CN201197905Y

CN201197905Y - Bead tube

Info

Publication number: CN201197905Y
Application number: CNU2008201083092U
Authority: CN
Inventors: 陈左生
Original assignee: Peking University
Current assignee: Peking University
Priority date: 2008-05-29
Filing date: 2008-05-29
Publication date: 2009-02-25
Anticipated expiration: 2018-05-29

Abstract

The utility model discloses a bead tube. The bead tube comprises an outer tube 2, a middle tube 3, a center tube 4 and a solid helix tube which are embedded in sequence from outside to inside. The lower end of the middle tube 3 is provided with a bent tube 5 which is convenient for discharging liquid and preventing gas from entering and a space is remained between the middle tube 3 and the outer tube 2; a space is remained between the center tube 4 and the middle tube 3; the tube wall at the upper end of the center tube 4 is jointed with the inner wall of the outer tube 2, and a space is remained between the tube wall at the upper end of the center tube 4 and the upper end of the middle tube 3; the solid helix tube 1 is composed of a column-shaped core 8 and a snake-shaped bar 6, the inner edge of which is sealed with the outer wall of the column-shaped core 8; and the lower end of the snake-shaped bar 6 is provided with a gas hole for ensuring steam to enter, and the upper end of the snake-shaped bar 6 is provided with a gas hole for ensuring the steam to flow out. The utility model has high plate number of the unit height of the bead tube, good distillation separation effect, small volume and convenient use, and can be used for the high purification of a small quantity of organic solvent for laboratory investigation.

Description

A kind of bead tube

Technical field

The utility model relates to a kind of bead tube, particularly relates to a kind of unit height number of plates height that has, and rectifying good separating effect volume is little, bead tube easy to use.

Background technology

Some detect the analysis of dense residual material, dioxins materials need reach very high purity, could guarantee result's accuracy.Analyze neat solvent and can not reach requirement, and farming residual level solvent is with the price of bioxin level solvent is very expensive, price reaches tens times that analyze neat solvent.

At present, be specifically designed to the rectifier unit that the high-purity organic solvent is purified, because requirement to the number of plates etc., all are large distillation towers, volume is big, and it is big to take up room, the expense height, the shortcomings such as purification of inapplicable a small amount of solvent, discomfort are used as the laboratory of scientific research research and set up purification devices voluntarily, and the purification laboratory is with high-purity analysis solvent.

Use the small size distillation cascade, because its number of plates is low, need repeatedly distills and could improve purity, purity does not reach requirement, and solvent loss is big, has improved solvent cost greatly.

The utility model content

The purpose of this utility model provides a kind of unit height number of plates height that has, the rectifying good separating effect, and volume is little, bead tube easy to use.

For achieving the above object, the utility model is taked technical scheme: a kind of bead tube, and it includes nested successively from outside to inside outer tube 2, intervalve 3, central tube 4 and solid helix tube; The lower end of described intervalve 3 is provided with and makes things convenient for liquid to flow out, and prevents the bend pipe 5 that gas enters simultaneously, leaves the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of described intervalve 3 and outer tube 2; Leave the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of described central tube 4 and described intervalve 3, the upper end tube wall of described central tube 4 engages with the inwall of described outer tube 2, and leave the space with the upper end of described intervalve 3, the space between intervalve 3 and the central tube 4 is communicated with space between the outer tube 2 by intervalve 3 upper ends and intervalve 3; Described solid coiled pipe 1 is made up of the snake 6 of cylindricality core 8 and inner edge and the 8 outer wall driving fits of cylindricality core, and the lower end of described snake 6 has the pore that guarantees that steam enters, and the upper end of described snake 6 has the pore that guarantees that steam flows out.

Operation for convenience and washing, the material of described bead tube can be glass and/or quartz.

