CN203736885U - Water separating equipment - Google Patents
Water separating equipment Download PDFInfo
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- CN203736885U CN203736885U CN201420091743.XU CN201420091743U CN203736885U CN 203736885 U CN203736885 U CN 203736885U CN 201420091743 U CN201420091743 U CN 201420091743U CN 203736885 U CN203736885 U CN 203736885U
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- cooler
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- fluid reservoir
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Abstract
Water separating equipment for separating little water in an organic solvent forming an azeotrope with water comprises a distillation still, a distillation column, a condenser, a cooler, a product tank, an intermediate liquid storage tank and a reflux valve, wherein the outlet of the cooler is connected with the product tank, and a product extracting valve is arranged on an extracting pipe; multiple layers of packing are arranged in the distillation column in an overlapped way, an input opening of the product extracting valve is connected with an input opening of the reflux valve, an output opening of the reflux valve is connected with an inlet of the intermediate liquid storage tank, and an outlet of the intermediate liquid storage tank is connected with a reflux liquid distributing pipeline on the distillation column. The water is fully enriched in the top of the distillation column through a reflux pipe and the intermediate liquid storage tank by a full-reflux intermittent distillation method. Under the same conditions, the enrichment times of the water in the top of the distillation column by the operation method is larger than enrichment times at any other refluxes, the distillation separating effect is best, and the water in the organic solvent can be controlled smaller than or equal to 0.05%.
Description
Technical field
The utility model belongs to chemical industry equipment, relates in particular to a kind of divisor.
Background technology
Organic solvent, as basic chemical products, is applied widely in industrial acquisition.But along with industrial expansion, especially electronics industry and synthetic the developing rapidly of medicine, stricter to the moisture requirement in organic solvent, as: require moisture≤0.05%.Conventionally must moisture could be reduced to specific process≤0.05%, as vaporize infiltration embrane method, molecular sieve adsorption, azeotropic distillation, reaction distillation etc. but these methods are often invested greatly, complicated operation, and be often only suitable for the large batch of production of single variety.
Utility model content
Based on this, a kind of batch distillation divisor of efficient and easy operating is provided, effectively separate with water and form moisture a small amount of in the organic solvent of azeotropic mixture, make moisture≤0.05% in organic solvent.
The divisor of a small amount of moisture in the organic solvent of a kind of separation and water formation azeotropic mixture, comprise distillation still, destilling tower, condenser, cooler and the products pot being connected with the outlet of this cooler, described destilling tower is located between described distillation still and described condenser, the condensed fluid collection dish outlet of described destilling tower is connected to the import of cooler by extraction pipe, fluid reservoir and return valve in the middle of also comprising, and on described extraction pipe, be provided with product extraction valve, described destilling tower has the filler of multilayer laminated setting, the input port of described product extraction valve is connected with the input port of described return valve, the delivery outlet of described return valve is connected with the import of described middle fluid reservoir, in the middle of described, the outlet of fluid reservoir is connected with the backflow liquid distributor road on described destilling tower.
Further, the described middle volume of fluid reservoir and the volume ratio of described distillation still are 1:50～1:100.
Further, between the top exit of described condenser and the import of described cooler, connect by an equalizing main.
Further, also comprise first flow meter, described first flow meter pipeline is connected between the input port and the import of described cooler of described product extraction valve.
Further, also comprise the second flowmeter, described the second flowmeter pipeline is connected between the delivery outlet and described middle fluid reservoir of described return valve.
Above-mentioned divisor utilizes return duct and middle fluid reservoir, adopts infinite reflux batch distillation method, makes moisture obtain sufficient enrichment at distillation tower top.Under equal conditions, this method of operating make moisture the multiple of distillation tower top enrichment than other any reflux ratio under the multiple of enrichment all large, separated effect is best, because be total reflux operation method, just need not control reflux ratio, make operation become extremely simple and convenient, be particularly suited for reflux ratio and change still-process greatly, make easier≤0.05% of moisture in organic solvent.
Brief description of the drawings
Fig. 1 is the structural representation of divisor.
Detailed description of the invention
In order to make the technical problems to be solved in the utility model, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the utility model is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain the utility model, and be not used in restriction the utility model.
