CN113413627B

CN113413627B - Energy-saving separation device for high-molecular polymer intermediate

Info

Publication number: CN113413627B
Application number: CN202110977863.4A
Authority: CN
Inventors: 李金江; 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: 2021-11-09
Anticipated expiration: 2041-08-25
Also published as: CN113413627A

Abstract

The invention relates to an energy-saving separation device for a high-molecular polymer intermediate, which relates to the technical field of chemical equipment and comprises a shell, a heating pipe and a liquid cylinder, wherein the shell is in a cylindrical pipe shape, the heating pipe is fixedly connected to the middle part of the shell, the upper part of the shell is fixedly connected with a cylindrical upper cover, the lower part of the shell is fixedly connected with a cylindrical lower cover, the top of the upper cover is fixedly connected with a liquid inlet pipe, the bottom of the lower cover is fixedly connected with a liquid outlet pipe, and the liquid inlet pipe and the liquid outlet pipe are both communicated with an inner cavity of the shell; the liquid cylinder is embedded in the lower cover, the top of the liquid cylinder is fixedly connected with an air outlet pipe, and the bottom of the liquid cylinder is fixedly connected with two liquid flow pipes; the invention has the advantages that reactants can be heated and methanol can be purified without an additional separation device.

Description

Energy-saving separation device for high-molecular polymer intermediate

Technical Field

The invention relates to the technical field of chemical equipment, in particular to an energy-saving separation device for 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 method of the high 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 flocculating group formed by the cationic polymers such as DAC (acryloyloxyethyl trimethyl ammonium chloride, [ CAS accession number ] 46830-22-2) is far better than that of the flocculating agent such as DMC (methacryloyloxyethyl trimethyl ammonium chloride, [ CAS accession number ] 5039-78-1), and the high polymer flocculating agent is a high polymer flocculating agent product which is most widely applied and used in most amount at present. DA (dimethylamino ethyl acrylate, CAS (CAS) accession number) 2439-35-2, hereinafter referred to as acrylic acid) 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 DAC cationic high polymer, and the quality of DA products depends on a production device for esterification reaction.

Compared with the prior device, the device has the problems of insufficient reaction depth of the monomer reaction kettle, low separation precision and recovery rate of the catalyst and the intermediate product of the device and low thermal efficiency, thereby causing low energy conversion rate. To ensure good output, more power needs to be consumed, and lower energy conversion yields more waste of resources than theoretically required energy values. For example, much of the heat generated by the heater is dissipated to the external environment and cannot participate in heating the raw materials, so that the thermal efficiency of the heater is relatively low, only 73% of the electric energy directly participates in heating the raw materials, and the rest is substantially dissipated to the external environment and is wasted.

Therefore, in view of the above disadvantages, it is desirable to provide an energy-saving separation apparatus for a high molecular polymer intermediate.

Disclosure of Invention

Technical problem to be solved

The invention aims to solve the technical problem that the existing heater is low in heat efficiency.

(II) technical scheme

In order to solve the technical problems, the invention provides an energy-saving separation device for a high molecular polymer intermediate, which comprises a shell, a heating pipe and a liquid cylinder, wherein the shell is in a cylindrical pipe shape, the heating pipe is fixedly connected to the middle part of the shell, the upper part of the shell is fixedly connected with a cylindrical upper cover, the lower part of the shell is fixedly connected with a cylindrical lower cover, the top of the upper cover is fixedly connected with a liquid inlet pipe, the bottom of the lower cover is fixedly connected with a liquid outlet pipe, and the liquid inlet pipe and the liquid outlet pipe are both communicated with an inner cavity of the shell; the liquid cylinder is embedded in the lower cover, the top of the liquid cylinder is fixedly connected with an air outlet pipe, and the bottom of the liquid cylinder is fixedly connected with two liquid flow pipes; wherein, the liquid inlet pipe and the liquid outlet pipe flow the mixed liquid of methyl acrylate, dimethylethanolamine and catalyst, and the liquid cylinder stores deionized water dissolved with methanol.

As a further explanation of the present invention, preferably, two liquid flow pipes both penetrate through the lower cover to communicate with the liquid cylinder, wherein one liquid flow pipe is communicated with an outlet end of the n-hexane washing tank, and the other liquid flow pipe is connected with the water tank.

As a further explanation of the present invention, it is preferable that the air outlet pipe extends into the cavity of the housing and the upper cover, and the air outlet end of the air outlet pipe extends out of the upper cover and is connected with a methanol condenser.

