CN104353259B - Combined type rectifying column and application thereof - Google Patents

Combined type rectifying column and application thereof Download PDF

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CN104353259B
CN104353259B CN201410611740.9A CN201410611740A CN104353259B CN 104353259 B CN104353259 B CN 104353259B CN 201410611740 A CN201410611740 A CN 201410611740A CN 104353259 B CN104353259 B CN 104353259B
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inner sleeve
intermediate casing
combined type
cylindrical body
outer cylindrical
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CN104353259A (en
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李桂芳
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Abstract

The present invention relates to combined type rectifying column and application thereof.Specifically, the present invention relates to a kind of combined type rectifying column, it is characterized in that, it comprises: outer cylindrical body, intermediate casing and inner sleeve, and three's main part is separately the tube that concentric is arranged.The invention still further relates to a kind of rectifier unit comprising this combined type rectifying column, and use combined type rectifying column of the present invention and rectifier unit to treat the method that rectifying material carries out rectifying.Apparatus of the present invention and method have easy cleaning, multiple filler can be used and change conveniently, product purity is high, steady quality, rectifying productive rate is higher, separation costs is low, distillation process is without the feature of potential safety hazard, and can need to change filling kind and use amount according to difference, there is solvent and purify, reclaim, the multiple uses such as natural product extraction.

Description

Combined type rectifying column and application thereof
Technical field
The application relates to the compound separation purification devices in chemical field, and the parts being specifically related to rectifying and the composite and multi-purpose rectifier unit using these parts, also relate to their purposes.
Background technology
Rectifying is a kind of utilizes backflow to make liquid mixture obtain the distillating method of high purity separation, its general principle is by liquid mixture partial gasification, utilize the characteristic that wherein each component volatility (relative volatility) is different, realize the unit operations being separated object.Rectifying column is the tower vapor-liquid contacting apparatus of one carrying out rectifying, is also called destilling tower.Traditionally, industrial large-scale rectifier unit is called rectifying column, and the rectifier unit of laboratory middle and small scale is called rectifying column.Current small-scale rectifying column mostly is the design of simple single hose, usually selects applicable filler according to the size of caliber.Such rectifying column is difficult to realize small size and high tray-number simultaneously, because under the condition that treating capacity is certain, increases column length and can increase the number of plates, but also cause rectifying column volume to increase simultaneously.Realize small size by minimizing treating capacity then to deviate from mutually with the original intention improving rectification efficiency with high tray-number.
The open CN101642630A of application for a patent for invention devises a kind of rectification column for laboratory, comprises some rectifying column bodies in parallel in outer tube and outer tube.This invention, by being arranged in parallel for rectifying by some rectifying column bodies, solving the contradiction between the length, caliber etc. of single rectifying column in prior art and treating capacity, achieves high flux in distillation technology, high efficiency requirement.But this invention is some rectifying columns due to parallel connection, the purity of its rectifying product is subject to the minimum rectifying column restriction of the number of plates, and the quality of rectifying product is wayward.
Utility model patent CN201299982Y discloses a kind of series-connected multi-level rectification solvent recovery device, and this recover is in series with three groups of heaters, tower body and condensers successively.This equipment largely solves conventional solvent separation and recovery tower can only carry out optionally some solvents for the system containing multi-solvents and carry out being separated and be separated incomplete problem.There is compact conformation, the feature such as with low cost and simple to operate simultaneously.
In novel organic reagent atmospheric distillation equipment for purifying disclosed in utility model patent CN201426987Y, rectifying still is provided with heating jacket, rupture pressure disc, Pressure gauge, relief valve and electrostatic let-off gear(stand) to improve the security performance of equipment.This equipment composition is relatively numerous and diverse, is not suitable for separated from solvent and recovery on a small scale.
A kind of pressure-reduced rectification instrument with rotary evaporation for extracting Rosa Damascana from rose is related in the open CN101433773A of application for a patent for invention.Comprise rectifying instrument, condenser; Rectifying instrument comprises muff and is placed in the filling extract rectification post in muff, and muff is provided with import and the outlet of thermal liquid, and filling extract rectification post lower port is equipped with decelerator; Condenser is positioned at the top of rectifying instrument; Condenser comprises housing and is placed in the two snake condensers in housing, filling extract rectification post upper port communicates with the housing of condenser, and suction mouth is established in housing upper end, and material outlet is established in housing lower end, material outlet is equipped with vacuum cock, and lower housing portion establishes condensing water inlet and condensation-water drain.This device structure is simple, and the Rosa Damascana fragrance nature of extraction, the content of moisture and wax is extremely low.This invention also can be used for other material and extracts.
Therefore, this area still needs chemicals rectifier unit, expect that it has easy cleaning, can use multiple filler and change conveniently, product purity is high, steady quality, and rectifying productive rate is higher, separation costs is low, distillation process is without the feature of potential safety hazard, and can need to change filling kind and use amount according to difference, there is solvent and purify, reclaim, the multiple uses such as natural product extraction.In addition, still there is the method using said apparatus to carry out chemicals purifying this area.
Summary of the invention
The object of the present invention is to provide a kind of chemicals rectifier unit, expect that it has easy cleaning, multiple filler can be used and change conveniently, product purity is high, steady quality, rectifying productive rate is higher, separation costs is low, and distillation process without the feature of potential safety hazard, and can need to change filling kind and use amount according to difference, there is solvent purify, reclaim, the multiple uses such as natural product extraction.In addition, another object of the present invention is to provide a kind of method using said apparatus to carry out chemicals purifying.Expect that these devices of the present invention can use multiple filler and change conveniently, the multiple fields such as the High Purity compound preparation of small-scale, solvent recovery and natural volatile product separation can be widely used in.