Batch distillation is that a batch materials is added in distillation still once, and material carries out part vaporization and partial condensation by repeated multiple times, material is carried out to a kind of distillation technique of separating-purifying.Because it adapts to different material and separation requirement in same set of equipment, have flexibility strong, invest the advantages such as little, in small-scale fine chemistry industry and spent organic solvent are recycled industry, obtain and be widely used.Batch distillation mainly contains two kinds of methods of operating at present: a kind of is the method for operating of permanent distillate composition, and it is refluxed and recently maintained the composition of distillate by continuous increase, obtains product; The second is the method for operating of constant reflux ratio, and it recently obtains product by constant backflow.It has flexible and convenient operation, simple in structure, invest littlely, obtain application widely in small quantities of output, factory wide in variety.
As shown in Figure 1, a kind of infinite reflux batch distillation divisor that adopts, it comprises distillation still 1, destilling tower 2, condenser 3, cooler 4 and the products pot 5 being connected with the outlet of this cooler 4.Destilling tower 2 is located between distillation still 1 and condenser 3, and in distillation still 1, the suitable height of configuration destilling tower 2(is several theoretical trays), destilling tower 2 has the filler of multilayer laminated setting.In addition, condenser 3 has and have a condensed fluid collection dish 31 between destilling tower, and this condensed fluid collection dish 31 is also connected to the import of cooler 4 by extraction pipe.
Especially, batch distillation divisor also comprises the middle fluid reservoir 8 and the return valve 9 that are arranged on return duct 7, and on extraction pipe, be provided with product extraction valve 10, extraction pipe comprises the product extraction pipe 14 between total extraction pipe 6 and product extraction valve 10 and the import of cooler 4 between product extraction valve 10 and condensed fluid collection dish 31.Return duct 7 is connected between the input port and destilling tower 2 of product extraction valve 10, and the interface of return duct 7 and destilling tower 2 is the interface with destilling tower 2 lower than extraction pipe 6; The input port of product extraction valve 10 is connected with the input port of return valve 9, and the delivery outlet of return valve 9 is connected with the import of middle fluid reservoir 8, and the outlet of middle fluid reservoir 8 is connected with the backflow liquid distributor road on destilling tower 2.
Utilize return duct 7 and middle fluid reservoir 8, adopt infinite reflux batch distillation method, make moisture obtain sufficient enrichment on destilling tower 2 tops.Under equal conditions, this method of operating make moisture the multiple of distillation tower top enrichment than other any reflux ratio under the multiple of enrichment all large, separated effect is best, because be total reflux operation method, just need not control reflux ratio, make operation become extremely simple and convenient, be particularly suited for reflux ratio and change still-process greatly.When the physical-chemical datas such as the vapor liquid equilibrium data of water-containing organic solvent to be separated are incomplete or unknown, while being difficult to determine suitable reflux ratio, the micro-moisture advantage that adopts this utility model to separate is wherein given prominence to
Preferably, the volume ratio of the volume of middle fluid reservoir 8 and distillation still 1 is 1:50～1:100.
In a further embodiment, between the top exit 32 of condenser 3 and the import of cooler 4, connect by equalizing main 11, this equalizing main 11 makes point water operation of divisor more stable.
Batch distillation divisor also comprises first flow meter 13, and first flow meter 13 pipelines are connected between the delivery outlet of product extraction valve 10 and the import of cooler 4.
Batch distillation divisor also comprises that the second flowmeter 12, the second flowmeter 12 pipelines are connected between the delivery outlet and middle fluid reservoir 8 of return valve 9.
Formed by following steps with the micro-moisture in above-mentioned divisor Separation of Organic:
(1), organic solvent to be separated is added to distillation still 1, heat temperature raising distillation, closes product extraction valve 10, opens the return valve 9 of reflux pipeline, carries out the total reflux operation of product-free extraction, the vapour-liquid of destilling tower 2 is approached and reach balance.Moisture in distillation still 1, through infinite reflux batch distillation, obtains sufficient enrichment at tower top;
(2), after the total reflux operation of regular hour (common 15～20 minutes), the concentration of the cut of middle fluid reservoir 8 reaches and approaches after balance, the liquid fraction of return duct 7 and extraction pipe 6 and middle fluid reservoir 8 is all emitted, be collected in packing container, be called " front-end volatiles ";
(3), according to moisture requirement in organic solvent product, concrete determine the number of times of " without extraction infinite reflux batch distillation---the liquid storage of fluid reservoir 8 in the middle of emitting ";
(4), when after several times " without extraction infinite reflux batch distillation---the liquid storage of fluid reservoir 8 in the middle of emitting ", in distillation still 1 still, the moisture of organic solvent reaches after requirement, closing volume valve 9, organic solvent in distillation still 1 still is steamed continuously, obtain the satisfactory organic solvent product of moisture;
(5), the processing of " front-end volatiles ": according to the different physicochemical properties of organic solvent, adopt diverse ways to carry out preliminary hydro-extraction, after preliminary hydro-extraction is processed, as raw material, more than pressing, (1)---the step of (4) operates, and can obtain the satisfactory organic solvent product of moisture.
