Acylation reaction kettle feeding system for preparing propargite technical intermediate through acylation reaction of aromatic cyclic alcohol and thionyl chloride
By designing a feeding system for the acylation reactor, precise control of the reactor temperature and continuous dripping of thionyl chloride were achieved, solving the problem of difficult temperature control in the acylation reactor and improving the production stability and automation level of propargite technical intermediate.
Patent Information
- Application Number
- CN202422705349.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-06
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2034-11-06
AI Technical Summary
In the existing technology, it is difficult to control the temperature of the acylation reactor for aromatic alcohols and thionyl chloride to be between -10 and -5°C, which affects the smooth progress of the acylation reaction. In addition, the addition of thionyl chloride is discontinuous, resulting in unstable production.
An acylation reactor feeding system was designed. The reactor temperature is monitored through an interlocking loop. A level gauge and flow meter are installed in the thionyl chloride high-level tank to achieve temperature control and continuous dripping of thionyl chloride. Combined with a cooling medium, the reactor temperature is maintained and integrated into a remote operation and automation control system.
The temperature of the acylation reactor was stably controlled at -10 to -5℃, ensuring the smooth progress of the acylation reaction and the continuous addition of thionyl chloride, thereby improving the stability and automation of the production process.
Smart Images
Figure CN223517468U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the production technology field of propargite, and particularly relates to an acylation reaction kettle feeding system for preparing a propargite intermediate through acylation reaction of aromatic ring alcohol and thionyl chloride. BACKGROUND
[0002] In the production of propargite, crude aromatic ring alcohol is generated from p-tert-butyl phenol and epoxy cyclohexane under alkaline conditions, the crude aromatic ring alcohol is washed with water and then acylated with thionyl chloride to generate a propargite intermediate, and the propargite intermediate is condensed with triethylamine and propargyl alcohol in toluene solvent to generate crude propargite, which is washed with water and desolventized to obtain propargite product. The specific process flow is as follows:
[0003] (1) Addition process: a certain amount of p-tert-butyl phenol and alkali solution is added to a synthesis kettle, a certain amount of epoxy cyclohexane is added dropwise, the temperature is raised to 100 DEG C after dropping, and the epoxy cyclohexane is removed after 8 hours of preservation, and finally the crude aromatic ring alcohol is obtained.
[0004] (2) Water washing of crude aromatic ring alcohol process: the crude aromatic ring alcohol in the synthesis kettle after removal of epoxy cyclohexane is transferred to a water washing kettle, a certain amount of alkali solution is added, and after stirring at 100 DEG C for 30 min, a certain amount of toluene and hot water are added through a slightly open steam valve, and after stirring at 70 DEG C for 30 min, the kettle is kept at 70 DEG C for 60 min. After the preservation, water is first removed, and after the first water removal, the stirring is started to add the prepared hot water into the water washing kettle, and after 30 min of stirring, the stirring is stopped and the kettle is kept at 70 DEG C for 60 min. After the preservation, the water is removed. After the second water removal, the above operation is repeated for the third water removal, and after the water removal, the pH value is measured, and then a certain amount of hydrochloric acid is taken from the hydrochloric acid absorption tank and added into the water washing kettle to adjust the pH value to 7. After the third water removal, the above operation is repeated for the fourth water removal. After the suspension separation, the toluene is removed by starting the vacuum pump. The desolventization is performed until the vacuum degree is greater than or equal to -0.098 MPa, and the maximum temperature is not higher than 130 DEG C.
[0005] (3) Acylation process: the aromatic ring alcohol toluene solution is transferred into an acylation reaction kettle, the stirring is started, the temperature is lowered to -10 DEG C to -5 DEG C, and then the thionyl chloride is added dropwise. After the dropping, the kettle is kept still, and then the vacuum pump is started to remove the thionyl chloride, and the propargite intermediate used in the condensation process is obtained.
[0006] (4) Condensation process: the toluene, triethylamine and propargyl alcohol are sequentially added into the acylation reaction kettle, the stirring is started, the temperature is lowered to a certain temperature, the propargite intermediate is added dropwise, and the propargite toluene solution is obtained after the preservation.
[0007] (5) water washing process: the propargite toluene solution is transferred into a water washing kettle, a certain amount of water is added, stirring is started, the pH value of the material is adjusted with dilute hydrochloric acid, and triethylamine hydrochloride is transferred into a triethylamine treatment kettle.
