CN209901286U - Tubular preparation reaction device for 3-chloro-2-hydroxypropyl trimethyl ammonium chloride - Google Patents
Tubular preparation reaction device for 3-chloro-2-hydroxypropyl trimethyl ammonium chloride Download PDFInfo
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- CN209901286U CN209901286U CN201920498796.6U CN201920498796U CN209901286U CN 209901286 U CN209901286 U CN 209901286U CN 201920498796 U CN201920498796 U CN 201920498796U CN 209901286 U CN209901286 U CN 209901286U
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Abstract
The utility model relates to a chemical products's synthesis technical field, concretely relates to 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride tubular preparation reaction unit, take place the mechanism, dispose the liquid mechanism of joining in marriage of trimethylamine hydrochloride solution and the elevated tank that is equipped with epichlorohydrin including the reaction, the reaction takes place the mechanism and includes the reaction tube, sets up SV type static mixer in the reaction tube, sets up in the cooling jacket outside the reaction tube, the reaction tube is provided with feed inlet and discharge gate, feed inlet and discharge gate are located the both ends of SV type static mixer respectively, join in marriage liquid mechanism and elevated tank and all communicate with the feed inlet. The utility model discloses a device can be fine with reaction raw materials mixing emulsification, the yield is higher, and the cooling effect is good, can carry out the continuous reaction, very big promotion reaction efficiency.
Description
Technical Field
The utility model relates to the technical field of chemical product synthesis, in particular to a tubular preparation reaction device for 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride.
Background
Epoxy chloropropane and trimethylamine hydrochloride are subjected to epoxidation ring-opening reaction to obtain 3-chloro-2-hydroxypropyl trimethyl ammonium chloride which is an important intermediate for preparing L-carnitine. The chemical equation is as follows:
however, there are many disadvantages in the synthesis process: firstly, because two substrates in the reaction have large polarity difference and are completely separated, the two substrates cannot be well mixed and emulsified by common stirring, so the reaction time is long, and the yield is low; secondly, the existing production is intermittent production, and the production efficiency is low; thirdly, the reaction is a strong exothermic reaction, the heat transfer efficiency of the existing kettle type reaction is low, the dropping speed of materials needs to be controlled, the dropping time and the reaction time are too long, and the production efficiency is influenced; how to improve the production efficiency and reduce the reaction time becomes the difficult problem in the preparation operation of the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, aiming at the problems, the utility model is specially designed to solve the problems.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride tubular preparation reaction unit, can be fine mix the emulsification with the reaction raw materials, the yield is higher, and the cooling effect is good, can carry out the continuous reaction, very big promotion reaction efficiency.
The utility model adopts the following technical scheme: the tubular preparation reaction device for the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride comprises a reaction generating mechanism, a liquid preparation mechanism for preparing a trimethylamine hydrochloride solution and a high-level trough filled with epoxy chloropropane, wherein the reaction generating mechanism comprises a reaction tube, an SV (vacuum pressure) type static mixer arranged in the reaction tube and a cooling jacket arranged outside the reaction tube, the reaction tube is provided with a feeding hole and a discharging hole, the feeding hole and the discharging hole are respectively positioned at two ends of the SV type static mixer, and the liquid preparation mechanism and the high-level trough are communicated with the feeding hole.
Preferably, the liquid preparation mechanism comprises a liquid preparation kettle, a trimethylamine head tank, a water head tank, a kettle cover, a stirrer and a pH meter which are arranged in the reaction kettle, and a liquid outlet which is arranged at the bottom of the reaction kettle, wherein the trimethylamine head tank, the water head tank and the kettle cover are arranged at the top of the liquid preparation kettle, the stirrer and the pH meter are arranged in the reaction kettle, and the liquid outlet is communicated with the feed inlet through a liquid conveying pipe.
Preferably, the infusion tube is provided with a metering pump for metering the addition amount of the trimethylamine hydrochloride solution.
Preferably, the reaction tube is a loop-type reaction tube, and a material blocking valve is arranged between the feeding hole and the discharging hole.
Preferably, the reaction tube is provided with an observation mechanism, and the observation mechanism comprises a U-shaped tube, an observation window, a first sampling valve and a second sampling valve, wherein the two ends of the U-shaped tube are communicated with the reaction tube, the observation window is arranged on the transverse tube of the U-shaped tube, and the first sampling valve and the second sampling valve are respectively arranged on the two vertical tubes of the U-shaped tube.
