CN212610367U - Hydroxyacetonitrile separation and purification device - Google Patents
Hydroxyacetonitrile separation and purification device Download PDFInfo
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- CN212610367U CN212610367U CN202021288145.3U CN202021288145U CN212610367U CN 212610367 U CN212610367 U CN 212610367U CN 202021288145 U CN202021288145 U CN 202021288145U CN 212610367 U CN212610367 U CN 212610367U
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- hydroxyacetonitrile
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Abstract
The utility model discloses a hydroxyl acetonitrile separation and purification device, including extraction tower, conveying pump, vacuum evaporator and cold-trap, the filler has been preset in the middle part of extraction tower, is equipped with heavy liquid entry and light liquid entry on the lateral wall of extraction tower respectively, and the top of extraction tower is equipped with the export of light liquid, the bottom of extraction tower is equipped with heavy liquid export, and heavy liquid export is connected with the conveying pump through first pipeline, and vacuum evaporator's bottom is equipped with the bin outlet that is used for discharging hydroxyl acetonitrile product, is equipped with the steam outlet who is used for discharging separation vapor on vacuum evaporator's the lateral wall, and steam outlet is connected with the cold-trap through first pipeline. The utility model discloses, utilize petroleum ether extraction industry hydroxyacetonitrile solution in order to detach harmful substance, through vacuum evaporation concentration hydroxyacetonitrile solution in order to obtain high yield, high-purity hydroxyacetonitrile.
Description
Technical Field
The utility model relates to a separation and purification field of hydroxyacetonitrile, concretely relates to hydroxyacetonitrile separation and purification device.
Background
The related terms in the technical field are explained as follows:
1) hydroxy acetonitrile: also known as Glycolonitrile, the English name Glycononitrile, chemical formula HOCH2CN, molecular weight 57.05, boiling point 183 deg.C, freezing point-72 deg.C, specific gravity 1.104, generally colorless oily liquid, hydrocyanic acid derivative, and simplest cyanohydrin.
2) Petroleum ether: also called as Petroleum English, the name of Petroleum Ether, pentane and hexane mixture, boiling point of 30-80 deg.c, freezing point lower than-73 deg.c, water insoluble, colorless and transparent liquid, and is one common weak limit organic solvent.
The hydroxyl acetonitrile is an important cyanohydrin organic intermediate and is widely applied to the fields of chemical industry, medicines, pesticides, dyes, electroplating, flotation and the like. As the industrial formaldehyde solution which is the main raw material for synthesizing the hydroxyl acetonitrile usually contains a large amount of water, the concentration of the industrial hydroxyl acetonitrile product is low, the content of the hydroxyl acetonitrile is only 45-50%, and the industrial formaldehyde solution contains a small amount of harmful impurities. In the organic synthesis process of chemical industry, medicine industry and pesticide industry, harmful impurities in industrial hydroxyacetonitrile solution can influence the yield of synthesized products, especially influence under the alkaline reaction condition, and a large amount of water in the hydroxyacetonitrile can increase the difficulty and cost of product post-treatment; in the flotation and electroplating industries, the purity of the hydroxy acetonitrile can directly influence the mineral flotation and metal electroplating effects. The hydroxyacetonitrile belongs to a highly toxic chemical, is easy to polymerize and poor in thermal stability, and is easily decomposed by heating to generate a highly toxic hydrocyanic acid gas, so that the conventional distillation method for concentrating the hydroxyacetonitrile has the advantages of low yield and great potential safety hazard.
The existing purification means at present mainly comprise the following two types:
1. extracting the hydroxyacetonitrile in the hydroxyacetonitrile solution by using ether, then drying and removing water, distilling and removing the ether at normal pressure, then distilling under reduced pressure, and collecting fractions at about 100 ℃ (1.33kPa) to obtain the high-purity hydroxyacetonitrile product. The device mainly comprises extraction equipment and reduced pressure distillation equipment. The drawbacks of this approach are: chemical reagents such as ether, drying agent and the like are consumed, the hydroxy acetonitrile is partially decomposed due to high distillation temperature (more than 100 ℃), the potential safety hazard of leakage of highly toxic gas exists, and the experimental operation and the device design are complex.
