Sectional fraction extraction device

Abstract

The utility model discloses a sectional type fraction extraction device which comprises a base, a support is fixedly installed on the base, a rectifying column is fixedly installed on the support, the bottom of the rectifying column is fixedly communicated with an evaporator, the top of the rectifying column is fixedly communicated with an air condenser, and the air condenser is fixedly communicated with an evaporator. And the right side of the air condenser fixedly communicates with a condensed water condenser. The condensation water condenser, the control assembly and the condensation assembly are arranged, the control assembly controls the condensation temperature by adjusting the temperature and the flow speed of the condensation water, so that multi-stage condensation and backflow of steam in the condensation water condenser are achieved, condensation and backflow of MMPA materials are achieved, the condensation efficiency and the operation flexibility of the device are improved, and the energy consumption is reduced. The multi-stage condensation and backflow device has the advantages that the multi-stage condensation and backflow of the material are realized, impurities with different boiling points are separated, and the purity of the MMPA product can be obviously improved.

Description

TECHNICAL FIELD

[0001] The utility model belongs to fractionation purification equipment technical field especially relates to a segmented type fraction extraction device. BACKGROUND

[0002] In the pharmaceutical, pesticide, fine chemical industry, often need to use some organic chemical intermediates, such as N, N-dimethyl-3-methoxy propionamide (MMPA), the purity of organic chemical intermediates directly influences the quality and performance of downstream products, therefore staff need to use extraction device to purify MMPA operation, such as the publication number: CN213885027U, disclosed a kind of based on medical organic intermediate impurity's purification device, including distillation tank, isolator and evaporating dish, the distillation tank is fixedly connected between isolator by connecting rod, the evaporating dish is engagedly connected between isolator, electric heating wire one is fixedly installed on the distillation tank, one plug block one is engagedly installed on the distillation tank, one water inlet pipe is fixedly installed on plug block one, and water inlet pipe penetrates plug block one and extends to distillation tank bottom, one plug block two and one dissolving tank are engagedly installed on the isolator, one cooling box is fixedly installed on plug block two, a plurality of cooling plates are fixedly installed on the cooling box, one distillation tube is communicated between the cooling box and distillation tank, the advantages are: improve the purity of the purified organism, accelerate the dissolution speed of organism and the quantity of organism's first purification, also improve the collection degree of precipitated organism, reduce the loss of organism.

[0003] However, the prior art has some problems: the existing equipment is evaporated by opening electric heating wire two to the organic body solution in evaporating dish, so that the organic body is precipitated, so as to complete the purification operation of organic body, but some organic chemical intermediates such as MMPA often contain two or more impurities, the existing technology can only separate one kind of impurity by simple heating, and the product purity is limited, therefore we propose a kind of segmented fraction extraction device. UTILITY MODEL CONTENT

[0004] In view of the problems existing in the prior art, the utility model aims at providing a kind of segmented fraction extraction device, by control assembly and condensing assembly, adjust condensing water temperature and flow rate control condensing temperature, so as to realize material multi-stage condensation and reflux, separate different boiling point impurities, can significantly improve MMPA product purity.

[0005] The utility model discloses a kind of sectional fraction extraction devices, including base, the bracket is fixedly installed on the base, the bracket is fixedly installed with rectifying column on it, the bottom of the rectifying column is fixedly communicated with evaporator, the top of the rectifying column is fixedly communicated with air condenser, the right side of the air condenser is fixedly communicated with condensate water condenser, air condenser, condensate water condenser and base are connected by control assembly between them, condensate water condenser is provided with condensing assembly, the right side of the condensate water condenser is fixedly communicated with first elbow pipe, collector is fixedly installed on the first elbow pipe, feed assembly and vacuum assembly are also provided on the base.

[0006] Optionally, the control assembly includes a reflux ratio controller, the reflux ratio controller is fixedly installed on the base, the reflux ratio controller is connected with a temperature sensor and a control head, the temperature sensor is fixedly installed on the air condenser, and the control head is fixedly installed on the condensate water condenser.

[0007] Optionally, the condensing assembly includes an inner tube, the inner tube is arranged inside the condensate water condenser, a refrigerated water bath circulator is fixedly installed on the base, and the refrigerated water bath circulator is connected with the inner tube through a water pipe.

