CN111298468A - Multi-component multi-working-condition short-path flash separation device - Google Patents
Multi-component multi-working-condition short-path flash separation device Download PDFInfo
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- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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Abstract
The invention discloses a multi-component multi-working-condition short-path flash separation device, which is a multi-component multi-working-condition continuous short-path flash separation device formed by combining a plurality of non-wiped-film short-path flash separation devices in a series-parallel mode, is applied to the continuous short-path flash separation of multi-component liquid organic compounds, and is particularly suitable for the separation and purification of temperature-sensitive natural substances and the distillation and purification of high-boiling-point materials; the film-scraping-free short-distance flash evaporation device changes the vertical falling flow of the traditional material into the falling circumferential flow along a spiral line by arranging the internal thread groove, the material stroke can be increased by 20-30 times in the same vertical distance, the heat exchange time is greatly prolonged, the distillation efficiency is high, the components with high and low boiling points are thoroughly separated, the heat transfer efficiency is improved, and the height of the whole device can be obviously reduced under the same distillation amount; the linear distance between the outer surface of the built-in condenser and the heating surface of the liner is only 300-600mm, so that the low-boiling-point components in the material can be flash evaporated instantly, the evaporation and condensation of the material can be completed within a few seconds, and the heating time is short.
Description
Technical Field
The invention relates to the technical field of distillation, in particular to a multi-component multi-working-condition short-path flash evaporation separation device.
Background
The separation and purification of multi-component liquid organic compounds has been a difficult problem. In particular, oily extracts derived from natural plants have a plurality of chemical components or groups of components, and the effective components and ineffective components are mixed together, so that the use effect of the extracts is influenced. It is necessary to separate a plurality of chemical components or component groups one by one.
The common method for separating and purifying the multi-component liquid organic compound is a distillation technology, materials are heated to a certain temperature in a distiller by utilizing the boiling point difference of various chemical components, wherein the component with the lower boiling point is heated and then converted into a gas state from a liquid state, the gas state component enters a condensation recoverer and is converted into the liquid state again after being cooled to the temperature below the boiling point, and the component with the higher boiling point keeps the liquid state and is remained in the distiller, so that the separation of the components with the high boiling point and the low boiling point is realized.
The distillation method is a simple and effective method for separating liquid organic compounds with simple components. However, the separation and purification of multi-component liquid organic compounds, especially the separation and purification of temperature-sensitive natural substances and the distillation of high-boiling materials are troublesome. Under the working condition of continuous feeding, one distillation operation corresponds to one set of distillation operation parameters in principle, and only one component can be separated. The separation of multiple components generally requires repeated multiple operations using different distillation operating parameters, the process is discontinuous, the operations are relatively cumbersome, and the operating time is long.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The invention aims to provide a multi-component multi-working-condition short-range flash separation device, and aims to solve the problems that the separation and purification of the existing multi-component liquid organic compound need to be repeatedly operated for many times by using different distillation operation parameters, the process is discontinuous, the operation is complicated, and the operation time is long.
The technical scheme of the invention is as follows: a multi-component multi-working-condition short-path flash separation device comprises at least two stages of flash separation units connected in series, wherein each stage of flash separation unit comprises at least one non-wiped film short-path flash device; a residual liquid outlet of one wiped film-free short-distance flash distillation device in the previous-stage flash separation unit is connected with a material inlet to be distilled of one or more wiped film-free short-distance flash distillation devices in the next-stage flash separation unit, and a material inlet to be distilled of one wiped film-free short-distance flash distillation device in the next-stage flash separation unit is connected with a residual liquid outlet of one or more wiped film-free short-distance flash distillation devices in the previous-stage flash separation unit; and distilling the material to be distilled through a step-by-step flash separation unit to realize continuous short-path flash separation of the multi-component liquid organic compound.
The multi-component multi-working-condition short-path flash separation device comprises 2 stages of flash separation units, each stage of flash separation unit comprises a non-wiped film short-path flash device, and a raffinate outlet of the non-wiped film short-path flash device in the previous stage of flash separation unit is connected with a to-be-distilled material inlet of the non-wiped film short-path flash device in the next stage of flash separation unit; or the flash separation unit comprises 2 stages, the previous stage flash separation unit comprises two non-wiped film short-path flash evaporation devices, the next stage flash separation unit comprises a non-wiped film short-path flash evaporation device, and a raffinate outlet of any non-wiped film short-path flash evaporation device in the previous stage flash separation unit is connected with a material to be distilled of the non-wiped film short-path flash evaporation device in the next stage flash separation unit; or the flash separation unit comprises 2 stages, the previous stage flash separation unit comprises a non-wiped film short-path flash evaporation device, the next stage flash separation unit comprises two non-wiped film short-path flash evaporation devices, and a raffinate outlet of the non-wiped film short-path flash evaporation device in the previous stage flash separation unit is respectively connected with a material inlet to be distilled of any non-wiped film short-path flash evaporation device in the next stage flash separation unit.
