CN214436588U - Rectification device for preparing high-purity low-boiling-point organic solvent in laboratory - Google Patents

Abstract

The utility model relates to the technical field of rectification and purification devices, in particular to a rectification device for preparing high-purity low-boiling-point organic solvent in a laboratory, which mainly comprises an intelligent heating electric furnace, a three-neck flask, a rectification column and a condenser, a three-neck flask is placed on the intelligent heating electric furnace, a side-opening bottle at one end of the three-neck flask is connected with a feeding device, a thermometer is inserted into a side mouth bottle at the other end of the three-neck flask, a rectification column is inserted into a middle mouth bottle of the three-neck flask, the gas outlet of the rectifying column is connected with the gas inlet of a condenser, the liquid outlet of the condenser is connected with a liquid collecting bottle, the condenser is connected with a circulating water pump below the circulating water tank through a water inlet silicon rubber pipe at the lower end of the condenser, the condenser passes through the return water silicone rubber pipe of condenser upper end and is connected with the gondola water faucet shower nozzle of circulation tank top, cooling blower is installed to the lateral wall department of circulation tank upper end. The utility model provides high low boiling organic solvent's purity has practiced thrift the rectification time, has improved rectification efficiency.

Description

Rectification device for preparing high-purity low-boiling-point organic solvent in laboratory

Technical Field

The utility model relates to a rectification purification technical field specifically is a laboratory preparation high purity low boiling organic solvent's rectification device.

Background

The rectification is a separation process for separating each component by utilizing different volatility of each component in the mixture, the evaporation rectification device is a sample separation and purification instrument widely applied in laboratories, and the separation and purification of products are realized through the processes of solvent evaporation, trace component concentration and the like. High-purity low-boiling organic solvents, such as methanol, ethanol, methyl formate, acetone, butanone, chloroform, benzene and the like, are common solvents in chemical laboratories and are synthesis raw materials of various chemicals. Depending on the production method and the source of raw materials, the organic solvents contain a small amount or trace amount of impurities, such as methanol often contains formaldehyde and formic acid; ethyl acetate often contains a trace amount of acetic acid, ethanol, etc. The acetone can be produced by an isopropanol method, an cumene method, a fermentation method, an acetylene hydration method, a propylene direct oxidation method and the like, a part of the commercially available acetone is from recovered acetone waste liquid, common acetone usually contains impurities such as isopropyl benzene, propanol, phenol, diethyl ether, ethanol, diisopropyl ether, propionaldehyde and the like, the content of the impurities is from 1% to 10%, and even the acetone of a chromatographic grade can always find trace impurities. In some instrumental analysis and preparation of high-purity substances, the low-boiling-point organic substances are often used as solvents or cleaning agents, impurities, particularly aromatic hydrocarbon impurities and alcohol impurities, are often deposited or adsorbed on the surface of the substances and are difficult to remove by cleaning, evaporation and the like, element blanks such as C, H are high when element analysis is carried out, the purity and the physical properties are influenced when the high-purity substances are prepared, and particularly when scientific research is carried out in a laboratory, the obtained results are used for production guidance, and serious deviation results can be generated.

Most of the existing low-boiling-point organic solvent purification devices are industrial devices, small devices used in laboratories are few, the rectification process is not emphasized, the column efficiency is low, the required purity can be reached by repeated distillation for many times, and the purification device takes time and has long time and low yield. Therefore, a rectification apparatus for efficiently producing a high-purity organic solvent is required.

SUMMERY OF THE UTILITY MODEL

For solving prior art's shortcoming and not enough, the utility model provides a laboratory preparation high purity low boiling organic solvent's rectifier unit, it has improved low boiling organic solvent's purity, has practiced thrift the rectification time, has improved rectification efficiency.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

a rectification device for preparing high-purity low-boiling-point organic solvent in a laboratory mainly comprises an intelligent heating electric furnace, a three-neck flask, a rectification column and a condenser, a three-neck flask is placed on the intelligent heating electric furnace, a side-opening bottle at one end of the three-neck flask is connected with a feeding device, a thermometer is inserted into a side mouth bottle at the other end of the three-neck flask, a rectification column is inserted into a middle mouth bottle of the three-neck flask, the gas outlet of the rectifying column is connected with the gas inlet of a condenser, the liquid outlet of the condenser is connected with a liquid collecting bottle, the condenser is connected with a circulating water pump below the circulating water tank through a water inlet silicon rubber pipe at the lower end of the condenser, the condenser is connected with a shower nozzle above the circulating water tank through a water return silicone rubber pipe at the upper end of the condenser, and a cooling fan is further installed on the outer side wall of the upper end of the circulating water tank and has the cooling effect on the circulating water tank.