2. The Chinese patent CN 201611170164.4 mentions a 'separation and purification method of hydroxyacetonitrile': extracting nonpolar organic impurities in the hydroxyacetonitrile solution by using a first extracting agent n-hexane, then extracting the hydroxyacetonitrile in the rest hydroxyacetonitrile solution by using a second extracting agent diethyl ether, then drying and removing water, distilling under reduced pressure to remove the diethyl ether, then performing nitrogen protection and reduced pressure distillation on the hydroxyacetonitrile in a Schlenk line system, and collecting 50-60 ℃ (0.20kPa) fractions to obtain a high-concentration hydroxyacetonitrile product. The drawbacks of this approach are: chemical reagents such as normal hexane, ether, drying agent and the like are consumed, the distillation temperature is higher (more than 60 ℃) to cause the partial decomposition of the hydroxy acetonitrile, a small amount of extremely toxic gas leakage potential safety hazards exist, and the experimental operation and the device design are complex.
In summary, there is a need for a device for separating and purifying hydroxyacetonitrile, which has simple structure, low cost, safety and reliability.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that simple structure, safe efficient hydroxyacetonitrile separation and purification equipment lacks at present.
In order to solve the technical problems, the technical proposal adopted by the utility model is to provide a separation and purification device of hydroxyl acetonitrile, which comprises an extraction tower, a material delivery pump, a vacuum evaporator and a cold trap which are connected in sequence by a first pipeline, the middle part of the extraction tower is pre-filled with filler, the side wall of the extraction tower is respectively provided with a heavy liquid inlet for injecting hydroxyl acetonitrile aqueous solution and a light liquid inlet for injecting petroleum ether, the top of the extraction tower is provided with a light liquid outlet for discharging petroleum ether, the bottom of the extraction tower is provided with a heavy liquid outlet for discharging the aqueous solution of hydroxyacetonitrile, the heavy liquid outlet is connected with the material conveying pump through the first pipeline, the bottom of the vacuum evaporator is provided with a discharge port for discharging the hydroxyl acetonitrile product, and a steam outlet for discharging and separating water vapor is arranged on the side wall of the vacuum evaporator, and the steam outlet is connected with the cold trap through the first pipeline.
In the above scheme, the side wall of the cold trap is connected with a vacuum pump for discharging non-condensable gas through the first pipeline, and the vacuum pump is provided with an exhaust port.
In the scheme, the vacuum evaporator is connected with a constant-temperature water bath circulating pump in parallel through a second pipeline.
In the scheme, the vacuum evaporator is a jacket pressure vessel with constant-temperature circulating water communicated in a jacket, and an electric magnetic stirrer is rotationally arranged in the vacuum evaporator.
In the scheme, the cold trap external jacket is connected with a freezing brine unit in parallel through a third pipeline.
In the scheme, the cold trap is a detachable stainless steel or pressure-resistant glass cold trap.
In the above scheme, the packing is random packing or regular packing, and the material of the packing is ceramic packing or metal packing
The utility model discloses the hydroxyacetonitrile separation and purification device that adopts possesses following advantage:
1) only low-cost extractant petroleum ether is used, so that the consumption cost of chemical reagents is greatly reduced;
2) the whole concentration process is operated at room temperature, so that the glycolonitrile is prevented from being decomposed by heating, and the experimental energy consumption is reduced;
3) experiment operation and device design are simple, have simplified the operating procedure, have reduced the device input cost.
Drawings
Fig. 1 is a schematic view of the connection structure of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The utility model discloses a hydroxyl acetonitrile separation and purification device, the technical personnel in the field can reference this text content, suitably improve technological parameter and realize. It is expressly noted that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be included in the invention and it is apparent to those skilled in the art that the inventive technique can be practiced and applied by modifying or appropriately combining the teachings herein without departing from the spirit and scope of the invention.
