CN216093572U - Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium - Google Patents

Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium Download PDF

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Publication number
CN216093572U
CN216093572U CN202122565427.4U CN202122565427U CN216093572U CN 216093572 U CN216093572 U CN 216093572U CN 202122565427 U CN202122565427 U CN 202122565427U CN 216093572 U CN216093572 U CN 216093572U
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reactor
raw material
pipeline
nitrogen
reaction
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耿智
朱树军
赵亮
朱晓东
钟向宏
胡晓宇
陈艳丹
吴宏伟
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Lianyungang Petrochemical Co Ltd
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Lianyungang Petrochemical Co Ltd
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Abstract

The utility model discloses a reaction system beneficial to recycling gas-phase raw material alcohol when active hydrogen-containing raw material alcohol reacts with sodium, which comprises a reactor and a condenser, wherein a stirrer is arranged in the reactor, and a discharge outlet is formed in the bottom of the reactor; the condenser is connected with a condensed water inlet pipe and a condensed water outlet pipe; the top of the reactor is provided with a feed inlet and a raw material recovery port, the feed inlet is connected with a feed pipeline, the raw material recovery port is connected with a gas phase inlet on a condenser through a gas phase discharge pipeline, and a condensate outlet on the condenser is connected with the raw material recovery port on the reactor through a condensate reflux pipeline; a coil pipe is arranged in the reactor, and circulating low-temperature water is introduced into the coil pipe; a jacket is arranged outside the reactor, and circulating hot water is introduced into the jacket; the top of the reactor is connected with a catalyst manual operation box. The reaction system provided by the utility model is beneficial to recovering the gas-phase raw material alcohol when the raw material alcohol containing active hydrogen reacts with sodium, and can reduce volatilization and discharge of the gas-phase raw material alcohol in the reaction process.