The multi-component multi-working-condition short-path flash separation device, wherein the non-wiped film short-path flash separation device comprises:
the heat transfer interlayer is used for supporting the whole structure, and a heat medium flows in the heat transfer interlayer;
the inner container is designed into a closed structure; the outer surface of the heat transfer interlayer is in contact with the inner surface of the heat transfer interlayer for heat exchange; an internal thread groove is arranged from top to bottom on the inner surface surrounding the inner container, the internal thread groove is distributed around the inner surface of the inner container and extends downwards in a spiral mode until reaching the bottom of the inner surface of the inner container, and the internal thread groove is used for converting vertical downward movement of materials into circular downward flow of a spiral line and prolonging heat exchange time;
the internal condenser is used for condensing the vaporized distillate in the inner container into liquid; cooling liquid is introduced into the interior;
the heat medium continuously circulates in the heat transfer interlayer; the material to be distilled enters the liner and flows downwards along the inner thread groove in a spiral line circumference from top to bottom, heat exchange is realized between the heat transfer of the liner and the heat transfer interlayer and a heat medium in the process that the material to be distilled flows along the inner thread groove, so that the component with lower boiling point in the material to be distilled is heated and then converted from liquid state to gaseous state, the component with higher boiling point continuously keeps the liquid state and flows downwards along the inner thread groove, and finally the component is discharged out of the liner; the gasified components are contacted with the outer surface of the inner condenser and then condensed into liquid again to be discharged.
The multi-component multi-working-condition short-path flash separation device is characterized in that the internal condenser is arranged in the inner container.
The multi-component multi-working-condition short-path flash evaporation separation device further comprises a vacuumizing port for vacuumizing the inner container, and the vacuumizing port is externally connected with vacuumizing equipment.
The multi-component multi-working-condition short-path flash evaporation separation device is characterized in that a nozzle used for spraying a material to be distilled onto the circumferential surface of the inner container in a high-speed tangential mode is arranged in the inner container, so that the material to be distilled forms a thin liquid layer on the surface of the inner thread groove.
The multi-component multi-working-condition short-path flash separation device further comprises a receiver used for collecting materials which are gasified and then contacted with the outer surface of the internal condenser to be condensed into liquid again, and the receiver is arranged in the inner container and is positioned right below the internal condenser.
The multi-component multi-working-condition short-path flash evaporation separation device is characterized in that the inner container is made of stainless steel plates, and the thickness of the inner container wall is 4-6 mm; the inner surface of the inner container is provided with a downward screwed internal thread groove (3).
The multi-component multi-working-condition short-path flash evaporation separation device is characterized in that the linear distance between the outer surface of the inner condenser and the inner surface of the inner container is 300-600 mm.
The multi-component multi-working-condition short-path flash evaporation separation device is characterized in that the inner condenser is made of stainless steel plates, the diameter of the inner condenser is 300mm-1000mm, and the thickness of the inner condenser is 1 mm-2 mm.
The invention has the beneficial effects that: the invention provides a multi-component multi-working-condition short-path flash separation device, which is a multi-component multi-working-condition continuous short-path flash separation device formed by combining a plurality of non-wiped-film short-path flash separation devices in a series-parallel mode, is applied to the continuous short-path flash separation of multi-component liquid organic compounds, and is particularly suitable for separation and purification of temperature-sensitive natural substances and distillation and purification of high-boiling-point materials; the wiped film-free short-distance flash evaporation device changes the vertical falling flow of the material to be distilled in the traditional falling film distiller/wiped film distiller into circular flow descending along a spiral line by arranging the internal thread groove, the material stroke can be increased by 20-30 times in the same vertical distance, the heat exchange time is greatly prolonged, the distillation efficiency is high, the separation of high and low boiling point components is thorough, the heat transfer efficiency is improved, the design height of the whole device can be obviously reduced under the condition of the same distillation amount, and the volume is smaller and more compact; the condenser is arranged in the inner container, the linear distance between the outer surface of the condenser and the heating surface of the inner container is only 300-600mm, the low-boiling-point components in the materials to be distilled can be flash evaporated instantly, the evaporation and condensation processes of the materials are completed within a few seconds, and the heating time is short.
Drawings
FIG. 1 is a schematic diagram of a multi-component, multi-regime, short-path flash separation apparatus of example A1 of the present invention.
FIG. 2 is a schematic structural diagram of a multi-component multi-operating-condition short-path flash separation device adopting a 2+1 combination in example A2 of the invention.
FIG. 3 is a schematic diagram of a 1+2 combination configuration of a multi-component, multi-regime, short-path flash separation apparatus according to example A3 of the present invention.
Fig. 4 is a schematic diagram of the structure of a single knifiess short-path flash apparatus of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; may be mechanically connected, may be electrically connected or may be in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
As shown in fig. 1, a multi-component multi-working-condition short-path flash separation device is applied to continuous short-path flash separation of multi-component liquid organic compounds, and is particularly suitable for separation and purification of temperature-sensitive natural substances and distillation and purification of high-boiling-point materials; the system comprises at least two stages of flash separation units connected in series, wherein each stage of flash separation unit comprises at least one knifing-free short-path flash evaporation device; a residual liquid outlet of one wiped film-free short-distance flash distillation device in the previous-stage flash separation unit is connected with a material inlet to be distilled of one or more wiped film-free short-distance flash distillation devices in the next-stage flash separation unit, and a material inlet to be distilled of one wiped film-free short-distance flash distillation device in the next-stage flash separation unit is connected with a residual liquid outlet of one or more wiped film-free short-distance flash distillation devices in the previous-stage flash separation unit; and distilling the material to be distilled through a step-by-step flash separation unit to realize continuous short-path flash separation of the multi-component liquid organic compound.
The number of the non-wiped film short-path flash devices included in each stage of flash separation unit is set according to actual needs, and the connection relationship between the non-wiped film short-path flash devices between two adjacent stages is set according to actual needs, and the following examples are listed for explanation:
example A1
As shown in figure 1, the two-stage flash separation unit series combination scheme is provided, each stage of flash separation unit comprises a non-wiped film short-path flash unit device, and the flash separation unit is suitable for flash separation of liquid organic compounds with large boiling point difference and small content difference of each component.