[0008] Optionally, the feed assembly includes a raw material storage tank, the raw material storage tank is fixedly installed on the base, a peristaltic pump is fixedly installed on the raw material storage tank, a connecting pipe is fixedly communicated with the peristaltic pump, and the other end of the connecting pipe is fixedly communicated with the evaporator.

[0009] Optionally, the vacuum assembly includes a vacuum pump, the vacuum pump is fixedly installed on the base, a second elbow pipe is fixedly communicated with the vacuum pump, and the other end of the second elbow pipe is fixedly communicated with the first elbow pipe.

[0010] Optionally, an oil bath pot is fixedly installed on the base, and the evaporator is arranged inside the oil bath pot.

[0011] Optionally, an electric heating tube is fixedly installed on the bracket, and the electric heating tube surrounds the bottom of the outer surface of the rectifying column.

[0012] Optionally, a three-way connector is arranged on the second elbow pipe, and a vacuum gauge is fixedly installed on the second elbow pipe between the first elbow pipe and the three-way connector.

[0013] Compared with the prior art, the utility model has the beneficial effects that:

[0014] 1. The utility model discloses a condensate water condenser, control assembly and condensing assembly are set up, and the control assembly is through the adjustment condensate water temperature and flow rate control condensing temperature to realize the steam multistage condensation and reflux in the condensate water condenser, is used for realizing the condensation and reflux of MMPA material, improves the condensation efficiency and the operation flexibility of device, and the liquid part after condensation is collected as product, and part is returned as reflux liquid to rectifying column, continues to carry out fractional distillation purification with different temperature again, separates the impurity of different boiling point, thereby can significantly improve the product purity.

[0015] 2. The utility model discloses a vacuum pump, three -way connector and vacuum gauge are set up, after feeding in evaporimeter, the staff starts vacuum pump, adjusts to proper vacuum degree through three -way connector, reduces material boiling point, prevents the generation of a large number of by -products of MMPA material in evaporimeter due to high temperature, and high -precision vacuum gauge can accurately show the vacuum degree of reaction device, and the staff is convenient for adjustment observation.

[0016] 3. The utility model discloses an oil bath pot and electric heating tube are set up, after the peristaltic pump is sent into evaporimeter with MMPA raw material, starts the oil bath pot and can preheat the MMPA raw material in evaporimeter to 50-60 DEG C, thereby can reduce raw material viscosity, and improve evaporation efficiency, and the mixed gas after pre-evaporation in evaporimeter enters rectifying column, heats through electric heating tube, thereby can stably provide the heat required in rectification process, guarantees rectification effect.

[0017] Other features of the utility model and its advantages will become clear from the following detailed description of exemplary embodiments of the utility model with reference to the accompanying drawings. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 It is the structure schematic drawing that the utility model provides;

[0019] Figure 2 It is the back structure schematic drawing that the utility model provides;

[0020] Figure 3 It is evaporimeter, rectifying column and air condenser connection structure schematic drawing that the utility model provides;

[0021] Figure 4 It is the sectional structure schematic drawing of condensate water condenser inside that the utility model provides;

[0022] Figure 5 It is Figure 2 The local amplification structure schematic drawing of place A in it.

[0023] In the figure: 1, base; 2, support; 3, rectifying column; 4, evaporator; 5, air condenser; 6, condenser water condenser; 7, inner tube; 8, refrigerated water bath circulator; 9, water pipe; 10, first elbow; 11, collector; 12, reflux ratio controller; 13, temperature sensor; 14, control head; 15, raw material storage tank; 16, peristaltic pump; 17, connecting pipe; 18, vacuum pump; 19, second elbow; 20, three-way connector; 21, vacuum gauge; 22, oil bath pot; 23, electric heating tube. DETAILED DESCRIPTION

[0024] In order to further understand the utility model content, characteristics and effects of the utility model, the following examples are given, and the details are described as follows with the help of the drawings.

[0025] As Figures 1 to 5 shown, the utility model embodiment provides a kind of extraction device of sectional type fraction, including base 1, base 1 is fixedly installed with support 2, support 2 is fixedly installed with rectifying column 3, the bottom of rectifying column 3 is fixedly communicated with evaporator 4, the top of rectifying column 3 is fixedly communicated with air condenser 5, the right side of air condenser 5 is fixedly communicated with condenser water condenser 6, air condenser 5, condenser water condenser 6 and base 1 are connected by control assembly between, condenser water condenser 6 is provided with condensing assembly, the right side of condenser water condenser 6 is fixedly communicated with first elbow 10, first elbow 10 is fixedly installed with collector 11, base 1 is also provided with feed assembly and vacuum assembly.

