CN115634650B - Alkyl phosphate oligomer's preparation facilities - Google Patents

Alkyl phosphate oligomer's preparation facilities Download PDF

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CN115634650B
CN115634650B CN202211375425.1A CN202211375425A CN115634650B CN 115634650 B CN115634650 B CN 115634650B CN 202211375425 A CN202211375425 A CN 202211375425A CN 115634650 B CN115634650 B CN 115634650B
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reaction
pipeline
reaction kettle
communicated
feeding
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CN115634650A (en
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梅连平
万邦隆
朱境
刘晨曦
马航
李云东
杨晓龙
陆忠海
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Yunnan Yuntianhua Co Ltd
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Yunnan Yuntianhua Co Ltd
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Abstract

The application relates to the field of chemical industry, in particular to a preparation device of an alkyl phosphate oligomer, which comprises a first reaction device, a plurality of second reaction devices and a distribution pipeline for communicating the first reaction device with the second reaction devices; a plurality of connecting pipelines are arranged on the distribution pipeline, and comprise a first connecting pipeline communicated with the first reaction device and a plurality of second connecting pipelines respectively communicated with a plurality of second reaction devices; the first reaction device is provided with a first discharge hole communicated with the first connecting pipeline, and a blocking device for preventing the accumulation of powdery materials is arranged at the first discharge hole. The blocking device is arranged at the first discharge hole of the first reaction kettle, so that the blocking phenomenon caused by accumulation of powdery materials in the first reaction kettle at the first discharge hole can be prevented, a first product can smoothly flow into a distribution pipeline, meanwhile, the powdery materials can be fully contacted with other materials, and the reaction rate is accelerated.

Description

Alkyl phosphate oligomer's preparation facilities
Technical Field
The application relates to the field of chemical industry, in particular to a preparation device of an alkyl phosphate oligomer.
Background
The alkyl phosphate is an important phosphorus-containing additive, has good abrasion resistance and oxidation resistance, and has good composite use performance when being used in combination with a sulfur-based antiwear agent. Meanwhile, alkyl phosphate plays a very important role in the preparation of pesticide organic phosphorus-containing corrosion inhibitors, plastic additives, dye additives and flame retardants, is an important fine chemical intermediate, and is prepared by mainly taking dodecanol and phosphorus pentoxide as raw materials for reaction during the synthesis of the alkyl phosphate, determining the optimal synthesis conditions by controlling the dosage of a catalyst, the loading capacity of the catalyst, the reaction time, the distilled water quantity and the temperature, polymerizing the phosphate, the phosphorus pentoxide and the ethylene oxide under the action of the catalyst to generate an alkyl phosphate oligomer, and removing residual ethylene oxide and phosphate in the alkyl phosphate oligomer to obtain a final product.
The traditional alkyl phosphate oligomer production uses a kettle reactor, the process is mature, the equipment is complex, the production period is long, and the production efficiency is low. The traditional kettle type production process has extremely low gas-liquid reaction efficiency in the synthesis process, and has a longer production period from the start of feeding to the acquisition of qualified products for at least 150 hours. The long production period leads the production cost of the finished product to be higher, which is not beneficial to the stable control of the quality of the product; in the reaction process, the unreacted powdery materials are deposited at the bottom to block the through hole, and the deposited materials are unfavorable for fully contacting and reacting with other materials and are unfavorable for the product to flow through the through hole; in the reaction process, a large amount of unreacted ethylene oxide is enriched at the upper part of the reaction kettle for a long time, so that the explosion and poisoning accidents of the ethylene oxide are easily caused, and the ethylene oxide enriched at the upper part of the reaction kettle can be self-polymerized to form local hot spots, so that the danger is further increased, and the difficulty of stably controlling the process conditions is further increased.
Disclosure of Invention
The present application aims to overcome one or more of the above-mentioned problems of the prior art and to provide an apparatus for preparing an alkyl phosphate oligomer.