In fig. 1, the upper and lower knifing-free short-path flash evaporation devices respectively adopt different distillation process parameters, so that the aim of continuously distilling and separating multiple components can be fulfilled.
Assuming that liquid organic compounds comprising three different components are required to be separated by distillation, the material to be distilled is fed through a material inlet a1-1 of a knifiess short-path flash device A1, and flash distillation is carried out by controlling certain process operation parameters (temperature, flow, vacuum degree and the like). Discharging the component with the lowest boiling point in the distillate from a distillate outlet b 1-1; the other components having higher boiling points flow out from the raffinate outlet c 1-1. The other components with higher boiling points which flow out of the non-wiped film short-path flash device A1 are sent to the material to be distilled inlet a2-1 of the non-wiped film short-path flash device A2 through a connecting pipe j1 which is connected with a raffinate outlet c1 and the material to be distilled inlet a2-1 of the non-wiped film short-path flash device A2. The wiped film-free short path flash unit a2 was controlled to flash using another set of process operating parameters (temperature, flow, vacuum, etc.). Discharging the low-boiling-point components in the material to be distilled from a distillate outlet b 2-1; the higher boiling components flow out of the raffinate outlet c 2-1. The three different components are separated one by one in a continuous process.
By analogy, n knifing-free short-path flash evaporation devices are combined in series and different process parameters are set theoretically, so that n +1 components can be separated.
Example A2
As shown in fig. 2, the two-stage flash separation unit and/or series combination scheme is provided, the first-stage flash separation unit comprises two non-wiped film short-path flash evaporation devices connected in parallel, and the second-stage flash separation unit comprises a non-wiped film short-path flash evaporation device, and is suitable for flash separation of liquid organic compounds with large boiling point difference and large content difference of each component.
In this embodiment, based on the conditions of a large proportion of low-boiling point components and a small proportion of high-boiling point components in the distillate, a combination of a "2 + 1" mode is used, so that the flow balance is conveniently realized. In the parallel-series combination of the three units shown in FIG. 2, two non-wiped film short-distance flash evaporation devices in the first-stage flash evaporation separation unit adopt the same distillation process parameters and work in parallel, and the working condition that the ratio of low-boiling-point components in the material to be distilled is large is responded by large flow; one non-wiped film short-path flash device in the second-stage flash separation unit is respectively connected with two non-wiped film short-path flash devices in the previous-stage flash separation unit in series, distillation process parameters different from those of the previous-stage flash separation unit are adopted, and the working condition that the high-boiling-point component ratio in the material to be distilled is small is met by using small flow. The aim of separating multiple components by continuous distillation can be achieved.
It is assumed that what needs to be separated by distillation is a liquid organic compound comprising three different components, the lowest boiling component content of which is particularly large. Materials to be distilled are respectively sent into a distiller through a material to be distilled inlet a1-2 of a non-wiped film short-distance flash device B1 and a material to be distilled inlet a2-2 of a non-wiped film short-distance flash device B2 in a first-stage flash separation unit, and the non-wiped film short-distance flash device B1 and the non-wiped film short-distance flash device B2 are controlled to carry out flash evaporation by adopting the same technological operation parameters (temperature, flow, vacuum degree and the like). Discharging the components with the lowest boiling point in the distillate from the distillate outlets b1-2 and b 2-2; other components with higher boiling points flow out of the raffinate outlets c1-2 and c 2-2. Through a connecting pipe j2, other components with higher boiling points flowing out of the non-wiped film short-path flash device B1 and the non-wiped film short-path flash device B2 are combined and then sent to a material to be distilled a3-2 of the non-wiped film short-path flash device B3, and the non-wiped film short-path flash device B3 is controlled to carry out flash evaporation by using another group of process operation parameters (temperature, flow, vacuum degree and the like). Discharging the low-boiling-point components in the material to be distilled from a distillate outlet b 3-2; the higher boiling components flow out of the raffinate outlet c-2. The three different components are separated one by one in a continuous process.
Example A3
As shown in fig. 3, a two-stage flash separation unit series/parallel combination scheme is adopted, the first-stage flash separation unit comprises a non-wiped film short-path flash evaporation device, and the second-stage flash separation unit comprises two non-wiped film short-path flash evaporation devices connected in parallel, and is suitable for flash separation of liquid organic compounds with large boiling point difference and large content difference of each component.
In this embodiment, based on the conditions of a small proportion of low-boiling point components and a large proportion of high-boiling point components in the distillate, a combination of "1 + 2" modes is used, so that the flow balance is conveniently realized. In the combination of three units in series and parallel, a non-knifing short-distance flash evaporation device in the first-stage flash evaporation separation unit adopts a distillation process parameter and corresponds to the working condition that the ratio of low-boiling point components in the material to be distilled is small by using small flow; two non-wiped film short-distance flash devices in the second-stage flash separation unit are respectively connected in series with one non-wiped film short-distance flash device in the previous-stage flash separation unit, and the two non-wiped film short-distance flash devices in the second-stage flash separation unit work in parallel, so that the working condition that the high-boiling-point component content in the material to be distilled is large is met by large flow. The aim of separating multiple components by continuous distillation can be achieved.
It is assumed that what needs to be separated by distillation is a liquid organic compound comprising three different components, of which the content of the high boiling component (i.e. the other two components having a higher boiling point than the lowest boiling component) is particularly large.
