CN216024865U - Low free alkali tert-butyl alcohol sodium intermittent synthesis device - Google Patents
Low free alkali tert-butyl alcohol sodium intermittent synthesis device Download PDFInfo
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- CN216024865U CN216024865U CN202122323230.XU CN202122323230U CN216024865U CN 216024865 U CN216024865 U CN 216024865U CN 202122323230 U CN202122323230 U CN 202122323230U CN 216024865 U CN216024865 U CN 216024865U
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Abstract
The utility model discloses a low free alkali sodium tert-butoxide intermittent synthesis device, which comprises a reaction kettle, wherein a first feed inlet of the reaction kettle is communicated with a liquid sodium methoxide storage tank through a first feed pipeline, and a second feed inlet is communicated with a tert-butanol storage tank through a second feed pipeline; a discharge port at the top of the reaction kettle is communicated with a methanol storage tank through a pre-rectifying tower and a rectifying tower; the utility model solves the problem that in the prior art, the free alkali is higher because the water as a byproduct of sodium tert-butoxide synthesis is difficult to remove from a production system.
Description
Technical Field
The utility model belongs to the technical field of alkoxide synthesis equipment, and particularly relates to a low-free-base sodium tert-butoxide intermittent synthesis device.
Background
Sodium tert-butoxide is used as a strong base, and is increasingly favored by industries such as chemical industry, medicine, pesticide and the like due to low cost, the demand of sodium tert-butoxide at home and abroad is increasingly large, at present, the synthesis process of common sodium tert-butoxide mainly comprises a metal method, an alkali method, an azeotropic distillation method and the like, and has the following defects: no water is generated in a metal method production system, but the moisture contained in the raw materials is difficult to discharge from a device, so that the production safety is poor, and the investment cost is high; although the alkaline production system has simple device, convenient operation and less equipment investment, the byproduct water in the sodium tert-butoxide prepared by the device is difficult to remove, so that the content of free alkali, namely sodium hydroxide in the product is higher, and the sodium hydroxide often has side effect when participating in the medical synthesis reaction, decomposes the reactant or the product and reduces the product yield; the azeotropic distillation production system also has the problem of recovery of tert-butyl alcohol, water and entrainer, so that the device cannot be widely applied.
Disclosure of Invention
In view of the above-mentioned drawbacks and deficiencies of the prior art, an object of the present invention is to provide a low free base sodium tert-butoxide batch synthesis apparatus, so as to solve the problem of high free base caused by the difficulty in removing the byproduct water from the production system in the prior art.
In order to achieve the purpose, the utility model adopts the following technical scheme:
a low free alkali sodium tert-butoxide intermittent synthesis device comprises a reaction kettle, wherein a first feed inlet of the reaction kettle is communicated with a liquid sodium methoxide storage tank through a first feed pipeline, and a second feed inlet is communicated with a tert-butanol storage tank through a second feed pipeline;
a discharge port at the top of the reaction kettle is connected with a feed port at the top of the methanol storage tank through a pre-rectifying tower and a rectifying tower;
and a bottom discharge hole of the reaction kettle is connected with a drying kettle, and the drying kettle is communicated with a tert-butyl alcohol storage tank through a condenser.
The utility model also has the following technical characteristics:
specifically, a first material transferring pump is further arranged on the first feeding pipeline.
Furthermore, a second material transferring pump is arranged on the second feeding pipeline.
Furthermore, a first condenser is arranged between the pre-rectifying tower and the rectifying tower, and a condensate discharging port of the first condenser is respectively connected with a top feeding port of the pre-rectifying tower and a middle feeding port of the rectifying tower.
Furthermore, a second condenser is arranged between the rectifying tower and the methanol storage tank, and a condensate discharge port of the second condenser is respectively connected with a top feed port of the rectifying tower and a top feed port of the methanol storage tank.
Furthermore, a reboiler is further arranged between the rectifying tower and the tert-butyl alcohol storage tank, a gas inlet of the reboiler is communicated with a liquid outlet of the rectifying tower, a gas outlet of the reboiler is communicated with a gas inlet of the rectifying tower, and a bottom discharge hole of the reboiler is communicated with a recovery port of the tert-butyl alcohol storage tank.