In order to achieve the above purpose, the present application provides the following technical solutions:
an apparatus for producing an alkyl phosphate oligomer, comprising:
a first reaction device, a plurality of second reaction devices, and a distribution pipeline for communicating the first reaction device with the plurality of second reaction devices;
a plurality of connecting pipelines are arranged on the distribution pipeline, and comprise a first connecting pipeline communicated with the first reaction device and a plurality of second connecting pipelines respectively communicated with a plurality of second reaction devices;
the first reaction device is provided with a first discharge hole communicated with the first connecting pipeline, and a blocking device for preventing the accumulation of powdery materials is arranged at the first discharge hole.
Preferably, the first reaction device further comprises a first reaction kettle, a first feeding device, a second feeding device and a first stirrer;
a first feeding port is formed in the top of the first reaction kettle, and a first discharging port is formed in the bottom of the first reaction kettle;
the first feeding holes are formed in two, the first feeding holes are respectively communicated with the first feeding device and the second feeding device, and the first discharging holes are communicated with the first connecting pipeline.
Preferably, the blocking means comprises a blocking cover, the first agitator being arranged in a telescopically movable configuration;
the blocking cover is fixedly connected with one end of the first stirrer, which is close to the first discharge hole;
the first stirrer stretches and contracts to control the blocking cover to open and close the first discharge hole.
Preferably, the blocking device comprises a vibrator arranged on the outer wall of the first reaction kettle;
the vibrator is arranged close to the first discharging hole.
Preferably, the second reaction device comprises a second reaction kettle, a third feeding device, a second stirrer, a baffle plate and a circulating spraying device;
a second feeding port is formed in the top of the second reaction kettle, and a second discharging port is formed in the bottom of the second reaction kettle;
the second feed inlet is provided with a plurality of second feed inlets, the second feed inlets are respectively communicated with one end of the circulating spraying device, the third feeding device and the second connecting pipeline correspondingly, and the second discharge outlet is communicated with the other end of the circulating spraying device.
Preferably, the baffle sets up the multilayer, and the interval sets up on the inside wall of second reation kettle, with the inside wall fixed connection of second reation kettle, and protruding in the inside wall of second reation kettle.
Preferably, the circulation spray device comprises a first pipeline, a second pipeline and a jet reactor;
one end of the first pipeline is communicated with the second feeding port, and the other end of the first pipeline is connected with the second discharging port;
the jet reactor is arranged on the first pipeline, one end of the second pipeline is communicated with the jet reactor, and the other end of the second pipeline is communicated with the top of the second reaction kettle.
Preferably, a cavity is arranged in the jet reactor, and a nozzle communicated with the first pipeline is arranged on the inner side wall of the cavity, which is far away from the second reaction kettle;
the second pipeline is communicated with the cavity.
Preferably, valves which are independently opened and closed are provided on a plurality of the connection pipes of the distribution pipe.
Preferably, a purge device is provided on the distribution pipe in communication with the distribution pipe;
inert gas is stored inside the purging device.