[0008] (6) desolventizing process: the water washed original drug is transferred into a toluene removal kettle, toluene is removed under a certain vacuum degree and temperature to obtain qualified propargite product.
[0009] In the acylation reaction of the water washed crude aromatic ring alcohol and thionyl chloride, the temperature of the acylation reaction kettle needs to be ensured at-10 to-5℃, otherwise the smooth progress of the acylation reaction will be affected. In addition, during the acylation reaction, thionyl chloride needs to be continuously added to ensure the continuous reaction and the normal operation of the production. Technical scheme of the utility model
[0010] The technical problem to be solved by the utility model is to overcome the shortcomings of the prior art, provide an acylation reaction kettle feeding system for preparing propargite original drug intermediates through acylation reaction of aromatic ring alcohol and thionyl chloride, realize the monitoring of the temperature of the acylation reaction kettle through an interlocking loop, keep the temperature at-10 to-5℃, ensure the smooth progress of the acylation reaction, and enable the whole system to realize remote operation and automatic control.
[0011] The technical scheme of the utility model is:
[0012] The acylation reaction kettle feeding system for preparing propargite original drug intermediates through acylation reaction of aromatic ring alcohol and thionyl chloride is connected with a thionyl chloride feeding pipeline, a toluene feeding pipeline, an aromatic ring alcohol feeding pipeline, a propargite original drug intermediate discharge pipeline and a hydrogen chloride tail gas discharge pipeline, a thionyl chloride feeding valve is arranged on the thionyl chloride feeding pipeline, a toluene feeding valve is arranged on the toluene feeding pipeline, an aromatic ring alcohol feeding valve is arranged on the aromatic ring alcohol feeding pipeline, and a vent valve is arranged on the hydrogen chloride tail gas discharge pipeline; the acylation reaction kettle is provided with a temperature sensor, and a cooling medium feeding pipeline and a cooling medium discharge pipeline are connected to the jacket of the acylation reaction kettle, and a cooling medium feeding valve is arranged on the cooling medium feeding pipeline; the thionyl chloride feeding pipeline is connected with a thionyl chloride high tank, the thionyl chloride high tank is connected with a thionyl chloride feeding pipeline, and a thionyl chloride feeding valve is arranged on the thionyl chloride feeding pipeline; the thionyl chloride feeding valve, the toluene feeding valve, the aromatic ring alcohol feeding valve, the vent valve, the temperature sensor, the cooling medium feeding valve and the thionyl chloride feeding valve are electrically connected with a control system.
[0013] Preferably, the thionyl chloride high tank is provided with a liquid level meter, and the liquid level meter is electrically connected with the control system.
[0014] Preferably, a thionyl chloride flow meter is arranged on the thionyl chloride feeding pipeline, and the thionyl chloride flow meter is electrically connected with the control system.
[0015] Preferably, a toluene flow meter is arranged on the toluene feeding pipeline, and the toluene flow meter is electrically connected with the control system.
[0016] Preferably, the acylation reactor is provided with a stirrer.
[0017] Preferably, the cooling medium fed into the cooling medium feeding pipeline is refrigerated brine.
[0018] Compared with the prior art, the acylation reactor feeding system for preparing an intermediate of an original fenbutatin-oxide by acylation reaction of aromatic ring alcohol and thionyl chloride has the following beneficial effects:
[0019] The acylation reactor feeding system for preparing an intermediate of an original fenbutatin-oxide by acylation reaction of aromatic ring alcohol and thionyl chloride of the utility model realizes the monitoring of the temperature of the acylation reactor through an interlock loop, so that the temperature of the acylation reactor is kept at-10 to-5 DEG C, thereby ensuring the smooth progress of the acylation reaction. In addition, the utility model also realizes the liquid level safety interlock of the thionyl chloride high tank, ensures the continuous dropping of the thionyl chloride, ensures the normal operation of the production, and enables the whole system to realize remote operation and automatic control. BRIEF DESCRIPTION OF DRAWINGS
[0020] Figure 1 is a structure schematic view of the acylation reactor feeding system for preparing an intermediate of an original fenbutatin-oxide by acylation reaction of aromatic ring alcohol and thionyl chloride of the utility model.
