CN219482685U - Pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate - Google Patents
Pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate Download PDFInfo
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- CN219482685U CN219482685U CN202320093146.XU CN202320093146U CN219482685U CN 219482685 U CN219482685 U CN 219482685U CN 202320093146 U CN202320093146 U CN 202320093146U CN 219482685 U CN219482685 U CN 219482685U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The utility model belongs to the technical field of hydrolysis of dimethyl oxalate, in particular to a prereaction device for preparing oxalic acid by hydrolysis of dimethyl oxalate, which comprises a hydrolysis mixing kettle and a pipeline mixer, wherein the pipeline mixer is arranged to fully mix dimethyl oxalate, desalted water and crystallization mother liquor before entering the hydrolysis mixing kettle, the dimethyl oxalate can be rapidly hydrolyzed in the hydrolysis mixing kettle, a feed inlet is arranged in the tangential direction of the side wall of the hydrolysis mixing kettle, and a guide plate is arranged in the hydrolysis mixing kettle to enable liquid in the hydrolysis mixing kettle to flow to the center of the hydrolysis mixing kettle when rotating, so that the liquid in the hydrolysis mixing kettle is rapidly transferred to the center of the hydrolysis mixing kettle after being heated on the inner wall of the kettle, the liquid in the kettle is heated more uniformly, and the phenomena that the temperature of dimethyl oxalate near the inner wall of the kettle is high in hydrolysis rate, and the temperature of dimethyl oxalate in the center of the kettle is low in hydrolysis rate are avoided; thereby improving the hydrolysis rate of the dimethyl oxalate and having the advantage of low power consumption.
Description
Technical Field
The utility model belongs to the technical field of hydrolysis of dimethyl oxalate, and particularly relates to a pre-reaction device for preparing oxalic acid by hydrolysis of dimethyl oxalate.
Background
Oxalic acid is an important organic chemical raw material and is often used as a raw material for fine chemical preparation. Oxalic acid has a wide range of industrial applications, such as in medicine, dye intermediates, refining rare metals, and defense industries. Among the existing industrial production methods of oxalic acid, sodium formate dehydrogenation is more typical. The calcification method still does not solve the problem of lag of the dehydrogenation process due to low sodium oxalate conversion rate and large sulfuric acid circulation amount in the acidification process in the calcification process. As the front-end flow of the process for synthesizing glycol by catalytic hydrogenation of dimethyl oxalate, the large-scale industrialization of the process for synthesizing dimethyl oxalate by CO and methyl nitrite can also realize the industrialization of oxalic acid production by hydrolysis of dimethyl oxalate.
The hydrolysis process of dimethyl oxalate is that dimethyl oxalate is first mixed fully in a hydrolysis mixing kettle under the stirring action and pre-reacted, and then fed into a reaction rectifying tower for full hydrolysis and rectification purification. The existing dimethyl oxalate hydrolysis mixing kettle is only a simple chemical raw material mixing kettle, the hydrolysis efficiency and the hydrolysis time of dimethyl oxalate when the dimethyl oxalate stays in the hydrolysis mixing kettle are not fully considered, particularly, the dimethyl oxalate and water just enter the hydrolysis mixing kettle and are not fully mixed, the hydrolysis efficiency is low, under the action of stirring, the oxalic acid and the water are gradually and uniformly mixed, and the hydrolysis efficiency is gradually improved. However, because the residence time of the dimethyl oxalate and the water in the hydrolysis mixing kettle is short, the mass content of oxalic acid of the dimethyl oxalate at the outlet of the hydrolysis mixing kettle is lower and is between 5 and 10 percent, the effect of the hydrolysis mixing kettle is not fully exerted, and the load of a subsequent reaction rectifying tower is increased.
Disclosure of Invention
Based on the problems existing in the prior art, the utility model aims to provide the pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate, which can improve the hydrolysis efficiency under the condition that the residence time of hydrolysis mixing kettles with the same volume is the same, improve the oxalic acid mass content at the outlet of the hydrolysis mixing kettles and reduce the load of a follow-up reaction rectifying tower.
In order to solve the technical problems, the technical scheme adopted by the utility model is as follows:
a pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate comprises a hydrolysis mixing kettle for hydrolyzing dimethyl oxalate, wherein an outlet of the hydrolysis mixing kettle is connected to an inlet of a reaction rectifying tower through a pipeline; the method is characterized in that: the device comprises a hydrolysis mixing kettle, a hydrolysis mother liquor inlet, a hydrolysis mixing kettle, a pipeline mixer, a mixed liquor outlet, a hydrolysis mixing kettle and a water inlet, wherein the mixed liquor outlet of the pipeline mixer is connected to the inlet of the hydrolysis mixing kettle through a pipeline; the crystallization mother liquor inlet is connected with a crystallization mother liquor pipeline; and the top of the hydrolysis mixing kettle is also provided with a methanol gas outlet which is communicated with the reaction rectifying tower.