Description

Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium
Technical Field
The utility model relates to the technical field of chemical equipment, in particular to a reaction system beneficial to recycling gas-phase raw material alcohol when active hydrogen-containing raw material alcohol reacts with sodium.
Background
At present, the following three methods are mainly adopted for preparing the macromonomer raw material initiator of the polycarboxylic acid water reducing agent: (1) the chain initiator is prepared by the reaction of sodium methoxide and raw material alcohol, the reaction is mild, methanol is generated, and the quality of the macromonomer for producing the water reducer is very unfavorable, so that a rectification tower is required to completely remove the byproduct methanol from the system, and the byproduct can be stably and efficiently removed by accurately controlling the pressure and the temperature in the tower, so that the purity of the chain initiator is greatly improved, the preparation time is prolonged, and the production cost is increased. (2) The chain-forming initiator is prepared by reacting the powdery alkali metal compound with the raw material alcohol, and although the chain-forming initiator prepared by reacting the powdery alkali metal compound with the raw material alcohol does not generate moisture and does not need vacuum dehydration, the reaction is violent in the preparation process of the initiator, hydrogen is generated, the risk is high, the initiator is easy to catch fire and cause explosion, and many accidents have occurred in domestic production enterprises. (3) Solid alkali metal reacts with raw material alcohol to prepare a chain-forming initiator for alkoxylation reaction; the method is characterized in that solid alkali metal and raw material alcohol are reacted in a stirring kettle, although the reaction is mild, the reaction of the raw material alcohol and the solid alkali metal is exothermic, so that the volatilization of the raw material alcohol is caused, and the method is still an unstable factor for the environment.
With respect to the above-mentioned method of 3, there is a need for improvement of existing production facilities, reduction of volatilization of raw material alcohol, and recycling of a volatilized portion of gas-phase raw material alcohol as much as possible. In the existing chemical production equipment, a condenser is connected to a reaction kettle, so that materials volatilized from the reaction kettle are condensed in the condenser and then recycled. However, since the polycarboxylic acid water reducer macromonomer raw material initiator needs to adopt raw material alcohol containing active hydrogen and metal sodium with very active chemical property as a catalyst during preparation, a reactor and a condensing system in the existing production equipment cannot meet the special requirement and needs to be improved.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model aims to provide a reaction system which is beneficial to recovering gas-phase raw material alcohol when active hydrogen-containing raw material alcohol reacts with sodium, and can reduce volatilization and discharge of the gas-phase raw material alcohol in the reaction process.
The technical scheme adopted by the utility model for solving the technical problem is as follows: a reaction system for recovering gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium is favorable, and comprises a reactor and a condenser, wherein a stirrer is arranged in the reactor, and a discharge outlet is formed in the bottom of the reactor; the condenser is connected with a condensed water inlet pipe and a condensed water outlet pipe; the top of the reactor is provided with a feed inlet and a raw material recovery port, the feed inlet is connected with a feed pipeline, the raw material recovery port is connected with a gas phase inlet on the condenser through a gas phase discharge pipeline, and a condensate outlet on the condenser is connected with the raw material recovery port on the reactor through a condensate reflux pipeline; a coil pipe is arranged in the reactor, and circulating low-temperature water is introduced into the coil pipe; a jacket is arranged outside the reactor, and circulating hot water is introduced into the jacket; the top of the reactor is connected with a catalyst manual operation box.
Furthermore, the top of the reactor is also provided with a first nitrogen port and a second nitrogen port, the first nitrogen port and the second nitrogen port form a loop through an outer nitrogen pipeline, and the outer nitrogen pipeline is connected with a nitrogen source; an inner nitrogen pipeline is arranged in the reactor and is communicated with the outer nitrogen pipeline through the first nitrogen port.
Furthermore, the nitrogen inner pipeline is vertically arranged close to the inner wall of the reactor, the upper end of the nitrogen inner pipeline is connected with the first nitrogen port, and the lower end of the nitrogen inner pipeline extends to the bottom in the reactor.
Further, the condenser is arranged above the reactor; the gas phase discharge pipeline is vertically arranged by adopting a straight pipe; the condensate return line is obliquely arranged by adopting a straight pipe.
Further, the pipe diameter ratio of the gas phase discharge pipeline to the condensate reflux pipeline is 3-5: 1; the inclination angle of the condensate reflux pipeline is 30-45 degrees relative to the vertical direction.
Further, the condenser is also provided with an exhaust port, and the exhaust port is connected to an out-of-range flare system through a flare discharge pipeline.
Before the reaction system works, nitrogen replacement is carried out in the reactor through a first nitrogen port, a second nitrogen port, a nitrogen outer pipeline and a nitrogen inner pipeline, and the inert gas atmosphere in the reactor is kept; raw material alcohol enters the reactor from a feeding pipeline through the feeding hole, solid catalyst metal sodium is put into the catalyst putting tank through the manual operation box, and after nitrogen replacement is carried out on the manual operation box, the metal sodium catalyst in the catalyst putting tank is put into the reactor; raw material alcohol is stirred to react with solid catalyst metal sodium in a reactor to generate a chain initiator, and hot water circulation is carried out through a jacket outside the reactor in the early stage of the reaction, so that the initiation reaction is facilitated; after the catalytic reaction is initiated, the circulating hot water is removed, and the reaction heat is carried away by the circulating low-temperature water in the coil pipe. The gas-phase alcohol generated in the reaction process enters a condenser through a gas-phase discharge pipeline, and the condensed raw material alcohol returns to the reactor through a condensate reflux pipeline to participate in the reaction again. The non-condensable gas such as hydrogen generated in the reaction process is discharged to an out-of-range flare system through a flare discharge pipeline.
The utility model has the beneficial effects that: compared with the prior art, the reaction system provided by the utility model has the following advantages:
1) only one raw material recovery port is arranged on the reactor, volatilized gas-phase raw material alcohol enters the condenser through the raw material recovery port and the gas-phase discharge pipeline for condensation, and condensed liquid-phase raw material alcohol returns to the reactor through the condensate return pipeline and the raw material recovery port, so that only one raw material recovery port is arranged for simultaneously discharging gas-phase raw material alcohol and feeding liquid-phase raw material alcohol, the purpose of reducing the interfaces of the reactor is to better ensure the closed environment of a reaction system; and because gaseous phase discharging pipeline is vertical setting, the pipe diameter is far more than condensate backflow pipeline and when actual production, gaseous phase discharging pipeline keeps normally open, and the condensate backflow pipeline adopts intermittent type formula to open, consequently can ignore the influence that gaseous phase raw materials alcohol got into condensate backflow pipeline production almost.