As a further explanation of the present invention, preferably, the heating pipes are infrared heaters, the housing is fixedly connected with a heat insulating ring, an electronic device is arranged in the heat insulating ring, the plurality of heating pipes are fixedly connected to the bottom of the heat insulating ring at annular intervals, and the heating pipes are electrically connected with the electronic device; one side of the heat insulation ring is fixedly connected with a heating pipeline which is electrically connected with the electronic device and extends out of the shell.

As a further explanation of the present invention, preferably, the bottom of the heating tube is fixedly connected with a support ring, the outer ring of the support ring is welded on the inner wall of the housing, and the liquid cylinder is partially embedded in the support ring.

As a further explanation of the present invention, preferably, the liquid cylinder includes a fixed cylinder and a volume cylinder, both the fixed cylinder and the volume cylinder are cylindrical hollow shell cylinders, and the fixed cylinder is fixedly connected to the top of the volume cylinder and is communicated with the volume cylinder; the solid fixed cylinder external diameter equals the lock ring internal diameter, and in the solid fixed cylinder embedding lock ring, a volume section of thick bamboo external diameter is the same with the lower cover internal diameter, and in the volume section of thick bamboo embedding lower cover, the liquid flow of the interior liquid inlet pipe is through solid fixed cylinder and volume section of thick bamboo flow direction drain pipe.

As a further explanation of the present invention, preferably, the outer side of the fixed cylinder is provided with a liquid inlet channel, the outer side of the volume cylinder is provided with a liquid flow channel, the liquid flow channel is communicated with the liquid inlet channel, the liquid inlet channel is communicated with the inner cavity of the housing, and the liquid flow channel is communicated with the liquid outlet pipe.

As a further explanation of the present invention, preferably, the inside of the liquid inlet channel and the liquid flow channel is fixedly connected with a zigzag partition plate, a part of the partition plate with a large axial distance from the lower cover is fixedly connected in the liquid flow channel, and the axial distance from the partition plate and the lower cover is smaller than the inner diameter of the volume cylinder.

As a further explanation of the present invention, preferably, the bottom of the volume cylinder is abutted with an annular gasket, and the radius of the inner ring of the gasket is larger than the maximum distance between the partition plate and the axis of the lower cover, so that the cavity of the gasket located right below the liquid flow channel is a flow hole, and the flow hole is communicated with the liquid outlet pipe.

As a further illustration of the present invention, it is preferable that the fixed cylinder and the volume cylinder contain methanol in deionized water in a volume smaller than the total volume of the liquid cylinder, and the gas outlet pipe is connected to the fixed cylinder.

(III) advantageous effects

The technical scheme of the invention has the following advantages:

according to the invention, the methanol distillation method is added into the reaction heater through creative design, the methanol is extracted from the deionized water by utilizing the heat emitted outwards by the heater, the normal heating of the heater to reactants is not influenced, in addition, an additional distillation tower and a heating device are not required to be additionally arranged for carrying out distillation purification on the deionized water containing the methanol, the heat efficiency of the heater is improved, and the waste of additional resources is reduced.

Drawings

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

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

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

FIG. 4 is a view of the cartridge of the present invention;

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

In the figure: 1. a housing; 11. an upper cover; 12. a lower cover; 13. a liquid inlet pipe; 14. a liquid outlet pipe; 2. heating a tube; 21. a heat insulating ring; 22. a heating line; 23. a support ring; 3. a liquid cylinder; 31. a containment cylinder; 32. a fixed cylinder; 33. a liquid inlet passage; 34. a fluid passage; 35. a partition plate; 36. a gasket; 37. an orifice; 38. an air outlet pipe; 39. a liquid flowing pipe.

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.

The utility model provides an energy-conserving separator of high molecular polymer intermediate, combines fig. 1, fig. 2, including casing 1, heating pipe 2 and liquid section of thick bamboo 3, casing 1 is the cylinder tubulose, and heating pipe 2 links firmly at 1 middle part of casing, and 1 upper portion of casing has linked firmly the upper cover 11 of tube-shape, and 1 lower part of casing has linked firmly the lower cover 12 of tube-shape, and upper cover 11 top has linked firmly feed liquor pipe 13, and lower cover 12 bottom has linked firmly drain pipe 14, and feed liquor pipe 13 and drain pipe 14 all communicate with each other with 1 inner chamber of casing. The liquid inlet pipe 13 is connected with an esterification reaction kettle, the esterification reaction kettle injects a mixed liquid of methyl acrylate, dimethylethanolamine and a catalyst into the liquid inlet pipe 13, and the temperature of the mixed liquid reaches the temperature capable of generating forward reaction by heating the heating pipe 2, so that heat is provided for the esterification reaction. The liquid cylinder 3 is embedded in the lower cover 12, the top of the liquid cylinder 3 is fixedly connected with an air outlet pipe 38, the bottom of the liquid cylinder 3 is fixedly connected with two liquid flow pipes 39, and deionized water dissolved with methanol is stored in the liquid cylinder 3 in a flowing manner.

