℃ of boilings, collect cut, obtain trifluoroacetic acid (310ml, purity 96%).
Embodiment 10
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 900ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 900ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, behind the backflow 0.5h, and rectifying, collect cut, obtain trifluoroacetic acid (390ml, purity 98%).
Embodiment 11
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 800ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, behind the backflow 1.0h, and rectifying, collect cut, obtain trifluoroacetic acid (270ml, purity 99%).
Embodiment 12
At room temperature, the synthetic middle explosive waste water that produces of explosive is added in the distiller, under reduced pressure, distill then, collect trifluoroacetic acid-water mixed solution.Trifluoroacetic acid-water mixed solution is distilled, collect 105 ℃ of-106 ℃ of cuts that steam, obtain trifluoroacetic acid-water azeotrope.Under the room temperature, 700ml trifluoroacetic acid-water azeotrope is added in the reactor, under agitation slowly add 98% vitriol oil 1120ml, heat up then, solution is 72 ℃ of-75 ℃ of boilings, behind the backflow 1.0h, and rectifying, collect cut, obtain trifluoroacetic acid (310ml, purity 99%).
Although invention has been described with reference to explanatory embodiment of the present invention here, the foregoing description only is preferred implementation of the present invention, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and embodiment will drop within the disclosed principle scope and spirit of the application.
Claims (7)
1. method of extracting trifluoroacetic acid from explosive waste water is characterized in that may further comprise the steps:
Step 1: the explosive waste water that explosive is produced in synthetic distills, collect trifluoroacetic acid-water mixed solution;
Step 2: trifluoroacetic acid-water mixed solution is distilled, collect 105～106 ℃ cut, obtain trifluoroacetic acid-water azeotrope;
Step 3: add solvent in trifluoroacetic acid-water azeotrope, distillation is collected cut and is trifluoroacetic acid.
2. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 1 is characterized in that further comprising the steps of: the mother liquor distillation with after the step 3 distillation, the moisture in the mother liquor is distilled out, and obtain reclaiming solvent.
3. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 1 and 2 is characterized in that described solvent is not for all to form azeotrope with water and trifluoroacetic acid.
4. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 3 is characterized in that described solvent is a kind of in the oleum and the vitriol oil.
5. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 4, the consumption that it is characterized in that described solvent are that every gram trifluoroacetic acid-water azeotrope adds 1～1.6g solvent.
6. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 5 is characterized in that the described distillation of step 1 is air distillation or underpressure distillation.
7. a kind of method of extracting trifluoroacetic acid from explosive waste water according to claim 5 is characterized in that the described distillation of step 3 is air distillation or rectifying.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5240566A (en) * | 1992-12-07 | 1993-08-31 | The Goodyear Tire & Rubber Company | Separation process |
| CN101878189A (en) * | 2007-09-28 | 2010-11-03 | 罗地亚管理公司 | Method for recovering fluorocarboxylic acids |
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2013
- 2013-04-18 CN CN2013101361515A patent/CN103214362A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5240566A (en) * | 1992-12-07 | 1993-08-31 | The Goodyear Tire & Rubber Company | Separation process |
| CN101878189A (en) * | 2007-09-28 | 2010-11-03 | 罗地亚管理公司 | Method for recovering fluorocarboxylic acids |
Non-Patent Citations (1)
| Title |
|---|
| ZHOU XIAO-QING ET AL.: "A New Recycling Technique of Trifluoroacetic Acid in Synthesis of LLM-105 Explosive", 《含能材料》 * |
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Application publication date: 20130724 |