For this reason, first aspect present invention provides a kind of combined type rectifying column, it is characterized in that,
It comprises: outer cylindrical body, intermediate casing and inner sleeve, and three's main part is separately the tube that concentric is arranged;
The lower ending opening of described outer cylindrical body, and this lower ending opening place be provided with for rectifier unit in device (the such as rectifying bottle etc. of rectifying steam are provided, they are the conventional components in a kind of distillation operation, treat the liquid material of rectifying for splendid attire) interface that connects; The interior edge of described outer cylindrical body upper end is used for sealing fit with described intermediate casing upper end;
The bore of the bottom of described intermediate casing reduces gradually and forms the crotch of opening upwards, thus the U-shaped tube shape that can realize fluid-tight function is formed in the bottom of intermediate casing, the side of U-shaped pipe is little opening upwards, and opposite side bore increases gradually and forms one with the main part of intermediate casing;
The bore of described intermediate casing upper end increases to form intermediate casing bulge gradually, the outer of this intermediate casing bulge and the interior of described outer cylindrical body upper end are along sealing fit, and the interior edge of this intermediate casing bulge is used for and described inner sleeve top seal fit;
The below of described intermediate casing bulge is provided with some through holes and passes through for steam;
The bore on described inner sleeve top increases to form inner sleeve bulge, and the outer of this inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit;
Described inner sleeve bottom is provided with sieve plate, this sieve plate can for steam by but can not to make in distillation operation filler pass through;
The top of described inner sleeve bulge is inner sleeve upper shed, and the caliber of this inner sleeve upper shed is less than this inner sleeve bulge, and this inner sleeve upper shed can be used for being connected with other rectifier unit parts;
Described outer cylindrical body, intermediate casing and inner sleeve three seal fit thus, form steam and enter from the lower ending opening of outer cylindrical body, leave the rectifying loop of rectifying column from the upper shed of inner sleeve.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the radius of described outer cylindrical body main part is 1: 0.4 ~ 0.9 with the ratio of the radius of intermediate casing main part.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the radius of described intermediate casing main part is 1: 0.4 ~ 0.9 with the ratio of the radius of inner sleeve main part.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the manufacture material of described outer cylindrical body, intermediate casing and inner sleeve three is selected from glass or stainless steel independently of one another.In one embodiment, the manufacture material of described outer cylindrical body, intermediate casing and inner sleeve three is glass.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the interface (like this, make the bore of the relative aperture of this interface connected rectifying bottle little) of outer grinding port structure that what described outer cylindrical body lower ending opening place was arranged for the interface be connected with rectifying bottle is.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the interior edge of described outer cylindrical body upper end is used for sealing fit with the outer of described intermediate casing bulge, and sealing fit is integrally formed structure or dismountable structure.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the interior edge of described outer cylindrical body upper end is used for sealing fit with the outer of described intermediate casing bulge, sealing fit is integrally formed structure, thus, outer cylindrical body and intermediate casing are integral types, and the two can not be disassembled.Such design benefit is significant, namely integrally formed both outer cylindrical body and intermediate casing, strengthens the two sealing in this position.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the interior edge of described outer cylindrical body upper end seals fit with the outer of described intermediate casing bulge, sealing fit is dismountable structure, thus, both outer cylindrical body and intermediate casing are separable, and the two is disassembled.Such design benefit is significant, and namely both outer cylindrical body and intermediate casing can distinguish processing, as long as the two can be made at this position seals fit; Also be convenient to internal washing; If the two one of have damage, replace one of them can with another unspoiled Component composition.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, in described outer cylindrical body upper end along and the outer of described intermediate casing bulge seal fit state under, described in the hook portion of tube shape that takes the shape of the letter U can not contact with the inwall of outer cylindrical body.In one embodiment, described intermediate casing main part overlook viewed circle, described in the take the shape of the letter U hook portion of tube shape be in this circle.This design of hook portion of tube shape of taking the shape of the letter U is favourable, such as, when both outer cylindrical body and intermediate casing are separable, disassembled designs, because of the contact internal walls of the hook portion of U-shaped tube shape and outer cylindrical body, each self-damage can not be even caused when entering intermediate casing to outer cylindrical body interpolation.In addition, take the shape of the letter U tube shape hook portion for extend rectifying time steam operating path be useful, namely in distillation process, the phegma dripped from such as inner sleeve because temperature reduces remains at this U-shaped pipe, can fluid-tight be realized when phegma is accumulated to a certain amount of and avoid steam directly to enter intermediate casing from this U-shaped pipe, can overflow from U-shaped tube opening one end when phegma continues accumulation and reenter rectifying bottle.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the edge, intermediate casing top be positioned at above intermediate casing bulge forms the edge, top that described in relative aperture, outer cylindrical body external diameter is large.The edge, top designed thus, can make both outer cylindrical body and intermediate casing when in separable, disassembled design, avoid intermediate casing can not fall into outer cylindrical body (top of intermediate casing along the upper end being just in time stuck in outer cylindrical body, and can not fall into wherein completely) completely.In addition, the edge, top designed thus, is also convenient to disassemble both outer cylindrical body and intermediate casing, and namely this edge, top of a hand-held outer cylindrical body, another hand-held intermediate casing, can easily make outer cylindrical body be separated with both intermediate casings.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the below of described intermediate casing bulge is provided with some through holes and passes through for steam, size and number design (usually determining according to the specification of combined type rectifying column) of through hole enters intermediate casing be as the criterion can guarantee to realize steam in outer cylindrical body, and/or can guarantee that intermediate casing has enough structural strengths to be as the criterion.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the outer of described inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit, and sealing fit is integrally formed structure or dismountable structure.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the outer of described inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit, sealing fit is integrally formed structure, thus, intermediate casing and inner sleeve are integral types, and the two can not be disassembled.Such design benefit is significant, namely integrally formed both intermediate casing and inner sleeve, strengthens the two sealing in this position.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the outer of described inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit, sealing fit is dismountable structure, thus, both intermediate casing and inner sleeve are separable, and the two is disassembled.Such design benefit is significant, and namely both intermediate casing and inner sleeve can distinguish processing, as long as the two can be made at this position seals fit; Also be convenient to internal washing; If the two one of have damage, replace one of them can with another unspoiled Component composition; And inner sleeve is convenient to its filling filler when disassembling, even in distillation process, replacing is filled with the inner sleeve of variety classes filler to realize more complicated distillation operation.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, along seal fit in the outer that the interior edge of described outer cylindrical body upper end is used for seal with the outer of described intermediate casing bulge fit and described inner sleeve bulge and described intermediate casing bulge, it is be integrally formed structure or be dismountable structure independently of one another that this two place seals fit.That is:
Outer cylindrical body, intermediate casing, inner sleeve three are integrally formed, namely single-piece cover (under this single-piece cover state, outer cylindrical body, non-removable between intermediate casing and inner sleeve three, be connected); Or
Both outer cylindrical body and intermediate casing are integrally formed and form disassembled two-piece-dress (under this two-piece-dress state with inner sleeve, outer cylindrical body and intermediate casing therebetween non-removable, be connected, and be dismountable between they and inner sleeve); Or
Both intermediate casing and inner sleeve are integrally formed and form disassembled two-piece-dress (under this two-piece-dress state with outer cylindrical body, intermediate casing and inner sleeve therebetween non-removable, be connected, and be dismountable between they and outer cylindrical body); Or
It is disassembled formation three-piece (under this three-piece state, outer cylindrical body, intermediate casing and inner sleeve three are all dismountable each other) between outer cylindrical body, intermediate casing, inner sleeve three.
According to different use occasion, suitable design is selected to be easy, such as when needs use with commercial scale, for strengthening the structural strength of combined type rectifying column of the present invention, adopting stainless steel, to prepare this combined type rectifying column be useful, be now integrally formed single-piece cover with outer cylindrical body, intermediate casing, inner sleeve three is useful.Again such as, when using with laboratory scale, two-piece-dress or three-piece design is used to be more flexibly, easily; Particularly when using glass for material, be more useful.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, the sieve plate that described inner sleeve bottom is arranged is provided with sieve aperture, and the size and number of sieve aperture is with such Program design: but can for steam up by, condensation reflux liquid descending to pass through to make in distillation operation filler pass through.
The combined type rectifying column of arbitrary embodiment, is characterized in that according to a first aspect of the present invention, and the interior edge of described inner sleeve upper shed is used for being connected in the mode sealing fit with other rectifier unit parts.
The combined type rectifying column of arbitrary embodiment according to a first aspect of the present invention, it is characterized in that, described outer cylindrical body, intermediate casing, three seals fit with inner sleeve, when carrying out distillation operation, the steam of rectifying is entered from the lower ending opening of described outer cylindrical body, in distillation process, the U-shaped pipe of intermediate casing is refluxed liquid fluid-tight, the through hole on steam up arrival intermediate casing top in outer cylindrical body and enter in intermediate casing, steam is descending along intermediate casing, the sieve plate being passed inner sleeve bottom because of U-shaped pipe by fluid-tight enters in inner sleeve, steam contacts to carry out rectification working process with the filler wherein loaded in inner sleeve, the upper shed of the up arrival inner sleeve of last steam and leave rectifying column, enter other rectifier unit parts.
In arbitrary embodiment of either side of the present invention, in this area, it also can be described as rectifying column to described rectifying column.
Further, second aspect present invention provides a kind of rectifier unit, it is characterized in that, it comprises: combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, as described in described combined type rectifying column embodiment as arbitrary in first aspect present invention.Described rectifying bottle is for holding the liquid material treating rectifying.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and described rectifying bottle is connected in the mode sealing fit with the interface of described combined type rectifying column outer cylindrical body lower end.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and one end of described condensing unit is connected in the mode sealing fit with the upper shed of described combined type rectifying column inner sleeve.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and the other end of described condensing unit is connected in the mode sealing fit with returnable bottle.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and described filler is filled in the inner sleeve of described combined type rectifying column.In one embodiment, the mode that described filler inclining is filled in the inner sleeve of described combined type rectifying column.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and described condensing unit is such as condenser pipe, such as serpentine condenser, spherical condensation tube, straight cold finger etc.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, and described filler is such as bead (such as quartz glass pearl), molecular sieve and stainless steel ring/ball etc.
The rectifier unit of arbitrary embodiment, is characterized in that according to a second aspect of the present invention, between described combined type rectifying column and condensing unit, and between described condensing unit and returnable bottle, connects independently of one another optionally through intermediate connector.