In the present application, unless otherwise specified, scientific and technical terms used herein have the meanings as commonly understood by one of ordinary skill in the art.
As shown in figure 1, the utility model provides a pair of hydroxy acetonitrile separation and purification device, include by the extraction tower 1, feeding pump 2, vacuum evaporator 3 and the cold trap 5 that first pipeline connects in order, preset in the middle part of extraction tower 1 and pack 14, pack 14 can be random packing and one of regular packing, consider that the cost is preferred random packing, and the packing material can be one of plastics, pottery, metal, considers cost and surface wettability, preferred ceramic packing.
The side wall of the extraction tower 1 is respectively provided with a heavy liquid inlet 11 for injecting a hydroxy acetonitrile aqueous solution and a light liquid inlet 12 for injecting petroleum ether, the top of the extraction tower 1 is provided with a light liquid outlet 13 for discharging the petroleum ether, the bottom of the extraction tower 1 is provided with a heavy liquid outlet 15 for discharging the hydroxy acetonitrile aqueous solution, and the heavy liquid outlet 15 is connected with the delivery pump 2 through a first pipeline.
The bottom of vacuum evaporator 3 is equipped with the bin outlet 31 that is used for discharging the hydroxyl acetonitrile product, is equipped with the steam outlet 33 that is used for discharging separation vapor on the 3 lateral walls of vacuum evaporator, and steam outlet 33 is connected with cold trap 5 through first pipeline, and it has constant temperature water bath circulating pump 4 still to have parallelly connected through the second pipeline on the vacuum evaporator 3 in addition. The vacuum evaporator 3 is a jacket pressure vessel, constant temperature circulating water is introduced into the jacket, and an electric magnetic stirrer 32 is arranged in the vacuum evaporator 3.
The side wall of the cold trap 5 is connected with a vacuum pump 7 for discharging non-condensable gas through a first pipeline, and the vacuum pump 7 is provided with an exhaust port 71. The cold trap 5 is a detachable stainless steel (or pressure-resistant glass) cold trap. The external jacket of the cold trap 5 is connected in parallel with a freezing brine unit 6 through a third pipeline.
The utility model provides a hydroxyacetonitrile separation and purification device utilizes petroleum ether extraction industry hydroxyacetonitrile solution in order to detach harmful impurity, through vacuum evaporation concentration hydroxyacetonitrile solution in order to obtain high yield, high-purity hydroxyacetonitrile, compares in traditional evaporative concentration, more is applicable to the high temperature easily decomposed heat sensitive solution.
The utility model discloses a concrete process flow: the commercial aqueous solution of the hydroxyacetonitrile (with the content of 45% -50%) enters an extraction tower 1 from a heavy liquid inlet 11, petroleum ether enters the extraction tower 1 from a light liquid inlet 12, light and heavy two-phase liquids are fully mixed in the filler extraction tower 1, the non-polar organic impurities (harmful impurities) in the aqueous solution of the hydroxyacetonitrile are extracted and separated by the petroleum ether, the petroleum ether is discharged from a light liquid outlet 13, then the petroleum ether is distilled and separated and recycled, and the aqueous solution of the hydroxyacetonitrile enters the next working procedure unit through a heavy liquid outlet 15 at the bottom of the tower. The water solution of the hydroxyacetonitrile after the impurity removal enters a vacuum evaporator 3 through a delivery pump 2, the water solution is evaporated in vacuum at room temperature (20-25 ℃) and under the pressure of 0.2kPa until the quality of the hydroxyacetonitrile solution is not reduced any more, then the hydroxyacetonitrile product is discharged from a discharge hole 31, the separated water vapor is fully condensed and collected by a cold trap 5 and a matched frozen brine unit 6, and the non-condensable gas is discharged from an exhaust hole 71 of a vacuum pump 7. The purity of the hydroxy acetonitrile product is detected to be 93 percent, no harmful impurities exist, and the calculated yield is 95 percent.