2) The reactor is externally provided with a jacket, and circulating hot water is introduced into the jacket, so that the reactor is favorably heated in the early stage of the reaction, and the initiation of the reaction is promoted; the coil pipe is arranged in the reactor, and circulating low-temperature water is introduced into the coil pipe, so that reaction heat generated in the middle and later stages of the reaction can be removed in time; the timely removal of the reaction heat has two effects, namely, the reaction can be stably carried out, the side reaction is reduced, the volatilization of the raw material alcohol can be reduced, and the reaction efficiency is improved.
3) The reactor is provided with a first nitrogen port and a second nitrogen port, the two nitrogen ports form a loop through an outer nitrogen pipeline and then are connected with a nitrogen source, and the first nitrogen port is communicated with an inner nitrogen pipeline in the reactor; the method is favorable for keeping the nitrogen atmosphere in the reactor and ensures the safe and efficient reaction.
Drawings
In order that the embodiments of the utility model may be more readily understood, reference should now be made to the following detailed description taken in conjunction with the accompanying drawings. It should be noted that, in accordance with industry standard practice, various components are not necessarily drawn to scale and are provided for illustrative purposes only. In fact, the dimensions of the various elements may be arbitrarily expanded or reduced for clarity of discussion.
FIG. 1 is a schematic structural diagram of a reaction system provided by the present invention.
Wherein, 1-a condensed water outlet pipe; 2-flare discharge line; 3-a condenser; 4-a condensed water inlet pipe; 5-a gas phase discharge line; 6-condensate return line; 7-a feed line; 8-a raw material recovery port; 9-a feed inlet; 10-a reactor; 11-a coil pipe; 12-a discharge outlet; 13-a jacket; 14-nitrogen inner line; 15-a second nitrogen port; 16-a first nitrogen port; 17-nitrogen external line.
Detailed Description
The utility model is further illustrated by the following specific examples. These examples are intended to illustrate the utility model and are not intended to limit the scope of the utility model.
Examples
A reaction system for recovering gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium is favorable, the reaction system comprises a reactor 10 and a condenser 3, a stirrer is arranged in the reactor 10, and a discharge outlet 12 is arranged at the bottom of the reactor 10; the condenser 3 is connected with a condensed water inlet pipe 4 and a condensed water outlet pipe 1; the condenser 3 is also provided with a gas outlet which is connected to an out-of-range flare system through a flare discharge pipeline 2. The top of the reactor 10 is connected with a catalyst manual operation box, and the catalyst manual operation box is connected with a catalyst feeding tank.
A feed inlet 9 and a raw material recovery port 8 are arranged at the top of the reactor 10, the feed inlet 9 is connected with a feed pipeline 7, the raw material recovery port 8 is connected with a gas phase inlet on the condenser 3 through a gas phase discharge pipeline 5, and a condensate outlet on the condenser 3 is connected with the raw material recovery port 8 on the reactor 10 through a condensate reflux pipeline 6; the condenser 3 is arranged above the reactor 10; the gas-phase discharge pipeline 5 is vertically arranged by adopting a straight pipe; the pipe diameter ratio of the gas-phase discharge pipeline 5 to the condensate reflux pipeline 6 is 4: 1; the condensate backflow pipeline 6 is obliquely arranged by adopting a straight pipe, and the inclination angle of the condensate backflow pipeline 6 is 30 degrees relative to the vertical direction. Only one raw material recovery port 8 is formed in the reactor 10, volatilized gas-phase raw material alcohol enters the condenser 3 through the raw material recovery port 8 and the gas-phase discharge pipeline 5 for condensation, and condensed liquid-phase raw material alcohol returns to the reactor 10 through the condensate return pipeline 6 and the raw material recovery port 8, so that only one raw material recovery port 8 is formed for simultaneously supplying gas-phase raw material alcohol out and liquid-phase raw material alcohol in, the number of interfaces of the reactor 10 is reduced, and the closed environment of a reaction system is better ensured; and because gaseous phase discharging pipeline 5 is vertical setting, the pipe diameter is far more than condensate backflow pipeline 6 and during actual production, gaseous phase discharging pipeline 5 keeps normally open, and condensate backflow pipeline 6 adopts the intermittent type formula to open, therefore can ignore the influence that gaseous phase raw materials alcohol got into condensate backflow pipeline 6 and produces almost.
The jacket 13 is arranged outside the reactor 10, and circulating hot water is introduced into the jacket 13, so that the reactor 10 is heated in the early stage of the reaction, and the initiation of the reaction is promoted; the coil pipe 11 is arranged in the reactor 10, and circulating low-temperature water is introduced into the coil pipe 11, so that reaction heat generated in the middle and later stages of the reaction can be removed in time; the timely removal of the reaction heat has two effects, namely, the reaction can be stably carried out, the side reaction is reduced, the volatilization of the raw material alcohol can be reduced, and the reaction efficiency is improved.
The top of the reactor 10 is also provided with a first nitrogen port 16 and a second nitrogen port 15, the first nitrogen port 16 and the second nitrogen port 15 form a loop through an outer nitrogen pipeline 17, and the outer nitrogen pipeline 17 is connected with a nitrogen source; an inner nitrogen line 14 is provided in the reactor 10, the inner nitrogen line 14 being in communication with the outer nitrogen line 17 via the first nitrogen port 16. The inner nitrogen pipeline 14 is vertically arranged close to the inner wall of the reactor 10, the upper end of the inner nitrogen pipeline 14 is connected with the first nitrogen port 16, and the lower end of the inner nitrogen pipeline 14 extends to the bottom in the reactor 10; the nitrogen atmosphere in the reactor 10 can be kept, and the safe and efficient reaction can be ensured.
Before the reaction system works, nitrogen is replaced in the reactor 10 through a first nitrogen port 16, a second nitrogen port 15, an outer nitrogen pipeline 17 and an inner nitrogen pipeline 14, and the inert gas atmosphere in the reactor 10 is kept; raw material alcohol enters a reactor 10 from a feeding pipeline 7 through a feeding hole 9, solid catalyst metal sodium is put into a catalyst putting tank through a manual operation box, nitrogen gas replacement is carried out on the manual operation box, and then the metal sodium catalyst in the catalyst putting tank is put into the reactor 10; raw material alcohol is stirred to react with solid catalyst metal sodium in the reactor 10 to generate a chain initiator, and hot water circulation is carried out through a jacket 13 outside the reactor 10 in the early stage of the reaction, so that the initiation reaction is facilitated; after the catalytic reaction is initiated, the circulating hot water is removed, and the reaction heat is taken away by the circulating low-temperature water in the coil pipe 11. The gas phase alcohol generated in the reaction process enters the condenser 3 through the gas phase discharge pipeline 5, and the condensed raw material alcohol returns to the reactor 10 through the condensate reflux pipeline 6 to participate in the reaction again. Noncondensable gases such as hydrogen generated in the reaction process are discharged to an external flare system through a flare discharge pipeline 2.
The above embodiments are only for illustrating the utility model and are not to be construed as limiting the utility model, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the utility model, therefore, all equivalent technical solutions also belong to the scope of the utility model, and the scope of the utility model is defined by the claims.