And (3) respectively feeding the material to be distilled into a distiller through a material inlet a1-3 of a first wiped film-free short-path flash device C1 in the first-stage flash separation unit, and controlling the first wiped film-free short-path flash device C1 to carry out flash evaporation by adopting process operation parameters (temperature, flow, vacuum degree and the like). Discharging the component with the lowest boiling point in the distillate from a distillate outlet b 1-3; the other components with higher boiling points flow out of the raffinate outlet c 1-3. Through a connecting pipe j3, other components with higher boiling points flowing out of the first wiped film-free short-path flash device C1 are shunted to a material to be distilled a2-3 of a second wiped film-free short-path flash device C2 and a material to be distilled a3-3 of a third wiped film-free short-path flash device C3 in the second-stage flash separation unit, and the second wiped film-free short-path flash device C2 and the third wiped film-free short-path flash device C3 are controlled to carry out flash evaporation by using another set of process operation parameters (temperature, flow, vacuum degree and the like). Discharging the low-boiling-point components in the distillate from the distillate outlets b2-3 and b 3-3; the higher boiling components flow out of the raffinate outlets c2-3, c 3-3. The three different components are separated one by one in a continuous process.
As shown in fig. 4, the wiped film-free short-path flash evaporation device comprises:
the heat transfer interlayer 1 is used for supporting the whole structure, and a heat medium circulates in the heat transfer interlayer 1;
the inner container 2 is designed into a closed structure; the outer surface of the heat transfer interlayer 1 is in contact with the inner surface of the heat transfer interlayer 1 for heat exchange; an internal thread groove 3 is arranged from top to bottom on the inner surface surrounding the inner container 2;
an internal condenser 4 for condensing the vaporized distillate in the inner container 2 into a liquid; cooling liquid is introduced into the interior;
the heat medium continuously circulates in the heat transfer interlayer 1; the material to be distilled enters the liner 2, flows downwards along the inner thread groove 3 in a spiral line circumference from top to bottom, and exchanges heat with a heat medium through heat transfer of the liner 2 and the heat transfer interlayer 1 in the process that the material to be distilled flows along the inner thread groove 3, so that the component with lower boiling point in the material to be distilled is heated and then converted from liquid state to gas state, the component with higher boiling point continuously keeps the liquid state and flows downwards along the inner thread groove 3, and finally is discharged out of the liner 2; the gasified components are condensed into liquid again and discharged after contacting with the outer surface of the inner condenser 4.
This technical scheme is through setting up internal thread groove 3, change the vertical whereabouts of waiting to distill the material in traditional falling film distiller/wiped film distiller and flow into along the circumference that the helix descends, material stroke in same vertical distance can increase 20-30 times, prolong heat transfer time by a wide margin, distillation efficiency is high, the separation of high low boiling point component is more thorough, heat transfer efficiency improves, under the condition of same distillation volume, whole no wiped film short distance flash distillation plant's design height can obviously reduce, the volume can be done littleer, compacter.
As a preferred embodiment, the internal thread groove 3 is directly engraved on the inner surface of the inner container 2. Preferably, the female thread groove 3 has a depth of 2.5mm and a vertical width of 50mm, and extends downward along the spiral line. In the technical scheme, the internal thread groove 3 is used for converting the vertical downward movement of the material to be distilled in the traditional falling film distiller along the surface of the heating wall into the spiral circular movement, so that the stroke of the material to be distilled can be greatly prolonged. Taking an inner container with the diameter of 1000mm as an example, 10 circles of internal thread grooves 3 can be engraved in the vertical height of 1m, the circumference of each circle is 3.14m, and the total length of 10 circles is 31.4 m. After the material to be steamed originally vertically moves down for 1m along the smooth surface and flows along the internal thread groove 3, the rectification stroke is changed into 31.4m within the vertical distance of 1m, and the stroke is prolonged by more than 30 times. Obviously, after the stroke is prolonged, the heat transfer time can be greatly increased, the heat transfer efficiency is improved, the materials to be distilled are fully heated, and the low-boiling-point components can be basically gasified and cleaned in the stroke. Therefore, under the condition of the same distillation amount, the design height of the knifing-free short-path flash evaporation device can be obviously reduced, and the manufacture, the transportation and the installation are facilitated.
In a preferred embodiment, the inner container 2 is made of stainless steel plate, the thickness of the side wall is 4 mm-6 mm, and the inner surface is a heating surface. The inner thread groove 3 can be carved on the inner surface of the inner container 2 by adopting the stainless steel plate with the thickness of 4 mm-6 mm, and meanwhile, the thicker steel plate can be used as a heat storage carrier by preheating through the heat transfer interlayer 1, so that the temperature fluctuation caused by the fact that materials to be distilled enter the non-film-scraping short-distance flash evaporation device is reduced.
As a preferred embodiment, said internal condenser 4 is arranged inside the internal bladder 2. When in operation, the inside of the internal condenser 4 is continuously introduced with cooling liquid through an inlet and outlet pipeline to form a low-temperature outer wall. The linear distance between the outer surface of the inner condenser 4 and the heating surface of the inner container 2 (namely the inner surface of the inner container 2) is only 300mm-600mm, the distance between low boiling point components in the material to be distilled from gasification to condensation is 300mm-600mm, the heating time is short, and the flash evaporation effect is achieved. In addition, the size of the whole set of the wiped film-free short-distance flash evaporation device can be reduced by the nested integrated design of the evaporator and the condenser, the whole complete equipment is convenient to leave a factory, and transportation and field installation are facilitated.
As a preferred embodiment, the internal condenser 4 is made of stainless steel plate material, the diameter is 300mm-1000mm, and the thickness is 1 mm-2 mm.
As a preferred embodiment, a condenser inlet g is provided at the top of the inner condenser 4, and a condenser outlet f is provided at the bottom of the inner condenser 4; the cooling liquid is passed into the internal condenser 4 at the condenser inlet g and flows out of the internal condenser 4 at the condenser outlet f.