Preferably, the horizontal pipe of U type pipe still is provided with high-pressure air valve and appearance valve, high-pressure air valve and appearance valve branch are located the both sides of observation window.
Preferably, an axial flow pump is arranged at the feeding port of the reaction tube.
Preferably, the cooling jacket is provided with a condensate inlet and a condensate outlet.
The utility model discloses following beneficial effect has: (1) materials can be more fully mixed and emulsified in the reaction tube through the SV type static mixer, the reaction speed is higher, a jacket well cools a reaction system, the cooling energy consumption is lower than that of a kettle type reaction, the consequences of material flushing and side reaction increase caused by over intense heat release are prevented, the reaction can be carried out while feeding, the discharge can be carried out while cooling, and the reaction continuity can be realized;
(2) the tubular reaction occupies small area, a plurality of tubular reactions can be carried out simultaneously, and the reaction efficiency is higher.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
The labels in the figures are: 1-stirring paddle, 2-liquid preparation kettle, 3-kettle cover, 4-water valve, 5-water head tank, 6-stirring motor, 7-trimethylamine head tank, 8-trimethylamine valve, 9-pH meter, 10-bottom valve, 11-liquid conveying pipe, 12-head tank, 13-epichlorohydrin valve, 14-metering pump, 15-condensed water outlet, 16-axial flow pump, 17-cooling jacket, 18-SV type static mixer, 19-reaction pipe, 20-condensed water inlet, 21-first sampling valve, 22-high pressure air valve, 23-observation window, 24-sample outlet valve, 25-second sampling valve, 26-discharge valve, 27-material blocking valve and 28-sampling pipe.
Detailed Description
The following description is made with reference to the accompanying drawings and examples, but not to be construed as limiting the invention.
As shown in fig. 1, the utility model relates to a 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride tubular preparation reaction unit, including reaction generating mechanism, the liquid mechanism of joining in marriage of configuration trimethylamine hydrochloride solution and the elevated tank 12 that is equipped with epichlorohydrin, reaction generating mechanism includes reaction tube 19, set up SV type static mixer 18 in reaction tube 19, set up cooling jacket 17 outside reaction tube 19, reaction tube 19 is provided with feed inlet and discharge gate, feed inlet and discharge gate are located SV type static mixer 18's both ends respectively, join in marriage liquid mechanism and elevated tank 12 and all communicate with the feed inlet.
The utility model discloses a reaction unit, during the reaction, the trimethylamine hydrochloride solution of liquid preparation mechanism and the epichlorohydrin of elevated position silo 12 are added the reaction tube 19 through the feed inlet respectively, and reaction material can more fully mix emulsification through SV type static mixer 18 in reaction tube 19, and reaction rate is faster, and reaction material flows towards the discharge gate of reaction tube 19 end along with SV type static mixer 18, can take out the reaction product from the discharge gate of reaction tube 19 after the reaction is accomplished; the cooling jacket 17 can be fine cool down the reaction system, use the utility model discloses a reaction unit can realize the while feeding reaction, and the while cooling ejection of compact can realize the serialization of reaction.
A discharge valve 26 is arranged at the discharge outlet, an epichlorohydrin valve 13 is arranged between the elevated feed tank 12 and the feed inlet, and a bottom valve 10 is arranged between the liquid distribution mechanism and the feed inlet. The elevated tank 12 is provided with scales for quantitative liquid feeding.
In this embodiment, the liquid preparation mechanism includes a liquid preparation kettle 2, a trimethylamine elevated tank 7, a water elevated tank 5, a kettle cover 3, a stirrer and a pH meter 9, which are arranged in the reaction kettle, and a liquid outlet arranged at the bottom of the reaction kettle, which are arranged at the top of the liquid preparation kettle 2, and the liquid outlet is communicated with the feed inlet through a liquid conveying pipe 11.
A trimethylamine valve 8 is arranged between the trimethylamine head tank 7 and the liquid preparation kettle 2, a water valve 4 is arranged between the water head tank 5 and the liquid preparation kettle 2, and a bottom valve 10 is arranged between the liquid outlet and the feed inlet. Scales are arranged on the trimethylamine elevated tank 7 and the water elevated tank 5 for quantitative liquid adding. The agitator is including setting up in joining in marriage the stirring rake 1 of liquid cauldron 2 and setting up in joining in marriage the outside agitator motor 6 who is connected with stirring rake 1 of liquid cauldron 2.