Based on the above, the application has the beneficial effects that:
1. according to the scheme provided by the application, two steps of reactions for preparing the alkyl phosphate oligomer are respectively carried out by using two reaction kettles, and meanwhile, as the reaction time of the second step is far longer than that of the first step, a plurality of second reaction kettles are arranged, a plurality of second steps of reactions can be carried out simultaneously, and more final products can be obtained in the same time compared with the traditional technology;
2. according to the scheme, the distribution pipeline is arranged to simultaneously connect the first reaction device and the plurality of second reaction devices, valves are arranged among the first reaction device, the second reaction device and the distribution pipeline, and the first product in the first reaction device is conveyed in a positioning way through opening and closing the valves;
3. according to the scheme, the blocking device is arranged at the first discharge hole of the first reaction kettle, so that the blocking phenomenon caused by accumulation of powdery materials in the first reaction kettle at the first discharge hole can be prevented, a first product can smoothly flow into the distribution pipeline, meanwhile, the powdery materials can be fully contacted with other materials, and the reaction rate is accelerated;
4. according to the scheme, the purging device connected with the distribution pipeline is arranged, inert gas is stored in the purging device, the distribution pipeline can be subjected to impurity removal treatment before the first product enters the distribution pipeline, meanwhile, after the first product enters the distribution pipeline, the purging device can squeeze the first product into the corresponding second reaction kettle, so that the first product is ensured to fully enter the second reaction kettle to react, materials are fully utilized, and accumulation and waste are not caused;
5. according to the scheme, the second reaction device further comprises a circulating spraying device, liquid in the second reaction kettle can be pumped out from the bottom of the second reaction kettle and conveyed into the inner cavity of the jet reactor along the first pipeline, the liquid can be sprayed out in a dispersed manner due to the arrangement of the nozzles, meanwhile, a second pipeline is arranged at the top of the second reaction kettle, third material in the second reaction kettle can be pumped, the other end of the second pipeline is communicated with the cavity of the spraying reactor, the third material is conveyed into the cavity of the spraying reactor and fully contacted with the dispersed sprayed liquid, and then the liquid returns into the second reaction kettle again from the top of the second reaction kettle along the first pipeline, so that the reaction rate of the second reaction can be accelerated, the first product is fully contacted with the third material, the preparation rate of alkyl phosphate oligomer is increased, and meanwhile, the circulating spraying device can also avoid that ethylene oxide is greatly enriched at the top of the second reaction kettle, and danger is avoided;
6. according to the scheme, the baffle plate is arranged on the inner side wall of the second reaction kettle and protrudes out of the inner side wall of the second reaction kettle, when the second reaction kettle is stirred, the liquid in the second reaction kettle is in a vortex shape, the central liquid level is low, the liquid level close to the inner wall of the second reaction kettle is high, when the circulating spraying device sucks the liquid in the second reaction kettle from the bottom of the second reaction kettle, if the liquid level of the liquid is too low, the circulating spraying device sucks the gas in the circulating spraying device, the liquid cannot be sucked, the second reaction rate cannot be accelerated, and due to the baffle plate, when the liquid is in a vortex shape, the high liquid level close to the inner side wall of the second reaction kettle can be blocked by the baffle plate and cannot be lifted, the fact that the whole liquid level difference of the liquid is not large is guaranteed, meanwhile, part of the liquid blocked by the baffle plate falls towards the position close to the center of the liquid level can be fully contacted with the third material, and simultaneously part of the third material can be wrapped, the third material can fall together, the whole liquid and the third material can be fully contacted, the reaction rate is accelerated, and the preparation rate of alkyl phosphate oligomer is increased.
Drawings
FIG. 1 schematically shows the overall structure of an apparatus for producing an alkylphosphonate oligomer according to one embodiment of the application;
FIG. 2 schematically shows a schematic structure of a first reaction apparatus according to an embodiment of the present application;
FIG. 3 schematically shows a block arrangement according to an embodiment of the application;
FIG. 4 schematically shows a schematic structure of a second reaction apparatus according to an embodiment of the present application.
Reference numerals illustrate: the device comprises a first reaction device 10, a first reaction kettle 101, a first feeding device 102, a second feeding device 103, a first stirrer 104, a first feeding port 105, a first discharging port 106, a blocking device 107, a blocking cover 1071, a second reaction device 20, a second reaction kettle 201, a third feeding device 202, a second stirrer 203, a baffle 204, a circulating spraying device 205, a first pipeline 2051, a second pipeline 2052, a spraying reactor 2053, a second feeding port 206, a second discharging port 207, a distribution pipeline 30, a connecting pipeline 301, a first connecting pipeline 3011, a second connecting pipeline 3012, a valve 302 and a purging device 303.
Detailed Description
The present disclosure will now be discussed with reference to exemplary embodiments, it being understood that the embodiments discussed are merely for the purpose of enabling those of ordinary skill in the art to better understand and thus practice the present disclosure and do not imply any limitation to the scope of the present disclosure.
