CN113413641B

CN113413641B - Distillation cooler applied to production of high-molecular polymer intermediate and cooling method

Info

Publication number: CN113413641B
Application number: CN202110977860.0A
Authority: CN
Inventors: 李金江; 钟华东; 荣洪杰
Original assignee: Shandong Lanwan New Material Co Ltd
Current assignee: Shandong Lanwan New Material Co Ltd
Priority date: 2021-08-25
Filing date: 2021-08-25
Publication date: 2021-11-16
Anticipated expiration: 2041-08-25
Also published as: CN113413641A

Abstract

The invention relates to a distillation cooler and a cooling method applied to the production of a high molecular polymer intermediate, which relate to the technical field of chemical equipment and comprise a tank body, a heat insulation layer, a spray head, a filter table, a screen plate and a collecting pipe, wherein the tank body is a columnar tank, the heat insulation layer is also a columnar tank, the heat insulation layer is embedded in the tank body, the heat insulation layer is fixedly connected with an air inlet pipe on the tank body, the air inlet pipe penetrates through the heat insulation layer and the tank body to be connected with the spray head, the spray head is positioned in the heat insulation layer, and nitrogen gas with the temperature of-100 ℃ to-125 ℃ flows in the air inlet pipe; the filter table is fixedly connected to the lower part of the heat insulation layer, a plurality of flow holes are formed in the middle of the filter table at intervals, the screen plate is laid on the upper end face of the filter table, the mesh opening diameter of the screen plate is smaller than that of the flow holes, the collecting pipe is fixedly connected to the bottom end face of the filter table, and the collecting pipe abuts against the bottom of the tank body.

Description

Distillation cooler applied to production of high-molecular polymer intermediate and cooling method

Technical Field

The invention relates to the technical field of chemical equipment, in particular to a distillation cooler and a cooling method applied to the production of a high molecular polymer intermediate.

Background

The high molecular polymer is a large class of water-soluble polymers with the widest application range at present, has high application value in the fields of petrochemical industry, papermaking, textile printing and dyeing, daily chemicals, particularly as a flocculating agent in the fields of water treatment, sludge dewatering and the like, and has the advantages of increasing the market demand year by year and good prospect. The production mode of the high molecular polymer mainly adopts the polymerization of cationic monomers such as quaternary ammonium salt, quaternary phosphonium salt, quaternary sulfonium salt and the like, wherein the mechanical force survivability of the DAC cationic polymer for forming floccules is far better than that of a DMC flocculant, and the high molecular flocculant is a high molecular flocculant product which is most widely applied and used at present. DA is a main intermediate for producing DAC cationic polymers at present, the quality of DA products directly influences the product quality and yield of the subsequent DAC cationic high-molecular polymers, and the quality of DA products depends on a production device for esterification.

As the domestic complete equipment for realizing the DA industrial production is less, compared with the existing equipment, the problems of insufficient reaction depth of a monomer reaction kettle, low separation precision and recovery rate of a catalyst and an intermediate product of the equipment, low automation control level, poor continuous production capacity, unstable product quality and the like exist. Particularly, the separation accuracy of the intermediate product is generally low, and if a chemical method is adopted, such as precipitation or vaporization separation of materials except the intermediate product by adding reactants, although the separation accuracy can be improved, the cost for adding the reactants is higher, and even exceeds the commercial value which can be created by the intermediate product. However, the separation accuracy is not high because some impurity liquid is still carried away in the flowing process of water by a physical method such as a water washing method with different solubility.

Therefore, in view of the above disadvantages, it is desirable to provide a distillation cooler and a cooling method for use in the production of a high molecular polymer intermediate.

Disclosure of Invention

Technical problem to be solved

The invention aims to solve the technical problem of low separation precision of the existing intermediate product.