[0021] In the figure, 1, acylation reactor; 101, stirrer; 102, jacket; 2, thionyl chloride feeding pipeline; 201, thionyl chloride feeding valve; 202, thionyl chloride flow meter; 3, toluene feeding pipeline; 301, toluene feeding valve; 302, toluene flow meter; 4, aromatic ring alcohol feeding pipeline; 401, aromatic ring alcohol feeding valve; 5, intermediate of an original fenbutatin-oxide outfeeling pipeline; 6, hydrogen chloride tail gas outfeeling pipeline; 601, vent valve; 7, temperature sensor; 8, cooling medium feeding pipeline; 801, cooling medium feeding valve; 9, cooling medium outfeeling pipeline; 10, thionyl chloride high tank; 11, thionyl chloride feeding pipeline; 1101, thionyl chloride feeding valve; 12, liquid level meter. DETAILED DESCRIPTION
[0022] In order to enable the personnel in the technical field to better understand the technical scheme in the utility model, the technical scheme of the utility model will be described clearly and completely in combination with the embodiments of the utility model.
[0023] Embodiment 1
[0024] As Figure 1As shown, the embodiment provides an acylation reactor feed system for preparing an azocyclotin intermediate from aromatic alcohol and thionyl chloride through acylation reaction. The acylation reactor 1 is connected with a thionyl chloride feed pipeline 2, a toluene feed pipeline 3, an aromatic alcohol feed pipeline 4, an azocyclotin intermediate discharge pipeline 5 and a hydrogen chloride tail gas discharge pipeline 6. The acylation reactor 1 is provided with a stirrer 101. The thionyl chloride feed pipeline 2 is provided with a thionyl chloride feed valve 201. The toluene feed pipeline 3 is provided with a toluene feed valve 301. The aromatic alcohol feed pipeline 4 is provided with an aromatic alcohol feed valve 401. The hydrogen chloride tail gas discharge pipeline 6 is provided with a vent valve 601.
[0025] As shown in the figure, Figure 1 The acylation reactor 1 is provided with a temperature sensor 7. The jacket 102 of the acylation reactor 1 is connected with a cooling medium feed pipeline 8 and a cooling medium discharge pipeline 9. The cooling medium fed into the cooling medium feed pipeline 8 is refrigerated brine. The cooling medium feed pipeline 8 is provided with a cooling medium feed valve 801. The thionyl chloride feed pipeline 2 is connected with a thionyl chloride high tank 10. The thionyl chloride high tank 10 is connected with a thionyl chloride supplement pipeline 11. The thionyl chloride supplement pipeline 11 is provided with a thionyl chloride supplement valve 1101. The thionyl chloride feed valve 201, the toluene feed valve 301, the aromatic alcohol feed valve 401, the vent valve 601, the temperature sensor 7, the cooling medium feed valve 801 and the thionyl chloride supplement valve 1101 are electrically connected with the control system.
[0026] As shown in the figure, Figure 1 The thionyl chloride high tank 10 is provided with a liquid level meter 12. The thionyl chloride feed pipeline 2 is provided with a thionyl chloride flow meter 202. The toluene feed pipeline 3 is provided with a toluene flow meter 302. The liquid level meter 12, the thionyl chloride flow meter 202 and the toluene flow meter 302 are electrically connected with the control system.
[0027] Working principle:
[0028] 1) Preparation stage
[0029] When the thionyl chloride is prepared, the thionyl chloride supplement valve 1101 of the thionyl chloride high tank 10 is opened, the thionyl chloride feed valve 201 is closed, and the thionyl chloride is filled into the thionyl chloride high tank 10. The low limit value and the high limit value of the liquid level of the thionyl chloride high tank 10 are preset in the control system. When the liquid level reaches the preset high limit value, the thionyl chloride supplement valve 1101 is closed. When the thionyl chloride is added dropwise into the acylation reactor 1 in the subsequent process, when the liquid level of the thionyl chloride high tank 10 reaches the low limit value, the control system opens the thionyl chloride supplement valve 1101 to supplement the thionyl chloride into the thionyl chloride high tank 10, so that the liquid level reaches the high limit value, thereby ensuring the smooth progress of the acylation reaction.