As used herein, the term "comprising" and variants thereof are to be interpreted as meaning "including but not limited to" open-ended terms. The terms "based on" and "based at least in part on" are to be construed as "at least one embodiment.
FIG. 1 schematically shows a schematic overall structure of an apparatus for producing an alkylphosphonate oligomer according to one embodiment of the application, as shown in FIG. 1, comprising:
a first reaction device 10, a plurality of second reaction devices 20, and a distribution pipe 30 communicating the first reaction device 10 with the plurality of second reaction devices 20;
in the process of preparing the alkyl phosphate oligomer, the alkyl phosphate oligomer is required to be prepared through two steps of reactions, wherein the first step of reaction is to react phosphorus pentoxide with triethyl phosphate to generate a first product, the second step of reaction is to react the first product with ethylene oxide to generate the alkyl phosphate oligomer, in the conventional technology, the two steps of reactions are usually carried out in one reaction vessel, in the common general knowledge, phosphorus pentoxide can react with ethylene oxide to generate byproducts, and heat is generated at the same time, so that the explosion phenomenon is easy to cause by carrying out the two steps of reactions in one reaction vessel, equipment is damaged, and the personal safety is endangered.
According to the application, the two-step reaction for preparing the alkyl phosphate oligomer is divided into two reaction devices to react respectively, so that phosphorus pentoxide and ethylene oxide can be effectively prevented from contacting, and hazard is effectively avoided; in the scheme of the application, a plurality of second reaction devices 20 are arranged and are simultaneously communicated with one first reaction device 10 through a distribution pipeline 30, in common knowledge, the reaction time of phosphorus pentoxide and triethyl phosphate under normal conditions is 4 hours, and the reaction time of the generated first product and ethylene oxide under normal conditions is 150 hours, and the application is provided with a plurality of second reaction devices 20, so that a plurality of second-step reactions can be simultaneously carried out, more alkyl phosphate oligomers can be prepared in the same time, and the preparation efficiency is improved.
Providing a plurality of connection pipes 301 on the distribution pipe 30, including a first connection pipe 3011 communicating with the first reaction device 10 and a plurality of second connection pipes 3012 respectively communicating with a plurality of second reaction devices 20; the plurality of connection pipes 301 of the distribution pipe 30 are provided with valves 302 that are independently opened and closed.
By controlling the opening and closing of the valve 302, it is possible to freely control whether or not the communication between one of the second reaction devices 20 and the distribution pipe 30 is required, and whether or not the first product of the first reaction device 10 needs to be fed into the second reaction device 20, and the movement path of the first product can be selectively controlled.
The distribution pipe 30 may be provided in the shape of a ring, square or diamond, etc., preferably in the shape of a ring.
To achieve the above object, the apparatus for producing an alkylphosphate oligomer of the present application further comprises a purge means 303 provided outside the distribution pipe 30 and communicating with the distribution pipe 30;
the purge device 303 stores an inert gas therein.
Before the first product enters the distribution pipeline 30, all valves 302 connected with the second reaction device 20 are opened, the purging device 303 is started, inert gas is continuously filled into the distribution pipeline 30, impurities such as air in the device are removed, impurities in the second reaction device 20 can be removed, and the purity of the product is ensured.
After the reaction of the first reaction device 10 is completed to generate the first product, a valve 302 between the first reaction device 10 and the distribution pipeline 30 is opened, the first product enters the distribution pipeline 30, a valve 302 between the distribution pipeline 30 and one of the second reaction devices 20 is opened, a purging device 303 is opened, the first product is extruded into the second reaction device 20, and the subsequent second-step reaction is performed.
The setting of sweeping device 303 can remove impurity to the device before the reaction, guarantees the product purity, also can make the whole second reaction unit 20 that gets into of first product simultaneously, can not cause partial first product to remain in distribution pipeline 30, avoids reducing the output of final product, make full use of material simultaneously.