The rectifier unit of arbitrary embodiment according to a second aspect of the present invention, comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connects their intermediate connector.Operate as laboratory scale conventional rectification, rectifying bottle can be typically there-necked flask, and wherein flatly and combined type rectifying column of the present invention, other two mouthfuls can be accessed agitator or thermometer to control distillation operation process conditions.In addition, above combined type rectifying column of the present invention, can be connected with a three-way pipe, one of them mouth is connected with condensing unit, another mouth can the monitoring device such as cut-in temperature meter to control distillation operation process conditions.
The rectifier unit of arbitrary embodiment according to a second aspect of the present invention, comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connects their intermediate connector.Optionally, between the condensing unit other end of the present invention and returnable bottle, three-way pipe can be used to connect, and a mouth more than needed can be connected with the external world, be connected with optional exhaust gas processing device (and/or drying tower), be connected and/or be connected with vacuum extractor with safety device.
The rectifier unit of arbitrary embodiment according to a second aspect of the present invention, comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connects their intermediate connector.Optionally, in rectifier unit of the present invention, described rectifying bottle can use heater to carry out the temperature heating to obtain required for distillation operation.
Further, third aspect present invention provides treats the method that rectifying material carries out rectifying, and the method comprises the following steps:
(1) provide and assemble combined type rectifying column as described in embodiment as arbitrary in first aspect present invention, and/or providing or assemble rectifier unit described in the arbitrary embodiment of second aspect present invention, in inner sleeve wherein, adding filler;
(2) in rectifying bottle, rectifying material is treated in interpolation, and this rectifying bottle is connected with the interface of combined type rectifying column lower end;
(3) condensing unit is made to be connected optionally by intermediate connector with the inner sleeve upper shed of combined type rectifying column;
(4) condensing unit is connected optionally by intermediate connector with returnable bottle, and be connected with the external world optionally by intermediate connector, (and/or drying tower is connected, be connected with safety device and/or be connected with vacuum extractor with optional exhaust gas processing device;
(5) according to treating the physicochemical property of rectifying material and the physicochemical property of target product, heat to start distillation operation to rectifying bottle, optional startup exhaust gas processing device (and/or drying tower), safety device and/or vacuum extractor, obtain rectifying target product by returnable bottle.
Arbitrary technical characteristic that arbitrary embodiment of either side of the present invention or this either side has is suitable for arbitrary embodiment of other arbitrary embodiment or other either side equally, as long as they can not be conflicting, certainly at where applicable each other, necessary words can be done suitably to modify to individual features.Be further described with feature to various aspects of the present invention below.
All documents that the present invention quotes from, their full content is incorporated to herein by reference, and if the implication expressed by these documents and the present invention inconsistent time, be as the criterion with statement of the present invention.In addition, the various term that the present invention uses and phrase have and well known to a person skilled in the art general sense, nonetheless, the present invention still wishes to be described in more detail at this these terms and phrase and to explain, the term mentioned and phrase, if any inconsistent with common art-recognized meanings, are as the criterion with the implication that the present invention states.
Be further described to various aspects of the present invention below.
In one embodiment, combined type rectifying column of the present invention comprises outer cylindrical body, intermediate casing and inner sleeve three part, filler is placed in inner sleeve, inner sleeve has outer grinding port, outer cylindrical body and intermediate casing form one and have interior ground, inner sleeve is contained in intermediate casing by the opening sleeve on outer cylindrical body and intermediate casing top, and the two is sealed by ground; Hold in rectifying bottle and treat rectifying sample, rectifying bottle is placed in heater; The bottom of outer cylindrical body of combined type rectifying column application of sample bottle and the bottleneck compact siro spinning technology at the top of heating bottle; The top of combined type rectifying column is connected to the top of condensing unit by tube connector; The bottom of condensing unit is connected to returnable bottle; Rectifying product is obtained in returnable bottle.
In one embodiment, both outer cylindrical body and intermediate casing are integrally formed, and become double glazing tubular construction, the bottom of outer layer glass tube is provided with steam inlet, the bottleneck compact siro spinning technology at the top of steam inlet and rectifying bottle; Inner layer glass tube and outer layer glass tube airtight on top, and airtight place is provided with interior ground; The top sidewall of inner layer glass tube is provided with equally distributed multiple through hole, and the internal diameter of bottom reduces gradually and forms elbow, and the shape of elbow is semicircle.According to the difference treating rectifying sample in inner sleeve, fill corresponding filler; Top is provided with outer grinding port, thus with double-layer glass tube sealing structure; Top end opening place is provided with interior ground, thus seals with tube connector; Bottom inner diameter reduces to form refluxing opening; On refluxing opening, be provided with sieve plate, sieve plate is provided with sieve aperture.Be placed on and after rectifying sample heats in heater, produce steam in rectifying bottle, the steam of rectifying component enters between outer cylindrical body and the double-layer glass tube of intermediate casing from rectifying bottle by steam inlet, rise to top, enter in intermediate casing by multiple through holes of side-walls, and then enter inner sleeve by the sieve aperture of sieve plate, contact with the filler in inner sleeve, the crotch of product liquid U-shaped tube shape bottom intermediate casing of backflow turns back in rectifying bottle; The steam of rectifying component is through steam repeatedly and backflow, and the steam arriving combined type rectifying column top enters condensing unit from the opening at top through tube connector.The present invention adopts the three-decker of combined type rectifying column, adds disjoint paths, have effectively achieved and increases rectifying column length, thus improve discrimination, serves the effect promoting heat transfer simultaneously; Further, rectifying column adopts knockdown structure, can be designed to fixed or detachable between each layer pipe, can according to actual needs, according to the filler treating rectifying sample to select to be applicable to, after rectifying terminates, can also cleaning be changed, can Reusability, and meet multiple use.
The fire brought in order to avoid electric heating cover, electric shock and the hidden danger such as poisoning, the firing equipment in the present invention adopts the firing equipment of oil bath or METAL HEATING PROCESS mode.
In one embodiment, rectifying bottle can adopt single port bottle, two-mouth bottle, or there-necked flask.For single port bottle, bottleneck is positioned at the top of rectifying bottle, with the bottom compact siro spinning technology of the outer cylindrical body of combined type rectifying column; For two-mouth bottle, be positioned at the bottom compact siro spinning technology of the bottleneck at the top of rectifying bottle and the outer cylindrical body of combined type rectifying column, another is used for laying temperature meter or temperature sensor, or is used for interpolation and treats rectifying sample; For there-necked flask, be positioned at the bottom compact siro spinning technology of the bottleneck of the top vertical of rectifying bottle and the outer cylindrical body of combined type rectifying column, another two bottlenecks are used for laying temperature meter or temperature sensor respectively, and are used for interpolation and treat rectifying sample; Or can agitating device be used.
Further, can also comprise in the various embodiment of the present invention: drying tower, safety flack and/or vavuum pump; Between condensing unit and returnable bottle, adopt three-limb tube, the first end of tube connector connects condensing unit, and the second end connects returnable bottle, three-terminal link drying tower; Drying tower is connected to safety flack by tube connector; Connect bottle and be connected to vavuum pump by tube connector.
In some embodiments, the invention provides the multiduty compound normal pressure/decompression rectification device of a kind of novel combination type, it is applicable to the rectification and purification of organic solvent, natural volatile product.The feature of this device is: combined type rectifying column easy cleaning, and can use multiple filler according to demand and change conveniently, product purity is high, steady quality, and rectifying productive rate is higher, separation costs is low, and distillation process is without potential safety hazard.
Especially, embodiment of the present invention adopt three layer interlayer sleeve structures, and simultaneously its advantage to play the effect increasing rectifying column length and promote heat transfer.
Embodiment of the present invention can regulate heating-up temperature according to the requirement of rectifying product type and purity, change filler in rectifying column and regulate reflux ratio, make the product purity of purifying through this device can reach chromatographically pure level, obtain higher product recovery rate simultaneously.