(II) technical scheme

In order to solve the technical problems, the invention provides a distillation cooler applied to the production of a high molecular polymer intermediate, which comprises a tank body, a heat insulation layer, a spray head, a filter table, a screen plate and a collecting pipe, wherein the tank body is a columnar tank, the heat insulation layer is also a columnar tank, the heat insulation layer is embedded in the tank body, the heat insulation layer is fixedly connected with an air inlet pipe on the tank body, the air inlet pipe penetrates through the heat insulation layer and the tank body to be connected with the spray head, the spray head is positioned in the heat insulation layer, and nitrogen gas at the temperature of-100 ℃ to-125 ℃ flows in the air inlet pipe; the filter table is fixedly connected to the lower portion of the heat insulation layer, a plurality of flow holes are formed in the middle of the filter table at intervals, the screen plate is laid on the upper end face of the filter table, the mesh aperture of the screen plate is smaller than the aperture of the flow holes, the collecting pipe is fixedly connected to the bottom end face of the filter table, and the collecting pipe is abutted to the bottom of the tank body.

As a further explanation of the invention, preferably, the top of the tank body is fixedly connected with a feed inlet, and the feed inlet is communicated with the inner cavity of the heat insulation layer; the bottom of the tank body is fixedly connected with a discharge port which is communicated with the collecting pipe.

As a further explanation of the invention, preferably, the top of the heat insulation layer is lower than the height of the inner cavity of the tank body, the top of the heat insulation layer is fixedly connected with a tubular joint, and the joint is connected with the feed inlet; a mixed liquid containing n-hexane and methanol flows in the feed inlet and the joint.

As a further explanation of the present invention, preferably, one side of the top of the thermal insulation layer is fixedly connected with an exhaust pipe, the exhaust pipe penetrates through the tank body and extends out of the tank body, and the exhaust pipe is connected to the recovery tank.

As a further description of the present invention, preferably, the collecting pipe is an inverted circular truncated cone casing, the outer diameter of the top of the collecting pipe is the same as the outer diameter of the filter stage, the bottom port of the collecting pipe abuts against the discharge port, and the caliber of the bottom of the collecting pipe is equal to the caliber of the discharge port.

As a further explanation of the present invention, it is preferable that the filter stage has a disk-like structure made of the same material as the heat insulating layer.

The invention also provides a cooling method of the distillation cooler applied to the production of the high molecular polymer intermediate, which comprises the following steps:

i, connecting an outlet end of a nitrogen tank in which liquid nitrogen exists at a gasification tank, introducing the liquid nitrogen into the gasification tank, gradually gasifying the liquid nitrogen into a gaseous state by a heating mode, and heating the nitrogen to-100-125 ℃;

after the temperature of the nitrogen rises to the specified temperature, a valve on the air inlet pipe is opened to enable the nitrogen to enter the thermal insulation layer through the spray head, the temperature in the thermal insulation layer is detected in real time through a temperature sensor and a pressure sensor in the thermal insulation layer, and meanwhile, a valve of the air exhaust pipe is opened to exhaust redundant gas in the thermal insulation layer, so that the air pressure in the thermal insulation layer is kept stable;

when the temperature in the thermal insulation layer is kept at about-100 ℃, a mixed solution containing normal hexane and methanol is filled into the thermal insulation layer through a feed inlet and a connector, and most of liquid is condensed into solid in a low-temperature environment and falls onto the screen plate;

after the content of the heat insulation layer meets the design requirement, closing a valve between an air inlet pipe and a gasification tank, opening a valve between the air inlet pipe and a recovery tank, keeping the temperature of nitrogen in the recovery tank between-94 ℃ and-97 ℃, then filling the nitrogen in the recovery tank into the heat insulation layer through the air inlet pipe, keeping the temperature in the heat insulation layer between-95.6 ℃ and-96.8 ℃, starting to liquefy solid methanol, percolating the solid methanol into a collecting pipe through a screen plate and a filter platform, guiding the liquid to a discharge port through the collecting pipe, and guiding the liquid to a methanol storage area through a multi-way valve of the discharge port;

after no liquid is generated in the thermal insulation layer, continuously heating the nitrogen in the recovery tank to ensure that the temperature of the gas in the recovery tank is higher than-93 ℃, then introducing the gas into the thermal insulation layer to liquefy the solid n-hexane, and guiding the liquefied n-hexane to a n-hexane storage area through a multi-way valve of a discharge port; separation of methanol and n-hexane was accomplished.

As a further description of the present invention, it is preferable that an atomizer is attached to the joint to disperse the liquid flowing through the joint into water drops.

