CN214051620U - Simple device for raising reaction temperature of mixed system under normal pressure - Google Patents
Simple device for raising reaction temperature of mixed system under normal pressure Download PDFInfo
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- CN214051620U CN214051620U CN202022483375.1U CN202022483375U CN214051620U CN 214051620 U CN214051620 U CN 214051620U CN 202022483375 U CN202022483375 U CN 202022483375U CN 214051620 U CN214051620 U CN 214051620U
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Abstract
The utility model discloses a simple and easy ordinary pressure rises mixed system reaction temperature's device down, including the heating member and set up in the reaction unit of heating member, reaction unit has the reaction chamber and the backward flow chamber of intercommunication, and the reaction intracavity holds the liquid mixture of multiple liquid mixture, and the backward flow chamber is provided with the backward flow piece, and wherein, the liquid mixture who is located the reaction chamber heats the back to make the lower liquid boiling of boiling point and flow to the backward flow piece, in order to form the liquid seal at the backward flow piece. After heating the liquid mixture in the reaction cavity, the liquid with lower boiling point forms gas and flows to the reflux cavity, a reflux piece is arranged in the reflux cavity, the gas formed after boiling can form liquid seal through the reflux piece, and the proportion of the liquid with low boiling point in the liquid mixture in the reaction cavity is gradually reduced, so that the reaction temperature of the liquid mixture staying in the reaction cavity is improved.
Description
Technical Field
The utility model belongs to the technical field of the chemical industry, concretely relates to simple and easy ordinary pressure rises mixed system reaction temperature's device down.
Background
In common chemical reactions, many of the reactions are required to be carried out under high temperature conditions, and in a certain temperature region, the reaction speed is obviously accelerated along with the increase of the temperature. This is because most of the reaction materials require a certain activation energy (material temperature) to be able to carry out the reaction, but the reaction temperature of the mixed solution is often fixed, for example, if methanol and water are mixed in a certain ratio without forming an azeotropic mixture whose boiling point depends on the low boiling point solvent (methanol); if the two substances are miscible and form an azeotrope, most of them form a low boiling mixture, i.e., the boiling point of the mixed system is lower than that of either component; if the two substances are immiscible, for example water and diethyl ether, the boiling point of the system depends on the component with the lower boiling point (diethyl ether).
In order to increase the temperature during the reaction, pressurization is generally used, and the pressurization reaction is not easily realized under laboratory conditions. The reaction system is often accompanied by acid and alkali and other catalytic components, is not suitable for reaction by stainless steel equipment, and the pressurization reaction belongs to a pure closed device, which is not beneficial to conventional experimental operations such as feeding, material separation, quality control, process color and other characteristics in the reaction process; or, the reaction temperature of the material is increased by adopting the tubular reactor, but the tubular reactor also needs to determine the material reaction parameters such as more favorable equipment parameters (height-diameter ratio), reaction temperature, material proportion, catalyst selection and the like on the basis of a laboratory routine experiment, so the tubular reactor is often more suitable for application in an industrial production stage rather than a laboratory parameter research stage, and the operation and parameter control of the tubular reactor are generally more complicated and are not beneficial to operation.
SUMMERY OF THE UTILITY MODEL
To foretell not enough, the utility model provides a simple and easy ordinary pressure rises mixed system reaction temperature's device down can improve the stability of the during operation of leading boots device.
The utility model discloses a realize through following technical scheme:
the utility model provides a simple and easy ordinary pressure rises mixed system reaction temperature's device down, includes the heating member and sets up in the reaction unit of heating member, and reaction unit has the reaction chamber and the backward flow chamber of intercommunication, and the reaction intracavity holds the liquid mixture that multiple liquid mixes, and the backward flow chamber is provided with the backward flow piece, and wherein, the liquid mixture who is located the reaction chamber heats the back to make the lower liquid boiling of boiling point and flow to the backward flow piece, in order to form the liquid seal at the backward flow piece.
Further, the backflow piece is one or more of a wire mesh packing, a ring packing and a spring packing.
Furthermore, the simple device for increasing the reaction temperature of the mixed system at normal pressure also comprises a condenser communicated with the reflux cavity, and the gas flowing through the reflux cavity flows into the condenser to form liquid.
Furthermore, the simple device for increasing the reaction temperature of the mixing system under normal pressure also comprises a receiving container communicated with the condenser, and the communication position of the condenser and the receiving container is lower than the communication position of the condenser and the reflux cavity.
Furthermore, the reaction device also comprises a stirring piece extending into the reaction cavity.
Furthermore, the reaction device also comprises a temperature detection piece extending into the reaction cavity.
The utility model discloses following beneficial effect has:
1. after heating the liquid mixture in the reaction cavity, the liquid with lower boiling point forms gas and flows to the reflux cavity, a reflux piece is arranged in the reflux cavity, the gas formed after boiling can form liquid seal through the reflux piece, and the proportion of the liquid with low boiling point in the liquid mixture in the reaction cavity is gradually reduced, so that the reaction temperature of the liquid mixture staying in the reaction cavity is improved.