Combine fig. 2, fig. 3, optional infrared heating pipe of

heating pipe

2, 1 upper portion of casing has linked firmly annular heat insulating ring 21, heat insulating ring 21 inside cavity just is equipped with electronic device in, generally be the circuit board, a plurality of heating pipe 2 is annular interval and links firmly in heat insulating ring 21 bottom, 2 one end imbeds in heat insulating ring 21 with circuit board electric connection, heat insulating ring 21 one side has linked firmly heating pipeline 22, heating pipeline 22 stretches out 1 external connection power supply of casing and industrial computer, be used for heating pipe 2 power supplies and adjust calorific capacity. The bottom of the heating pipe 2 is fixedly connected with an annular support ring 23, the outer ring of the support ring 23 is welded on the inner wall of the shell 1, and the part of the liquid cylinder 3 is embedded into the support ring 23. The support ring 23 can support the heating pipe 2 and can also be used for fixing the liquid cylinder 3.

With reference to fig. 2, 4 and 5, the liquid cylinder 3 includes a fixed cylinder 32 and a volume cylinder 31, and both the fixed cylinder 32 and the volume cylinder 31 are cylindrical hollow shells and are formed by blow molding of PVC material, so that the liquid cylinder 3 has certain flexibility, and has better compression resistance compared with metal material. The fixed cylinder 32 is fixedly connected to the top of the volume cylinder 31 and communicated with the volume cylinder 31; the outer diameter of the fixed cylinder 32 is equal to the inner diameter of the support ring 23, the fixed cylinder 32 is embedded into the support ring 23, the outer diameter of the volume cylinder 31 is equal to the inner diameter of the lower cover 12, the volume cylinder 31 is embedded into the lower cover 12, and a gap is formed between the volume cylinder 31 and the support ring 23, so that not only can liquid reactants be accommodated for heat exchange, but also the pressure on the support ring 23 can be buffered when the volume cylinder 31 is cracked due to overlarge air pressure, and the probability of damage to the heating pipe 2 is reduced. Two liquid flow pipes 39 penetrate through the lower cover 12 and are communicated with the volume cylinder 31, one liquid flow pipe 39 is communicated with the outlet end of the n-hexane washing tank, and the other liquid flow pipe 39 is connected with the water tank. Deionized water containing methanol discharged from the water washing tank is introduced into the liquid cartridge 3 through the liquid flow pipe 39. The air outlet pipe 38 extends into the cavities of the shell 1 and the upper cover 11, the air inlet end of the air outlet pipe 38 is fixedly connected to the top of the fixed cylinder 32, and the air outlet end of the air outlet pipe 38 extends out of the upper cover 11 and is connected with a methanol condenser for guiding and condensing methanol gas, so that secondary use is facilitated. In addition, the air outlet pipe 38 is made of thin-wall PVC materials, a pressure sensor is additionally arranged at the bottom of the heat insulating ring 21, when the air pressure in the liquid cylinder 3 is too high, the air outlet pipe 38 can be firstly squeezed and broken, the air pressure in the shell 1 is instantly increased at the moment, after the pressure sensor detects the pressure change, a signal is transmitted to the industrial personal computer through the heating pipeline 22, the industrial personal computer controls the circulation heating and water washing equipment for stopping the esterification reaction kettle, and further development of accidents can be effectively avoided.

With reference to fig. 2, 4 and 5, an inlet channel 33 is formed on an outer side of the fixed cylinder 32, a fluid channel 34 is formed on an outer side of the volume cylinder 31, the fluid channel 34 is communicated with the inlet channel 33, the inlet channel 33 is communicated with an inner cavity of the housing 1, and the fluid channel 34 is communicated with the outlet pipe 14, so that the fluid in the inlet pipe 13 can flow through the fixed cylinder 32 and the volume cylinder 31 to flow to the outlet pipe 14 through the inlet channel 33 and the fluid channel 34. The inner sides of the liquid inlet channel 33 and the liquid flow channel 34 are fixedly connected with a zigzag partition plate 35, the part of the partition plate 35 with large axial distance with the lower cover 12 is fixedly connected in the liquid flow channel 34, and the axial distance between the partition plate 35 and the lower cover 12 is smaller than the inner diameter of the volume cylinder 31. An annular gasket 36 is abutted to the bottom of the volume cylinder 31, the radius of the inner ring of the gasket 36 is larger than the maximum distance between the partition plate 35 and the axis of the lower cover 12, so that the cavity of the gasket 36, which is positioned right below the liquid flow channel 34, is a flow hole 37, and the flow hole 37 is communicated with the liquid outlet pipe 14. The fixed cylinder 32 with the liquid inlet channel 33 is arranged and embedded into the support ring 23, so that the liquid cylinder 3 can be fixed by matching with the lower cover 12, the infiltration speed of the liquid reactant can be reduced, the heating pipe 2 can fully heat the liquid reactant, the contact time of the liquid reactant and the liquid cylinder 3 can be prolonged, and the heat exchange is more thorough.