As a further explanation of the present invention, it is preferable that the valves on the air intake pipe and the air exhaust pipe are electromagnetic valves, the temperature sensor and the pressure sensor in the thermal insulation layer are connected to the industrial personal computer, and the air intake amount and the air exhaust amount of the nitrogen in the thermal insulation layer are automatically adjusted by detecting the temperature and the air pressure in the thermal insulation layer, so as to keep the changes of the temperature and the air pressure within a safe range.

As a further explanation of the present invention, it is preferable that the number of recovery tanks is two or more.

(III) advantageous effects

The technical scheme of the invention has the following advantages:

according to the invention, the traditional distillation tower structure is improved, and the intermediate product n-hexane and methanol are separated by using a condensation method, so that the separation precision is high, the temperature control can be simpler and more accurate compared with the traditional heating distillation mode, no additional energy input is required in the separation process, and the electric power cost is saved.

Drawings

FIG. 1 is a diagram of the overall assembly effect of the present invention;

FIG. 2 is a cross-sectional view of the present invention;

FIG. 3 is a side view of the present invention;

FIG. 4 is a block diagram of the filter stage of the present invention;

fig. 5 is a cross-sectional view of a manifold of the present invention.

In the figure: 1. a tank body; 11. an upper cover; 12. a feed inlet; 13. a discharge port; 2. a thermal insulation layer; 21. a joint; 3. a spray head; 31. an air inlet pipe; 32. an air exhaust pipe; 4. filtering the table; 41. an orifice; 5. a screen plate; 6. a header pipe; 61. and (7) supporting legs.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.

A distillation cooler and a cooling method applied to production of a high molecular polymer intermediate are combined with a figure 1 and a figure 2 and comprise a tank body 1, a heat insulation layer 2, a spray head 3, a filter table 4, a screen plate 5 and a collecting pipe 6, wherein the tank body 1 is a columnar tank, the heat insulation layer 2 is also a columnar tank, the heat insulation layer 2 is embedded into the tank body 1, the spray head 3 is positioned in the heat insulation layer 2, the filter table 4 is fixedly connected to the lower part of the heat insulation layer 2, the screen plate 5 is paved on the upper end surface of the filter table 4, the collecting pipe 6 is fixedly connected to the bottom end surface of the filter table 4, and the collecting pipe 6 is abutted to the bottom of the tank body 1.

With reference to fig. 1 and 2, the top end of the tank body 1 is open and is fixedly connected with an upper cover 11 through a flange and a bolt, and the upper cover is used for sealing the tank body 1 after the thermal insulation layer 2 is assembled. The upper cover 11 is fixedly connected with a feed inlet 12, the top of the heat insulating layer 2 is lower than the height of the inner cavity of the tank body 1, the top of the heat insulating layer 2 is fixedly connected with a tubular joint 21, and the joint 21 is connected with the feed inlet 12 so as to enable the feed inlet 12 to be communicated with the inner cavity of the heat insulating layer 2 and be used for injecting mixed liquid containing normal hexane and methanol into the heat insulating layer 2. The bottom of the tank body 1 is fixedly connected with a discharge port 13, the discharge port 13 is communicated with the collecting pipe 6, and the discharge port 13 is externally connected with a multi-way valve for leading out separation liquid and leading to different storage areas respectively.

With reference to fig. 2 and 3, the thermal insulation layer 2 has the same structure as a dewar flask, and a temperature sensor and a pressure sensor are arranged in the thermal insulation layer 2 for monitoring the temperature and the air pressure in the thermal insulation layer 2 in real time, so as to determine whether the purification work is performed normally or whether a safety problem exists. The heat insulation layer 2 and the tank body 1 are fixedly connected with an air inlet pipe 31, and nitrogen with the temperature of-100 ℃ to-125 ℃ flows in the air inlet pipe 31. The air inlet pipe 31 penetrates through the heat insulation layer 2 and the tank body 1 to be connected with the spray head 3 and is used for spraying nitrogen into the heat insulation layer 2 in a large range so as to enlarge the contact range of the nitrogen and the mixed liquid. 2 top one sides on heat insulating layer have linked firmly exhaust tube 32, and outside exhaust tube 32 runs through jar body 1 and stretches out jar body 1, exhaust tube 32 connected on retrieving the jar for take out heat insulating layer 2 with the nitrogen gas that heaies up and retrieve outward and recycle. Retrieve jar quantity more than or equal to two, be convenient for save different temperature's nitrogen gas, set up a plurality of recovery jars in addition, and some recovery jars of vacant for when heat insulating layer 2 atmospheric pressure is too high, carry out the pressure release in the recovery jar of vacant with unnecessary nitrogen gas pump income, avoid direct discharge polluted environment.