Each nested pipe is centrosymmetric in the described bead tube, the diameter of outer tube 2 is 4 times of central tube 4 diameters, the diameter of the cylindricality core 8 of solid coiled pipe 1 is 1/2 of central tube 4 diameters, and the ratio of intervalve 3 outer walls and outer tube 2 inwall spacings and intervalve 3 inwalls and central tube 4 outer wall spacings is 5/2.

In the above-mentioned bead tube, the top and bottom of described outer tube 2 are provided with the convenient frosted opening that is connected with piston or flask.

Bead tube of the present utility model is designed to 3 layers of inner sleeve, makes approach total length three times above outer tube 2 effective lengths, the number of plates height of unit height, the rectifying good separating effect, volume is little, easy to use, make things convenient for the purifying of the required high-purity organic solvent of laboratory research to make simultaneously.The quality that experiment showed, the organic solvents such as toluene that obtained by this bead tube rectifying can reach the purity that the dioxins materials analysis need reach, and promptly when being concentrated into 10,000 times, can not detect dioxin-like chemical in this distillate.

Description of drawings

Fig. 1 is a front view of the present utility model.

The specific embodiment

As shown in Figure 1, be bead tube provided by the utility model, it includes:

Nested successively from outside to inside outer tube 2, intervalve 3, central tube 4 and solid helix tube 1;

Leave the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of intervalve 3 and outer tube 2; The lower end of intervalve is provided with and makes things convenient for liquid to flow out, and prevents the bend pipe 5 that gas enters simultaneously;

Leave the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of central tube 4 and intervalve 3, the upper end tube wall of central tube 4 engages with the inwall of outer tube 2, and leave the space with the upper end of intervalve 3, space between intervalve 3 and the central tube 4 is communicated with space between the outer tube 2 by intervalve 3 upper ends and intervalve 3, and spaces and outer tube 2 do not communicate in the central tube 4 with space between the central tube 4; Can make steam travel up to central tube 4 and outer tube 2 joints like this, continue to flow downward along the space between intervalve 3 and the central tube 4 along the inwall of outer tube 2.

Solid coiled pipe 1 is made up of the snake 6 of the outer wall driving fit of cylindricality core 8 and inner edge and cylindricality core 8, the snake 6 outer rim driving fits of the solid coiled pipe 1 of the inwall of central tube 4 or leave the slit, the lower end of described snake 6 has the pore that guarantees that steam enters, and the upper end of described snake 6 has the pore that guarantees that steam flows out.

Central tube 4 lower ending openings, recessed two projections 7 that hold up described snake 6 of the inner symmetry in its lower end.

The material of above-mentioned bead tube is a glass material.

In the above-mentioned bead tube, the top and bottom of described outer tube are provided with the convenient frosted opening that is connected with piston or flask.

Each nested pipe of above-mentioned bead tube is centrosymmetric, the diameter of outer tube 2 is 4 times of central tube 4 diameters, the diameter of the cylindricality core rod 8 of solid coiled pipe 1 is 1/2 of central tube 4 diameters, the ratio of intervalve outer wall and outer tube wall spacing and intervalve inwall and central tube 4 outer wall spacings is 5/2, intervalve upper end and bottom respectively have the pore of 4 symmetries, and it is mobile to guarantee that steam is pressed certain orientation.

In the present embodiment, being specially of bead tube: 1. outer tube 2 diameters are 40mm, and central tube 4 diameters are 10mm; 2. interpolation solid glass rod 8, diameter is 5mm; 3. intervalve 3 outer walls and outer tube 2 inwall spacings are 5mm, and intervalve 3 inwalls and central tube 4 outer wall spacings are 2mm; 4. intervalve 3 upper ends and bottom respectively have the pore of 4 symmetries, and it is mobile to guarantee that steam is pressed certain orientation; The number of turn of snake 6 is 35 circles.

