CN103386211A - Device and method for separating acetonitrile-water-methanol mixture - Google Patents
Device and method for separating acetonitrile-water-methanol mixture Download PDFInfo
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- CN103386211A CN103386211A CN2013102947444A CN201310294744A CN103386211A CN 103386211 A CN103386211 A CN 103386211A CN 2013102947444 A CN2013102947444 A CN 2013102947444A CN 201310294744 A CN201310294744 A CN 201310294744A CN 103386211 A CN103386211 A CN 103386211A
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Abstract
The invention discloses a device and a method for separating an acetonitrile-water-methanol mixture. The separating device comprises a heating device, a temperature measurement couple, a rectification tower and a product collection tank. The rectification tower, which is located in the heating device, comprises a tower bottom, in which the temperature measurement couple is arranged, a rectification section connected to the tower bottom, a condensing tower above the rectification section, and a liquid transfer tube. The separating method utilizes the device and the differences of solubilities of all components of the mixture in dichloromethane to remove methanol first, the dichloromethane in the lower layer flows back into the rectification tower, and sodium chloride is added into the remaining mixture of acetonitrile and water for breaking and separating the azeotrope to obtain the acetonitrile and the water. The separating device is simple in structure, easy to operate, low in energy consumption, and suitable for industrial production. The device and the method achieve separation of acetonitrile, water and methanol with low costs and energy consumption, and are environmentally friendly and convenient for applications.
Description
Technical field
The present invention relates to the separating technology of mixture, be specifically related to a kind of separator and separation method of acetonitrile-water-carbinol mixture.
Background technology
Methyl alcohol and acetonitrile are important industrial chemicals and solvents, be to be also important mobile phase in liquid chromatographic detection, therefore easily produce methyl alcohol and the mixture of acetonitrile two components or the mixture of methyl alcohol, acetonitrile and water three components in the processes such as Chemical Manufacture and detection., in order to prevent that these mixtures from damaging usually and will reclaim environment, after reclaiming, mixture is reclaimed and can apply at this; No matter yet be that mixture or the mixture of three components of two components all easily forms azeotropic mixture under normal pressure, therefore be difficult to separate with common rectificating method.
Separating of the mixture of methyl alcohol and acetonitrile two components, be mainly to separate by the method for variable-pressure rectification, and the variable-pressure rectification separating effect is better, but the variable-pressure rectification cost is high, and vacuum tower tower reactor temperature is too low, need to expend huge energy consumption.Chinese patent application CN102068831A discloses the intermittent extraction, distillation and separation method of a kind of acetonitrile-methanol azeotropic mixture, the extracting rectifying mode separating acetonitrile of employing interpolation DMF-methanol azeotropic mixture, although solved the problem of energy consumption, but DMF has higher toxicity, there is potential safety hazard, be unfavorable for industrial promotion and application.
Separating of the mixture of methyl alcohol, acetonitrile and water three components, utilize variable-pressure rectification to be difficult to reach the effect of separation; Due to during water and methyl alcohol and DMF can dissolve each other, so said method can not be used for and will separate in ternary mixture.Up to the present also do not have a kind of can separation of methanol, the method for the mixture of acetonitrile and water three components, so be all to sell waste product reagent to reclaim company's burning disposal greatly, but acetonitrile burns and easily produces the hydrogen cyanide extremely toxic substance, and environment is damaged.Therefore, the ternary mixture of separating-purifying acetonitrile methanol water not only has economic worth and also possesses the value of environmental protection.
Summary of the invention
, for overcoming the defect of prior art, the object of the present invention is to provide a kind of separator of acetonitrile-water-carbinol mixture.
Another object of the present invention is to provide a kind of separation method of acetonitrile-water-carbinol mixture, by realizing the separation between acetonitrile-water-methyl alcohol three, cost is low, and energy consumption is little, and environmental protection, convenient application.