In sum, the present invention is a kind of compound normal pressure/decompression rectification device of novel composite and multi-purpose.It is applicable to the rectification and purification of multiple organic solvent, natural volatile product, and final products can realize high-purity and high-recovery simultaneously.In addition, distillation process is repeatable strong and without obvious potential safety hazard.
Apparatus of the present invention belong to the compound separation purification devices in chemical field.It utilizes each component in mixture to have the characteristic of different vapour pressures at a certain temperature, by heating liquid mixture, by repeatedly gasification and condensation, mass transfer and the heat transfer of liquid phase is carried out in rectifying column, the component making high vapour pressure content in the gas phase obviously more than the content in liquid phase, thus reaches the object this component be separated from mixed liquor.Apparatus of the present invention can be widely used in the field such as the preparation of High Purity compound, solvent recovery and natural volatile product separation of small-scale.By improving its structural strength, such as use stainless steel to replace glass material, apparatus of the present invention as the even production-scale equipment of the pilot-scale of chemical field, can play its corresponding function.
Advantage of the present invention is extremely significant, such as but not limited to:
(1) by using multiloop structure, device has less volume, preferably heat-transfer effect and the higher number of plates;
(2) filler is replaceable, is applicable to different separation demand;
(3) rectifying column is combiner, is easier to manufacture and use;
(4) oil bath mode of heating can be used to avoid disaster hidden-trouble;
(5) apparatus of the present invention regulate reflux ratio by thermometer or temperature sensor precise temperature control, reach the balance of product high-purity and high-recovery.
Accompanying drawing explanation
Fig. 1 shows the outer cylindrical body of combined type rectifying column of the present invention, intermediate casing and inner sleeve three schematic diagram in the assembled state, and outer cylindrical body, intermediate casing and the inner sleeve three top mode in sealing fit that shows in figure combines.
Fig. 2 shows the outer cylindrical body of combined type rectifying column of the present invention, intermediate casing and inner sleeve three schematic diagram in a disassembled state, it is disassembled formation three-piece between outer cylindrical body, intermediate casing, inner sleeve three, under this three-piece state, outer cylindrical body, intermediate casing and inner sleeve three are all dismountable each other.In figure, left hand view is outer cylindrical body, and middle graph is intermediate casing, and right part of flg is inner sleeve, and wherein inner sleeve is for insert in intermediate casing and to seal fit, and intermediate casing is for insert in outer cylindrical body and to seal fit.
It is integrally formed and form disassembled two-piece-dress with inner sleeve that Fig. 3 shows both the outer cylindrical body of combined type rectifying column of the present invention and intermediate casing, under this two-piece-dress state, outer cylindrical body and intermediate casing therebetween non-removable, be connected, and be dismountable between they and inner sleeve.
It is integrally formed and form disassembled two-piece-dress with outer cylindrical body that Fig. 4 shows both the intermediate casing of combined type rectifying column of the present invention and inner sleeve, under this two-piece-dress state, intermediate casing and inner sleeve therebetween non-removable, be connected, and be dismountable between they and outer cylindrical body.
Fig. 5 schematically depict the divide a word with a hyphen at the end of a line route of steam in combined type rectifying column of the present invention of rectifying, and rectifying divides a word with a hyphen at the end of a line route as one of the arrows.
Fig. 6 depicts some basic elements of character of rectifier unit of the present invention, comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connects their intermediate connector.
Fig. 7 depicts some basic elements of character of rectifier unit of the present invention, comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connects their intermediate connector.Optionally, between the condensing unit other end of the present invention and returnable bottle, three-way pipe can be used to connect, the mouth that this three-way pipe is had more than needed can be connected with the external world, be connected with optional exhaust gas processing device (and/or drying tower), be connected with safety device and/or be connected with vacuum extractor; Optionally, in rectifier unit of the present invention, described rectifying bottle can use heater to carry out the temperature heating to obtain required for distillation operation.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.They are only preferred embodiments more of the present invention, protection scope of the present invention be not only confined to these embodiments, and all technical schemes belonged under thinking of the present invention all belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, some improvements and modifications without departing from the principles of the present invention, should be considered as protection scope of the present invention.
Fig. 1 to Fig. 7 of the present invention schematically depict the structure of various aspects of the present invention and spatial relationship thereof and working method, is described further below in conjunction with accompanying drawing.
As depicted in figs. 1 and 2, present the assembled state figure of the combined type rectifying column 1 of first aspect present invention and a kind of decomposing state figure of embodiment respectively, this combined type rectifying column 1 comprises: outer cylindrical body 11, intermediate casing 12 and inner sleeve 13, and three's main part is separately the tube that concentric is arranged;
The lower ending opening of described outer cylindrical body 11, and this lower ending opening place be provided with for rectifier unit in device (the such as rectifying bottle etc. of rectifying steam are provided, they are the conventional components in a kind of distillation operation, treat the liquid material of rectifying for splendid attire) interface 111 that connects; Described outer cylindrical body 11 upper end interior along 112 for sealing fit with described intermediate casing 12 upper end;
The bore of the bottom of described intermediate casing 12 reduces gradually and forms the crotch 121 of opening upwards, thus the U-shaped tube shape that can realize fluid-tight function is formed in the bottom of intermediate casing 12, the side of U-shaped pipe is little opening upwards, and opposite side bore increases gradually and forms one with the main part of intermediate casing 12;
The bore of described intermediate casing 12 upper end increases to form intermediate casing bulge 122 gradually, outer and the interior of described outer cylindrical body 11 upper end of this intermediate casing bulge 122 seal fit along 112, and the interior edge of this intermediate casing bulge 122 is used for and described inner sleeve 13 top seal fit;
The below of described intermediate casing 12 bulge 122 is provided with some through holes 123 and passes through for steam;
The bore on described inner sleeve 13 top increases to form inner sleeve bulge 131, and the outer of this inner sleeve bulge 131 and the interior of described intermediate casing 12 bulge 122 are along sealing fit;
Described inner sleeve 13 bottom is provided with sieve plate 132, this sieve plate 132 can for steam by but can not to make in distillation operation filler pass through;
The top of described inner sleeve bulge 131 is inner sleeve upper shed 133, and the caliber of this inner sleeve upper shed 133 is less than this inner sleeve bulge 131, and this inner sleeve upper shed 133 can be used for being connected with other rectifier unit parts;
Described outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three seal fit thus, form steam and enter from the lower ending opening of outer cylindrical body 11, leave the rectifying loop of rectifying column 1 from the upper shed 133 of inner sleeve 13.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the radius of described outer cylindrical body main part is 1: 0.4 ~ 0.9 with the ratio of the radius of intermediate casing main part.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the radius of described intermediate casing main part is 1: 0.4 ~ 0.9 with the ratio of the radius of inner sleeve main part.
As shown in Figure 1, which show the outer cylindrical body 11 of combined type rectifying column 1 of the present invention, intermediate casing 12 and inner sleeve 13 three schematic diagram in the assembled state, outer cylindrical body 11, intermediate casing 12 and the inner sleeve 13 three top mode in sealing fit that shows in figure combines.
