CN214416006U - HCl absorbing device of low water content for trimethyl orthoacetate - Google Patents
HCl absorbing device of low water content for trimethyl orthoacetate Download PDFInfo
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- CN214416006U CN214416006U CN202022700962.1U CN202022700962U CN214416006U CN 214416006 U CN214416006 U CN 214416006U CN 202022700962 U CN202022700962 U CN 202022700962U CN 214416006 U CN214416006 U CN 214416006U
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Abstract
The utility model discloses a trimethyl orthoacetate is with HCl absorbing device of low water content, including absorption cauldron, desicator and agitator, be equipped with the HCl charge door on the HCl charge door, the desicator setting is at the top of HCl charge door, and the desicator passes through HCl charge door and absorption cauldron intercommunication, and in the agitator stretched into absorption cauldron, absorption cauldron's upper portion was equipped with liquid charge door and nitrogen gas entry, and absorption cauldron's bottom was equipped with liquid discharge mouth 7. The dryer is a multi-stage dryer, the nonpolar solvent is added into the absorption kettle through a liquid charging port, and nitrogen is introduced into the absorption kettle through a nitrogen inlet. The utility model discloses a physical drying (multistage/single-stage desicator) and nitrogen protection (let in nitrogen atmosphere protection) synergism have reduced the water content who gets into among the HCl absorbing device. The HCl absorption device further comprises a refrigerant jacket, the refrigerant jacket is arranged at the lower part of the absorption kettle and attached to the outer side of the absorption kettle, a refrigerant inlet is formed in the bottom of the refrigerant jacket, and a refrigerant outlet is formed in the upper part of the refrigerant jacket.
Description
Technical Field
The utility model belongs to the technical field of chemical product production, concretely relates to HCl absorbing device of low water content for trimethyl orthoacetate.
Background
Trimethyl orthoacetate, also known as 1,1, 1-trimethoxyethane, is an important orthoester. The structural formula is CH3C (OCH3) 3. Is insoluble in water, and soluble in organic solvent such as ethanol and diethyl ether. Mainly used as an organic intermediate for synthesizing medicines and pesticides. Trimethyl orthoacetate is an intermediate raw material for synthesizing pyrethrin pesticides such as cypermethrin, cyhalothrin and the like; is also a synthetic vitamin B1And A1Intermediates required for sulfadiazine drugs; it can also be used as raw material for producing dye, perfume, food additive, and paint.
At present, the main synthesis method of trimethyl orthoacetate is as follows: acetonitrile, methanol and dry hydrogen chloride are used as raw materials, in the presence of a non-polar solvent, ethylimine methyl ether hydrochloride is prepared, and trimethyl orthoacetate is generated through methanol alcoholysis. Trimethyl orthoacetate is easy to decompose when meeting water, so that moisture existing in a reaction system is one of main factors influencing the product yield, and the requirements of methanol, acetonitrile and an organic solvent in raw materials on the moisture content are severe, but the total moisture content still reaches 0.2 percent or even higher. After the small amount of water is brought into a reaction system, the synthesis yield is reduced, and the removal and reduction of the water in the system by taking measures becomes an important way for improving the product yield.
A plurality of unit equipment are involved in the production process of trimethyl orthoacetate, and an HCl absorption device is one of basic equipment and is key equipment for effectively reducing water substituted into a reaction system.
SUMMERY OF THE UTILITY MODEL
To the deficiencies existing in the prior art, the object of the utility model is to provide a HCl absorbing device with low water content for trimethyl orthoacetate.
In order to achieve the above purpose, the technical scheme of the utility model is that: a HCl absorbing device with low water content for trimethyl orthoacetate is characterized in that: including absorption cauldron, desicator and agitator, be equipped with the HCl charge door on the absorption cauldron, the desicator setting is at the top of HCl charge door, and the desicator passes through HCl charge door and absorption cauldron intercommunication, and in the agitator stretched into the absorption cauldron, the upper portion of absorption cauldron was equipped with liquid charge door and nitrogen gas entry.
Furthermore, the HCl absorption device further comprises a refrigerant jacket, the refrigerant jacket is arranged at the lower part of the absorption kettle, the refrigerant jacket is attached to the outer side of the absorption kettle, a refrigerant inlet is formed in the bottom of the refrigerant jacket, and a refrigerant outlet is formed in the upper part of the refrigerant jacket.
Furthermore, a conduit is arranged at the lower part of the HCl feeding port, one end of the conduit is communicated with the HCl feeding port, and the other end of the conduit extends into the absorption kettle to be below the liquid level of the added nonpolar solvent.
Furthermore, the HCl absorption device further comprises a transmission device, the transmission device is arranged at the top of the absorption kettle, one end of the stirrer is connected with the transmission device, and the other end of the stirrer stirs liquid in the absorption kettle.