[0026] Further, control assembly includes reflux ratio controller 12, reflux ratio controller 12 is fixedly installed on base 1, temperature sensor 13 and control head 14 are connected on reflux ratio controller 12, temperature sensor 13 is fixedly installed on air condenser 5, control head 14 is fixedly installed on condenser water condenser 6.

[0027] Flow controller is provided on control head 14, reflux ratio controller 12 controls condensing temperature by adjusting condenser water temperature and flow rate, to realize multi-stage condensation and reflux, for realizing the condensation and reflux of MMPA material, improve condensation efficiency and the operating flexibility of device, liquid part after condensation is collected as product, part is returned to rectifying column 3 as reflux liquid, to maintain operation balance, to realize the efficient separation and purification of MMPA.

[0028] Further, condensing assembly includes inner tube 7, inner tube 7 is arranged in condenser water condenser 6, base 1 is fixedly installed with refrigerated water bath circulator 8, refrigerated water bath circulator 8 is connected between inner tube 7 by water pipe 9.

[0029] After the steam enters the condensate condenser 6, the refrigerated water bath circulator 8 can adjust the condensate temperature and circulate to the inside of the inner tube 7 through the water pipe 9, so that the steam in the condensate condenser 6 can be condensed into water droplets by cooling, part of which is collected as a product, and part of which returns to the rectification column 3 as reflux liquid to maintain the operation balance.

[0030] Further, the feeding assembly comprises a raw material storage tank 15 fixedly installed on the base 1, a peristaltic pump 16 fixedly installed on the raw material storage tank 15, and a connecting pipe 17 fixedly communicated with the peristaltic pump 16 and fixedly communicated with the evaporator 4 at the other end.

[0031] The staff can make the peristaltic pump 16 extract the MMPA raw material in the raw material storage tank 15 by starting the peristaltic pump 16, and then deliver it to the inside of the evaporator 4 through the connecting pipe 17, so as to perform the fractionation operation.

[0032] Further, the vacuum assembly comprises a vacuum pump 18 fixedly installed on the base 1, and a second elbow 19 fixedly communicated with the vacuum pump 18 and fixedly communicated with the first elbow 10 at the other end.

[0033] After the raw material is fed into the evaporator 4, the staff starts the vacuum pump 18, which can reduce the boiling point of the MMPA material by adjusting the appropriate vacuum degree, so as to prevent the generation of a large amount of by-products in the evaporator 4 due to high temperature.

[0034] Further, an oil bath pot 22 is fixedly installed on the base 1, and the evaporator 4 is arranged in the oil bath pot 22.

[0035] After the peristaltic pump 16 sends the MMPA raw material into the evaporator 4, the oil bath pot 22 is started to preheat the organic chemical intermediate raw material in the evaporator 4 to 50-60℃, so as to reduce the viscosity of the MMPA raw material and improve the evaporation efficiency.

[0036] Further, an electric heating pipe 23 is fixedly installed on the support 2 and surrounds the bottom of the outer surface of the rectification column 3.

[0037] The mixed gas pre-evaporated from the evaporator 4 enters the rectification column 3 and is heated by the electric heating pipe 23, so as to stably provide the heat required for the rectification process and ensure the rectification effect.

[0038] Further, a three-way connector 20 is arranged on the second elbow 19, and a vacuum gauge 21 is fixedly installed on the second elbow 19 between the first elbow 10 and the three-way connector 20.

[0039] The worker adjusts the three-way connector 20 to -75KPa, reduces the boiling point of the MMPA material, prevents a large amount of by-products from being generated in the evaporator 4 due to high temperature, and the high-precision vacuum gauge 21 can accurately display the vacuum degree of the reaction device, so that the worker can adjust and observe.