FIG. 2 schematically shows a schematic structure of a first reaction apparatus according to an embodiment of the present application, as shown in FIG. 2:
further, the first reaction device 10 of the present application comprises a first reaction kettle 101, a first feeding device 102, a second feeding device 103 and a first stirrer 104;
a first feeding port 105 is arranged at the top of the first reaction kettle 101, and a first discharging port 106 is arranged at the bottom of the first reaction kettle 101;
the first feeding ports 105 are provided in two, and communicate with the first feeding device 102 and the second feeding device 103, respectively, and the first connecting pipe 3011 communicates with the first feeding port 106.
Specifically, the number of the first feeding ports 105 is two, one of the first feeding ports 105 is communicated with the first feeding device 102, phosphorus pentoxide powder is stored in the first feeding device 102, the other first feeding port 105 is communicated with the second feeding device 103, and triethyl phosphate liquid is stored in the second feeding device 103.
The first stirrer 104 is arranged in the first reaction kettle 101 and is connected with the top center of the first reaction kettle 101, and the first stirrer 104 is driven by an external motor to rotate, so that materials in the first reaction kettle 101 are stirred, and the material reaction rate is accelerated. FIG. 3 schematically shows a block arrangement according to an embodiment of the application; further, as shown in fig. 3:
the first reaction device 10 further comprises a blocking device 107 capable of preventing the accumulation of unreacted complete powdered material at the first outlet 106.
In the first embodiment of the present application, the blocking means 107 blocks the cover 1071, and the first agitator 104 is provided in a telescopically movable structure; the blocking cover 1071 is fixedly connected with one end, close to the first discharge hole 106, of the first stirrer 104, the first discharge hole 106 can be opened and closed through expansion of the first stirrer 104, and the diameter of the opening of the blocking cover 1071 is larger than that of the opening of the first discharge hole 106, so that the blocking cover 1071 can completely cover the first discharge hole 106.
The first stirrer 104 comprises a telescopic rod (not shown) and stirring blades (not shown), the telescopic rod is vertically inserted inwards from the top of the first reaction kettle 101, the non-insertion end of the telescopic rod is connected with a motor (not shown), and the telescopic rod can be driven to vertically move in a telescopic manner or rotate through the motor; stirring leaf setting is on the telescopic link lateral wall, with telescopic link fixed connection, when the telescopic link is rotatory, drives stirring leaf stirring liquid, and then can accelerate the reaction rate of first material and second material.
Further, in the reaction process of phosphorus pentoxide and triethyl phosphate, the phosphorus pentoxide powder gradually moves to the center due to the stirring action of the first stirrer 104, and is further accumulated at the bottom center of the first reaction kettle 101, namely at the first discharge port 106, so that the first discharge port 106 is blocked, the first material generated in the first step of reaction cannot smoothly enter the distribution pipeline 30 through the first discharge port 106, and the preparation rate of the alkyl phosphate oligomer is reduced;
by the arrangement of the application, before the first material and the second material are placed in the first reaction kettle 101, the first stirrer 104 is extended until the bottom of the blocking device 107 contacts with the inner wall of the first reaction kettle 101, at this time, the blocking device 107 completely shields the first discharge hole 106, then the first material and the second material are placed into the first reactor to perform a first step reaction, the first stirrer 104 rotates to stir the first material and the second material to make them fully contact, so as to accelerate the reaction rate, while the first material which does not participate in the reaction is blocked at the outer wall of the blocking device 107, and still rotates along with the liquid along with the stirring of the first stirrer 104 because the first material is not positioned at the center of the liquid vortex, so that the reaction is fully performed; when the first reaction is completed, the first stirrer 104 is contracted, and the blocking device 107 does not block the first discharge port 106, but if the first material is not completely reacted, the first material is not accumulated at the first discharge port 106, so that the first product can smoothly enter the distribution pipeline 30 through the first discharge port 106.