Further, a cooling medium enters the refrigerant jacket from a refrigerant inlet, the temperature in the absorption kettle is controlled to be 0-minus 5 ℃, nitrogen is introduced into the absorption kettle through the nitrogen inlet to fully replace the air in the reaction kettle, quantitative anhydrous methanol is added into the absorption kettle through the liquid charging port, and after the anhydrous methanol is uniformly stirred, HCl is introduced into the absorption kettle through the drier and the HCl charging port.
Further, the desicator is the multilayer desicator, and transmission is the motor, and the agitator includes stirring head and connecting axle, and the one end of connecting axle and the output shaft of motor, stirring head connection are at the other end of connecting axle.
Adopt the utility model discloses technical scheme's advantage does:
1. the nitrogen is required to be continuously introduced for better reducing the moisture in the system; in order to obtain better HCl absorption effect, a mode of introducing HCl gas under liquid is preferably adopted; in order to obtain better HCl gas drying effect, a multi-stage dryer is adopted compared with a single-stage dryer.
2. The utility model reduces the water content entering the HCl absorption device through the synergistic effect of physical drying (multi-stage dryer) and nitrogen protection (nitrogen atmosphere protection is introduced); the absorption device has high HCl absorption efficiency, the water content is lower than 500ppm, and the absorption device provides guarantee for improving the subsequent reaction conversion rate and the product yield.
Drawings
The invention will be described in further detail with reference to the following drawings and detailed description:
fig. 1 is a schematic structural view of the HCl absorption device of the present invention.
The labels in the above figures are respectively: 1. a dryer; 2. an HCl feed port; 3. a nitrogen inlet; 4. a refrigerant outlet; 5. a stirrer; 51. a stirring head; 52. a connecting shaft; 6. a refrigerant inlet; 7. a liquid discharge port; 8. A conduit; 9. a refrigerant jacket; 11. a liquid feed port; 12. a transmission device; 13. and (5) an absorption kettle.
Detailed Description
In the present invention, it is to be understood that the term "length"; "Width"; "Up"; "Down"; "front"; "Back"; "left"; "Right"; "vertical"; "horizontal"; "Top"; "bottom" "inner"; "outer"; "clockwise"; "counterclockwise"; "axial"; "planar direction"; the directional or positional relationship indicated as "circumferential" or the like is based on the directional or positional relationship shown in the drawings, and is only for convenience of description and simplified description, and does not indicate or imply that the device or element referred to must have a particular orientation; constructed and operative in a particular orientation and therefore should not be construed as limiting the invention.
As shown in figure 1, a HCl absorption device with low water content for trimethyl orthoacetate is characterized in that: including absorption kettle 13, desicator 1 and agitator 5, be equipped with HCl charge door 2 on absorption kettle 13, desicator 1 sets up at the top of HCl charge door 2, and desicator 1 communicates with absorption kettle 13 through HCl charge door 2, and agitator 5 stretches into in absorption kettle 13, and absorption kettle 13's upper portion is equipped with liquid charge door 11 and nitrogen gas entry 3, and absorption kettle 13's bottom is equipped with liquid discharge gate 7. The dryer 1 is a multistage dryer, the nonpolar solvent is added into the absorption kettle through a liquid feed inlet 11, and nitrogen is introduced into the absorption kettle 13 through a nitrogen inlet 3. The utility model discloses a physical drying (multistage/single-stage desicator) and nitrogen protection (let in nitrogen atmosphere protection) synergism have reduced the water content who gets into among the HCl absorbing device.
The HCl absorption device further comprises a cooling medium jacket 9, the cooling medium jacket 9 is arranged at the lower part of the absorption kettle 13, the cooling medium jacket 9 is attached to the outer side of the absorption kettle 13, a cooling medium inlet 6 is arranged at the bottom of the cooling medium jacket 9, and a cooling medium outlet 4 is arranged at the upper part of the cooling medium jacket 9.
The lower part of the HCl feeding port 2 is provided with a conduit 8, one end of the conduit 8 is communicated with the HCl feeding port 2, and the other end of the conduit 8 extends into the absorption kettle 13 to be below the liquid level of the added nonpolar solvent.
The HCl absorption device further comprises a transmission device 12, the transmission device 12 is arranged at the top of the absorption kettle 13, one end of the stirrer 5 is connected with the transmission device 12, and the other end of the stirrer 5 stirs liquid in the absorption kettle 13. The transmission device 12 is a motor, the stirrer 5 comprises a stirring head 51 and a connecting shaft 52, one end of the connecting shaft 52 is connected with an output shaft of the motor, and the stirring head 51 is connected at the other end of the connecting shaft 52.