Furthermore, valves are arranged on the first feeding pipeline and the second feeding pipeline.
Furthermore, a third material transferring pump is arranged between the reaction kettle and the drying kettle.
Compared with the prior art, the utility model has the following technical effects:
(1) according to the utility model, reaction and rectification are combined, the reaction and rectification can be carried out simultaneously, methanol generated by the reaction is rapidly taken out through tertiary butanol steam, no water is introduced into the device in the reaction process, no water is generated, and even if trace water exists, the methanol can be evaporated out along with the methanol in the rectification process, so that the effect of extremely low free alkali is achieved.
(2) The utility model can be used for batch synthesis, namely, all raw materials are initially put into a reaction kettle at one time, each link can be independently carried out, and the production of the next kettle can be carried out after the completion. The order type production can be carried out according to the requirement, the operation is simple and flexible, and the arrangement of workshop personnel is free.
(3) The utility model realizes the recycling of the raw materials and effectively reduces the production cost of enterprises.
(4) The utility model has simple structure, convenient operation and value popularization.
Drawings
Fig. 1 is a schematic structural view of the present invention.
The reference numbers in the figures represent:
the method comprises the following steps of 1-a reaction kettle, 2-a first feeding pipeline, 3-a liquid sodium methoxide storage tank, 4-a second feeding pipeline, 5-a tert-butyl alcohol storage tank, 6-a pre-rectifying tower, 7-a rectifying tower, 8-a methanol storage tank, 9-a drying kettle, 10-a third condenser, 11-a first material transfer pump, 12-a second material transfer pump, 13-a first condenser, 14-a second condenser, 15-a reboiler and 16-a third material transfer pump.
The solution according to the utility model is further explained and illustrated below with reference to the figures and examples.
Detailed Description
All parts in the present invention are those known in the art, unless otherwise specified.
As used herein, the terms "upper," "lower," "front," "back," "top," "bottom," and the like are used in an orientation or positional relationship that is indicated for convenience in describing the utility model and to simplify the description, but does not indicate or imply that the referenced devices or elements must be in a particular orientation, constructed and operative in a particular orientation, "inner" and "outer" refer to the inner and outer of the contours of the corresponding parts and are not to be construed as limiting the utility model.
In the present invention, the terms "mounted," "connected," "fixed," and the like are used broadly and may be, for example, fixedly connected, detachably connected, or integrated without being described to the contrary; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The present invention will be described in further detail with reference to specific examples.
Example 1
Following the above technical solution, as shown in fig. 1, this embodiment provides a low free alkali sodium tert-butoxide intermittent synthesis device, which includes a reaction kettle 1, a first feed inlet of the reaction kettle 1 is communicated with a liquid sodium methoxide storage tank 3 through a first feed pipe 2, and a second feed inlet is communicated with a tert-butanol storage tank 5 through a second feed pipe 4; liquid sodium methoxide storage tank 3 is used for storing liquid sodium methoxide, the liquid sodium methoxide is sent into reaction kettle 1 through first feeding pipeline 2, tert-butyl alcohol storage tank 5 is used for storing tert-butyl alcohol, the tert-butyl alcohol is sent into reaction kettle 1 through second feeding pipeline 4, and the tert-butyl alcohol and the liquid sodium methoxide react in reaction kettle 1;
a discharge port at the top of the reaction kettle 1 is connected with a feed inlet of a methanol storage tank 8 through a pre-rectifying tower 6 and a rectifying tower 7; the methanol generated in the reaction kettle 1 is quickly distilled by tertiary butanol steam generated by volatilizing the reaction kettle 1 in the pre-rectifying tower 6, the mixed gas of the tertiary butanol and the methanol is discharged from the top of the pre-rectifying tower 6 and is sent to the first condenser 13, and the rectifying tower 7 is used for separating the mixed liquid of the tertiary butanol and the methanol sent by the first condenser 13 again.
A discharge port at the bottom of the reaction kettle 1 is connected with a drying kettle 9, and the drying kettle 9 is communicated with a tert-butyl alcohol storage tank 5 through a third condenser 10. The drying kettle 9 is used for drying the liquid sodium tert-butoxide fed into the reaction kettle, and feeding the tert-butanol generated in the drying process into a third condenser 10 for cooling; and (3) sending the cooled tert-butyl alcohol into a tert-butyl alcohol storage tank 5, and discharging the sodium tert-butoxide solid obtained after drying.