In the second embodiment of the present application, the blocking device 107 is configured as a vibrator (not shown in the drawings), and the first stirrer 104 is not specifically configured; the vibrator is arranged at the position, close to the first discharge port 106, of the outer wall of the first reaction kettle 101, and vibration of the vibrator enables first materials stacked at the first discharge port 106 to be dispersed, so that the first materials are prevented from blocking the first discharge port 106, and meanwhile the dispersed first materials are fully contacted with second materials, so that the reaction rate can be accelerated.
FIG. 4 schematically shows a schematic structural view of a second reaction apparatus according to an embodiment of the present application, as shown in FIG. 4:
the second reaction device 20 of the present application comprises a second reaction kettle 201, a third feeding device 202, a second stirrer 203, a baffle 204 and a circulation spraying device 205;
a second feeding port 206 is arranged at the top of the second reaction kettle 201, and a second discharging port 207 is arranged at the bottom of the second reaction kettle 201;
the second feeding ports 206 are respectively communicated with one end of the circulating spraying device 205, the third feeding device 202 and the second connecting pipeline 3012, and the second discharging ports 207 are communicated with the other end of the circulating spraying device 205.
And ethylene oxide is stored in the third feeding device 202, when the first product enters the second reaction kettle 201 through the second connecting pipeline 3012 and the second feeding port 206, the third feeding device 202 introduces the third material, namely ethylene oxide, into the second reaction kettle 201, and then the third material is stirred by the second stirrer 203, so that the first product fully contacts with the third material to react, and the final product alkyl phosphate oligomer is generated.
In the process of performing the second reaction, the circulation spraying device 205 can suck the liquid from the bottom of the second reaction kettle 201, and move the top of the second reaction kettle 201 along the pipeline to spray the liquid from the top of the second reaction kettle 201, so that the liquid at the bottom of the second reaction kettle 201 is fully contacted with the gas at the top of the second reaction kettle 201, and the reaction rate is accelerated.
Further, in the solution of the present application, the baffle 204 is disposed on the inner sidewall of the second reaction kettle 201, fixedly connected to the inner sidewall of the second reaction kettle 201, and protruding from the inner sidewall of the second reaction kettle 201 toward the center of the second reaction kettle 201.
Specifically, the baffles 204 are provided in multiple layers at different heights of the second reaction kettle 201, and are arranged at the inner side wall of the second reaction kettle 201 at intervals and in a ring shape;
when the second stirrer 203 stirs, the liquid is stirred to rotate to form a vortex, so that the centers of the two sides of the liquid level are high, and the circulating spraying device 205 only circulates the gas in the second reaction kettle 201, so that the contact area of the gas and the liquid is not quickened, the reaction rate is increased, and the circulating spraying device 205 loses the set meaning because the circulating spraying device 205 pumps the liquid from the bottom of the second reaction kettle 201, if the second stirrer 203 rotates too fast, or the liquid in the second reaction kettle 201 is less, and the liquid level at the center of the liquid is close to the second discharge hole 207, so that the circulating spraying device 205 pumps the gas in the second reaction kettle 201, but not pumps the liquid or pumps the less liquid.
The baffle 204 of the application is arranged so that when liquid rotates to form vortex, high liquid levels at two sides can touch the bottom plane of the baffle 204 and can not be lifted any more because of being blocked by the bottom plane of the baffle 204, and the excessive difference between the liquid levels at two sides and the liquid level at the center can be avoided, so that the liquid level at the center can not be too low, and the circulating spraying device 205 can be prevented from sucking gas; meanwhile, the liquid blocked by the baffle 204 can reversely drop to the center of the liquid, so that the contact area with the gas is increased, and part of the gas can be rolled up to drop, so that the liquid can be contacted with the gas, the reaction rate is further accelerated, and the alkyl phosphate oligomer can be prepared more quickly.
Further, the circulation spray device 205 includes a first line 2051, a second line 2052, and a jet reactor 2053;
the first pipe 2051 has one end communicating with the second feed port 206 and the other end communicating with the second discharge port 207, the jet reactor 2053 is provided on the first pipe 2051 and is provided near the second feed port 206, the second pipe 2052 has one end communicating with the jet reactor 2053 and the other end communicating with the top of the second reaction tank 201.