With reference to fig. 4 and 5, the filter stage 4 is a disk made of the same material and structure as the thermal insulation layer 2, and a plurality of flow holes 41 are spaced in the middle of the filter stage 4 for guiding the liquid out of the tank body 1. The screen plate 5 is a disc-shaped screen formed by weaving conventional stainless steel wires, and the aperture of the screen plate 5 is smaller than that of the flow hole 41 and is used for receiving condensed solid methanol and n-hexane. The collecting main 6 is an inverted circular truncated cone shell, a plurality of square steel supporting legs 61 are fixedly connected to the periphery of the collecting main 6 at intervals, and the supporting legs 61 are abutted to the bottom end face of the tank body 1 and used for supporting the collecting main 6 and the heat insulation layer 2. The 6 top external diameters of pressure manifold are the same with 4 external diameters of straining platform, and 6 bottom ports of pressure manifold and 13 butts of discharge gate and 6 bottom bores of pressure manifold equal to 13 bores of discharge gate for collect 13 departments of discharge gate with liquid and avoid the deposit in jar body 1.

Through the comparatively simple cooler structure of the aforesaid, cooperation low temperature nitrogen gas can purify methyl alcohol and n-hexane, can not mix other impurity moreover for the methyl alcohol and the n-hexane purity homoenergetic that separate out at last can reach more than 99%, in addition at the disengaging process, except that air pump and oil pump produce the electric energy loss, do not use other electric energy, compare traditional distillation purification, not only purification precision is high, and energy consumption is few moreover, and the purification cost is low. In addition, the liquid nitrogen has low acquisition cost, cannot be mixed into an intermediate product, cannot react with the intermediate product, and is very practical.

connecting an outlet end of a nitrogen tank in which liquid nitrogen exists at a gasification tank, introducing the liquid nitrogen into the gasification tank, gradually gasifying the liquid nitrogen into a gaseous state in an environment temperature rise and pressure reduction mode, and raising the temperature of the nitrogen to between-100 ℃ and-125 ℃, so that accidents caused by rapid temperature change due to direct filling of liquid nitrogen are avoided.

After the temperature of the nitrogen rises to a specified temperature, a valve on the air inlet pipe 31 is opened to enable the nitrogen to enter the heat insulation layer 2 through the spray head 3, the temperature in the heat insulation layer 2 is detected in real time through a temperature sensor and a pressure sensor in the heat insulation layer 2, meanwhile, a valve of the exhaust pipe 32 is opened to exhaust redundant gas in the heat insulation layer 2, and the air pressure in the heat insulation layer 2 is guaranteed to be kept stable; and the function of precooling is achieved, and the phenomenon that the temperature change amplitude in the later-stage heat insulation layer 2 is too large is avoided.

And III, when the temperature in the heat insulation layer 2 is kept at about minus 100 ℃, pouring a mixed solution containing normal hexane and methanol into the heat insulation layer 2 through a feed inlet 12 and a connector 21, wherein most of liquid is condensed into a solid and falls onto the screen plate 5 in a low-temperature environment because the melting point of the methanol is minus 97.8 ℃ and the melting point of the normal hexane is minus 95 ℃. The atomizer can additionally be installed in joint 21 department, makes the liquid of flowing through in the joint 21 split into the water droplet form, can not only make liquid condense sooner, can also avoid appearing the condition of bold "ice package water", prevents effectively that bold "ice package water" from dropping and pounces bad otter board 5 and strain platform 4 on otter board 5, can also avoid liquid outflow to freeze the mesh of otter board 5 and influence subsequent liquid infiltration in addition. Water drops are condensed into small ice bodies in a low-temperature environment and fall onto the screen plate 5, and the ice bodies can be limited to continuously fall by using fine holes on the screen plate 5, so that subsequent heating separation work is performed.