As a preferred embodiment, the heat transfer interlayer 1 is disposed between the outer wall and the inner wall of the housing 11; the shell 11 is made of stainless steel materials and is in the shape of a cylindrical cone bottom and a flat top, the inner diameter of the cylindrical section is 600 mm-1500 mm, and the thickness of the outer wall is 4mm-8 mm. Hot water or heat conducting oil without pressure can be used as a heating source in the heat transfer interlayer 1, the designed working temperature is 60-250 ℃, and the designed working pressure is less than or equal to 0.8 MPa. The heat transfer interlayer 1 can also use steam with the pressure of less than or equal to 0.6MPa as a heat source after being designed by a pressure container, and the temperature design range is 100-165 ℃.
An interlayer inlet d is formed in the top of the shell 11, and an interlayer outlet e is formed in the bottom of the shell 11; the heat medium flows into the heat transfer interlayer 1 from the interlayer inlet d and flows out of the heat transfer interlayer 1 from the interlayer outlet e.
In order to conveniently discharge the materials which are condensed into liquid again, the scrapless short-distance flash evaporation device also comprises a receiver 5 which is used for collecting the materials which are condensed into liquid again after being gasified and contacted with the outer surface of the inner condenser 4, and the receiver 5 is arranged in the inner container 2 and is positioned right below the inner condenser 4.
In a preferred embodiment, the receiver 5 is designed in a funnel shape, is made of stainless steel plate, has a thickness of 2mm, and is used for preventing the condensed low-boiling-point distilled component and the unvaporized high-boiling-point component from being mixed together, and separately collecting and outputting the low-boiling-point distilled component.
As a preferred embodiment, a distillate outlet b is provided at the bottom of the receiver 5, through which the low-boiling components are discharged.
In order to conveniently convey the material to be distilled into the inner container 2, an inlet a which penetrates through the side wall of the shell 11 and the side wall of the inner container 2 simultaneously is arranged, a nozzle 6 is arranged at the inlet a of the material to be distilled, the nozzle 6 is arranged in the inner container 2 and conveys the material to be distilled through a pipeline, the nozzle 6 sprays the material to be distilled into the circumferential surface of the inner container 2 in a high-speed tangential mode, so that the material to be distilled forms a thin liquid layer on the surface of the internal thread groove 3, the material to be distilled which vertically moves downwards is changed into circular flow which descends along a spiral line, and the material is in contact with the internal thread groove 3 of the heating surface of the inner container 2 for heat exchange, and the distillation stroke of.
As a preferred embodiment, a residual liquid outlet c which penetrates through the bottom of the shell 11 and the bottom of the inner container 2 simultaneously is arranged at the bottom of the shell 11, the distillate is sprayed into the inner container 2 from the nozzle 6, and the residual liquid after the distillation treatment is discharged through the residual liquid outlet c.
As a preferred embodiment, a vacuum-pumping port h is arranged on a pipeline connected with the distilled liquid outlet b, and the vacuum-pumping port h is externally connected with a vacuum-pumping device. The vacuum-pumping equipment vacuumizes the inner container 2 through the vacuum-pumping port h to realize reduced-pressure distillation operation, so that the knifing-free short-distance flash evaporation device is suitable for distillation of high-boiling-point materials.
The working principle of the knifing-free short-distance flash evaporation device is as follows:
1. the heat-conducting medium with the required temperature is continuously sent into the heat-conducting interlayer 1, and the inner wall of the inner container 2 reaches the set working temperature after a plurality of times. The inner wall temperature of the inner container 2 can be kept constant by adjusting the flow velocity of the heat-conducting medium.
2. If the distillation is carried out under reduced pressure, the air in the inner container 2 is removed through the vacuum-pumping port h, so that the inside of the device is in a vacuum state.
3. Cooling water is continuously introduced into the internal condenser 4.
4. Starting a metering pump which is additionally and cooperatively installed, feeding materials into the inner container 2 through the first material inlet a1 and the second material inlet a2 to be distilled, wherein the distillation quantity can be adjusted through flow speed and flow rate and is determined according to the physical properties of the materials to be distilled.
5. The material to be distilled enters the surface of the internal thread groove 3 which has been preheated through the nozzle 6 and moves downwards along the circumferential spiral. The material is heated during its downward travel, the low-boiling components of which are vaporized into a gaseous state and the high-boiling components, which are still in a liquid state, are separated.
6. The gaseous low-boiling point component contacts with the low-temperature outer wall of the internal condenser 4, is converted into liquid again, moves downwards along the low-temperature outer wall of the internal condenser 4 by gravity, enters the receiver 5, passes through the evaporated liquid outlet b and is output to another matched storage tank.
7. The high boiling point components still in liquid state are downward along the inner wall of the inner container 2 and finally are output to another matched storage tank through a residual liquid outlet c.
8. The film-scraping-free short-distance flash evaporation device can continuously and stably operate for a long time.
9. And (5) closing the heating, cooling, material conveying pump and vacuum pump, and finishing an operation period.
The short-path flash evaporation device without a scratch film described above is illustrated by the following examples:
the multi-component multi-working-condition short-path flash separation device is illustrated by the following examples:
example 1
The main engineering dimensions of the base unit of the wiped film-free short-path flash apparatus used in this example were: the outer diameter of the heat transfer interlayer 1 is 1200mm, and the height of the heat transfer interlayer is 3250 mm; the outer diameter of the inner container 2 is 1000mm, the wall thickness is 4mm, and the height is 2800 mm; the depth of the internal thread groove 3 is 2.5mm, the vertical width is 50mm, and the internal thread groove extends downwards along the spiral line; the total height of the inner wall carved with the internal thread groove 3 in the inner container 2 is 2200mm, 22 circles of internal thread grooves 3 are carved, the circumference of each circle of internal thread groove 3 is 3.14m, and the total length of 22 circles of internal thread grooves 3 is about 69 m; the diameter of the internal condenser 4 is 500mm, and the linear distance between the heating surface of the inner container 2 and the outer wall of the internal condenser 4 is 250 mm.