[0030] 2) Feeding stage
[0031] After the preparation of thionyl chloride is completed, a certain amount of toluene solvent is added to the acylation reaction kettle 1 through the toluene feeding valve 301 and the toluene flowmeter 302, and the cooling medium feeding valve 801 of the acylation reaction kettle 1 jacket 102 is opened, the temperature value range of the temperature sensor 7 in the control system is preset, the temperature of the acylation reaction kettle 1 is kept at-10~ -5℃ by adjusting the opening of the cooling medium feeding valve 801, when the temperature sensor 7 detects that the temperature of the acylation reaction kettle 1 reaches the preset range, the thionyl chloride feeding valve 201 is opened, and a certain amount of thionyl chloride is added to the acylation reaction kettle 1 at one time. In the aromatic ring alcohol feeding stage, the aromatic ring alcohol feeding valve 401 and the vent valve 601 of the acylation reaction kettle 1 are opened, and when the weighing module of the acylation reaction kettle 1 reaches the set value, the aromatic ring alcohol feeding valve 401 is closed, and the acylation reaction is started by dropping thionyl chloride into the acylation reaction kettle 1 through the thionyl chloride feeding valve 201 and the thionyl chloride flowmeter 202.
Claims
1. An acylation reactor feed system for the preparation of an intermediate for the acylation of fenpyroximate technical material by acylation of an aromatic ring alcohol with thionyl chloride, characterized in that, The acylation reaction kettle (1) is connected with a thionyl chloride feeding pipeline (2), a toluene feeding pipeline (3), an aromatic ring alcohol feeding pipeline (4), a propargite original pesticide intermediate discharging pipeline (5) and a hydrogen chloride tail gas discharging pipeline (6), the thionyl chloride feeding pipeline (2) is provided with a thionyl chloride feeding valve (201), the toluene feeding pipeline (3) is provided with a toluene feeding valve (301), the aromatic ring alcohol feeding pipeline (4) is provided with an aromatic ring alcohol feeding valve (401), and the hydrogen chloride tail gas discharging pipeline (6) is provided with a vent valve (601); the acylation reaction kettle (1) is provided with a temperature sensor (7), and the jacket (102) of the acylation reaction kettle (1) is connected with a cooling medium feeding pipeline (8) and a cooling medium discharging pipeline (9), and the cooling medium feeding pipeline (8) is provided with a cooling medium feeding valve (801); the thionyl chloride feeding pipeline (2) is connected with a thionyl chloride high-level tank (10), the thionyl chloride high-level tank (10) is connected with a thionyl chloride supplement pipeline (11), and the thionyl chloride supplement pipeline (11) is provided with a thionyl chloride supplement valve (1101); the thionyl chloride feeding valve (201), the toluene feeding valve (301), the aromatic ring alcohol feeding valve (401), the vent valve (601), the temperature sensor (7), the cooling medium feeding valve (801) and the thionyl chloride supplement valve (1101) are electrically connected with a control system.
2. The acylation reactor feed system for preparing the intermediate of the fenbutatin oxide original drug by acylation reaction of the aromatic ring alcohol and the sulfuric chloride according to claim 1, characterized in that, The thionyl chloride high-level tank (10) is provided with a liquid level meter (12), and the liquid level meter (12) is electrically connected with the control system.
3. The acylation reactor feed system for preparing the intermediate of the fenbutatin oxide original pesticide by acylation reaction of the aromatic ring alcohol and the sulfuric chloride according to claim 1, characterized in that, The thionyl chloride feeding pipeline (2) is provided with a thionyl chloride flow meter (202), and the thionyl chloride flow meter (202) is electrically connected with the control system.
4. The acylation reactor feed system for preparing the intermediate of the fenbutatin oxide original pesticide by acylation reaction of the aromatic ring alcohol and the sulfuric chloride according to claim 1, characterized in that, The toluene feeding pipeline (3) is provided with a toluene flow meter (302), and the toluene flow meter (302) is electrically connected with the control system.
5. The acylation reactor feed system for the preparation of the intermediate of the fenbutatin oxide original drug by acylation reaction of the aromatic ring alcohol and the sulfuric chloride, according to claim 1, characterized in that, The acylation reaction kettle (1) is provided with a stirrer (101).
6. The acylation reactor feed system for the preparation of the intermediate of the fenbutatin oxide original drug by acylation reaction of the aromatic ring alcohol and the sulfuric chloride, according to claim 1, characterized in that, The cooling medium fed into the cooling medium feeding pipeline (8) is refrigerated brine.