And IV, after the internal volume of the heat insulation layer 2 meets the design requirement, closing a valve between the air inlet pipe 31 and the gasification tank, opening the valve between the air inlet pipe 31 and the recovery tank, reducing the pressure of nitrogen in the recovery tank or exchanging heat with the outside, keeping the temperature between-94 ℃ and-97 ℃, then filling the nitrogen in the recovery tank into the heat insulation layer 2 through the air inlet pipe 31, keeping the temperature in the heat insulation layer 2 between-95.6 ℃ and-96.8 ℃, starting to liquefy solid methanol, percolating the solid methanol into a collecting pipe 6 through a screen plate 5 and a filter table 4, guiding the liquid to a discharge port 13 through the collecting pipe 6, and guiding the liquid to a methanol storage area through a multi-way valve of the discharge port to finish the purification of the methanol.

And V, after no liquid is generated in the heat insulation layer 2, continuing to heat the nitrogen in the recovery tank so as to ensure that the temperature of the gas in the recovery tank is higher than-93 ℃, and if the liquid contains water, not enabling the temperature to be higher than 0 ℃. Then, introducing the gas into the heat insulation layer 2 to liquefy the solid n-hexane, and guiding the liquefied n-hexane to a n-hexane storage area through a multi-way valve of a discharge port; separation of methanol and n-hexane was accomplished. And the rest intermediate products such as water and the like can be liquefied by heating for three times, or other heavy component products are separated out in a distillation mode before entering the feed inlet, and only methanol and normal hexane or water are reserved to further improve the separation precision.

In addition, the valves on the air inlet pipe 31 and the air exhaust pipe 32 can be set as electromagnetic valves, the temperature sensor and the pressure sensor in the thermal insulation layer 2 are connected with an industrial personal computer, the air inflow and the air exhaust of nitrogen in the thermal insulation layer 2 are automatically adjusted through detecting the temperature and the air pressure in the thermal insulation layer 2, and the change of the temperature and the air pressure is kept in a safe range, so that the safety of purification work is improved.

In conclusion, the invention can separate the intermediate product with high precision by designing the cooler with simple structure and combining the use method, and has the advantages of low energy consumption and extremely low cost, even if some recovery tanks or other safety facilities are additionally arranged, although some cost is generated, the cost is basically negligible compared with the total economic benefit and the requirement of safe production. And no matter methyl alcohol and n-hexane are melting point or boiling point all very close, adopt distillation heating temperature wayward, the high temperature then can evaporate simultaneously, the temperature crosses lowly then can not evaporate, and carry out the mode that heaies up through make-up gas, direct control air input can, easy operation is convenient, adjusts the degree of difficulty and hangs down, changes the assurance.

Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims

1. The cooling method of the distillation cooler applied to the production of the high molecular polymer intermediate comprises the steps that the distillation cooler comprises a tank body (1), a heat insulation layer (2), a spray head (3), a filter table (4), a screen plate (5) and a collecting pipe (6), wherein the tank body (1) is a columnar tank, the heat insulation layer (2) is also a columnar tank, the heat insulation layer (2) is embedded into the tank body (1), the heat insulation layer (2) and the tank body (1) are fixedly connected with an air inlet pipe (31), the spray head (3) is positioned in the heat insulation layer (2), and nitrogen gas at the temperature of-100 ℃ to-125 ℃ flows in the air inlet pipe (31); the filter table (4) is fixedly connected to the lower part of the heat insulation layer (2), a plurality of flow holes (41) are arranged in the middle of the filter table (4) at intervals, the screen plate (5) is laid on the upper end face of the filter table (4), the mesh aperture of the screen plate (5) is smaller than the aperture of the flow holes (41), the collecting pipe (6) is fixedly connected to the bottom end face of the filter table (4), and the collecting pipe (6) is abutted to the bottom of the tank body (1); wherein the top of the tank body (1) is fixedly connected with a feed inlet (12), and the feed inlet (12) is communicated with the inner cavity of the heat insulation layer (2); the bottom of the tank body (1) is fixedly connected with a discharge port (13), and the discharge port (13) is communicated with the collecting pipe (6); the top of the heat insulation layer (2) is lower than the height of the inner cavity of the tank body (1), the top of the heat insulation layer (2) is fixedly connected with a tubular joint (21), and the joint (21) is connected with the feed inlet (12); a mixed liquid containing normal hexane and methanol flows in the feed inlet (12) and the joint (21); one side of the top of the heat insulation layer (2) is fixedly connected with an air extraction pipe (32), the air extraction pipe (32) penetrates through the tank body (1) and extends out of the tank body (1), and the air extraction pipe (32) is connected to the recovery tank; exhaust tube (3) are connected on retrieving the jar for take out heat insulating layer (2) with the nitrogen gas of intensification and retrieve outward and recycle, retrieve jar quantity more than or equal to two, its characterized in that: comprises the following steps of (a) carrying out,