As shown in Figure 2, which show the outer cylindrical body 11 of combined type rectifying column 1 of the present invention, intermediate casing 12 and inner sleeve 13 three schematic diagram in a disassembled state, left hand view is outer cylindrical body 11, middle graph is intermediate casing 12, right part of flg is inner sleeve 13, wherein inner sleeve 13 is for insert in intermediate casing 12 and to seal fit, and intermediate casing 12 is for insert in outer cylindrical body 11 and to seal fit.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the manufacture material of described outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three is selected from glass or stainless steel independently of one another.In one embodiment, the manufacture material of described outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three is glass.When combined type rectifying column 1 of the present invention uses the specification of scale to provide with laboratory, its material is good with glass, be easy to like this to manufacture, be easy to cleaning, have to be easy to during damaged components to replace, glass ground joint is easy to sealing, be easy to change experiment condition etc., when particularly outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three are all can arrange in the mode mutually dismantled according to specific experiment demand.And when combined type rectifying column 1 of the present invention provides with the specification of pilot scale or production and application scale, its material is good with stainless steel, high-strength structure requirement can be realized like this, now outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three are all arranged in integrally formed non-removable mode, or with wherein adjacent both to arrange in integrally formed non-removable mode be preferred.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the interface (like this, make the bore of the relative aperture of this interface 111 connected rectifying bottle little) of outer grinding port structure that what described outer cylindrical body 11 lower ending opening place was arranged for the interface 111 be connected with rectifying bottle is.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, described outer cylindrical body 11 upper end interior is along 112 for sealing fit with the outer of described intermediate casing 12 bulge 122, and sealing fit is integrally formed structure or dismountable structure.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, described outer cylindrical body 11 upper end interior along 112 for sealing fit with the outer of described intermediate casing 12 bulge 122, sealing fit is integrally formed structure, thus, outer cylindrical body 11 and intermediate casing 12 are integral types, and the two can not be disassembled.Such design benefit is significant, and namely outer cylindrical body 11 is integrally formed with both intermediate casings 12, the sealing in this position both strengthening.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the interior of described outer cylindrical body 11 upper end seals fit along 112 and the outer of described intermediate casing 12 bulge 122, sealing fit is dismountable structure, thus, outer cylindrical body 11 and both intermediate casings 12 are separable, and the two is disassembled.Such design benefit is significant, and namely outer cylindrical body 11 and both intermediate casings 12 can distinguish processing, as long as the two can be made at this position seals fit; Also be convenient to internal washing; If the two one of have damage, replace one of them can with another unspoiled Component composition.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, under the state sealing fit along 112 with the outer of described intermediate casing 12 bulge 122 in described outer cylindrical body 11 upper end, described in take the shape of the letter U crotch 121 part of tube shape can not contact with the inwall of outer cylindrical body 11.In one embodiment, described intermediate casing 12 main part overlook viewed circle, described in take the shape of the letter U crotch 121 part of tube shape be in this circle.This design of crotch 121 part of tube shape of taking the shape of the letter U is favourable, such as, when outer cylindrical body 11 and both intermediate casings 12 are separable, disassembled designs, because of the contact internal walls of crotch 121 part of U-shaped tube shape and outer cylindrical body 11, each self-damage can not be even caused when inserting intermediate casing 12 in outer cylindrical body 11.In addition, take the shape of the letter U tube shape crotch 121 part for extend rectifying time steam operating path be useful, namely in distillation process, the phegma dripped from such as inner sleeve 13 because temperature reduces remains at this U-shaped pipe, can fluid-tight be realized when phegma is accumulated to a certain amount of and avoid steam directly to enter intermediate casing 12 from this U-shaped pipe, can overflow from U-shaped tube opening one end when phegma continues accumulation and reenter rectifying bottle.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, is positioned at intermediate casing top above intermediate casing bulge 122 along forming top that described in relative aperture, outer cylindrical body 11 external diameter is large along 124.The top designed thus is along 124, can make outer cylindrical body 11 and both intermediate casings 12 when in separable, disassembled design, (top of intermediate casing 12 is just in time stuck in the upper end of outer cylindrical body 11 along 124 to avoid intermediate casing 12 can not fall into outer cylindrical body 11 completely, and can not fall into wherein completely, avoid causing dismounting difficulty).In addition, the top designed thus is along 124, and be also convenient to disassemble outer cylindrical body 11 and both intermediate casings 12, namely this top of a hand-held outer cylindrical body 11, another hand-held intermediate casing 12 is along 124, can easily make outer cylindrical body 11 be separated with both intermediate casings 12.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention; the below of described intermediate casing 12 bulge 122 is provided with some through holes 123 and passes through for steam; the size and number design (usually determining according to the use scale of combined type rectifying column 1 or specification) of through hole 123 enters intermediate casing 12 be as the criterion can guarantee to realize steam in outer cylindrical body 11, and/or can guarantee that intermediate casing 12 has enough structural strengths to be as the criterion.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the outer of described inner sleeve bulge 131 and the interior of described intermediate casing 12 bulge 122 are along sealing fit, and sealing fit is integrally formed structure or dismountable structure.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the outer of described inner sleeve bulge 131 and the interior of described intermediate casing 12 bulge 122 are along sealing fit, sealing fit is integrally formed structure, thus, intermediate casing 12 and inner sleeve 13 are integral types, and the two can not be disassembled.Such design benefit is significant, and namely intermediate casing 12 is integrally formed with both inner sleeves 13, the sealing in this position both strengthening.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the outer of described inner sleeve bulge 131 and the interior of described intermediate casing 12 bulge 122 are along sealing fit, sealing fit is dismountable structure, thus, intermediate casing 12 and both inner sleeves 13 are separable, and the two is disassembled.Such design benefit is significant, and namely intermediate casing 12 and both inner sleeves 13 can distinguish processing, as long as the two can be made at this position seals fit; Also be convenient to internal washing; If the two one of have damage, replace one of them can with another unspoiled Component composition; And inner sleeve 13 is convenient to its filling filler when disassembling, even in distillation process, replacing is filled with the inner sleeve 13 of variety classes filler to realize more complicated distillation operation.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, described outer cylindrical body 11 upper end interior is along 112 for sealing along seal fit in the outer of fit and described inner sleeve bulge 131 and described intermediate casing 12 bulge 122 with the outer of described intermediate casing 12 bulge 122, and this two place sealing fit is in integrally formed structure independently of one another or is dismountable structure.That is:
Outer cylindrical body 11, intermediate casing 12, inner sleeve 13 three are integrally formed, namely (typical structure is see Fig. 1 for single-piece cover, under this single-piece cover state, outer cylindrical body 11, non-removable between intermediate casing 12 and inner sleeve 13 three, be connected); Or
Outer cylindrical body 11 is integrally formed and form disassembled two-piece-dress with inner sleeve 13 (typical structure is see Fig. 3 with both intermediate casings 12, under this two-piece-dress state, outer cylindrical body 11 and intermediate casing 12 therebetween non-removable, be connected, and be dismountable between they and inner sleeve 13); Or
Intermediate casing 12 is integrally formed and form disassembled two-piece-dress with outer cylindrical body 11 (typical structure is see Fig. 4 with both inner sleeves 13, under this two-piece-dress state, intermediate casing 12 and inner sleeve 13 therebetween non-removable, be connected, and be dismountable between they and outer cylindrical body 11); Or
That (typical structure is see Fig. 2 for disassembled formation three-piece between outer cylindrical body 11, intermediate casing 12, inner sleeve 13 three, under this three-piece state, outer cylindrical body 11, intermediate casing 12 and inner sleeve 13 three are all dismountable each other).
According to design spirit of the present invention, for different use occasion, suitable design is selected to be easy.Such as when needs use with commercial scale, for strengthening the structural strength of combined type rectifying column 1 of the present invention, adopting stainless steel, to prepare this combined type rectifying column 1 be useful, be now integrally formed single-piece cover with outer cylindrical body 11, intermediate casing 12, inner sleeve 13 three is useful.Again such as, when using with laboratory scale, two-piece-dress or three-piece design is used to be more flexibly, easily; Particularly when using glass for material, be more useful.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the sieve plate 132 that described inner sleeve 13 bottom is arranged is provided with sieve aperture, the size and number of sieve aperture is with such Program design: but can for steam up by, condensation reflux liquid descending by can not to make in distillation operation filler by (namely, typically, the aperture of sieve aperture should be less than the particle diameter of general filler).
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, the interior edge of described inner sleeve upper shed 133 is used for being connected (be such as connected with follow-up condensing unit, optionally adopt tube connector transition to connect therebetween) in the mode sealing fit with other rectifier unit parts.