2. The condenser can liquefy the gas generated after boiling into liquid again, so that the low boiling point liquid and the high boiling point liquid can be separated conveniently.
3. The communication position of the condenser and the receiving container is lower than the communication position of the condenser and the reflux cavity, and liquid formed in the condenser can flow into the receiving container under the action of gravity, so that the phenomenon that the low-boiling-point liquid flows back to the reaction cavity again to influence the reaction temperature is avoided.
4. The liquid mixture in the reaction cavity is stirred by the stirring piece, so that the temperature of the liquid mixture is homogenized, and meanwhile, each part in the liquid mixture is in a moving state, and the reaction speed is accelerated.
Drawings
FIG. 1 is a schematic diagram illustrating an exemplary embodiment of the present invention;
fig. 2 is a schematic structural diagram illustrating another exemplary embodiment of the present invention.
In the figure: 1. heating element, 2, reaction unit, 21, reaction chamber, 22, reflux chamber, 23, reflux element, 3, condenser, 4, receiving container, 5, stirring element, 6, temperature detection element.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
It should be noted that the terms of orientation such as left, right, up, down, front and back in the embodiments of the present invention are only relative concepts or are referred to the normal use state of the product, i.e. the traveling direction of the product, and should not be considered as limiting.
In addition, it should be noted that the dynamic terms such as "relative movement" mentioned in the embodiments of the present invention include not only a change in position but also a movement in which a state changes without a relative change in position such as rotation or rolling.
Finally, it is noted that when an element is referred to as being "on" or "disposed" to another element, it can be on the other element or intervening elements may also be present. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or intervening elements may also be present.
As shown in fig. 1 and fig. 2, a simple device for raising the reaction temperature of a mixed system under normal pressure comprises a heating element 1 and a reaction device 2 arranged on the heating element 1, wherein the reaction device 2 has a reaction chamber 21 and a reflux chamber 22 which are communicated, a liquid mixture formed by mixing a plurality of liquids is contained in the reaction chamber 21, and the reflux chamber 22 is provided with a reflux member 23, wherein after the liquid mixture in the reaction chamber 21 is heated, the liquid with a lower boiling point is boiled and flows to the reflux member 23, so that a liquid seal is formed on the reflux member 23; after the liquid mixture in the reaction chamber 21 is heated, the liquid with a lower boiling point forms gas and flows into the reflux chamber 22, the reflux piece 23 is arranged in the reflux chamber 22, the gas formed after boiling can form a liquid seal through the reflux piece 23, and the proportion of the liquid with a lower boiling point in the liquid mixture in the reaction chamber 21 is gradually reduced, so that the reaction temperature of the liquid mixture staying in the reaction chamber 21 is improved.
Because the boiling points of all the substances in the liquid mixture are different, the reaction temperature of the mixed solution is always fixed, the boiling point of the liquid mixture is always reduced by the low-boiling-point liquid, the low-boiling-point liquid is heated to become gas, and a liquid seal is formed at the position of the reflux piece 23, so that the reaction temperature of the liquid mixture is gradually increased, and because of the liquid seal formed by the low-boiling-point liquid, the high-boiling-point substance can quickly flow back into the reaction system when reaching the liquid seal, so that the proportion of the high-boiling-point substance and the low-boiling-point substance in the liquid mixture is changed, and the reaction temperature of the whole system is improved.
As for the reaction device 2, a flask can be selected, so that the method is convenient and easy to obtain, the cost is reduced, the operation is simple, and the use is safe.
Wherein, when the liquid seal is formed at the reflux member 23, the liquid seals with different heights can be formed at the reflux member 23 by controlling the heating power of the heating member 1, and the separation of product components is carried out, thereby increasing the boiling point of the reaction system, and achieving the purposes of improving the reaction yield and shortening the reaction time.
In the ionic reaction type of A + B → C + D, the device can selectively remove certain low-boiling point components generated, so that the reaction is carried out in a favorable direction.
The reflux piece 23 is one or more of silk screen packing, ring packing and spring packing; the above fillers are common fillers, are convenient and easy to obtain, are convenient to install and easy to realize, and can be made of single fillers when the backflow piece 23 is formed by the fillers, or different fillers are combined to form the backflow piece, so that different selections are performed according to actual conditions.
The simple device for increasing the reaction temperature of the mixed system under normal pressure also comprises a condenser 3 communicated with the reflux cavity 22, and gas flowing through the reflux cavity 22 flows into the condenser 3 to form liquid; the condenser 3 can re-liquefy the gas generated after boiling into liquid, so that the low boiling point liquid and the high boiling point liquid can be conveniently separated.