The material to be distilled is industrial crude turpentine produced in mountainous areas in Yuexi, the measured density is 0.868g/L, and the main components comprise 2.2 percent of low-boiling-point front fraction, 76.4 percent of α -pinene, 8.5 percent of β -pinene and 12.9 percent of the rest high-boiling-point components through gas chromatography detection.
This example employs the "2 + 1" parallel-series combination scheme of fig. 2.
The distillation operation adopts a working mode of continuous reduced pressure distillation, and aims to separate light and heavy components in the crude turpentine, the distillate is mainly collected α -pinene (containing part β -pinene) and longifolene (containing components with similar boiling points), and the distillation residue is tar.
1. Weigh 10 tons (approximately 11.5 m)3) Industrial crude turpentine is put into a storage tank for standby.
2. The heat conduction oil is used as a heat source, and the working temperature of the heat conduction oil furnace is set to be 200 ℃. And starting the device, and continuously feeding the heat transfer oil into the heat transfer interlayer 1 of the non-wiped film short-path flash evaporation device B1 and the non-wiped film short-path flash evaporation device B2. The inner wall temperature of the inner container 2 in the non-wiped film short-path flash device B1 and the non-wiped film short-path flash device B2 after 38 minutes and 42 minutes respectively reaches the set 80 ℃. The temperature is automatically adjusted by an automatic temperature control system to keep the temperature of the inner wall constant.
3. The vacuum pump is started. The pressure in the system is reduced to below 1000 Pa.
4. The two internal condensers 4 are each continuously charged with circulating cooling water at 23 ℃.
5. And starting the metering pump which is additionally and cooperatively installed, and setting the total flow rate to be 20L/min. Turpentine is respectively sent to a non-knifing short-path flash evaporation device B1 and a non-knifing short-path flash evaporation device B2 through a material inlet a1-2 and a2-2 to be distilled, and the flow rate of each path is set to be 10L/min.
6. The material to be distilled enters the internal thread groove 3 which is preheated to 80 ℃ through the nozzle 6 and moves downwards along the circumference, α -pinene with relatively low boiling point (containing part β -pinene) is output from the distillate outlets b1-2 and b2-2, other components with relatively high boiling point flow out from c1-2 and c2-2, and first-stage separation of low-boiling-point components and high-boiling-point components is realized.
7. Other components with higher boiling points which flow out of the non-wiped film short-path flash device B1 and the non-wiped film short-path flash device B2 are combined and then are sent to a to-be-steamed liquid inlet a3-2 of the non-wiped film short-path flash device B3 through a communicating pipe f 2. And heating the inner wall of the heat transfer interlayer 1 to 160 ℃ by a scratch-free short-path flash evaporation device B3 for flash evaporation. Taking out longifolene components (containing other components with similar boiling points) with low boiling points from the distilled liquid outlet b 3-2; the higher boiling tar component exits at raffinate outlet c 3-2. The three components are separated one by one in a continuous process.
8. Each flash evaporation unit stably operates in the distillation process. About 11 hours and 20 minutes, the distillation of the material was completed.
9. And (5) closing the material conveying pump, the heating furnace, the vacuum pump and the circulating cooling water, and finishing the operation.
The experimental data shows that 8.15t of α -pinene (containing low-boiling-point forecut and part of β -pinene) is obtained, the yield calculated by crude turpentine is 81.5%, 0.96t of longifolene component (containing close boiling-point component) is 9.6%, the yield calculated by crude turpentine is 7.5%, the loss is 0.14t, the total loss of materials is 1.4%, and the low-boiling-point distillate mainly comprises 1.7% of low-boiling-point forecut, 86.9% of α -pinene, 7.5% of β -pinene and 3.9% of the rest high-boiling-point components.
Example 2
The main engineering dimensions of the base unit of the wiped film-free short-path flash apparatus used in this example were: the outer diameter of the heat transfer interlayer 1 is 800mm, and the height of the heat transfer interlayer is 2500 mm; the outer diameter of the inner container 2 is 650mm, the wall thickness is 4mm, and the height is 2000 mm; the depth of the internal thread groove 3 is 2.5mm, the vertical width is 50mm, and the internal thread groove extends downwards along the spiral line; the total height of the inner wall carved with the internal thread groove 3 in the inner container 2 is 1600mm, 16 circles of internal thread grooves 3 are carved, the circumference of each circle of internal thread groove 3 is 2m, and the total length of 16 circles of internal thread grooves 3 is about 32 m; the diameter of the internal condenser 4 is 250mm, and the linear distance between the heating surface of the inner container 2 and the outer wall of the internal condenser 4 is 200 mm.
The material to be distilled is industrial crude cinnamon oil produced in mountainous areas in Yuexi, is light yellow oily liquid and has strong cinnamon smell. The density was 1.070 g/L. The main component of cinnamaldehyde (C) is detected by gas chromatography9H8O) content 62.4%.
This example employs the "1 + 1" series combination scheme of FIG. 1.
Distilling by continuous vacuum distillation to separate light and heavy components from the crude oleum Cinnamomi, and distilling to obtain cinnamaldehyde (C)9H8O) refined cinnamon oil with a content of more than 75%.
