CN203061178U - Reaction device capable of improving yield of product - Google Patents
Reaction device capable of improving yield of product Download PDFInfo
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- CN203061178U CN203061178U CN 201220705356 CN201220705356U CN203061178U CN 203061178 U CN203061178 U CN 203061178U CN 201220705356 CN201220705356 CN 201220705356 CN 201220705356 U CN201220705356 U CN 201220705356U CN 203061178 U CN203061178 U CN 203061178U
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Abstract
The utility model discloses a reaction device capable of improving the yield of a product. The reaction device comprises a charging device, a reaction device and a separation device, wherein the charging device comprises a raw material pool; the reaction device comprises a reaction kettle, a heating device for heating the reaction kettle, and a first receiving device; a charging port, a discharging port and an air outlet are formed in the reaction kettle; the charging port is connected with the raw material pool by virtue of a pipeline; the discharging port is connected with the first receiving device by virtue of the pipeline; a stirring device and a temperature monitoring device are also arranged in the reaction kettle; the separation device comprises a rectifying tower, a condenser and a second receiving device; the air inlet end of the rectifying tower is connected with an air outlet of the reaction kettle by virtue of the pipeline; the outlet end of the rectifying tower is connected with the inlet end of the condenser; and the outlet end of the condenser is connected with a second receiving device. By using the reaction device, a separation technology in which a reaction product effectively separated by the rectifying tower and raw materials/solvents are miscible and azeotropic is adopted, so that the yield of the reaction product is improved, and the reaction cost is also reduced.
Description
Technical field
The utility model relates to organic chemical products synthesis technical field, is specifically related to a kind of reaction unit that improves product yield.
Background technology
In chemical organic chemical industry's product synthetic, often with the generation of side reaction, the generation of accessory substance all has a significant impact separation purification and the yield thereof of target compound.The generation of accessory substance changes the equilibrium constant on the one hand, causes reaction can not carry out thoroughly.Even the change reaction condition, as: prolong the reaction time, improve reaction temperature, can not obviously increase reaction yield, and excessive high temperature heats and the long reaction time usually can make product decompose, and increases the complexity of reaction.On the other hand, accessory substance normal with product or the solvent azeotropic that dissolves each other, cause difficulty to the separation purification of product.
For overcoming the above problems, in production practices, adopt following method usually: 1. control reaction condition, as the control reaction temperature, change feeding sequence etc., improve the primary product yield.2. the use catalyst reduces activation energy, increases the reaction selectivity, improves reaction yield.3. from system, tell product/accessory substance, promote the molecular balance forward to move, improve reaction yield.In actual production, telling product/accessory substance from system is comparatively cost-effective method.The method of separated product/accessory substance commonly used has: the branch water law, extraction etc. can be obtained effect preferably usually.But if product, accessory substance are with solvent dissolves each other or azeotropic, tell product/accessory substance by said method so and then have greatly difficulty.
The above-mentioned azeotropic system that dissolves each other, separation method commonly used has:
1. compression rectification technology.Utilize binary system that Raoult's law is produced deviation, improve system pressure, destroy the solvent azeotropic point and come separating by-products.This technology is not introduced new component in reaction system, avoid producing more side reactions, and technology is simple, easy to operate.But compression rectification equipment precision, operating cost is higher, and operation easier is higher relatively.
2. variable-pressure rectification technology.Because the composition of azeotropic mixture is obvious with pressure change, by the two-tower rectification of two different pressures, realize the separation of azeotropic mixture.This technical energy saving is efficient, does not need to add other components to reaction system, has avoided the generation of side reaction.But the control of the automation between two towers has big difficulty, and the operation of reaction is had relatively high expectations.
3. azeotropic distillation technology.In former reaction system, add new component, form new azeotropic system, thereby realize separating.This technology recycling flow process is short, and equipment is simple, handling safety.But owing in former system, introduce new component, tend to increase uncertain side reaction, and alternative azeotropic mixture system is few, alternative little.
4. extraction and distillation technology.Add high boiling extractant in former reaction system, any component azeotropic not can significantly change the relative amount in the former reactive component in this extractant and the reaction system, reaches the separation purpose.Extractant range of choice in this technology is wide, and the variation of operating parameters scope is big, and energy consumption is low, but owing to introduce new component in the former system, usually can bring uncertain side reaction.
Above-mentioned various distillation technology respectively has characteristics, and wherein variable-pressure rectification and compression rectification technology are comparatively advanced, but the equipment complexity is expensive; Though azeotropic distillation and extracting rectifying operation are simple, need to introduce new component, cause the side reaction that can not expect, increase the product complexity.