Firstly, a nonpolar solvent is added into an absorption kettle through a liquid charging port 11, a refrigerant medium is started, the refrigerant medium enters a refrigerant jacket 9 through a refrigerant inlet 6, the temperature in the absorption kettle 13 is controlled to be 0-5 ℃, in order to prevent moisture in air from entering absorption in the cooling process, nitrogen is introduced into the absorption kettle through a nitrogen inlet 3, after the air in the reaction kettle is fully replaced, quantitative anhydrous methanol is added into the absorption kettle 13 through the liquid charging port 11, and after the stirring is uniform, HCl is introduced into the absorption kettle through a drier 1 through an HCl charging port 2, so that HCl gas is fully absorbed.
In order to better reduce the moisture in the system, the nitrogen needs to be continuously introduced; in order to obtain better HCl absorption effect, a mode of introducing HCl gas under liquid is preferably adopted; in order to obtain better HCl gas drying effect, a multi-stage dryer is adopted compared with a single-stage dryer.
The utility model reduces the water content entering the HCl absorption device through the synergistic effect of physical drying (multi-stage dryer) and nitrogen protection (nitrogen atmosphere protection is introduced); the absorption device has high HCl absorption efficiency, the water content is lower than 500ppm, and the absorption device provides guarantee for improving the subsequent reaction conversion rate and the product yield.
The present invention has been described above with reference to the accompanying drawings, and it is obvious that the present invention is not limited by the above-mentioned manner, and various insubstantial improvements can be made without the technical solutions of the present invention, or the present invention can be directly applied to other occasions without the improvements, and all are within the protection scope of the present invention.
Claims (6)
1. A HCl absorbing device with low water content for trimethyl orthoacetate is characterized in that: including reation kettle (13), desicator (1) and agitator (5), be equipped with HCl charge door (2) on reation kettle (13), desicator (1) sets up the top at HCl charge door (2), and desicator (1) communicates with reation kettle (13) through HCl charge door (2), and in agitator (5) stretched into reation kettle (13), the upper portion of reation kettle (13) was equipped with liquid charge door (11) and nitrogen gas entry (3).
2. The apparatus for absorbing HCl with low water content for trimethyl orthoacetate according to claim 1, wherein: the HCl absorption device further comprises a cooling medium jacket (9), the cooling medium jacket (9) is arranged at the lower part of the absorption kettle (13), the cooling medium jacket (9) is attached to the outer side of the absorption kettle (13), a cooling medium inlet (6) is formed in the bottom of the cooling medium jacket (9), and a cooling medium outlet (4) is formed in the upper part of the cooling medium jacket (9).
3. The apparatus for absorbing HCl with low water content for trimethyl orthoacetate according to claim 1 or 2, wherein: the lower part of the HCl feeding port (2) is provided with a conduit (8), one end of the conduit (8) is communicated with the HCl feeding port (2), and the other end of the conduit (8) extends into the absorption kettle (13) to be below the liquid level of the added nonpolar solvent.
4. The apparatus for absorbing HCl with a low water content in trimethyl orthoacetate according to claim 3, wherein: the HCl absorption device further comprises a transmission device (12), the transmission device (12) is arranged at the top of the absorption kettle (13), one end of the stirrer (5) is connected with the transmission device (12), and the other end of the stirrer (5) stirs liquid in the absorption kettle (13).
5. The apparatus for absorbing HCl with a low water content in trimethyl orthoacetate according to claim 2, wherein: refrigerant medium enters a refrigerant jacket (9) from a refrigerant inlet (6), the temperature in an absorption kettle (13) is controlled to be 0 ℃ to-5 ℃, nitrogen is introduced into the absorption kettle through a nitrogen inlet (3) to fully displace the air in the reaction kettle, quantitative anhydrous methanol is added into the absorption kettle (13) through a liquid feed inlet (11), and HCl is introduced into the absorption kettle through a drier (1) and an HCl feed inlet (2) after being uniformly stirred.
6. The apparatus for absorbing HCl with a low water content in trimethyl orthoacetate according to claim 4, wherein: the dryer (1) is a multilayer dryer, the transmission device (12) is a motor, the stirrer (5) comprises a stirring head (51) and a connecting shaft (52), one end of the connecting shaft (52) is connected with an output shaft of the motor, and the stirring head (51) is connected to the other end of the connecting shaft (52).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022700962.1U CN214416006U (en) | 2020-11-20 | 2020-11-20 | HCl absorbing device of low water content for trimethyl orthoacetate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022700962.1U CN214416006U (en) | 2020-11-20 | 2020-11-20 | HCl absorbing device of low water content for trimethyl orthoacetate |
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| CN214416006U true CN214416006U (en) | 2021-10-19 |
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| CN202022700962.1U Active CN214416006U (en) | 2020-11-20 | 2020-11-20 | HCl absorbing device of low water content for trimethyl orthoacetate |
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Denomination of utility model: A Low Moisture Content HCl Absorption Device for Trimethyl Acetate Effective date of registration: 20230904 Granted publication date: 20211019 Pledgee: Agricultural Bank of China Limited Dongzhi County Branch Pledgor: Anhui Xintai New Material Co.,Ltd. Registration number: Y2023980055122 |