Further, the hydrolysis mixing kettle is a jacketed reaction kettle, and is made of zirconium.
Further, a guide plate is arranged in the hydrolysis mixing kettle.
Further, the inlet of the hydrolysis mixing kettle is arranged in the tangential direction of the side wall of the kettle body.
Further, the pipeline mixer is made of zirconium material or carbon steel lining plastic or carbon steel lining rubber.
Further, the hydrolysis mixing kettle further comprises a heat exchanger, and the heat exchanger is arranged on a pipeline connected with the mixed liquid outlet of the pipeline mixer and the hydrolysis mixing kettle inlet.
Advantageous effects
1. According to the utility model, through the pipeline mixer, stirring in the hydrolysis mixing kettle is replaced, dimethyl oxalate, desalted water and crystallization mother liquor are fully mixed before entering the hydrolysis mixing kettle, and dimethyl oxalate can be rapidly hydrolyzed after entering the hydrolysis mixing kettle, so that the condition that insufficient mixing hydrolysis rate is low when dimethyl oxalate, desalted water and crystallization mother liquor just enter the hydrolysis mixing kettle is avoided, and therefore dimethyl oxalate is hydrolyzed in the hydrolysis mixing kettle as much as possible, the hydrolysis rate of dimethyl oxalate is improved, and the load of a reaction rectifying tower of a subsequent device is reduced.
2. According to the utility model, the feed inlet is arranged in the tangential direction of the side wall of the hydrolysis mixing kettle, the guide plate is arranged in the hydrolysis mixing kettle, the kinetic energy of the mixed liquid entering the hydrolysis mixing kettle is utilized to push the liquid in the hydrolysis mixing kettle to rotate, and under the action of the guide plate, the liquid in the hydrolysis mixing kettle rotates and flows towards the center of the hydrolysis mixing kettle, so that the liquid in the hydrolysis mixing kettle can be quickly transferred to the center of the hydrolysis mixing kettle after the inner wall of the kettle is heated, the liquid in the hydrolysis mixing kettle is heated more uniformly, and the phenomena that the temperature of dimethyl oxalate near the inner wall of the hydrolysis mixing kettle is high, the hydrolysis rate is low, and the temperature of dimethyl oxalate in the center of the hydrolysis mixing kettle is low are avoided; thereby improving the hydrolysis rate of the dimethyl oxalate.
3. According to the utility model, through the pipeline mixer, the hydrolysis mixing kettle does not need to be provided with stirring, so that the consumption of power and electricity is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
FIG. 2 is a schematic view of a baffle structure of the present utility model;
FIG. 3 is a schematic view b of a baffle structure of the present utility model;
FIG. 4 is a schematic view of the arrangement of baffles in the hydrolysis mixing kettle of the present utility model;
FIG. 1-pipe mixer; 2-a hydrolysis mixing kettle; 3-a transfer pump; 4-a reactive rectifying tower; 5-a desalted water pipeline; a 6-dimethyl oxalate pipeline; 7-a crystallization mother liquor pipeline; 8-a deflector; 9-channel.
Detailed Description
Examples
In order to improve the hydrolysis efficiency of the dimethyl oxalate hydrolysis mixing kettle 2 and reduce the load of a reaction rectifying tower 4 of a subsequent device, the pre-reaction device for preparing oxalic acid by hydrolysis of dimethyl oxalate is provided by combining with fig. 1, 2, 3 and 4, and comprises a pipeline mixer 1 and a hydrolysis mixing kettle 2 for hydrolysis of dimethyl oxalate, wherein the hydrolysis mixing kettle 2 is a jacketed reaction kettle and is made of zirconium materials; the inlet of the hydrolysis mixing kettle 2 is arranged in the tangential direction of the side wall of the kettle body; a guide plate 8 is arranged in the hydrolysis mixing kettle 2, and the guide plate 8 is of a sieve plate structure with a slight radian; one end of the guide plate 8 connected with the inner wall of the hydrolysis mixing kettle 2 is provided with a channel 9 which is beneficial to the rotation of the liquid in the hydrolysis mixing kettle 2; the outlet of the hydrolysis mixing kettle 2 is connected to the inlet of the reaction rectifying tower 4 through a pipeline and a delivery pump 3; the mixed liquor outlet of the pipeline mixer 1 is connected to the inlet of the hydrolysis mixing kettle 2 through a pipeline, the pipeline mixer 1 is provided with three inlets, namely a dimethyl oxalate inlet and a desalted water inlet, a crystallization mother liquor inlet, the dimethyl oxalate inlet is connected with a dimethyl oxalate pipeline 6, and the desalted water inlet is connected with a desalted water pipeline 5; the crystallization mother liquor inlet is connected with a crystallization mother liquor pipeline 7; the top of the hydrolysis mixing kettle 2 is also provided with a methanol gas outlet which is communicated with the reaction rectifying tower 4.