The utility model content
In order to solve the technical problem that the azeotropic system that dissolves each other in the prior art can't realize that low-cost high-efficiency separates, the utility model provides a kind of reaction unit that improves product yield.By the dissolve each other isolation technics of azeotropic of efficient reaction product isolated and raw material/solvent, to improve reaction yield, save reaction cost.
The reaction unit of raising product yield of the present utility model comprises feeding device, reaction unit and separator, wherein:
Feeding device comprises feed reservoir;
Reaction unit comprises reactor, the heater that the heating reactor is used, and first receiving device; Wherein reactor is provided with charging aperture, discharging opening and gas outlet, and charging aperture is connected by pipeline with feed reservoir, and discharging opening is connected by pipeline with first receiving device, also is provided with agitating device and device for monitoring temperature in the reactor;
Separator comprises rectifying column, condenser and second receiving system; Wherein the rectifying column entrance point is connected by pipeline with the gas outlet of reactor, and the rectifying column port of export is connected with the entrance point of condenser, and the condensator outlet end connects second receiving system.
Preferably, described feed reservoir is a plurality of.More when material composition, be not suitable for adding simultaneously fashionable, can be contained in different feed reservoir respectively, add respectively as required, simple and convenient.
Preferably, described feed reservoir is connected by the pipeline that is provided with multiple-way valve with the reactor charging aperture.
Preferably, the pipeline that is connected with the reactor charging aperture of described feed reservoir is provided with the peristaltic pump that pump is got raw material.
Preferably, described agitator is mechanical agitator or magnetic stirring apparatus.
Preferably, described heater is electric heating film or steam heater.Electric heating film can be coated on the reactor periphery.
Preferably, described condenser makes water or ethanol as refrigerant.
Preferably, described discharging opening is located at the reactor bottom, and its pipeline that is communicated with first receiving device is provided with two-port valve; The reactor top is located in described gas outlet.
Preferably, the pipeline that is connected with first receiving device of described discharging opening is provided with two-port valve.
Preferably, described agitating device and device for monitoring temperature are independent control formula.
The utlity model has following beneficial effect:
Reaction unit of the present utility model is by arranging a rectifying column, the product of the azeotropic that dissolves each other that difficulty is separated separates with raw material, utilize the difference of its boiling point, making product continue to enter condenser reaction raw materials (solvent) with gaseous form then passes back into reactor with liquid form and proceeds reaction, realize the dissolve each other isolation technics of azeotropic of efficient reaction product isolated and raw material/solvent, not only improve the product yield, also saved reaction cost.
Description of drawings
Fig. 1 is the structural representation of the utility model reaction system.
The component symbol explanation:
1 feeding device; 2 reaction units;
3 separators; 7,9 feed reservoir;
6,8 peristaltic pumps; 10 triple valves;
11 reactors; 12 heaters;
13 agitating devices; 14 device for monitoring temperature;
15 two-port valves; 16 rectifying columns;
17 condensers; 5 first receiving devices;
4 second receiving systems
The specific embodiment
The utility model is described in further detail below in conjunction with the drawings and specific embodiments, so that those skilled in the art can better understand the utility model and being implemented, but illustrated embodiment is not as to restriction of the present utility model.
Embodiment 1 preparation 5 hydroxymethyl furfural
The entire reaction device comprises feeding device 1, reaction unit 2 and separator 3.Feeding device 1 comprises two independently feed reservoir 7 and 9, is connected with reactor 11 charging apertures by pipeline respectively, and the pipeline that feed reservoir 7 is communicated with reactor 11 is provided with peristaltic pump 6, and another pipeline is provided with peristaltic pump 8.Two pipelines are connected with the charging aperture of reactor 11 by a triple valve 10.
Reaction unit 2 comprises reactor 11, heater 12, agitating device 13, device for monitoring temperature 14 and first receiving device 5, and wherein, agitating device 13 and device for monitoring temperature 14 are built in the reactor, control its switch by external switch respectively; Heater can be electric heating film or steam heater, if use electric heating film it can be coated on reactor 11 peripheries, reactor 11 bottoms are provided with discharging opening and connect first receiving device 5 by pipeline, by two-port valve 15 gauge taps.
Separator 3 comprises a rectifying column 16, and the entrance point of rectifying column 16 is communicated with the gas outlet that the reactor upper end arranges, and the rectifying column port of export connects the entrance point of a condenser 17, and the port of export of condenser connects second receiving system 4.Condenser 17 is cooled off as refrigerant by recirculated water or ethanol.
Preparation process:
Close two-port valve 15.1kg fructose is mixed as reaction raw materials with 4L DMSO, place feed reservoir 7, the 5g concentrated sulfuric acid and 1L DMSO low-temperature mixed place feed reservoir 9 as catalyst.Open triple valve 10, opening peristaltic pump 6 pumps into raw material in the reactor 11, after turn on agitator 13 stirs 10min, opening peristaltic pump 8 slowly pumps into catalyst in the reactor 11, close triple valve 10, after the question response thing becomes homogeneous phase, open heater 12, open built-in device for monitoring temperature 14, open cold condenser 17.