With reference to fig. 2, 4 and 5, when a high molecular polymer is produced, the heating pipe 2 is started to heat the interior of the shell 1, the heating temperature is 80-110 ℃, then the liquid reactant flowing in through the liquid inlet pipe 13 enters the esterification reaction kettle added with the catalyst to perform esterification reaction, and then the liquid is continuously transported into the shell 1 through the pump body to maintain the reaction temperature in the reaction kettle to be constant. And (3) as a byproduct methanol is generated by the esterification reaction, the methanol and the normal hexane are azeotroped into gas by adding the normal hexane so as to be separated from the finished product liquid, so that the finished product has certain purity. And the methanol and the normal hexane are separated by a water washing method after condensation and liquefaction, namely the methanol is dissolved in water, and the normal hexane is not dissolved in water, so that the methanol can be stripped from the normal hexane by deionized water. Deionized water containing methanol is then introduced into liquid cartridge 3 through liquid flow tube 39.

Referring to fig. 4 and 5, the volumes of the deionized water containing methanol in the fixed cylinder 32 and the volume cylinder 31 are smaller than the total volume of the liquid cylinder 3, so as to provide a space for methanol gas to be separated out and prevent the liquid cylinder 3 from being exploded due to excessive expansion caused by heating. When deionized water containing methanol enters the liquid cylinder 3, liquid heated by the heating pipe 2 flows in the shell 1, at the moment, the liquid in the shell 1 and the liquid in the liquid cylinder 3 carry out heat exchange, the temperature of a liquid reactant is not lower than 90 ℃, the temperature in the liquid cylinder 3 can be between 70 and 90 ℃, the boiling point temperature of the methanol is 64.7 ℃, and the boiling point temperature of the water is 100 ℃, so that the methanol can be separated out of the deionized water into gas by utilizing the heat exchange with the liquid reactant, and then the gas flows out of the shell 1 through the gas outlet pipe 38 to be condensed, thereby realizing the purification of the methanol. And the temperature of the liquid reactant after heat exchange is reduced without influencing the normal reaction of the reactant, and the gas outlet pipe 38 extends into the shell 1 and the upper cover 11, so that the temperature of the liquid in the shell 1 can be used for preserving or heating the gas in the gas outlet pipe 38, and the problem that the methanol gas is liquefied in the pipeline due to the fact that the temperature is dissipated too fast in the gas outlet pipe 38 or in the pipeline outside the shell 1 is solved.

In conclusion, the liquid cylinder 3 is arranged in the heater, the methanol is purified and placed in the heater, the heat of the heated liquid reactant is utilized for vaporization and separation, and compared with the method of additionally arranging the distillation tower for separating the methanol, the method not only saves the purchase cost of equipment, but also reduces the use amount of electric energy. In addition, on the premise of not changing the heating power of the heating pipe 2, although the temperature of the liquid reactant is reduced by adding the deionized water containing methanol, because the reactant can be completely reacted in the initial stage, the heating pipe 2 can overheat the reactant (if the reactant is overheated, the heat can not be transferred to the middle part of the liquid or the reaction temperature is insufficient due to heat dissipation caused by heat exchange with the outside), the deionized water containing methanol can be added to recover the residual heat of the reaction, so that the heat efficiency is effectively improved, and under the condition that the heating power of the heating pipe 2 is not changed, the heat efficiency of the heating pipe 2 can be improved to about 80% by preliminary estimation, and the electric energy utilization rate can reach more than 95%. And set up feed liquor way 33 and flow liquid way 34 on liquid cylinder 3, can increase the area of contact of liquid reactant and liquid cylinder 3, and then increase the area of contact with deionized water, increase heat exchange efficiency, make methanol precipitate more fast. The partition plate 35 can keep the volume cylinder 3 with excellent reserve volume, so that the liquid cylinder 3 can purify more methanol once, the contact area between the liquid cylinder 3 and the liquid reactant can be further increased, and the heat exchange efficiency can be further improved.