Distillation operation
1. 500 kg (467L) of industrial crude cinnamon oil is weighed and put into a storage tank for standby.
2. The heat conduction oil is used as a heat source, and the working temperature of the heat conduction oil furnace is set to be 160 ℃. Starting the device, and continuously feeding the heat transfer oil into a heat transfer interlayer 1 of a non-wiped film short-distance flash evaporation device A1. After 23 minutes, the temperature of the inner wall of the inner container 2 reaches the set 70 ℃. The temperature is automatically adjusted by an automatic temperature control system to keep the temperature of the inner wall constant.
3. The vacuum pump is started. The pressure in the system is reduced to below 100 Pa.
4. The circulating cooling water at 23 ℃ is continuously introduced into the internal condenser 4.
5. Starting a metering pump which is additionally and cooperatively installed, and feeding the cinnamon oil into a distillation device through a material inlet a1-1 of a non-wiped film short-distance flash evaporation device A1, wherein the flow rate is set to be 3L/min.
6. The material enters the internal thread groove of the scrapless short-path flash apparatus a1, which has been preheated to 70 ℃, through the nozzle 6 and spirally moves downward along the circumference. After about 3 minutes, a distillate fraction (front cut) was discharged from the distillate outlet b1-1 to another holding tank. After about 5 minutes, the distillate (containing cinnamaldehyde and high boiling components) was discharged from the raffinate outlet c 1-1. The first-stage separation of the low-boiling point component and the high-boiling point component is realized.
7. Other components with higher boiling points which flow out of the non-wiped film short-path flash device A1 are sent to a liquid inlet a2-1 of the non-wiped film short-path flash device A2 through a communicating pipe f 1. The flash evaporation is carried out by controlling the temperature of the inner wall of the heat transfer interlayer 1 of the scratchproof short-path flash evaporation device A2 to be 110 ℃. Taking out cinnamyl aldehyde (containing other components with similar boiling points) with low boiling point in the distillate from a distillate outlet b 2-1; the other components having higher boiling points flow out from the raffinate outlet c 2-1. The three components are separated one by one in a continuous process.
8. About 3 hours and 05 minutes, the distillation was complete and the high-boiling fraction was separated off. The working temperature and the feeding flow rate in the distillation process are stable. The exit temperature of the circulating coolant from condenser outlet f1 was 52 ℃, and the inlet temperature of the coolant entering internal condenser 4 from condenser inlet g2 was maintained below 29 ℃. The multi-component multi-working-condition short-path flash separation device can stably operate.
9. And (5) closing the material conveying pump, the heating furnace, the vacuum pump and the circulating cooling water, and finishing the operation.
The experimental results are as follows: 34kg of the distillate before distillation was obtained, and the yield based on the crude cinnamon oil was 6.8%. 406 kg of cinnamaldehyde was distilled off, and the yield based on the crude cinnamon oil was 81.2%. 53.5 kg of a residue was distilled, and the yield based on the crude cinnamon oil was 10.7%. The material loss was 6.5 kg.
Detecting by gas chromatography to obtain target distillate cinnamaldehyde (C)9H8The content of O) is 76.1 percent, which is 13.7 percent higher than the content of the crude product before distillation which is 62.4 percent, and the product meets the requirement of quality standard. The distillation separation effect is good.
Compared with the prior art, the multi-component multi-working-condition short-path flash separation device has the following advantages:
(1) the multi-component multi-working-condition short-path flash evaporation separation device integrates the advantages of a falling film distiller and a molecular distiller, cancels a whole set of film scraping devices such as a stirring motor, a rotating shaft, a wall scraping paddle and the like, changes the movement of the traditional vertically falling material to be distilled into circular flow descending along a spiral line through the internal thread groove 3, can greatly increase the material stroke in the same vertical distance, prolongs the heat exchange time, has high distillation efficiency and more thoroughly separates high and low boiling point components; the built-in design of the internal condenser ensures that the space distance from the heating surface to the condensing surface is very short, and the processes of instant flash evaporation, material evaporation and condensation can be completed within a few seconds; is especially suitable for the separation and purification of natural substances sensitive to temperature and the distillation of high-boiling-point materials.
(2) Different series-parallel combination modes can be adopted according to actual needs, and different rectification needs are met.
In the description herein, references to the description of the terms "one embodiment," "certain embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Reference numerals
A wiped film-free short-path flash apparatus a 1; a wiped film-free short-path flash apparatus a 2; a wiped film-free short-path flash unit B1; a wiped film-free short-path flash unit B2; a wiped film-free short-path flash unit B3; a material to be distilled inlet a 1-1; a distillate outlet b 1-1; a raffinate outlet c 1-1; a material to be distilled inlet a 2-1; a distillate outlet b 2-1; a raffinate outlet c 2-1; a material to be distilled inlet a 1-2; a distillate outlet b 1-2; a raffinate outlet c 1-2; a material to be distilled inlet a 2-2; a distillate outlet b 2-2; a raffinate outlet c 2-2; a material to be distilled inlet a 3-2; a distillate outlet b 3-2; a raffinate outlet c 3-2; a material to be distilled inlet a 1-3; a distillate outlet b 1-3; a raffinate outlet c 1-3; a material to be distilled inlet a 2-3; a distillate outlet b 2-3; a raffinate outlet c 2-3; a material to be distilled inlet a 3-3; a distillate outlet b 3-3; a raffinate outlet c 3-3; a heat transfer interlayer 1; a housing 11; an inner container 2; an internal thread groove 3; an internal condenser 4; a receiver 5; a nozzle 6; a material to be distilled inlet a; a distillate outlet b; a raffinate outlet c; an interlayer inlet d; an interlayer outlet e; a condenser outlet f; condenser inlet g; and (4) vacuumizing a port h.