As follows for realizing above-mentioned first purpose the technical solution adopted in the present invention:
A kind of separator of acetonitrile-water-carbinol mixture, comprise heater, thermometric galvanic couple, rectifying column and product-collecting filling, described rectifying column comprises tower reactor, rectifying section, condensing tower, described rectifying column is arranged in heater, the thermometric galvanic couple is arranged in tower reactor, rectifying section is connected on tower reactor, and condensing tower is positioned at the top of rectifying section; It also comprises that one turns the liquid pipe, turns the liquid pipe and comprises vertical arm and horizontal arm, and described condensing tower bottom is provided with a high-position discharge mouth and low level discharging opening; Described low level discharging opening connects an end of vertical arm, the other end of vertical arm is equipped with only liquid valve, described rectifying section is provided with charging aperture, horizontal arm one end is connected on vertical arm, the other end connects the charging aperture of rectifying section, be provided with the first control valve on described horizontal arm, product-collecting is filled with by a drain pipe and is connected the high-position discharge mouth, is provided with the second control valve on drain pipe; Described rectifying section top is provided with temperature measuring equipment.
The present invention can also realize by following scheme:
As one embodiment of the present invention, in such scheme, described theoretical number of plates of rectifying tower is 50.
As one embodiment of the present invention, in such scheme, described heater comprises electric heating cover and insulation cotton-padded covering, and tower reactor is arranged in electric heating cover, and the insulation cotton-padded covering wraps rectifying section.
For realizing second purpose of the present invention, the technical solution adopted in the present invention is as follows:
A kind of separation method of acetonitrile-water-carbinol mixture, the method adopts above-mentioned acetonitrile-water-carbinol mixture separator, according to following steps, carries out:
1) acetonitrile-water-methyl alcohol mixed waste liquor is packed in tower reactor, add carrene, close simultaneously the first control valve, the second control valve and liquid valve only, stir and heat up, it is the cut of 36-40 ℃ that infinite reflux 0.4-0.8 hour, collection rectifying section push up temperature; Wherein the addition of carrene and acetonitrile-water-methyl alcohol mixed waste liquor is 1:(3-5 according to mass ratio) ratio mix;
2) above-mentioned cut cooling layering at the bottom of condensing tower, open the first control valve and the second control valve, to be methyl alcohol be recovered to during collection of products fills with by high-position discharge mouth on separator the upper strata cut, and lower floor's carrene enters and turns the liquid pipe and be back in tower reactor through the low level discharging opening;
3) after methyl alcohol phase fluid is completed, close the first control valve, the second control valve, continue to heat up, reflux, collecting rectifying section top temperature is 49 ~ 53 ℃ of cuts;
4) cut in step 3), cooling at the bottom of condensing tower, open only liquid valve, reclaim carrene;
5) step 4) reclaim complete after, near room temperature, add NaCl toward tower reactor in, be warming up to rectifying section top temperature and reach 70 ℃, infinite reflux, get the cut of 70 ~ 71 ℃, reflux ratio 1.3, recovery acetonitrile;
6) acetonitrile reclaim complete after, be saline solution at the bottom of cooling, tower reactor, distillation again, wholely go out most of water, reclaims salt.
In said method, the selection of solvent is most important, the solubility of carrene in water is very little, but can dissolve each other with methyl alcohol, add carrene in the mixture of three components after, there will be layering, upper strata is acetonitrile and the aqueous solution, lower floor is the solution of methyl alcohol and carrene, and after stirring boiling, at first the azeotropic mixture of methyl alcohol and carrene is separated.
the principle of said method separating acetonitrile of the present invention-water-methanol mixture is: utilize the difference of this carrene to each components dissolved of mixture, due to methyl alcohol and carrene mixes and boiling point is the most approaching, at the beginning after the heating, carrene and the formation of methanol azeotropic mixture, after rectifying column separates, condensation separatory under tower top end condenser, by rectifying, the methanol solution of carrene is separated from the tower top end, condensed carrene and methanol solution layering, upper strata methyl alcohol removes and obtains methyl alcohol, lower floor's methylene chloride reflux is to tower, after removing methyl alcohol, at the bottom of remaining tower acetonitrile and aqueous mixtures by add sodium chloride destroy azeotropic plus fifteen from, last separating acetonitrile and water.
As one embodiment of the present invention, in above-mentioned separation method, the addition of step 5) sodium chloride accounts for the 1-5% of acetonitrile-water-methyl alcohol mixed waste liquor gross weight.