Furthermore, the volume of the three-neck flask is 1000mL, a small amount of ceramic chips are placed in the three-neck flask to prevent the violent boiling of liquid to cause the explosive boiling of the flask, and the ceramic chips are more than or equal to 3g and less than or equal to 5 g.

Further, the inner diameter of the rectification column is 25mm, and the length of the rectification column is 800 mm; baffle plates are arranged on the inner wall of the rectification column in a staggered manner; the angle between the rectification column and the horizontal plane is 90 degrees. The rectification column is lengthened and the baffle plate is arranged, so that organic impurities with high boiling points can be effectively prevented from being carried in the organic solvent during rapid evaporation, the efficiency of separating the organic impurities with the boiling points close to that of the organic solvent is improved, and the purity of the distilled organic solvent is also improved.

Further, the condenser is snakelike spiral tube condenser pipe, and length is 600mm, the condenser adopts deionized water circulative cooling, can reduce the use of cooling water, reduces the water consumption, and does not have the scale deposit in the condenser, the contained angle of condenser and rectifying column is 45.

Furthermore, the liquid collecting bottle is a flat-bottomed glass bottle with a sealed opening, and the liquid collecting bottle is provided with a rubber sealing bottle plug, so that the steam leakage of the organic solvent can be prevented.

Furthermore, the rectification device of the utility model can purify the low boiling point organic solvent (purity is more than 90%) sold in the market to more than 99.5% by secondary rectification; or the low boiling point organic solvent waste liquid (the purity is more than 50%) is rectified for three times and purified to more than 99.5%; the low boiling point organic solvent with the purity of 99.5 percent can be purified to more than 99.8 percent by one-time rectification. In addition, the treatment capacity of purifying the low-boiling organic solvent can reach 300mL per hour, and the method is suitable for laboratory instrument analysis, high-purity sample preparation and the like.

Compared with the prior art, the utility model discloses following beneficial effect has:

1. the utility model effectively prevents organic impurities with high boiling point from being carried in the organic solvent during the rapid evaporation by lengthening the rectification column and installing the baffle plates in the rectification column in a staggered way, and improves the efficiency of separating the organic impurities with the boiling point close to that of the organic solvent, thereby improving the purity of the distilled organic solvent;

2. the utility model has strong sealing performance at each contact part, can effectively prevent the organic solvent steam from leaking, and improves the rectification yield and the safety of the rectification process;

3. the utility model adopts the intelligent electric heating furnace to adjust the temperature, can effectively control the distillation speed and is convenient to operate;

4. the utility model discloses a deionized water circulative cooling utilizes cooling blower simultaneously, and good control the temperature of deionized water, reduced the water consumption, and no scale deposit in the condenser.

Drawings

Fig. 1 is a schematic view of the device of the present invention.

In the figure: 1-intelligent heating electric furnace; 2-three-neck flask; 3-a feeding device; 4-a thermometer; 5-a rectification column; 6-a condenser; 7-liquid collecting bottle; 8-a circulating water tank; 9-a circulating water pump; 10-a water inlet silicone rubber pipe; 11-backwater silicone rubber pipe; 12-a shower head; 13-Cooling Fan.

Detailed Description

The following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings:

as shown in fig. 1, a rectification apparatus for preparing high-purity low-boiling organic solvent in laboratory mainly comprises: the device comprises an intelligent heating electric furnace 1, a three-neck flask 2, a rectifying column 5 and a condenser 6, wherein the three-neck flask 2 is placed on the intelligent heating electric furnace 1, the volume of the three-neck flask 2 is 1000mL, a small amount of ceramic chips are placed in the three-neck flask 2, and the ceramic chips are more than or equal to 3g and less than or equal to 5 g; a side-mouth bottle at one end of the three-neck flask 2 is connected with the feeding device 3, a thermometer 4 is inserted into a side-mouth bottle at the other end of the three-neck flask 2, a rectification column 5 is inserted into a middle-mouth bottle of the three-neck flask 2, the inner diameter of the rectification column 5 is 25mm, the length of the rectification column 5 is 800mm, baffle plates are installed on the inner wall of the rectification column 5 in a staggered mode, and the included angle between the rectification column 5 and the horizontal plane is 90 degrees; the gas outlet of the rectifying column 5 is connected with the gas inlet of a condenser 6, the condenser 6 is a coiled spiral pipe type condensing pipe, the length of the condensing pipe is 600mm, the condenser 6 is circularly cooled by deionized water, and the included angle between the condenser 6 and the rectifying column 5 is 45 degrees; the liquid outlet of the condenser 6 is connected with a liquid collecting bottle 7, and the liquid collecting bottle 7 is a flat-bottom glass bottle with a sealed opening. Condenser 6 is connected with circulating water pump 9 of 8 below in the circulating water tank through the silicon rubber pipe 10 of intaking of 6 lower extremes of condenser, condenser 6 is connected with the gondola water faucet shower nozzle 12 of 8 tops in the circulating water tank through return water silicon rubber pipe 11 of 6 upper ends in the condenser, cooling blower 13 is still installed to the lateral wall department of 8 upper ends in the circulating water tank, cooling blower 13 has cooling's effect to circulating water tank 8.