Referring to fig. 1, the simple apparatus for raising the reaction temperature of the mixed system at normal pressure further comprises a receiving container 4 communicated with the condenser 3, wherein the communication position between the condenser 3 and the receiving container 4 is lower than the communication position between the condenser 3 and the reflux cavity 22; the communication between the condenser 3 and the receiving container 4 is lower than the communication between the condenser 3 and the reflux cavity 22, and the liquid formed in the condenser 3 can flow into the receiving container 4 under the action of gravity, so that the low-boiling-point liquid is prevented from flowing back to the reaction cavity 21 again to influence the reaction temperature.
The reaction device 2 also comprises a stirring piece 5 extending into the reaction cavity 21; the liquid mixture in the reaction chamber 21 is stirred by the stirrer 5, so that the temperature of the liquid mixture is uniformed, and the reaction speed is increased by moving each part in the liquid mixture.
The reaction device 2 also comprises a temperature detection piece 6 extending into the reaction cavity 21; the temperature of the liquid mixture in the reaction cavity 21 can be detected at any time through the temperature detection piece 6, so that the reaction process is conveniently controlled.
The following will explain the present invention in a specific experiment.
Experiment one
50 g of glycine, 50ml of ethanol, 200ml of toluene and 20 g of 732 resin are refluxed until the reaction is finished to prepare glycine ethyl ester, and the key points of the reaction are water removal and temperature rise. The conventional method is to divide water by toluene reflux, but the reaction has the particularity that ternary azeotrope is formed by toluene-water-ethanol, so that water division is difficult to carry out.
In this experiment, the boiling point of the system was approximately close to the boiling point of ethanol (78 ℃), and the reaction rate was very slow at this temperature, and the reaction was carried out using the apparatus of the present application, and a trace amount of water produced by the reaction, water, toluene, and ethanol formed a ternary azeotropic system. The ternary system is stored in the filler of the filler pipe, so that the water content in the system is reduced (the forward movement of the esterification reaction is promoted), the temperature of the system is increased (90-110 ℃), the yield is greatly increased, and the reaction time is reduced from about 20 hours to about 6 hours.
Experiment two
When methyl benzoate and n-dodecanol are used for transesterification to prepare dodecyl benzoate, the conventional method is that the benzoic acid is made into benzoyl chloride by using thionyl chloride, and then condensed with sodium dodecanol in an inert solvent, wherein the catalysis of transition metal base is used; the yield is low and the post-treatment is difficult.
The device is used for reaction, slightly excessive methyl benzoate and dodecanol are mixed, and ester exchange is directly carried out under the heating condition. The methanol generated by the reaction stays at the lower layer of the reflux piece, and after the methanol serving as an ionic reaction product is continuously separated from the system, the temperature of the system is increased, the forward progress of the reaction is promoted, and the use of a solvent, a catalytic alkali and thionyl chloride which stimulates corrosivity in the traditional reaction is reduced. Meanwhile, the solvent waste caused by the solvent fractionation and the potential safety hazard caused by the solvent waste are avoided.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (6)
1. The utility model provides a simple and easy ordinary pressure rises device of mixed system reaction temperature, its characterized in that, including the heating member and set up in the reaction unit of heating member, reaction unit has reaction chamber and the backward flow chamber of intercommunication, the reaction intracavity holds the liquid mixture that multiple liquid mixes, the backward flow chamber is provided with backward flow spare, wherein, is located the reaction chamber the liquid mixture heats the back to make the lower liquid boiling of boiling point and flow to backward flow spare, with backward flow spare forms the liquid seal.
2. The simple apparatus for raising the reaction temperature of a mixing system under normal pressure according to claim 1, wherein the reflux member is one or more of a wire mesh packing, a ring packing and a spring packing.
3. The simplified apparatus for raising the reaction temperature of a mixing system at atmospheric pressure as set forth in claim 1, further comprising a condenser in communication with the reflux chamber, wherein the gas flowing through the reflux chamber flows into the condenser to form a liquid.
4. The simplified apparatus for raising the reaction temperature of a mixing system under normal pressure as set forth in claim 3, further comprising a receiving vessel in communication with the condenser, wherein the condenser is in communication with the receiving vessel at a position lower than the condenser is in communication with the reflux chamber.
5. The simple apparatus for increasing the reaction temperature of a mixing system under normal pressure as claimed in claim 1, wherein the reaction apparatus further comprises a stirring member extending into the reaction chamber.
6. The apparatus as claimed in claim 1, further comprising a temperature detecting member extending into the reaction chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022483375.1U CN214051620U (en) | 2020-10-30 | 2020-10-30 | Simple device for raising reaction temperature of mixed system under normal pressure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022483375.1U CN214051620U (en) | 2020-10-30 | 2020-10-30 | Simple device for raising reaction temperature of mixed system under normal pressure |
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| CN214051620U true CN214051620U (en) | 2021-08-27 |
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| CN202022483375.1U Active CN214051620U (en) | 2020-10-30 | 2020-10-30 | Simple device for raising reaction temperature of mixed system under normal pressure |
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