Beneficial effect of the present invention is: separator of the present invention, and simple in structure, easy to operate, less energy consumption, be applicable to suitability for industrialized production; The present invention adopts above-mentioned separator, by add carrene in acetonitrile-water-carbinol mixture, utilize each component of mixture and carrene between deliquescent difference, separate discontinuous rectifying through rectifying column and isolate three kinds of materials, whole separation process is carried out under normal pressure, energy consumption is little, and security performance is high, has realized the separation of acetonitrile-water-methyl alcohol ternary mixture; By three components that the method is separated, the methanol purity that wherein reclaims reaches 98.5%, and the rate of recovery reaches 98%; Acetonitrile purity is more than 98%, and the rate of recovery reaches 95%; The carrene rate of recovery reaches 98%; The rate of recovery of agent NaCl reaches 99.5%.
Below in conjunction with concrete embodiment, the present invention is described in further detail.
Description of drawings
Fig. 1 is the separator structural representation of acetonitrile-water-carbinol mixture of the present invention.
The specific embodiment
As shown in Figure 1, the separator of acetonitrile-water-carbinol mixture of the present invention, comprise heater, thermometric galvanic couple 2, rectifying column and product-collecting filling, described rectifying column comprises tower reactor 2, rectifying section 4, condensing tower 6, described rectifying column is arranged in heater, thermometric galvanic couple 3 is arranged in tower reactor, and rectifying section 4 is connected on tower reactor 2, and condensing tower 6 is positioned at the top of rectifying section 4; It also comprises that one turns the liquid pipe, turns the liquid pipe and comprises vertical arm 10 and horizontal arm 12, and at the bottom of described condensing tower, 6 ones are provided with a high-position discharge mouth and low level discharging opening; Described low level discharging opening connects an end of vertical arm 10, the other end of vertical arm 10 is equipped with only liquid valve 11, described rectifying section 4 is provided with charging aperture 13, horizontal arm 12 1 ends are connected on vertical arm 10, the other end connects the charging aperture 13 of rectifying section 4, be provided with the first control valve 14 on described horizontal arm 12, product-collecting is filled with 9 and is connected the high-position discharge mouth by a drain pipe 8, is provided with the second control valve 7 on drain pipe 8; Described rectifying section 4 tops are provided with temperature measuring equipment 5.
As one embodiment of the present invention, in such scheme, described theoretical number of plates of rectifying tower is 50.
As one embodiment of the present invention, in such scheme, described heater comprises electric heating cover 1 and insulation cotton-padded covering (not shown), and tower reactor 2 is arranged in electric heating cover 1, and the insulation cotton-padded covering wraps rectifying section.
Be below specific embodiment of the present invention, in an embodiment of the present invention, adopt device of the present invention to separate water 52.6% in the waste liquid that contains methyl alcohol-acetonitrile-water, acetonitrile 32.2%, methyl alcohol 15.2%, the content of above component is calculated by percentage to the quality.
Embodiment 1
Adopt above-mentioned separator, 20kg waste liquid, 5kg carrene are added the rectifying tower reactor, close simultaneously the first control valve, the second control valve and stop the liquid valve, open and stir, and slowly heat up; Come to life to 50 ℃, infinite reflux 0.5 hour, 38 ℃ of top temperature, start discharging, and after the condensing tower condensation,, at the condensing tower bottom slice, open the first control valve and the second control valve and reclaim methyl alcohol, and the backflow carrene, control reflux ratio 1.2; After the discharging of methyl alcohol phase is complete, close the first control valve and the second control valve, again be warming up to 70 ℃, get 50 ~ 51 ℃ of cuts, open only liquid valve and reclaim additive, reclaim after complete and be down to room temperature, close apolipsis liquid valve, add NaCl0.1kg in the still tower, be warming up to 90 ℃, 70 ℃ of top temperature, infinite reflux, then get 70 ~ 71 ℃ of cuts, reflux ratio 1.3, reclaim acetonitrile; Reclaim completely, cooling, be saline solution at the bottom of still,, by distillation again, steams absolutely large most of water, and reclaim salt.The methanol purity 98.5% that wherein reclaims, the rate of recovery reaches 98%; Acetonitrile purity 98%, the rate of recovery 95%; The carrene rate of recovery 98%; The rate of recovery 99.5% of agent NaCl.