Another embodiment differs from embodiment 1 in that: the pipeline mixer 1 is carbon steel lining plastic.
Another embodiment differs from embodiment 1 in that: the pipeline mixer 1 is carbon steel lining rubber.
Another embodiment differs from embodiment 1 in that: the hydrolysis mixing kettle further comprises a heat exchanger, wherein the heat exchanger is arranged on a pipeline connected with the mixed liquid outlet of the pipeline mixer 1 and the inlet of the hydrolysis mixing kettle 2.
The working principle of the utility model is as follows: through the pipeline mixer 1, stirring in the hydrolysis mixing kettle 2 is replaced, dimethyl oxalate, desalted water and crystallization mother liquor are fully mixed before entering the hydrolysis mixing kettle 2, and the dimethyl oxalate can be rapidly hydrolyzed after entering the hydrolysis mixing kettle 2, so that the condition of low hydrolysis rate when the dimethyl oxalate, the desalted water and the crystallization mother liquor just enter the hydrolysis mixing kettle 2 and are insufficiently mixed is avoided, the dimethyl oxalate is hydrolyzed in the hydrolysis mixing kettle 2 as much as possible, the hydrolysis rate of the dimethyl oxalate is improved, and the load of a reaction rectifying tower 4 of a subsequent device is reduced; meanwhile, a feed inlet is formed in the tangential direction of the side wall of the hydrolysis mixing kettle 2, a guide plate 8 is arranged in the hydrolysis mixing kettle, the kinetic energy of mixed liquid entering the hydrolysis mixing kettle 2 is utilized to push the liquid in the hydrolysis mixing kettle 2 to rotate, the liquid in the hydrolysis mixing kettle 2 rotates and flows towards the center of the hydrolysis mixing kettle 2 under the action of the guide plate 8, the liquid in the hydrolysis mixing kettle 2 can be quickly transferred to the center of the hydrolysis mixing kettle 2 after the inner wall of the kettle is heated, the liquid in the hydrolysis mixing kettle 2 is heated more uniformly, and the phenomenon that the dimethyl oxalate temperature near the inner wall of the hydrolysis mixing kettle 2 is high, the hydrolysis rate is high, and the dimethyl oxalate temperature in the center of the hydrolysis mixing kettle 2 is low, and the hydrolysis rate is low is avoided; thereby improving the hydrolysis rate of the dimethyl oxalate.
Modifications and variations of this utility model will be apparent to those skilled in the art and are intended to be within the scope of the utility model and are not limited to the embodiments described.
Claims (6)
1. A pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate comprises a hydrolysis mixing kettle for hydrolyzing dimethyl oxalate, wherein an outlet of the hydrolysis mixing kettle is connected to an inlet of a reaction rectifying tower through a pipeline; the method is characterized in that: the device also comprises a pipeline mixer, a mixed liquid outlet of the pipeline mixer is connected to an inlet of the hydrolysis mixing kettle through a pipeline, the pipeline mixer is provided with three inlets, the device comprises a dimethyl oxalate inlet, a desalted water inlet and a crystallization mother liquor inlet, wherein the dimethyl oxalate inlet is connected with a dimethyl oxalate pipeline; the desalted water inlet is connected with a desalted water pipeline; the crystallization mother liquor inlet is connected with a crystallization mother liquor pipeline; and the top of the hydrolysis mixing kettle is also provided with a methanol gas outlet which is communicated with the reaction rectifying tower.
2. The pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate according to claim 1, wherein the pre-reaction device comprises: the hydrolysis mixing kettle is a jacketed reaction kettle and is made of zirconium materials.
3. The pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate according to claim 1, wherein the pre-reaction device comprises: and a guide plate is arranged in the hydrolysis mixing kettle.
4. The pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate according to claim 1, wherein the pre-reaction device comprises: the inlet of the hydrolysis mixing kettle is arranged in the tangential direction of the side wall of the kettle body.
5. The pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate according to claim 1, wherein the pre-reaction device comprises: the pipeline mixer is made of zirconium materials or carbon steel lining plastics or carbon steel lining rubber.
6. The pre-reaction device for preparing oxalic acid by hydrolyzing dimethyl oxalate according to claim 1, wherein the pre-reaction device comprises: the heat exchanger is arranged on a pipeline connected with the mixed liquid outlet of the pipeline mixer and the inlet of the hydrolysis mixing kettle.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN117263297A (en) * | 2023-11-24 | 2023-12-22 | 山东无棣海丰电缆有限公司 | A processing apparatus for high salt dense water |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN117263297A (en) * | 2023-11-24 | 2023-12-22 | 山东无棣海丰电缆有限公司 | A processing apparatus for high salt dense water |
CN117263297B (en) * | 2023-11-24 | 2024-02-13 | 山东三岳化工有限公司 | A processing apparatus for high salt dense water |
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