An embodiment of combined type rectifying column 1 according to a first aspect of the present invention, exemplarily as shown in Figure 1, described outer cylindrical body 11, intermediate casing 12, fit is sealed with inner sleeve 13 three, when carrying out distillation operation, the steam of rectifying is entered from the lower ending opening of described outer cylindrical body 11, in distillation process, the U-shaped pipe of intermediate casing 12 is refluxed liquid fluid-tight, the through hole 123 on steam up arrival intermediate casing 12 top in outer cylindrical body 11 and enter in intermediate casing 12, steam is descending along intermediate casing 12, the sieve plate 132 being passed inner sleeve 13 bottom because of U-shaped pipe by fluid-tight enters in inner sleeve 13, steam contacts to carry out rectification working process with the filler wherein loaded in inner sleeve 13, the upper shed 133 of the up arrival inner sleeve 13 of last steam and leave rectifying column 1, enter other rectifier unit parts.Fig. 5 schematically depict the divide a word with a hyphen at the end of a line route of steam in combined type rectifying column 1 of the present invention of rectifying, as one of the arrows.
The combined type rectifying column 1 of arbitrary embodiment according to a first aspect of the present invention, it also can be described as rectifying column, particularly when the scale of industrial production or scale up test uses.
Further, as shown in Fig. 6 and/or Fig. 7, an embodiment of rectifier unit according to a second aspect of the present invention, this comprises: combined type rectifying column 1, rectifying bottle 2, condensing unit 3, returnable bottle 4 and filler 5, as described in described combined type rectifying column 1 embodiment as arbitrary in first aspect present invention.Described rectifying bottle 2 is for holding the liquid material treating rectifying.
An embodiment of rectifier unit according to a second aspect of the present invention, described rectifying bottle 2 is connected in the mode sealing fit with the interface 111 of described combined type rectifying column 1 outer cylindrical body 11 lower end.
An embodiment of rectifier unit according to a second aspect of the present invention, one end of described condensing unit 3 is connected in the mode sealing fit with described combined type rectifying column 1 inner sleeve upper shed 133.
An embodiment of rectifier unit according to a second aspect of the present invention, the other end of described condensing unit 3 is connected in the mode sealing fit with returnable bottle 4.
An embodiment of rectifier unit according to a second aspect of the present invention, described filler 5 is filled in the inner sleeve 13 of described combined type rectifying column 1.In one embodiment, the mode that described filler 5 inclining is filled in the inner sleeve 13 of described combined type rectifying column 1.
An embodiment of rectifier unit according to a second aspect of the present invention, described condensing unit 3 is such as condenser pipe, such as serpentine condenser, spherical condensation tube, straight cold finger etc.
An embodiment of rectifier unit according to a second aspect of the present invention, described filler 5 is such as bead (such as quartz glass pearl), molecular sieve and stainless steel ring/ball etc.
An embodiment of rectifier unit, between described combined type rectifying column 1 and condensing unit 3, and between described condensing unit 3 and returnable bottle 4, connects optionally through intermediate connector 31 independently of one another according to a second aspect of the present invention.
Such as, as shown in Figure 6, wherein depict some basic elements of character of rectifier unit of the present invention, comprise combined type rectifying column 1, rectifying bottle 2, condensing unit 3, returnable bottle 4 and filler 5, and connect their intermediate connector 31.Operate as laboratory scale conventional rectification, rectifying bottle 2 can be typically there-necked flask, wherein a bite and combined type rectifying column 1 of the present invention, other two mouthfuls (a mouth of Fig. 6 and b mouth) can access agitator or thermometer or conduct and add item to control distillation operation process conditions.In addition, above combined type rectifying column 1 of the present invention, can be connected with a three-way pipe, a mouth of this three-way pipe is connected with condensing unit 3, another mouth (the c mouth of Fig. 6) can the monitoring device such as cut-in temperature meter to control distillation operation process conditions.Delivery port when the d mouth of Fig. 6 and e mouth are using condenser pipe as condensing unit respectively and water inlet).
In addition, as shown in Figure 7, optionally, between condensing unit 3 other end of the present invention and returnable bottle 4, three-way pipe can be used to connect, the more than needed mouth (the f mouth of Fig. 6) of this three-way pipe can be connected with the external world, connect with optional exhaust gas processing device (and/or drying tower, Fig. 7 62), be connected (Fig. 7 63) and/or be connected with vacuum extractor (Fig. 7 64) with safety device; When being connected with these peripheral units, their order of connection well known to a person skilled in the art, (and/or drying tower, safety device, vacuum extractor is connected the more than needed mouth of such as this three-way pipe is a kind of common connected mode with exhaust gas processing device successively.
In addition, as shown in Figure 7, optionally, in rectifier unit of the present invention, described rectifying bottle 2 can use heater 61 to carry out the temperature heating to obtain required for distillation operation.
Further, describe with reference to Fig. 1 to Fig. 7 of the present invention and the present invention described in detail above, third aspect present invention provides a kind ofly treats the method that rectifying material carries out rectifying, and the method comprises the following steps:
(1) provide and assemble combined type rectifying column 1 as described in embodiment as arbitrary in first aspect present invention, and/or providing or assemble rectifier unit described in the arbitrary embodiment of second aspect present invention, in inner sleeve 13 wherein, adding filler 5;
(2) in rectifying bottle 2, rectifying material is treated in interpolation, and this rectifying bottle 2 is connected with the interface 111 of combined type rectifying column 1 lower end;
(3) condensing unit 3 is made to be connected optionally by intermediate connector 31 with the inner sleeve upper shed 133 of combined type rectifying column 1;
(4) condensing unit 3 is made to be connected optionally by intermediate connector 31 with returnable bottle 4, and is connected with the external world optionally by intermediate connector 31, with optional exhaust gas processing device (and/or drying tower, Fig. 7 62) connection, is connected (Fig. 7 63) with safety device and/or is connected with vacuum extractor (Fig. 7 64);
(5) according to treating the physicochemical property of rectifying material and the physicochemical property of target product, heat to start distillation operation to rectifying bottle 2, optional startup exhaust gas processing device (and/or drying tower), safety device and/or vacuum extractor, obtain rectifying target product by returnable bottle 4.
embodiment 1
In the present embodiment, for the atmospheric distillation of n-hexane, with the preparative scale glass device in laboratory (example is as Fig. 6), with the package assembly of three-piece shown in Fig. 2, and the method for third aspect present invention, illustrate operation of the present invention.The method of operating of the present embodiment, comprises the following steps:
1) in the inner sleeve 13 of combined type rectifying column, load appropriate glass column filler 5, the inner sleeve 13 installing filler is contained in intermediate casing 12 by the opening sleeve on intermediate casing 12 top, screws slightly, the two interface is sealed by glass ground joint; Then make them be contained in outer cylindrical body 11 by the opening sleeve on outer cylindrical body 11 top, screw slightly, the two interface is sealed by glass ground joint;
2) 2000mL is analyzed pure hexane reagent, be injected in three mouthfuls of rectifying bottles 2 of 3L by the bottleneck a of rectifying bottle 2, add appropriate zeolite, then bottleneck a grinding port plug is sealed, in bottleneck b, fill in thermometer or temperature sensor and seal, rectifying bottle 2 is placed in oil bath firing equipment 61, and the steam inlet of the outer cylindrical body 11 of combined type rectifying column 1 and interface 111 pass through glass ground joint compact siro spinning technology with the bottleneck at the top of rectifying bottle; The condensation mouth of pipe e with d is connected circulating condensing water inlet and outlet respectively, opens recirculated water switch and refrigeration switch, makes the cooling water of 10 DEG C by serpentine condenser 3;
3) open the heating function of oil bath firing equipment 61, temperature is adjusted between 120 ~ 150 DEG C, and when n-hexane liquid reaches its boiling point, n-hexane comes to life and gasifies, and produces steam;
4) steam of n-hexane enters in the double-layer glass tube between outer cylindrical body 11 and intermediate casing 12 from rectifying bottle 2 by steam inlet and interface 111, rise to top, enter in the double-layer glass tube between intermediate casing 12 and inner sleeve 13 by the through hole of side-walls above intermediate casing 12, steam comes downwards to bottom and enters in inner sleeve 13 from the sieve plate of inner sleeve 13, and then contact with the filler in inner sleeve 13, through continuous rectifying and backflow, the U-shaped pipe crotch 121 of product liquid bottom intermediate casing 12 of backflow turns back in rectifying bottle 2;
5) steam of n-hexane is through steam repeatedly and backflow, and the steam arriving combined type rectifying column top enters condensing unit 3 from the opening at top through tube connector, finally enters the n-hexane rectifying product obtaining chromatographically pure level in returnable bottle 4.