Adopt above-mentioned separator, 20kg waste liquid, 6.5kg carrene are added the rectifying tower reactor, close simultaneously the first control valve, the second control valve and stop the liquid valve, open and stir, and slowly heat up; Come to life to 50 ℃, infinite reflux 0.5 hour, 38 ℃ of top temperature, start discharging, and after the condensing tower condensation,, at the condensing tower bottom slice, open the first control valve and the second control valve and reclaim methyl alcohol, and the backflow carrene, control reflux ratio 1.2; After the discharging of methyl alcohol phase is complete, close the first control valve and the second control valve, again be warming up to 70 ℃, get 50 ~ 51 ℃ of cuts, open only liquid valve and reclaim additive, reclaim after complete and be down to room temperature, close apolipsis liquid valve, add NaCl0.1kg in the still tower, be warming up to 90 ℃, 70 ℃ of top temperature, infinite reflux, then get 70 ~ 71 ℃ of cuts, reflux ratio 1.3, reclaim acetonitrile; Reclaim completely, cooling, be saline solution at the bottom of still,, by distillation again, steams absolutely large most of water, and reclaim salt.The methanol purity 96.4% that wherein reclaims, the rate of recovery reaches 98.2%; Acetonitrile purity 98.6%, the rate of recovery 95%; The carrene rate of recovery 97%; The rate of recovery 99% of agent NaCl.
Adopt above-mentioned separator, 20kg waste liquid, 4kg carrene are added the rectifying tower reactor, close simultaneously the first control valve, the second control valve and stop the liquid valve, open and stir, and slowly heat up; Come to life to 50 ℃, infinite reflux 0.5 hour, 38 ℃ of top temperature, start discharging, and after the condensing tower condensation,, at the condensing tower bottom slice, open the first control valve and the second control valve and reclaim methyl alcohol, and the backflow carrene, control reflux ratio 1.2; After the discharging of methyl alcohol phase is complete, close the first control valve and the second control valve, again be warming up to 70 ℃, get 50 ~ 51 ℃ of cuts, open only liquid valve and reclaim additive, reclaim after complete and be down to room temperature, close apolipsis liquid valve, add NaCl0.1kg in the still tower, be warming up to 90 ℃, 70 ℃ of top temperature, infinite reflux, then get 70 ~ 71 ℃ of cuts, reflux ratio 1.3, reclaim acetonitrile; Reclaim completely, cooling, be saline solution at the bottom of still,, by distillation again, steams absolutely large most of water, and reclaim salt.The methanol purity 97% that wherein reclaims, the rate of recovery reaches 97.3%; Acetonitrile purity 98.1%, the rate of recovery 94%; The carrene rate of recovery 96.5%; The rate of recovery 98% of agent NaCl.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of those skilled in the art does on basis of the present invention any unsubstantiality and replacement all belong to the present invention's scope required for protection.
Claims (5)
1. the separator of an acetonitrile-water-carbinol mixture, comprise heater, thermometric galvanic couple, rectifying column and product-collecting filling, described rectifying column comprises tower reactor, rectifying section, condensing tower, described rectifying column is arranged in heater, the thermometric galvanic couple is arranged in tower reactor, rectifying section is connected on tower reactor, and condensing tower is positioned at the top of rectifying section; It is characterized in that: it also comprises that one turns the liquid pipe, turns the liquid pipe and comprises vertical arm and horizontal arm, and described condensing tower bottom is provided with a high-position discharge mouth and low level discharging opening; Described low level discharging opening connects an end of vertical arm, the other end of vertical arm is equipped with only liquid valve, described rectifying section is provided with charging aperture, horizontal arm one end is connected on vertical arm, the other end connects the charging aperture of rectifying section, be provided with the first control valve on described horizontal arm, product-collecting is filled with by a drain pipe and is connected the high-position discharge mouth, is provided with the second control valve on drain pipe; Described rectifying section top is provided with temperature measuring equipment.