In this embodiment, the infusion tube 11 is provided with a metering pump 14 for metering the amount of trimethylamine hydrochloride solution to be added.
In this embodiment, the reaction tube 19 is a loop-type reaction tube 19, and a material blocking valve 27 is disposed between the feeding hole and the discharging hole.
The reaction tube 19 is set to be of a loop type, so that incomplete reaction when the reaction raw materials flow from the feed inlet to the discharge outlet of the reaction tube 19 can be avoided, and the reaction raw materials can flow in the reaction tube 19 for a week again, so that the reaction is complete.
In this embodiment, the reaction tube 19 is provided with an observation mechanism, and the observation mechanism includes a U-shaped tube having both ends communicated with the reaction tube 19, an observation window 23 disposed on the horizontal tube of the U-shaped tube, and a first sampling valve 21 and a second sampling valve 25 respectively disposed on two vertical tubes of the U-shaped tube.
Still be provided with sampling tube 28 on the U type pipe, make things convenient for the experimenter to take a sample. The degree of reaction can be observed at any time through observation window 23, and during the reaction, the accessible is observed the material and is had an interpretation reaction condition by separating liquid-muddy-emulsification-clear change, but the reaction condition is comparatively difficult to the clear observation reaction situation of current kettle formula, and when sample gas phase analysis raw materials consumption degree, need open 3 samples of kettle cover, and the volatilizing of solution can influence the operator healthy, also can cause environmental pollution the utility model discloses set up the reaction window and can clearly observe the reaction situation, sampling device makes things convenient for the operating personnel sample more, and under the condition that the individual reaction has not completely gone on, can circulate continuation reaction. The direction from the feeding hole to the discharging hole is defined to be from front to back, and the discharging hole is positioned behind the observation mechanism.
In this embodiment, the horizontal tube of the U-shaped tube is further provided with a high-pressure air valve 22 and a sample outlet valve 24, and the high-pressure air valve 22 and the sample outlet valve 24 are respectively arranged on two sides of the observation window 23.
In this embodiment, an axial flow pump 16 is disposed at the feed inlet of the reaction tube 19.
The solution of the reaction material can be made to flow better from the inlet port to the outlet port by the axial flow pump 16.
In this embodiment, the cooling jacket 17 is provided with a condensate inlet 20 and a condensate outlet 15.
The cooling purpose is achieved by introducing condensed water into the cooling jacket 17.
The utility model discloses a theory of operation is: before working, all valves are closed. A water valve 4 is opened to add a certain amount of water into the liquid preparation kettle 2. And starting the stirring motor 6 to drive the stirring paddle 1 to stir the solution in the kettle. Opening the kettle cover 3, and adding a certain amount of trimethylamine hydrochloride solid to prepare the trimethylamine hydrochloride solution. And opening a trimethylamine valve, dropwise adding the trimethylamine solution into the solution in the kettle, and adjusting the pH value to 8.5, wherein the pH value is read by a pH meter 9. The reaction tube 19 is cooled by introducing condensed water into the cooling jacket 17. The axial flow pump 16, the bottom valve 10, the first sampling valve 21, the second sampling valve 25 and the discharge valve 26 are opened. Then, the epichlorohydrin valve 13 and the metering pump 14 are simultaneously opened, and the epichlorohydrin and the prepared trimethylamine hydrochloride solution are injected into the reaction tube 19 to carry out tubular reaction according to a certain proportion relation. The solution is mixed and reacted by an SV type static mixer, and is cooled by a cooling jacket, so that the generation of flushing and side reaction caused by reaction overheating is prevented. The final reaction can be monitored through the observation window 23, and when the solution reaches the discharge valve 26, the metering pump 14, the epichlorohydrin valve 13, the axial flow pump 16, the first sampling valve 21 and the second sampling valve 25 are closed. The high pressure air valve 22 and the sample outlet valve 24 are opened, and the sample in the sampling tube 28 is pressed out by the high pressure air for sampling gas phase analysis. If the reaction liquid is qualified, the axial flow pump 16 is started to discharge qualified reaction liquid out of the reaction pipe 19 through the discharge valve 26. If the reaction is not completed, the high-pressure air valve 22 and the sample outlet valve 24 are closed, the material blocking valve 27, the axial-flow pump 16, the first sampling valve 21 and the second sampling valve 25 are opened, the reaction liquid is circulated and reacted in the reaction pipe 19 again, and after the sampling is qualified, the material blocking valve 27 is closed, and the reaction liquid is discharged out of the system. And opening an epichlorohydrin valve 13 and a metering pump 14 to perform the next reaction process. Through the accumulation of experimental experience of a certain time, the length of the reaction tube 19 can be determined according to the reaction time, and the reaction raw materials are completely reacted in the flowing process from the feeding hole to the discharging hole, so that the step of sampling and analyzing can be omitted in the reaction process, and continuous feeding and discharging of the continuous reaction are realized.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood that the invention is not limited thereto, and that various modifications and changes can be made by those skilled in the art without departing from the principles of the invention.