When the bead tube of the foregoing description uses, the frosted mouth of the lower end of the outer tube 2 of bead tube is connected with twoport flask mouth, connect three-way connector in the top, be connected with serpentine condenser by the three-way connector side, the boiling point that thermometer detects the control different solvents is inserted in the upper end, the lower end of serpentine condenser is connected with the exhaust connector, the exhaust connector is connected with separatory funnel, after can purifying by the bead tube of present embodiment simultaneously, use serpentine condenser, separatory funnel reclaims, and can purify and reclaim as toluene, n-hexane, carrene, acetone and other organic solvent.

The operation principle of the bead tube of the foregoing description: organic solvent that will be to be purified is packed in the twoport flask, through heating twoport flask, the organic vapor volatilization enters bead tube, rise along bead tube outer tube 2 inwalls, the solvent vapo(u)r that rises enters intervalve 3 fractionation through intervalve 3 upper ends of upper end, flow downward along intervalve 3 inwalls again, steam enters central tube 4 by the perforate of central tube 4 lower ends, under pressure, the solid snakelike glass bar of steam in the central tube 4 shape in the shape of a spiral rises and is distillated, until flowing out bead tube; Rectifying steam by connector, enters serpentine condenser and is condensed into liquid after flowing out; Enter separatory funnel, be received.

3 layers of inner sleeve approach total length of above-mentioned utility model surpass three times of outer tube 2 effective lengths, number of plates height, rectifying good separating effect.

When homemade analytically pure toluene (110.5 ℃), n-hexane (68.5 ℃), carrene (40.0 ℃) and acetone (56.6 ℃) directly concentrated 10000 times without purifying, finding when HRGC-HRMS tests had 4-8 chlorine De bioxin with the interference impurity of bioxin furans.Bead tube with the foregoing description connects recovery as toluene, n-hexane, carrene and acetone according to above-mentioned same method, with homemade analytically pure toluene (110.5 ℃ of boiling points), n-hexane (68.5 ℃ of boiling points), carrene (40.0 ℃ of boiling points) and acetone (56.6 ℃ of boiling points) is raw material, carries out purifying respectively.The solvent that obtains behind the purifying concentrates 10 respectively ⁴Doubly, the test of carrying out on high-resolution gaschromatographic mass spectrometry device (HRGC-HRMS) is not then found to detect the above dioxins materials of lower limit and other impurity, checks 10 of all reagent through HRGC-HRMS ⁴Times concentrate, its spectrogram baseline is steady, and noise is little, and without any the disturbance spectrum peak, the full operation blank all is lower than the detection lower limit (10 of instrument ^-15G flies gram level) requirement.Bead tube of the present utility model is described, the organic solvent after the rectification and purification can reach the requirement of bioxin level solvent.

Claims

1. bead tube, it includes nested successively from outside to inside outer tube (2), intervalve (3), central tube (4) and solid coiled pipe (1); The lower end of described intervalve (3) is provided with and makes things convenient for liquid to flow out, and prevents the bend pipe (5) that gas enters simultaneously, leaves the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of described intervalve (3) and outer tube (2); Leave the spacing that guarantees that steam flows along the body direction between the inwall of the outer wall of described central tube (4) and described intervalve (3); The upper end tube wall of described central tube (4) engages with the inwall of described outer tube (2), and leave the space with the upper end of described intervalve (3), the space between intervalve (3) and the central tube (4) is communicated with space between the outer tube (2) by intervalve (3) upper end and intervalve (3); Described solid coiled pipe (1) is made up of the snake (6) of cylindricality core (8) and inner edge and cylindricality core (8) outer wall driving fit, the lower end of described snake (6) has the pore that guarantees that steam enters, and the upper end of described snake (6) has the pore that guarantees that steam flows out.

2. bead tube according to claim 1 is characterized in that: described central tube (4) lower ending opening, recessed two projections (7) that hold up described snake (6) of the inner symmetry in its lower end.

3. bead tube according to claim 2 is characterized in that: the top and bottom of described outer tube (2) are provided with the convenient frosted opening that is connected with piston or flask.

4. bead tube according to claim 3 is characterized in that: the material of described bead tube is glass and/or quartzy material.