[0040] The working principle and use process of the utility model are as follows:

[0041] Firstly, the worker starts the peristaltic pump 16, the MMPA material in the raw material storage tank 15 is transported into the evaporator 4 through the connecting pipe 17 due to the operation of the peristaltic pump 16, then the vacuum pump 18 is started, the appropriate vacuum degree is adjusted through the three-way connector 20, the boiling point of the MMPA material can be reduced, and a large amount of by-products can be prevented from being generated in the evaporator 4 due to high temperature, after the peristaltic pump 16 sends the MMPA raw material into the evaporator 4, the worker starts the oil bath pot 22, the MMPA raw material in the evaporator 4 can be preheated to 50-60 DEG C, so that the raw material viscosity can be reduced, and the evaporation efficiency can be improved, after preheating, the temperature of the oil is controlled to be 220-230 DEG C through the oil bath pot 22, low-boiling-point impurities start to evaporate, at this time, the condensing water in the refrigerated water bath circulator 8 is set to 3-8 DEG C, and the circulation is started, when the steam reaches the rectifying column 3, the electric heating tube 23 is used for heating, so that the heat required in the rectification process can be stably provided, the rectification effect is guaranteed, after the steam reaches the air condenser 5, the full reflux is controlled for about half an hour through the reflux ratio controller 12, the top temperature in the rectifying column 3 is stably controlled at about 110-115 DEG C, the appropriate reflux ratio is adjusted through the reflux ratio controller 12, the low-boiling-point impurities are gradually extracted, and the collector 11 is used for collecting, then, the worker adjusts different temperatures, vacuum degrees and reflux ratios, separates impurities with different boiling points, and collects the MMPA material after fractional distillation in sections, the purification efficiency is improved, the production cost is reduced, the purity of the MMPA product is significantly improved, and the demand of the high-end industry such as medicine, pesticide and dye for ultra-pure MMPA is met.

[0042] Although the embodiments of the utility model have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and variations can be made to the embodiments without departing from the principles and spirits of the utility model, the scope of the utility model is defined by the appended claims and their equivalents.

Claims

1. An apparatus for the extraction of fractionated distillates comprising a base (1) characterised in that: The base (1) is fixedly installed with a support (2), the support (2) is fixedly installed with a rectifying column (3), the bottom of the rectifying column (3) is fixedly communicated with an evaporator (4), the top of the rectifying column (3) is fixedly communicated with an air condenser (5), the right side of the air condenser (5) is fixedly communicated with a condensed water condenser (6), the air condenser (5), the condensed water condenser (6) and the base (1) are connected through a control assembly, the condensed water condenser (6) is provided with a condensing assembly, the right side of the condensed water condenser (6) is fixedly communicated with a first elbow pipe (10), the first elbow pipe (10) is fixedly installed with a collector (11), the base (1) is further provided with a feeding assembly and a vacuum assembly.

2. A segmented fraction extraction device according to claim 1, characterized in that: The control assembly comprises a reflux ratio controller (12), the reflux ratio controller (12) is fixedly installed on the base (1), the reflux ratio controller (12) is connected with a temperature sensor (13) and a control head (14), the temperature sensor (13) is fixedly installed on the air condenser (5), the control head (14) is fixedly installed on the condensed water condenser (6).

3. A segmented fraction extraction device according to claim 1, characterized in that: The condensing assembly comprises an inner tube (7), the inner tube (7) is arranged in the condensed water condenser (6), the base (1) is fixedly installed with a refrigerated water bath circulator (8), the refrigerated water bath circulator (8) and the inner tube (7) are connected through a water pipe (9).

4. A segmented fraction extraction device according to claim 1, characterized in that: The feeding assembly comprises a raw material storage tank (15), the raw material storage tank (15) is fixedly installed on the base (1), the raw material storage tank (15) is fixedly installed with a peristaltic pump (16), the peristaltic pump (16) is fixedly communicated with a connecting pipe (17), the other end of the connecting pipe (17) is fixedly communicated with the evaporator (4).

5. A segmented fraction extraction device according to claim 1, characterized in that: The vacuum assembly comprises a vacuum pump (18), the vacuum pump (18) is fixedly installed on the base (1), the vacuum pump (18) is fixedly communicated with a second elbow pipe (19), the other end of the second elbow pipe (19) is fixedly communicated with the first elbow pipe (10).

6. A segmented fraction extraction device according to claim 1, characterized in that: The base (1) is fixedly installed with an oil bath pot (22), the evaporator (4) is arranged in the oil bath pot (22).

7. A segmented fraction extraction device according to claim 1, characterized in that: The support (2) is fixedly installed with an electric heating tube (23), the electric heating tube (23) surrounds the bottom of the outer surface of the rectifying column (3).

8. A segmented fraction extraction device according to claim 5, characterized in that: The second elbow pipe (19) is provided with a three-way connector (20), the second elbow pipe (19) is fixedly installed with a vacuum gauge (21) between the first elbow pipe (10) and the three-way connector (20).

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