Claims (6)

1. A reaction system for recovering gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium is favorable, and comprises a reactor and a condenser, wherein a stirrer is arranged in the reactor, and a discharge outlet is formed in the bottom of the reactor; the condenser is connected with a condensed water inlet pipe and a condensed water outlet pipe; the method is characterized in that: the top of the reactor is provided with a feed inlet and a raw material recovery port, the feed inlet is connected with a feed pipeline, the raw material recovery port is connected with a gas phase inlet on the condenser through a gas phase discharge pipeline, and a condensate outlet on the condenser is connected with the raw material recovery port on the reactor through a condensate reflux pipeline; a coil pipe is arranged in the reactor, and circulating low-temperature water is introduced into the coil pipe; a jacket is arranged outside the reactor, and circulating hot water is introduced into the jacket; the top of the reactor is connected with a catalyst manual operation box.
2. The reaction system for facilitating the recovery of a gaseous starting alcohol upon reaction of a starting alcohol containing active hydrogen with sodium as set forth in claim 1, wherein: the top of the reactor is also provided with a first nitrogen port and a second nitrogen port, the first nitrogen port and the second nitrogen port form a loop through an outer nitrogen pipeline, and the outer nitrogen pipeline is connected with a nitrogen source; an inner nitrogen pipeline is arranged in the reactor and is communicated with the outer nitrogen pipeline through the first nitrogen port.
3. The reaction system for facilitating recovery of a gas-phase raw alcohol upon reaction of a raw alcohol containing active hydrogen with sodium as set forth in claim 2, wherein: the nitrogen inner pipeline is vertically arranged close to the inner wall of the reactor, the upper end of the nitrogen inner pipeline is connected with the first nitrogen port, and the lower end of the nitrogen inner pipeline extends to the bottom in the reactor.
4. The reaction system for facilitating the recovery of a gaseous starting alcohol upon reaction of a starting alcohol containing active hydrogen with sodium as set forth in claim 1, wherein: the condenser is arranged above the reactor; the gas phase discharge pipeline is vertically arranged by adopting a straight pipe; the condensate return line is obliquely arranged by adopting a straight pipe.
5. The reaction system for facilitating recovery of a gaseous phase raw alcohol upon reaction of a raw alcohol containing active hydrogen with sodium as set forth in claim 4, wherein: the pipe diameter ratio of the gas phase discharge pipeline to the condensate reflux pipeline is 3-5: 1; the inclination angle of the condensate reflux pipeline is 30-45 degrees relative to the vertical direction.
6. The reaction system for facilitating the recovery of a gaseous starting alcohol upon reaction of a starting alcohol containing active hydrogen with sodium as set forth in claim 1, wherein: the condenser is also provided with an exhaust port, and the exhaust port is connected to an out-of-range flare system through a flare discharge pipeline.
CN202122565427.4U 2021-10-25 2021-10-25 Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium Active CN216093572U (en)

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CN202122565427.4U CN216093572U (en) 2021-10-25 2021-10-25 Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium

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Application Number Priority Date Filing Date Title
CN202122565427.4U CN216093572U (en) 2021-10-25 2021-10-25 Reaction system beneficial to recycling gas-phase raw material alcohol during reaction of raw material alcohol containing active hydrogen and sodium

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CN216093572U true CN216093572U (en) 2022-03-22

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