2. the separator of acetonitrile-water-carbinol mixture according to claim 1, it is characterized in that: described theoretical number of plates of rectifying tower is 50.
3. the separator of acetonitrile-water-carbinol mixture according to claim 1 is characterized in that: described heater comprises electric heating cover and insulation cotton-padded covering, and tower reactor is arranged in electric heating cover, and the insulation cotton-padded covering wraps rectifying section.
4. the separation method of an acetonitrile-water-carbinol mixture is characterized in that: the separator that the method adopts acetonitrile-water-carbinol mixture claimed in claim 1, carry out according to following steps:
1) acetonitrile-water-methyl alcohol mixed waste liquor is packed in tower reactor, add carrene, close simultaneously the first control valve, the second control valve and liquid valve only, stir and heat up, it is the cut of 36-40 ℃ that infinite reflux 0.4-0.8 hour, collection rectifying section push up temperature; Wherein the addition of carrene and acetonitrile-water-methyl alcohol mixed waste liquor is 1:(3-5 according to mass ratio) ratio mix;
2) above-mentioned cut cooling layering at the bottom of condensing tower, open the first control valve and the second control valve, to be methyl alcohol be recovered to during collection of products fills with by high-position discharge mouth on separator the upper strata cut, and lower floor's carrene enters and turns the liquid pipe and be back in tower reactor through the low level discharging opening;
3) after methyl alcohol phase fluid is completed, close the first control valve, the second control valve, continue to heat up, reflux, collecting rectifying section top temperature is 49 ~ 53 ℃ of cuts;
4) cut in step 3), cooling at the bottom of condensing tower, open only liquid valve, reclaim carrene;
5) step 4) reclaim complete after, near room temperature, add NaCl toward tower reactor in, be warming up to rectifying section top temperature and reach 70 ℃, infinite reflux, get the cut of 70 ~ 71 ℃, reflux ratio 1.3, recovery acetonitrile;
6) acetonitrile reclaim complete after, be saline solution at the bottom of cooling, tower reactor, distillation again, wholely go out most of water, reclaims salt.
5. the separation method of acetonitrile-water-carbinol mixture according to claim 4, it is characterized in that: the addition of step 5) sodium chloride accounts for the 1-5% of acetonitrile-water-methyl alcohol mixed waste liquor gross weight.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
| CN106316883A (en) * | 2016-07-26 | 2017-01-11 | 安徽天地高纯溶剂有限公司 | Acetonitrile waste liquid recycling device capable of automatically adjusting heating effect |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
| CN110903167A (en) * | 2019-10-28 | 2020-03-24 | 重庆大学 | Method for separating acetonitrile-methanol-water mixture by heat-integrated three-tower vacuum extraction rectification |
| CN112194596A (en) * | 2020-11-06 | 2021-01-08 | 山东汇海医药化工有限公司 | Method for recovering acetonitrile in synthetic acetonitrile ammonia water |
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| CN102068831A (en) * | 2010-12-15 | 2011-05-25 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
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| JP2000344756A (en) * | 1999-05-31 | 2000-12-12 | Asahi Chem Ind Co Ltd | Purification of oxazole |
| CN101134736A (en) * | 2007-09-28 | 2008-03-05 | 天津大学 | Method for separating carbinol acetonitrile azeotrope |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
| CN106316883A (en) * | 2016-07-26 | 2017-01-11 | 安徽天地高纯溶剂有限公司 | Acetonitrile waste liquid recycling device capable of automatically adjusting heating effect |
| CN109231635A (en) * | 2018-11-20 | 2019-01-18 | 江苏九天高科技股份有限公司 | A kind of dichloroethanes/ethane nitrile wastewater New Process for Treatment |
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| CN110903167A (en) * | 2019-10-28 | 2020-03-24 | 重庆大学 | Method for separating acetonitrile-methanol-water mixture by heat-integrated three-tower vacuum extraction rectification |
| CN112194596A (en) * | 2020-11-06 | 2021-01-08 | 山东汇海医药化工有限公司 | Method for recovering acetonitrile in synthetic acetonitrile ammonia water |
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