As a preferable scheme of this embodiment, the first feeding pipe 2 is further provided with a first transferring pump 11, and the first transferring pump 11 is used for feeding liquid sodium methoxide into the reaction kettle 1 through the first feeding pipe 2.
As a preferable scheme of this embodiment, the second feeding pipe 4 is further provided with a second material transferring pump 12, and the second material transferring pump 12 is used for feeding tertiary butanol into the reaction kettle 1 through the second feeding pipe 4.
As a preferable scheme of this embodiment, a first condenser 13 is disposed between the pre-rectifying tower 6 and the rectifying tower, a condensate discharge port of the first condenser 13 is respectively connected to a top feed port of the pre-rectifying tower 6 and a middle feed port of the rectifying tower 7, the first condenser 13 is configured to condense part of the tert-butyl alcohol vapor discharged from the pre-rectifying tower 6, and then send the condensed part of the tert-butyl alcohol vapor back to the reaction kettle 1 through the pre-rectifying tower 6, and send part of the condensed tert-butyl alcohol vapor to the rectifying tower 7, so as to reduce the initial feeding amount of the tert-butyl alcohol.
As a preferable scheme of this embodiment, a second condenser 14 is disposed between the rectifying tower and the methanol storage tank 8, and a condensate discharge port of the second condenser 14 is respectively connected to the top feed port of the rectifying tower 7 and the top feed port of the methanol storage tank 8.
As a preferable scheme of this embodiment, a reboiler 15 is further disposed between the rectifying tower 7 and the tert-butyl alcohol storage tank 5, a gas inlet of the reboiler 15 is communicated with a liquid outlet of the rectifying tower 7, a gas outlet of the reboiler 15 is communicated with a gas inlet of the rectifying tower 7, and a bottom discharge port of the reboiler 15 is communicated with a recovery port of the tert-butyl alcohol storage tank 5.
The preset temperature of the reboiler 15 is 90-100 ℃, a small part of tertiary butanol is sent to the rectifying tower 7 after being reboiled for system balance, and a large part of tertiary butanol which is not boiled is sent to the tertiary butanol storage tank 5 for recycling.
As a preferable scheme of this embodiment, valves are provided on both the first feeding pipe 2 and the second feeding pipe 4.
As a preferable scheme of this embodiment, a third material transfer pump 16 is further disposed between reaction kettle 1 and drying kettle 9, and third material transfer pump 16 is used for sending the tert-butyl alcohol output from reaction kettle 1 to drying kettle 9.
The use process of the device is as follows:
starting a first material transfer pump 11 and a second material transfer pump 12, adding liquid sodium methoxide and tert-butyl alcohol into a reaction kettle 1 in proportion, reacting the liquid sodium methoxide and the tert-butyl alcohol at 140 ℃, setting the reflux ratio of a first condenser 13, discharging mixed gas of methanol and the tert-butyl alcohol from a gas discharge port at the top of a pre-rectifying tower 6 after reacting for a period of time, condensing the mixed gas into liquid in the first condenser 13, refluxing part of the methanol and the tert-butyl alcohol into the pre-rectifying tower 6, and conveying part of the methanol and the tert-butyl alcohol to the rectifying tower 6 for rectification and separation. Setting the reflux ratio of a second condenser 14, discharging methanol gas from a gas discharge port at the top of a rectifying tower 7, after the methanol gas is condensed into liquid in the second condenser 14, partially refluxing the methanol into the rectifying tower 7, and partially sending the methanol into a methanol storage tank 8 for later use, wherein a small part of tert-butyl alcohol as a tower bottom component of the rectifying tower 7 enters an air inlet of the rectifying tower 7 through an air outlet of a reboiler 15, and most of the tert-butyl alcohol which is not reboiled is transferred into a tert-butyl alcohol storage tank 5 through a bottom discharge port of a reboiler 15 for later use, meanwhile, liquid sodium tert-butoxide generated in a reaction kettle 1 is transferred into a drying kettle 9 for drying, the dried and distilled tert-butyl alcohol finally enters the tert-butyl alcohol storage tank 5 for later use, and after drying is finished, cooling and discharging the solid sodium tert-butoxide.