after the temperature of the nitrogen rises to a specified temperature, a valve on the air inlet pipe (31) is opened to enable the nitrogen to enter the heat insulation layer (2) through the spray head (3), the temperature in the heat insulation layer (2) is detected in real time through a temperature sensor and a pressure sensor in the heat insulation layer (2), and meanwhile, a valve of the air exhaust pipe (32) is opened to exhaust redundant air in the heat insulation layer (2) to ensure that the air pressure in the heat insulation layer (2) is kept stable;

when the temperature in the heat insulation layer (2) is kept at about-100 ℃, a mixed solution containing normal hexane and methanol is poured into the heat insulation layer (2) through a feeding hole (12) and a connector (21), and most of liquid is condensed into a solid in a low-temperature environment and falls onto the screen plate (5);

after the internal volume of the heat insulation layer (2) meets the design requirement, closing a valve between an air inlet pipe (31) and a gasification tank, opening the valve between the air inlet pipe (31) and a recovery tank, maintaining the temperature of nitrogen in the recovery tank between-94 ℃ and-97 ℃ at the moment, then filling the nitrogen in the recovery tank into the heat insulation layer (2) through the air inlet pipe (31), maintaining the temperature in the heat insulation layer (2) between-95.6 ℃ and-96.8 ℃, starting to liquefy solid methanol, seeping and flowing into a collecting pipe (6) through a screen plate (5) and a filter platform (4), wherein the collecting pipe (6) is an inverted circular truncated cone shell, the outer diameter of the top of the collecting pipe (6) is the same as that of the filter platform (4), the bottom port of the collecting pipe (6) is abutted against a discharge port (13), and the bottom caliber of the collecting pipe (6) is equal to that of the discharge port (13); the filtering table (4) is of a disc-shaped structure made of the same material as the heat insulation layer (2); liquid is guided to a discharge port (13) through a collecting pipe (6) and then guided to a methanol storage area through a multi-way valve of the discharge port (13);

after no liquid is generated in the heat insulation layer (2), continuously heating nitrogen in the recovery tank to ensure that the temperature of gas in the recovery tank is higher than-93 ℃, then introducing the gas into the heat insulation layer (2) to liquefy solid n-hexane, and guiding the liquefied n-hexane to a n-hexane storage area through a multi-way valve of a discharge hole (13); separation of methanol and n-hexane was accomplished.

2. The cooling method of a distillation cooler applied to production of a high molecular polymer intermediate according to claim 1, characterized in that: an atomizer can be additionally arranged at the joint (21) to enable the liquid flowing through the joint (21) to be dispersed into a water droplet shape.

3. The cooling method of a distillation cooler applied to production of a high molecular polymer intermediate according to claim 2, characterized in that: the valves on the air inlet pipe (31) and the air exhaust pipe (32) are electromagnetic valves, the electromagnetic valves, a temperature sensor and a pressure sensor in the heat insulation layer (2) are connected with an industrial personal computer, the air inflow and the air discharge of nitrogen in the heat insulation layer (2) are automatically adjusted through detecting the temperature and the air pressure in the heat insulation layer (2), and the change of the temperature and the air pressure is kept within a safe range.