Find in the present embodiment 1, when the radius of outer cylindrical body main part is in 1: 0.4 ~ 0.9 scope with the ratio of the radius of intermediate casing main part, rectifying productive rate reaches more than 85%, and when above-mentioned radius ratio is not within the scope of this, rectifying productive rate can sharply decline, particularly from this scope more away from then rectifying productive rate decline larger; Such as, the rectifying productive rate only 41% when the radius of outer cylindrical body main part is 1: 0.3 with the ratio of the radius of intermediate casing main part, and when the radius of outer cylindrical body main part is 1: 0.95 with the ratio of the radius of intermediate casing main part rectifying productive rate only 62%.In addition, also find in the present embodiment 1, when the radius of middle sleeve body portion is in 1: 0.4 ~ 0.9 scope with the ratio of the radius of inner sleeve main part, rectifying productive rate reaches more than 87%, and when above-mentioned radius ratio is not within the scope of this, rectifying productive rate can sharply decline, particularly from this scope more away from then rectifying productive rate decline larger; Such as, the rectifying productive rate only 46% when the radius of middle sleeve body portion is 1: 0.3 with the ratio of the radius of inner sleeve main part, and when the radius of middle sleeve body portion is 1: 0.95 with the ratio of the radius of inner sleeve main part rectifying productive rate only 57%.In addition, applicant carries out the operation of the present embodiment 1 respectively according to the upper disclosed device of CN101642630A, CN201299982Y, CN201426987Y, CN101433773A, their rectifying productive rate of result is all in 46% ~ 61% scope.In addition, applicant is through manufacturing and adjusting, find the device (all so that the specification of 2000mL material can be processed) of the upper disclosed device of CN101642630A, CN201299982Y, CN201426987Y, CN101433773A and the present embodiment 1, these existing apparatus make 2.6 ~ 4.1 times that cost is the present embodiment cost, be all significantly higher than the cost of the application's device.
embodiment 2
In the present embodiment, for the rectification under vacuum of Rosa Damascana, with the preparative scale glass device in laboratory (example is as Fig. 7), with the package assembly of two-piece-dress shown in Fig. 3, and the method for third aspect present invention, illustrate operation of the present invention.The method of operating of the present embodiment, comprises the following steps:
1) in the inner sleeve 13 of combined type rectifying column, appropriate stainless steel ring filler 5 is loaded, the inner sleeve 13 installing filler is contained in outer cylindrical body 11/ intermediate casing 12 two-piece-dress by the opening sleeve on intermediate casing 12 top, screw slightly, the two interface is sealed by glass ground joint;
2) 2000mL rose is slightly oily, be injected in three mouthfuls of rectifying bottles 2 of 3L by the bottleneck a of rectifying bottle 2, add appropriate zeolite, then bottleneck a grinding port plug is sealed, in bottleneck b, fill in thermometer or temperature sensor and seal, rectifying bottle 2 is placed in oil bath firing equipment 61, and the steam inlet of the outer cylindrical body 11 of combined type rectifying column 1 and interface 111 pass through glass ground joint compact siro spinning technology with the bottleneck at the top of rectifying bottle; The condensation mouth of pipe e with d is connected circulating condensing water inlet and outlet respectively, opens recirculated water switch and refrigeration switch, makes the cooling water of 4 DEG C by serpentine condenser 3;
3) connect drying tower 62, safety flack 63 and vavuum pump 64, for vavuum pump 64 is opened in rectification under vacuum, suitably regulate the vacuum that the valve on safety flack 63 makes internal system keep certain;
4) open the heating function of oil bath firing equipment 61, temperature is adjusted between 40 ~ 60 DEG C, and when the Rosa Damascana in rectifying bottle 2 reaches boiling point under vacuum conditions, Rosa Damascana comes to life and gasifies, and produces steam;
5) steam of Rosa Damascana enters in the double-layer glass tube between outer cylindrical body 11 and intermediate casing 12 from rectifying bottle 2 by steam inlet and interface 111, rise to top, enter in the double-layer glass tube between intermediate casing 12 and inner sleeve 13 by the through hole of side-walls above intermediate casing 12, steam comes downwards to bottom and enters in inner sleeve 13 from the sieve plate of inner sleeve 13, and then contact with the filler in inner sleeve 13, through continuous rectifying and backflow, the U-shaped pipe crotch 121 of product liquid bottom intermediate casing 12 of backflow turns back in rectifying bottle 2;
6) steam of Rosa Damascana is through steam repeatedly and backflow, and the steam arriving combined type rectifying column top enters condensing unit 3 from the opening at top through tube connector, finally enters the Rosa Damascana product obtaining high-quality in returnable bottle 4.
Find in the present embodiment 2, when the radius of outer cylindrical body main part is in 1: 0.4 ~ 0.9 scope with the ratio of the radius of intermediate casing main part, rectifying productive rate reaches more than 87%, and when above-mentioned radius ratio is not within the scope of this, rectifying productive rate can sharply decline, particularly from this scope more away from then rectifying productive rate decline larger; Such as, the rectifying productive rate only 44% when the radius of outer cylindrical body main part is 1: 0.3 with the ratio of the radius of intermediate casing main part, and when the radius of outer cylindrical body main part is 1: 0.95 with the ratio of the radius of intermediate casing main part rectifying productive rate only 66%.In addition, also find in the present embodiment 2, when the radius of middle sleeve body portion is in 1: 0.4 ~ 0.9 scope with the ratio of the radius of inner sleeve main part, rectifying productive rate reaches more than 84%, and when above-mentioned radius ratio is not within the scope of this, rectifying productive rate can sharply decline, particularly from this scope more away from then rectifying productive rate decline larger; Such as, the rectifying productive rate only 40% when the radius of middle sleeve body portion is 1: 0.3 with the ratio of the radius of inner sleeve main part, and when the radius of middle sleeve body portion is 1: 0.95 with the ratio of the radius of inner sleeve main part rectifying productive rate only 59%.In addition, applicant carries out the operation of the present embodiment 2 respectively according to the upper disclosed device of CN101642630A, CN201299982Y, CN201426987Y, CN101433773A, their rectifying productive rate of result is all in 43% ~ 66% scope.

Claims (31)

1. a combined type rectifying column, is characterized in that, it comprises: outer cylindrical body, intermediate casing and inner sleeve, and three's main part is separately the tube that concentric is arranged;
The lower ending opening of described outer cylindrical body, and be provided with at this lower ending opening place for the interface providing the device of rectifying steam to be connected in rectifier unit; The interior edge of described outer cylindrical body upper end is used for sealing fit with described intermediate casing upper end;
The bore of the bottom of described intermediate casing reduces gradually and forms the crotch of opening upwards, thus the U-shaped tube shape that can realize fluid-tight function is formed in the bottom of intermediate casing, the side of U-shaped pipe is little opening upwards, and opposite side bore increases gradually and forms one with the main part of intermediate casing;
The bore of described intermediate casing upper end increases to form intermediate casing bulge gradually, the outer of this intermediate casing bulge and the interior of described outer cylindrical body upper end are along sealing fit, and the interior edge of this intermediate casing bulge is used for and described inner sleeve top seal fit;
The below of described intermediate casing bulge is provided with some through holes and passes through for steam;
The bore on described inner sleeve top increases to form inner sleeve bulge, and the outer of this inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit;
Described inner sleeve bottom is provided with sieve plate, this sieve plate can for steam by but can not to make in distillation operation filler pass through;
The top of described inner sleeve bulge is inner sleeve upper shed, and the caliber of this inner sleeve upper shed is less than this inner sleeve bulge, and this inner sleeve upper shed can be used for being connected with other rectifier unit parts;
Described outer cylindrical body, intermediate casing and inner sleeve three seal fit thus, form steam and enter from the lower ending opening of outer cylindrical body, leave the rectifying loop of rectifying column from the upper shed of inner sleeve; And
The radius of described outer cylindrical body main part is 1: 0.4 ~ 0.9 with the ratio of the radius of intermediate casing main part, and the radius of intermediate casing main part is 1: 0.4 ~ 0.9 with the ratio of the radius of inner sleeve main part.