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 utility model provides an energy-conserving separator of high molecular polymer intermediate, includes casing (1) and heating pipe (2), and casing (1) is the cylinder tubulose, and heating pipe (2) link firmly at casing (1) middle part, its characterized in that: the device is characterized by also comprising a liquid cylinder (3), wherein the upper part of the shell (1) is fixedly connected with a cylindrical upper cover (11), the lower part of the shell (1) is fixedly connected with a cylindrical lower cover (12), the top of the upper cover (11) is fixedly connected with a liquid inlet pipe (13), the bottom of the lower cover (12) is fixedly connected with a liquid outlet pipe (14), and the liquid inlet pipe (13) and the liquid outlet pipe (14) are both communicated with the inner cavity of the shell (1); the liquid cylinder (3) is embedded in the lower cover (12), the top of the liquid cylinder (3) is fixedly connected with an air outlet pipe (38), and the bottom of the liquid cylinder (3) is fixedly connected with two liquid flow pipes (39); wherein, the liquid inlet pipe (13) and the liquid outlet pipe (14) flow the mixed liquid of methyl acrylate, dimethylethanolamine and catalyst, and the liquid cylinder (3) is stored with deionized water dissolved with methanol; the heating pipes (2) are infrared heaters, a heat insulation ring (21) is fixedly connected in the shell (1), electronic devices are arranged in the heat insulation ring (21), the heating pipes (2) are fixedly connected to the bottom of the heat insulation ring (21) at annular intervals, and the heating pipes (2) are electrically connected with the electronic devices; one side of the heat insulation ring (21) is fixedly connected with a heating pipeline (22), the heating pipeline (22) is electrically connected with the electronic device, and the heating pipeline (22) extends out of the shell (1); the bottom of the heating pipe (2) is fixedly connected with a support ring (23), the outer ring of the support ring (23) is welded on the inner wall of the shell (1), and the liquid cylinder (3) is partially embedded into the support ring (23); the liquid cylinder (3) comprises a fixed cylinder (32) and a volume cylinder (31), the fixed cylinder (32) and the volume cylinder (31) are both columnar hollow shell cylinders, and the fixed cylinder (32) is fixedly connected to the top of the volume cylinder (31) and communicated with the volume cylinder (31); the outer diameter of the fixed cylinder (32) is equal to the inner diameter of the support ring (23), the fixed cylinder (32) is embedded into the support ring (23), the outer diameter of the volume cylinder (31) is the same as the inner diameter of the lower cover (12), the volume cylinder (31) is embedded into the lower cover (12), and liquid in the liquid inlet pipe (13) flows to the liquid outlet pipe (14) through the fixed cylinder (32) and the volume cylinder (31).

2. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 1, wherein: two liquid flowing pipes (39) penetrate through the lower cover (12) and are communicated with the liquid cylinder (3), one liquid flowing pipe (39) is communicated with the outlet end of the n-hexane washing tank, and the other liquid flowing pipe (39) is connected with the water tank.

3. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 2, wherein: the air outlet pipe (38) extends into the cavity of the shell (1) and the upper cover (11), and the air outlet end of the air outlet pipe (38) extends out of the upper cover (11) and is connected with a methanol condenser.

4. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 3, wherein: the outer side of the fixed cylinder (32) is provided with a liquid inlet channel (33), the outer side of the volume cylinder (31) is provided with a liquid flow channel (34), the liquid flow channel (34) is communicated with the liquid inlet channel (33), the liquid inlet channel (33) is communicated with the inner cavity of the shell (1), and the liquid flow channel (34) is communicated with the liquid outlet pipe (14).

5. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 4, wherein: the inner sides of the liquid inlet channel (33) and the liquid flow channel (34) are fixedly connected with zigzag partition plates (35), the part with large axial line distance between the partition plates (35) and the lower cover (12) is fixedly connected in the liquid flow channel (34), and the axial line distance between the partition plates (35) and the lower cover (12) is smaller than the inner diameter of the volume cylinder (31).

6. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 5, wherein: the bottom of the volume cylinder (31) is abutted with an annular gasket (36), the radius of the inner ring of the gasket (36) is larger than the maximum distance between the partition plate (35) and the axis of the lower cover (12), so that a cavity of the gasket (36) right below the liquid flow channel (34) is a flow hole (37), and the flow hole (37) is communicated with the liquid outlet pipe (14).

7. The energy-saving separation device for the high molecular polymer intermediate as claimed in claim 6, wherein: the volumes of the deionized water containing methanol in the fixed cylinder (32) and the volume cylinder (31) are less than the total volume of the liquid cylinder (3), and the air outlet pipe (38) is connected with the fixed cylinder (32).