Compared with the conventional method and the patent method, the freeze concentration method of the utility model has the following advantages:
1) the whole process is operated at room temperature, so that the heat-sensitive component of the hydroxyacetonitrile is prevented from being decomposed by heating, and the recovery rate of the hydroxyacetonitrile is improved;
2) the production of hydrocyanic acid is avoided, and the potential safety hazard of highly toxic gas leakage is eliminated;
3) only low-cost extractant petroleum ether is used, so that the raw material cost is saved;
4) the experimental operation is simple, and the production efficiency and the operation safety are improved;
5) the experimental device is simple, and the equipment investment is reduced;
6) less three wastes (only a small amount of waste liquid and harmless tail gas are generated, no waste slag is generated), low energy consumption, environmental protection and energy saving.
The utility model discloses, utilize petroleum ether extraction industry hydroxyacetonitrile solution in order to detach harmful substance, through vacuum evaporation concentration hydroxyacetonitrile solution in order to obtain high yield, high-purity hydroxyacetonitrile.
The present invention is not limited to the above best mode, and any person should learn the structural changes made under the teaching of the present invention, all with the present invention has the same or similar technical solution, all fall into the protection scope of the present invention.
Claims (7)
1. A separation and purification device of hydroxyacetonitrile is characterized by comprising an extraction tower, a material delivery pump, a vacuum evaporator and a cold trap which are sequentially connected by a first pipeline, the middle part of the extraction tower is pre-filled with filler, the side wall of the extraction tower is respectively provided with a heavy liquid inlet for injecting hydroxyl acetonitrile aqueous solution and a light liquid inlet for injecting petroleum ether, the top of the extraction tower is provided with a light liquid outlet for discharging petroleum ether, the bottom of the extraction tower is provided with a heavy liquid outlet for discharging the aqueous solution of hydroxyacetonitrile, the heavy liquid outlet is connected with the material conveying pump through the first pipeline, the bottom of the vacuum evaporator is provided with a discharge port for discharging the hydroxyl acetonitrile product, and a steam outlet for discharging and separating water vapor is arranged on the side wall of the vacuum evaporator, and the steam outlet is connected with the cold trap through the first pipeline.
2. The apparatus for separating and purifying hydroxyacetonitrile according to claim 1, wherein a vacuum pump for discharging non-condensable gas is connected to the side wall of the cold trap through the first pipeline, and an exhaust port is provided on the vacuum pump.
3. The apparatus for separating and purifying hydroxyacetonitrile according to claim 1, wherein a constant temperature water bath circulating pump is connected in parallel to the vacuum evaporator through a second pipeline.
4. The apparatus for separating and purifying hydroxyacetonitrile according to claim 1, wherein the vacuum evaporator is a jacket pressure vessel having a jacket filled with circulating water at a constant temperature, and an electric magnetic stirrer is rotatably disposed in the vacuum evaporator.
5. The apparatus for separating and purifying hydroxyacetonitrile according to claim 4, wherein the external jacket of the cold trap is connected in parallel with the frozen brine unit through a third pipe.
6. The apparatus for separating and purifying hydroxyacetonitrile according to claim 1, wherein the cold trap is a detachable stainless steel or pressure-resistant glass cold trap.
7. The apparatus for separating and purifying hydroxyacetonitrile according to claim 1, wherein the packing is random packing or structured packing, and the material of the packing is ceramic packing or metal packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021288145.3U CN212610367U (en) | 2020-07-02 | 2020-07-02 | Hydroxyacetonitrile separation and purification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021288145.3U CN212610367U (en) | 2020-07-02 | 2020-07-02 | Hydroxyacetonitrile separation and purification device |
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| CN212610367U true CN212610367U (en) | 2021-02-26 |
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| CN202021288145.3U Active CN212610367U (en) | 2020-07-02 | 2020-07-02 | Hydroxyacetonitrile separation and purification device |
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