2. combined type rectifying column according to claim 1, is characterized in that described outer cylindrical body, the manufacture material of intermediate casing and inner sleeve three is selected from glass or stainless steel independently of one another.
3. combined type rectifying column according to claim 1, what it is characterized in that described outer cylindrical body lower ending opening place arranges is the interface of outer grinding port structure for the interface be connected with rectifying bottle.
4. combined type rectifying column according to claim 1, it is characterized in that the interior edge of described outer cylindrical body upper end is for sealing fit with the outer of described intermediate casing bulge, sealing fit is integrally formed structure.
5. combined type rectifying column according to claim 1, it is characterized in that the interior edge of described outer cylindrical body upper end seals fit with the outer of described intermediate casing bulge, sealing fit is dismountable structure.
6. combined type rectifying column according to claim 1, under it is characterized in that the state that edge and the outer of described intermediate casing bulge seal fit in described outer cylindrical body upper end, the hook portion of the tube shape that takes the shape of the letter U can not contact with the inwall of outer cylindrical body.
7. combined type rectifying column according to claim 1, is characterized in that the edge, intermediate casing top be positioned at above intermediate casing bulge forms the edge, top that described in relative aperture, outer cylindrical body external diameter is large.
8. combined type rectifying column according to claim 1, it is characterized in that the below of described intermediate casing bulge is provided with some through holes and passes through for steam, the size and number design of through hole enters intermediate casing be as the criterion can guarantee to realize steam in outer cylindrical body, and/or can guarantee that intermediate casing has enough structural strengths to be as the criterion.
9. combined type rectifying column according to claim 1, it is characterized in that the outer of described inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit, sealing fit is integrally formed structure.
10. combined type rectifying column according to claim 1, it is characterized in that the outer of described inner sleeve bulge and the interior of described intermediate casing bulge are along sealing fit, sealing fit is dismountable structure.
11. combined type rectifying columns according to claim 1, it is characterized in that the interior edge of described outer cylindrical body upper end is for sealing along seal fit in the outer of fit and described inner sleeve bulge and described intermediate casing bulge with the outer of described intermediate casing bulge, this two place sealing fit is in integrally formed structure independently of one another or is dismountable structure.
12. combined type rectifying columns according to claim 1, is characterized in that described outer cylindrical body, intermediate casing, inner sleeve three are integrally formed, be i.e. single-piece cover.
13. combined type rectifying columns according to claim 1, is characterized in that both described outer cylindrical body and intermediate casing are integrally formed and form disassembled two-piece-dress with inner sleeve.
14. combined type rectifying columns according to claim 1, is characterized in that both described intermediate casing and inner sleeve are integrally formed and form disassembled two-piece-dress with outer cylindrical body.
15. combined type rectifying columns according to claim 1, is characterized in that it being disassembled formation three-piece between described outer cylindrical body, intermediate casing, inner sleeve three.
16. combined type rectifying columns according to claim 1, it is characterized in that the sieve plate that described inner sleeve bottom is arranged is provided with sieve aperture, the size and number of sieve aperture is with such Program design: but can for steam up by, condensation reflux liquid descending by can not to make in distillation operation filler pass through.
17. combined type rectifying columns according to claim 1, is characterized in that the interior edge of described inner sleeve upper shed is for being connected in the mode sealing fit with other rectifier unit parts.
18. combined type rectifying columns according to claim 1, it is characterized in that, described outer cylindrical body, intermediate casing, three seals fit with inner sleeve, when carrying out distillation operation, the steam of rectifying is entered from the lower ending opening of described outer cylindrical body, in distillation process, the U-shaped pipe of intermediate casing is refluxed liquid fluid-tight, the through hole on steam up arrival intermediate casing top in outer cylindrical body and enter in intermediate casing, steam is descending along intermediate casing, the sieve plate being passed inner sleeve bottom because of U-shaped pipe by fluid-tight enters in inner sleeve, steam contacts to carry out rectification working process with the filler wherein loaded in inner sleeve, the upper shed of the up arrival inner sleeve of last steam and leave rectifying column, enter other rectifier unit parts.
19. 1 kinds of rectifier units, it is characterized in that, it comprises: combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and described combined type rectifying column is as described in any one of claim 1-18.
20. rectifier units according to claim 19, is characterized in that described rectifying bottle is connected in the mode sealing fit with the interface of described combined type rectifying column outer cylindrical body lower end.
21. rectifier units according to claim 19, is characterized in that one end of described condensing unit is connected in the mode sealing fit with the upper shed of described combined type rectifying column inner sleeve.
22. rectifier units according to claim 21, is characterized in that the other end of described condensing unit is connected in the mode sealing fit with returnable bottle.
23. rectifier units according to claim 19, is characterized in that described filler is filled in the inner sleeve of described combined type rectifying column.
24. rectifier units according to claim 19, is characterized in that the mode that described filler inclining is filled in the inner sleeve of described combined type rectifying column.
25. rectifier units according to claim 19, is characterized in that described condensing unit is condenser pipe, comprise serpentine condenser, spherical condensation tube, straight cold finger.
26. rectifier units according to claim 19, is characterized in that described filler is bead, molecular sieve and stainless steel ring/ball.
27. rectifier units according to claim 19, is characterized in that between described combined type rectifying column and condensing unit, and between described condensing unit and returnable bottle, connect independently of one another optionally through intermediate connector.
28. rectifier units according to claim 19, is characterized in that this rectifier unit comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connect their intermediate connector.
29. rectifier units according to claim 21, it is characterized in that this rectifier unit comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connect their intermediate connector, between the condensing unit other end and returnable bottle, use three-way pipe connects, and a mouth more than needed is connected with the external world, is connected with optional exhaust gas processing device, is connected and/or is connected with vacuum extractor with safety device.
30. rectifier units according to claim 19, it is characterized in that this rectifier unit comprises combined type rectifying column, rectifying bottle, condensing unit, returnable bottle and filler, and connecting their intermediate connector, described rectifying bottle uses heater to carry out the temperature heating to obtain required for distillation operation.
31. treat the method that rectifying material carries out rectifying, and the method comprises the following steps:
(1) provide and assemble combined type rectifying column as described in any one of claim 1-18, and/or providing or assemble rectifier unit described in claim 19, in inner sleeve wherein, adding filler;
(2) in rectifying bottle, rectifying material is treated in interpolation, and this rectifying bottle is connected with the interface of combined type rectifying column lower end;
(3) condensing unit is made to be connected optionally by intermediate connector with the inner sleeve upper shed of combined type rectifying column;
(4) condensing unit is connected optionally by intermediate connector with returnable bottle, and is connected with the external world optionally by intermediate connector, is connected with optional exhaust gas processing device, is connected with safety device and/or is connected with vacuum extractor;
(5) according to treating the physicochemical property of rectifying material and the physicochemical property of target product, heat to start distillation operation to rectifying bottle, optional startup exhaust gas processing device, safety device and/or vacuum extractor, obtain rectifying target product by returnable bottle.
CN201410611740.9A 2014-11-04 2014-11-04 Combined type rectifying column and application thereof Expired - Fee Related CN104353259B (en)

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CN110604938A (en) * 2018-12-18 2019-12-24 北矿检测技术有限公司 Spiral column plate column
CN109569003B (en) * 2018-12-31 2021-04-06 江西石华精细化工科技协同创新有限公司 Purification method of trimethylaluminum crude product
CN109569002B (en) * 2018-12-31 2021-06-22 江西石华精细化工科技协同创新有限公司 Method for large-scale purification of trimethylaluminum crude product
CN113912580B (en) * 2021-11-03 2023-06-02 瑞孚信江苏药业股份有限公司 Method for purifying 4- (hydroxymethyl) -5-methyl- [1,3] dioxol-2-one

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