Below to use above-mentioned divisor to carry out the concrete case study on implementation that organic solvent divides water:
Case one:
Moisture 10% acetonitrile solvent, add anhydrous calcium chloride as salting-out separation agent, carry out after initial gross separation dehydration, moisture in acetonitrile solvent drops to 1.4%, acetonitrile solvent after preliminary hydro-extraction is joined in 4000L distillation still 1, selecting tower diameter is the intermittent column 2 of 500mm, adopt the moisture in infinite reflux batch distillation method separating acetonitrile, the acetonitrile organic solvent product that to have obtained moisture be≤0.02%.
Case two:
Moisture about 2% 1-Methoxy-2-propyl acetate waste liquid is joined in 4000L distillation still 1, the intermittent column 2 that is 500mm with tower diameter, carry out the moisture in batch distillation separating propylene glycol methyl ether acetate by operation, obtained the 1-Methoxy-2-propyl acetate organic solvent product of moisture≤0.05%.
The foregoing is only preferred embodiment of the present utility model; not in order to limit the utility model; all any amendments of doing within spirit of the present utility model and principle, be equal to and replace and improvement etc., within all should being included in protection domain of the present utility model.
Claims (5)
1. a divisor, comprise distillation still, destilling tower, condenser, cooler and the products pot being connected with the outlet of this cooler, described destilling tower is located between described distillation still and described condenser, the condensed fluid collection dish outlet of described destilling tower is connected to the import of cooler by extraction pipe, it is characterized in that, fluid reservoir and return valve in the middle of also comprising, and on described extraction pipe, be provided with product extraction valve, described destilling tower has the filler of multilayer laminated setting, the input port of described product extraction valve is connected with the input port of described return valve, the delivery outlet of described return valve is connected with the import of described middle fluid reservoir, in the middle of described, the outlet of fluid reservoir is connected with the backflow liquid distributor road on described destilling tower.
2. divisor according to claim 1, is characterized in that, the described middle volume of fluid reservoir and the volume ratio of described distillation still are 1:50～1:100.
3. divisor according to claim 1, is characterized in that, between the top exit of described condenser and the import of described cooler, connects by an equalizing main.
4. according to the divisor described in claims 1 to 3 any one, it is characterized in that, also comprise first flow meter, described first flow meter pipeline is connected between the delivery outlet and the import of described cooler of described product extraction valve.
5. according to the divisor described in claims 1 to 3 any one, it is characterized in that, also comprise the second flowmeter, described the second flowmeter pipeline is connected between the delivery outlet and described middle fluid reservoir of described return valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420091743.XU CN203736885U (en) | 2014-02-28 | 2014-02-28 | Water separating equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420091743.XU CN203736885U (en) | 2014-02-28 | 2014-02-28 | Water separating equipment |
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| Publication Number | Publication Date |
|---|---|
| CN203736885U true CN203736885U (en) | 2014-07-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201420091743.XU Expired - Fee Related CN203736885U (en) | 2014-02-28 | 2014-02-28 | Water separating equipment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299203A (en) * | 2018-01-29 | 2018-07-20 | 淄博高新技术产业开发区精细化工和高分子材料研究院 | A method of PGMEA being recycled from PGMEA/ aqueous solutions using intermittent azeotropic rectifying |
-
2014
- 2014-02-28 CN CN201420091743.XU patent/CN203736885U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299203A (en) * | 2018-01-29 | 2018-07-20 | 淄博高新技术产业开发区精细化工和高分子材料研究院 | A method of PGMEA being recycled from PGMEA/ aqueous solutions using intermittent azeotropic rectifying |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140730 Termination date: 20200228 |