Claims (10)
1. A multi-component multi-working-condition short-path flash separation device is characterized by comprising at least two stages of flash separation units connected in series, wherein each stage of flash separation unit comprises at least one non-wiped film short-path flash device; a residual liquid outlet of one wiped film-free short-distance flash distillation device in the previous-stage flash separation unit is connected with a material inlet to be distilled of one or more wiped film-free short-distance flash distillation devices in the next-stage flash separation unit, and a material inlet to be distilled of one wiped film-free short-distance flash distillation device in the next-stage flash separation unit is connected with a residual liquid outlet of one or more wiped film-free short-distance flash distillation devices in the previous-stage flash separation unit; and distilling the material to be distilled through a step-by-step flash separation unit to realize continuous short-path flash separation of the multi-component liquid organic compound.
2. The multi-component multi-working-condition short-path flash separation device according to claim 1, wherein the flash separation unit comprises 2 stages, each stage of flash separation unit comprises a non-wiped film short-path flash device, and a raffinate outlet of the non-wiped film short-path flash device in the previous stage of flash separation unit is connected with a material to be distilled inlet of the non-wiped film short-path flash device in the next stage of flash separation unit; or the flash separation unit comprises 2 stages, the previous stage flash separation unit comprises two non-wiped film short-path flash evaporation devices, the next stage flash separation unit comprises a non-wiped film short-path flash evaporation device, and a raffinate outlet of any non-wiped film short-path flash evaporation device in the previous stage flash separation unit is connected with a material to be distilled of the non-wiped film short-path flash evaporation device in the next stage flash separation unit; or the flash separation unit comprises 2 stages, the previous stage flash separation unit comprises a non-wiped film short-path flash evaporation device, the next stage flash separation unit comprises two non-wiped film short-path flash evaporation devices, and a raffinate outlet of the non-wiped film short-path flash evaporation device in the previous stage flash separation unit is respectively connected with a material inlet to be distilled of any non-wiped film short-path flash evaporation device in the next stage flash separation unit.
3. The multi-component, multi-regime short-path flash separation device of any one of claims 1 or 2, wherein the scrapless short-path flash separation device comprises:
the heat transfer interlayer (1) is used for supporting the whole structure, and a heat medium circulates in the heat transfer interlayer (1);
the inner container (2) is designed into a closed structure; the outer surface of the heat transfer interlayer (1) is in contact with the inner surface of the heat transfer interlayer (1) for heat exchange; an internal thread groove (3) is arranged from top to bottom around the inner surface of the inner container (2), and the internal thread groove (3) is distributed around the inner surface of the inner container (2) and extends downwards in a spiral mode until reaching the bottom of the inner surface of the inner container (2);
an internal condenser (4) for condensing the vaporized distillate in the inner container (2) into a liquid; cooling liquid is introduced into the interior;
the heat medium continuously circulates in the heat transfer interlayer (1); the material to be distilled enters the inner container (2), flows downwards along the inner thread groove (3) in a spiral line shape from top to bottom, and exchanges heat with a heat medium through heat transfer of the inner container (2) and the heat transfer interlayer (1) in the process that the material to be distilled flows along the inner thread groove (3), so that the component with lower boiling point in the material to be distilled is heated and then converted into gas state from liquid state, the component with higher boiling point continuously keeps the liquid state and flows downwards along the inner thread groove (3), and finally the component is discharged out of the inner container; the gasified components are contacted with the outer surface of the inner condenser (4), and then condensed into liquid again to be discharged.
4. A multi-component multi-condition short-path flash separation device according to claim 3, characterized in that the internal condenser (4) is arranged in the inner container (2).
5. A multi-component multi-working-condition short-path flash separation device according to claim 3, further comprising a vacuum port (h) for performing vacuum treatment in the inner container (2), wherein the vacuum port (h) is externally connected with a vacuum device.
6. A multi-component multi-working-condition short-path flash evaporation separation device as claimed in claim 3, wherein a nozzle (6) for spraying the material to be distilled onto the circumferential surface of the inner container in a high-speed tangential manner is arranged in the inner container, so that the material to be distilled forms a thin liquid layer on the surface of the internal thread groove.
7. A multi-component multi-condition short-path flash separation device according to any one of claims 4 to 6, characterized by further comprising a receiver (5) for collecting the material which is gasified and then contacted with the outer surface of the internal condenser (4) to be condensed into liquid again, wherein the receiver (5) is arranged in the inner container (2) and is positioned right below the internal condenser (4).
8. The multi-component multi-working-condition short-path flash separation device according to any one of claims 4 to 6, wherein the inner container (2) is made of stainless steel plate, and the wall thickness of the inner container (2) is 4 mm-6 mm; the inner surface of the inner container (2) is carved with a downward rotary internal thread groove (3).
9. A multi-component multi-condition short-path flash separation device according to claim 4, characterized in that the straight-line distance between the outer surface of the internal condenser (4) and the inner surface of the inner container (2) is 300mm-600 mm.
10. A multi-component multi-regime short-path flash separation apparatus according to any one of claims 4 to 6, wherein the internal condenser (4) is made of stainless steel plate material, and has a diameter of 300mm to 1000mm and a thickness of 1 mm to 2 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010217123.6A CN111298468A (en) | 2020-03-25 | 2020-03-25 | Multi-component multi-working-condition short-path flash separation device |
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| CN202010217123.6A CN111298468A (en) | 2020-03-25 | 2020-03-25 | Multi-component multi-working-condition short-path flash separation device |
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