In order to make the device stability better, support and fix rectifying column 5 and condenser 6 through iron stand platform and iron clamp, fix three-neck flask 2 through the iron clamp, have the cushion on the iron clamp, have the effect of buffering stress.

In the rectification operation process, the connection of the determining device is correct and the sealing is good, organic solvent is added to two thirds of the volume of the three-neck flask 2 through a separating funnel on the feeding device 3, the intelligent electric heating furnace 1 is started to heat, meanwhile, cooling circulating water is started, the rectification operation is started, when rectification is carried out until a small amount of liquid is left at the bottom of the three-neck flask 2, the heating is stopped, and the rectification process is terminated. If continuous feeding and rectification are carried out, the organic solvent to be purified is added through a separating funnel of the feeding device 3, the volume of the organic solvent accounts for two thirds of that of the three-necked flask 2, the rectification operation is continuously carried out, and the treatment capacity of the purified organic solvent can reach 300mL per hour in the continuous rectification process; by adjusting the temperature of the intelligent heating electric furnace 1, the treatment capacity of the organic solvent can be adjusted between 100 mL/h and 300 mL/h.

The organic solvent obtained by rectification can be analyzed for purity by adopting a gas chromatography, and the organic solvent can be purified to 99.5% by once rectification through commercially available methanol, methyl formate, acetone and the like (the purity is more than 95%); and rectifying again to purify to 99.8%. Methyl formate and acetone waste liquid (purity is more than 50%) can be purified to 90.5% by primary rectification, and can be purified to 95.6% by secondary rectification; and (4) rectifying for three times, and purifying to 99.5%.

In conclusion, the rectification device for preparing the high-purity low-boiling-point organic solvent in the laboratory achieves the purpose of preparing the high-purity organic solvent in small batches in the laboratory by improving the separation efficiency of the rectification column, enhancing the sealing of the joint and using deionized water for circulating cooling, so that the rectification device can be used in the fields of instrument analysis, high-purity substance preparation and the like with high purity requirements.

The above embodiments and the description only illustrate the principles of the present invention and the more specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is familiar with the technical scope of the present invention.

Claims (5)

1. A rectification device for preparing high-purity low-boiling-point organic solvent in a laboratory is characterized in that: mainly comprises an intelligent heating electric furnace (1), a three-neck flask (2), a rectifying column (5) and a condenser (6), wherein the three-neck flask (2) is placed on the intelligent heating electric furnace (1), a feeding device (3) is connected with one end side mouth bottle of the three-neck flask (2), a thermometer (4) is inserted into the other end side mouth bottle of the three-neck flask (2), a rectifying column (5) is inserted into a middle mouth bottle of the three-neck flask (2), an air inlet of the condenser (6) is connected with an air outlet of the rectifying column (5), a liquid outlet of the condenser (6) is connected with a liquid collecting bottle (7), the condenser (6) is connected with a circulating water pump (9) below the circulating water tank (8) through a water inlet silicon rubber tube (10) at the lower end of the condenser (6), and a shower nozzle (12) above the circulating water tank (8) are connected with the condenser (6) through a water return silicon rubber tube (11) at the upper end of the condenser (6), and a cooling fan (13) is further installed on the outer side wall of the upper end of the circulating water tank (8).

2. The rectification apparatus for laboratory preparation of high-purity low-boiling organic solvent according to claim 1, characterized in that: the volume of the three-neck flask (2) is 1000mL, a small number of ceramic tiles are placed in the three-neck flask (2), and the ceramic tiles are larger than or equal to 3g and smaller than or equal to 5 g.

3. The rectification apparatus for laboratory preparation of high-purity low-boiling organic solvent according to claim 1, characterized in that: the inner diameter of the rectifying column (5) is 25mm, and the length is 800 mm; baffle plates are arranged on the inner wall of the rectification column (5) in a staggered manner; the angle between the rectification column (5) and the horizontal plane is 90 degrees.

4. The rectification apparatus for laboratory preparation of high-purity low-boiling organic solvent according to claim 1, characterized in that: condenser (6) are snakelike spiral tube condenser pipe, and length is 600mm, the contained angle of condenser (6) and rectifying column (5) is 45.

5. The rectification apparatus for laboratory preparation of high-purity low-boiling organic solvent according to claim 1, characterized in that: the liquid collecting bottle (7) is a flat-bottom glass bottle with a sealed opening.

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