Specifically, a cavity is provided in the jet reactor 2053, and a nozzle communicating with the first pipe 2051 is provided on an inner side wall of the cavity far from the second reaction vessel 201, so that the liquid conveyed by the first pipe 2051 can be jetted in bulk and into the cavity.
One end of the second pipeline 2053 is communicated with the second reaction kettle 201, and the other end is communicated with the cavity, so that the sprayed liquid sprayed from the nozzle is fully contacted with the gas conveyed by the second pipeline 2053 to react, and then returns to the bottom of the second reaction kettle 201 along with the first pipeline 2051 through the second feed port 206.
A first circulation pump is arranged on the first pipeline 2051 near the second discharge port 207, so that the liquid at the bottom of the second reaction kettle 201 can be pumped, and a second circulation pump is arranged on the second pipeline 2052 near the second feed port 206, so that the gas at the top of the second reaction kettle 201 can be pumped.
The circulating spraying device 205 arranged as described above can continuously suck the liquid at the bottom of the second reaction kettle 201, so that the liquid in a spray shape is fully contacted with the gas, the reaction rate is accelerated, the liquid stirred at the bottom of the second reaction kettle 201 by the second stirrer 203 can react in the spraying reactor 2053 while reacting, the reaction rate is further accelerated, and the efficiency of preparing the alkyl phosphate oligomer is improved; meanwhile, as the ethylene oxide at the top of the second reaction kettle 201 is pumped, a large amount of enrichment of the ethylene oxide at the top of the second reaction kettle 201 is avoided, and the occurrence of harm is effectively reduced.
In summary, the apparatus for preparing an alkylphosphonate oligomer of the present application, by providing the distribution pipe 30 and simultaneously communicating with the plurality of second reaction apparatuses 20, can simultaneously perform a plurality of second reactions, and can prepare more alkylphosphonate oligomer in the same time, thereby improving the preparation efficiency compared to the conventional technique; meanwhile, the circulating spraying device 205 is arranged to circulate the liquid, so that the second-step reaction is not limited to the reaction at the bottom of the second reaction kettle 201, the contact area of the liquid and the gas is further increased, the reaction rate is further increased, and the preparation rate of the alkyl phosphate oligomer is improved.
The above description is only illustrative of the preferred embodiments of the present application and of the principles of the technology employed. It will be appreciated by persons skilled in the art that the scope of the application referred to in the present application is not limited to the specific combinations of the technical features described above, but also covers other technical features formed by any combination of the technical features described above or their equivalents without departing from the inventive concept. Such as the above-mentioned features and the technical features disclosed in the present application (but not limited to) having similar functions are replaced with each other.
It should be understood that, the sequence numbers of the steps in the summary and the embodiments of the present application do not necessarily mean the order of execution, and the execution order of the processes should be determined by the functions and the internal logic, and should not be construed as limiting the implementation process of the embodiments of the present application.