By built-in device for monitoring temperature 14 monitoring reactions, reaction temperature rises to steadily backflow of beginning in 166 ℃ of afterreaction stills, the gas that the reactant liquor backflow produces is the mixture of steam and DMSO, gas outlet by the reactor upper end enters rectifying column 16 backs because the DMSO condensing temperature is lower than water vapour, makes the DMSO of generating gasification separate with water byproduct.DMSO reenters reactor 11 by the rectifying column pipeline, continues to participate in reaction as solvent.Water byproduct enters condenser 17 with the steam form, is condensed into aqueous water rapidly, enters second receiving system 4.
When the reacting liquid temperature in the reaction unit 2 was down to 140 ℃, it was comparatively complete to judge that the fructose dehydration is carried out.Close heater 12, open two-port valve 15, reaction mixture is entered first receiving device 5, carry out further separation and purification.
More than for synthesizing a full unit of 5 hydroxymethyl furfural.
Behind the emptying reactor, open triple valve 10, open pump 6, pump 8, in reactor 11, feed in raw material as requested, begin second pot of reaction, realize the continuous production of 5 hydroxymethyl furfural.
The above embodiment is the preferred embodiment that proves absolutely that the utility model is lifted, and protection domain of the present utility model is not limited thereto.Being equal to that those skilled in the art do on the utility model basis substitutes or conversion, all within protection domain of the present utility model.Protection domain of the present utility model is as the criterion with claims.
Claims (10)
1. a reaction unit that improves product yield comprises feeding device, reaction unit and separator, it is characterized in that:
Feeding device comprises feed reservoir;
Reaction unit comprises reactor, the heater that the heating reactor is used, and first receiving device; Wherein reactor is provided with charging aperture, discharging opening and gas outlet, and charging aperture is connected by pipeline with feed reservoir, and discharging opening is connected by pipeline with first receiving device, also is provided with agitating device and device for monitoring temperature in the reactor;
Separator comprises rectifying column, condenser and second receiving system; Wherein the rectifying column entrance point is connected by pipeline with the gas outlet of reactor, and the rectifying column port of export is connected with the entrance point of condenser, and the condensator outlet end connects second receiving system.
2. the reaction unit of raising product yield according to claim 1 is characterized in that, described feed reservoir is a plurality of.
3. the reaction unit of raising product yield according to claim 2 is characterized in that, described feed reservoir is connected by the pipeline that is provided with multiple-way valve with the reactor charging aperture.
4. the reaction unit of raising product yield according to claim 1 is characterized in that, the pipeline that described feed reservoir is connected with the reactor charging aperture is provided with the peristaltic pump that pump is got raw material.
5. the reaction unit of raising product yield according to claim 1 is characterized in that, described agitator is mechanical agitator or magnetic stirring apparatus.
6. the reaction unit of raising product yield according to claim 1 is characterized in that, described heater is electric heating film or steam heater.
7. the reaction unit of raising product yield according to claim 1 is characterized in that, described condenser makes water or ethanol as refrigerant.
8. the reaction unit of raising product yield according to claim 1 is characterized in that, described discharging opening is located at the reactor bottom, and its pipeline that is communicated with first receiving device is provided with two-port valve; The reactor top is located in described gas outlet.
9. the reaction unit of raising product yield according to claim 1 is characterized in that, the pipeline that described discharging opening is connected with first receiving device is provided with two-port valve.
10. the reaction unit of raising product yield according to claim 1 is characterized in that, described agitating device and device for monitoring temperature are independent control formula.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220705356 CN203061178U (en) | 2012-12-19 | 2012-12-19 | Reaction device capable of improving yield of product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220705356 CN203061178U (en) | 2012-12-19 | 2012-12-19 | Reaction device capable of improving yield of product |
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| CN203061178U true CN203061178U (en) | 2013-07-17 |
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| CN 201220705356 Expired - Fee Related CN203061178U (en) | 2012-12-19 | 2012-12-19 | Reaction device capable of improving yield of product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021022469A1 (en) * | 2019-08-06 | 2021-02-11 | 吉林凯莱英医药化学有限公司 | Continuous synthesis-purification integrated device and continuous reaction system containing same |
-
2012
- 2012-12-19 CN CN 201220705356 patent/CN203061178U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021022469A1 (en) * | 2019-08-06 | 2021-02-11 | 吉林凯莱英医药化学有限公司 | Continuous synthesis-purification integrated device and continuous reaction system containing same |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130717 Termination date: 20131219 |