Claims (8)
1. A tubular preparation reaction device of 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride is characterized in that: the reaction generating mechanism comprises a reaction tube, an SV type static mixer arranged in the reaction tube and a cooling jacket arranged outside the reaction tube, wherein the reaction tube is provided with a feed inlet and a discharge outlet which are respectively arranged at two ends of the SV type static mixer, and the liquid preparing mechanism and the high-level trough are communicated with the feed inlet.
2. The tubular preparation reaction device of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 1, wherein: the liquid preparation mechanism comprises a liquid preparation kettle, a trimethylamine head tank, a water head tank, a kettle cover, a stirrer and a pH meter which are arranged in the reaction kettle, and a liquid outlet which is arranged at the bottom of the reaction kettle, wherein the trimethylamine head tank, the water head tank and the kettle cover are arranged at the top of the liquid preparation kettle, the stirrer and the pH meter are arranged in the reaction kettle, and the liquid outlet is communicated with the feed inlet through a liquid conveying pipe.
3. The tubular production reaction apparatus of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 2, characterized in that: the infusion tube is provided with a metering pump for metering the addition amount of the trimethylamine hydrochloride solution.
4. The tubular preparation reaction device of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 1, wherein: the reaction tube is a loop type reaction tube, and a material blocking valve is arranged between the feeding hole and the discharging hole.
5. The tubular preparation reaction device of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 1, wherein: the reaction tube is provided with an observation mechanism, the observation mechanism comprises a U-shaped tube, an observation window, a first sampling valve and a second sampling valve, wherein the two ends of the U-shaped tube are communicated with the reaction tube, the observation window is arranged on the transverse tube of the U-shaped tube, and the first sampling valve and the second sampling valve are respectively arranged on the two vertical tubes of the U-shaped tube.
6. The tubular production reaction apparatus of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 5, wherein: the horizontal pipe of U type pipe still is provided with high-pressure air valve and appearance valve, high-pressure air valve and appearance valve branch are located the both sides of observation window.
7. The tubular preparation reaction device of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 1, wherein: and an axial flow pump is arranged at the feed inlet of the reaction tube.
8. The tubular preparation reaction device of 3-chloro-2-hydroxypropyltrimethylammonium chloride according to claim 1, wherein: the cooling jacket is provided with a condensed water inlet and a condensed water outlet.
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CN201920498796.6U CN209901286U (en) | 2019-04-12 | 2019-04-12 | Tubular preparation reaction device for 3-chloro-2-hydroxypropyl trimethyl ammonium chloride |
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CN201920498796.6U CN209901286U (en) | 2019-04-12 | 2019-04-12 | Tubular preparation reaction device for 3-chloro-2-hydroxypropyl trimethyl ammonium chloride |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114427881A (en) * | 2021-10-12 | 2022-05-03 | 福建龙氟化工有限公司 | Double-scale metering device for hydrogen fluoride production and metering method thereof |
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2019
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114427881A (en) * | 2021-10-12 | 2022-05-03 | 福建龙氟化工有限公司 | Double-scale metering device for hydrogen fluoride production and metering method thereof |
CN114427881B (en) * | 2021-10-12 | 2023-09-29 | 福建省龙氟新材料有限公司 | Double weighing apparatus metering device for hydrogen fluoride production and metering method thereof |
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Granted publication date: 20200107 Termination date: 20210412 |
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CF01 | Termination of patent right due to non-payment of annual fee |