Claims (3)

1. An apparatus for producing an alkyl phosphate oligomer, comprising:
a first reaction device, a plurality of second reaction devices, and a distribution pipeline for communicating the first reaction device with the plurality of second reaction devices;
a plurality of connecting pipelines are arranged on the distribution pipeline, and valves which are independently opened and closed are arranged on the plurality of connecting pipelines, wherein the plurality of connecting pipelines comprise a first connecting pipeline communicated with the first reaction device and a plurality of second connecting pipelines respectively communicated with the plurality of second reaction devices correspondingly;
a first discharge hole communicated with the first connecting pipeline is formed in the first reaction device, and a blocking device for preventing powder materials from accumulating is arranged at the first discharge hole;
the first reaction device further comprises a first reaction kettle, a first feeding device, a second feeding device and a first stirrer;
a first feeding port is formed in the top of the first reaction kettle, and a first discharging port is formed in the bottom of the first reaction kettle;
the two first feeding ports are respectively communicated with the first feeding device and the second feeding device, and the first discharging port is communicated with the first connecting pipeline;
the second reaction device comprises a second reaction kettle, a third feeding device, a second stirrer and a circulating spraying device;
a second feeding port is formed in the top of the second reaction kettle, and a second discharging port is formed in the bottom of the second reaction kettle;
the second feeding holes are respectively communicated with one end of the circulating spraying device, the third feeding device and the second connecting pipeline correspondingly, and the second discharging holes are communicated with the other end of the circulating spraying device;
the second reaction device comprises a baffle plate,
the baffle plates are arranged in multiple layers, are arranged on the inner side wall of the second reaction kettle at intervals, are fixedly connected with the inner side wall of the second reaction kettle, and protrude out of the inner side wall of the second reaction kettle;
the blocking device comprises a blocking cover, and the first stirrer is arranged in a telescopic moving structure;
the blocking cover is fixedly connected with one end of the first stirrer, which is close to the first discharge hole;
the first stirrer stretches and contracts to control the blocking cover to open and close the first discharge hole;
the blocking device comprises a vibrator arranged on the outer wall of the first reaction kettle;
the vibrator is arranged close to the first discharge hole;
the circulating spraying device comprises a first pipeline, a second pipeline and a jet reactor;
one end of the first pipeline is communicated with the second feeding port, and the other end of the first pipeline is connected with the second discharging port;
the jet reactor is arranged on the first pipeline, one end of the second pipeline is communicated with the jet reactor, and the other end of the second pipeline is communicated with the top of the second reaction kettle;
a cavity is arranged in the jet reactor, and a nozzle communicated with the first pipeline is arranged on the inner side wall of the cavity, which is far away from the second reaction kettle;
the second pipeline is communicated with the cavity.
2. The apparatus for producing an alkylphosphate oligomer according to claim 1, wherein valves which are independently opened and closed are provided in a plurality of said connecting pipes of said distribution pipe.
3. The apparatus for producing an alkylphosphate oligomer according to claim 1, wherein a purge means is provided on the distribution pipe in communication with the distribution pipe;
inert gas is stored inside the purging device.
CN202211375425.1A 2022-11-04 2022-11-04 Alkyl phosphate oligomer's preparation facilities Active CN115634650B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2810740Y (en) * 2005-01-05 2006-08-30 武汉化工学院 Vertical circulative impinging stream reactor
CN101400724A (en) * 2006-03-07 2009-04-01 托塔尔石油化学产品研究弗吕公司 Method and system for degassing polymer powder
WO2020014211A1 (en) * 2018-07-09 2020-01-16 Blue Cube Ip Llc Eductor nozzle to improve gas hold up in gas-liquid reactor
CN211070043U (en) * 2019-09-29 2020-07-24 安徽海螺新材料科技有限公司 Production system of polyether
CN216125612U (en) * 2021-10-27 2022-03-25 上海东庚设备工程技术有限公司 Reation kettle measures charging equipment
CN114768743A (en) * 2022-05-24 2022-07-22 云南云天化股份有限公司 Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2810740Y (en) * 2005-01-05 2006-08-30 武汉化工学院 Vertical circulative impinging stream reactor
CN101400724A (en) * 2006-03-07 2009-04-01 托塔尔石油化学产品研究弗吕公司 Method and system for degassing polymer powder
WO2020014211A1 (en) * 2018-07-09 2020-01-16 Blue Cube Ip Llc Eductor nozzle to improve gas hold up in gas-liquid reactor
CN211070043U (en) * 2019-09-29 2020-07-24 安徽海螺新材料科技有限公司 Production system of polyether
CN216125612U (en) * 2021-10-27 2022-03-25 上海东庚设备工程技术有限公司 Reation kettle measures charging equipment
CN114768743A (en) * 2022-05-24 2022-07-22 云南云天化股份有限公司 Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method

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