The above are only preferred embodiments of the present invention, and are not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A low free alkali sodium tert-butoxide intermittent synthesis device comprises a reaction kettle (1) and is characterized in that a first feed inlet of the reaction kettle (1) is communicated with a liquid sodium methoxide storage tank (3) through a first feed pipeline (2), and a second feed inlet is communicated with a tert-butanol storage tank (5) through a second feed pipeline (4);
a top discharge port of the reaction kettle (1) is connected with a top feed inlet of a methanol storage tank (8) through a pre-rectifying tower (6) and a rectifying tower (7);
and a bottom discharge hole of the reaction kettle (1) is connected with a drying kettle (9), and the drying kettle (9) is connected with a tert-butyl alcohol storage tank (5) through a third condenser (10).
2. A low free base sodium tert-butoxide batch synthesis plant as claimed in claim 1, characterised in that the first feed line (2) is also provided with a first transfer pump (11).
3. A low free base sodium tert-butoxide batch synthesis unit as claimed in claim 1, in which a second transfer pump (12) is also provided in the second feed line (4).
4. The batch synthesis device of sodium tert-butoxide with low free base as in claim 1, characterized in that a first condenser (13) is arranged between the pre-rectifying column (6) and the rectifying column, and the condensate discharge outlet of the first condenser (13) is respectively connected with the top feed inlet of the pre-rectifying column (6) and the middle feed inlet of the rectifying column (7).
5. The batch synthesis device of sodium tert-butoxide with low free base as claimed in claim 1, characterized in that a second condenser (14) is arranged between the rectification column (7) and the methanol storage tank (8), and the condensate discharge outlet of the second condenser (14) is connected to the top feed inlet of the rectification column (7) and the top feed inlet of the methanol storage tank (8), respectively.
6. The batch synthesis device of low free alkali sodium tert-butoxide of claim 1, characterized in that a reboiler (15) is further disposed between the rectification column (7) and the tert-butanol storage tank (5), the gas inlet of the reboiler (15) is communicated with the liquid outlet of the rectification column (7), the gas outlet of the reboiler (15) is communicated with the gas inlet of the rectification column (7), and the bottom outlet of the reboiler (15) is communicated with the recovery port of the tert-butanol storage tank (5).
7. A low free base sodium tert-butoxide batch synthesis plant as claimed in claim 1, in which valves are provided in both the first feed line (2) and the second feed line (4).
8. The batch synthesizer of sodium tert-butoxide with low free base as claimed in claim 1, characterized in that a third transfer pump (16) is arranged between the reactor (1) and the drying vessel (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122323230.XU CN216024865U (en) | 2021-09-24 | 2021-09-24 | Low free alkali tert-butyl alcohol sodium intermittent synthesis device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122323230.XU CN216024865U (en) | 2021-09-24 | 2021-09-24 | Low free alkali tert-butyl alcohol sodium intermittent synthesis device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115301173A (en) * | 2022-07-18 | 2022-11-08 | 临沂金朗化工有限公司 | Preparation device and method of sodium tert-butoxide |
| CN115318229A (en) * | 2022-08-31 | 2022-11-11 | 安徽金邦医药化工有限公司 | Granular sodium tert-butoxide preparation system and preparation process thereof |
| CN115301173B (en) * | 2022-07-18 | 2024-05-14 | 临沂金朗化工有限公司 | Preparation device and method of sodium tert-butoxide |
-
2021
- 2021-09-24 CN CN202122323230.XU patent/CN216024865U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115301173A (en) * | 2022-07-18 | 2022-11-08 | 临沂金朗化工有限公司 | Preparation device and method of sodium tert-butoxide |
| CN115301173B (en) * | 2022-07-18 | 2024-05-14 | 临沂金朗化工有限公司 | Preparation device and method of sodium tert-butoxide |
| CN115318229A (en) * | 2022-08-31 | 2022-11-11 | 安徽金邦医药化工有限公司 | Granular sodium tert-butoxide preparation system and preparation process thereof |
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