SUMMERY OF THE UTILITY MODEL
In view of the above-mentioned shortcomings of the prior art, the present invention provides a continuous polymer tackifying reactor, which can continuously remove small molecules or volatile components from a polymer, and at the same time, can ensure that the polymer keeps good fluidity in the reactor, so as to solve the problems of the prior art, such as difficulty in flowing the polymer in a horizontal reactor, low productivity, etc.
To achieve the above and other related objects, the basic solution of the present invention is: a polymer continuous tackifying reactor comprises a vertical shell, wherein a high-efficiency heat exchanger is arranged at the top of the shell, the high-efficiency heat exchanger is a tube type heat exchanger, the tube type heat exchanger comprises a vertical barrel, a material inlet is formed in the top of the barrel, a plurality of vertically arranged heat exchange tubes communicated with the material inlet are arranged in the barrel, and the lower ends of the heat exchange tubes are communicated with the inside of the shell; the shell is internally provided with a fluid distributor and a plurality of layers of liquid holding heating plates which are arranged in a staggered manner from top to bottom in sequence, the liquid holding heating plates are heat exchange plates which are communicated with a heating medium and are arranged obliquely, the upper part of the side wall of the shell is provided with a gas phase outlet, and the bottom of the shell is provided with a material outlet; and the upper part and the lower part of the side wall of the shell are respectively provided with a heating medium inlet and outlet communicated with the inside of the cylinder, and the upper part and the lower part of the side wall of the shell are respectively provided with a heating medium inlet and outlet communicated with the inside of the heat exchange plate.
The working principle of the basic scheme is as follows:
the high-efficiency heat exchanger is arranged above the tackifying reactor, high-viscosity polymer fluid enters the heat exchange pipe from the material inlet, is heated by the high-efficiency heat exchanger and then enters the fluid distributor of the tackifying reactor, and then falls onto the liquid-holding heat exchange plate and flows along the inclined direction of the liquid-holding heat exchange plate under the action of gravity, so that the polymer is continuously heated on the liquid-holding heat exchange plate to supplement the heat carried by the gasification of small molecular substances after entering the tackifying reactor, and the high-molecular polymer is ensured to keep good fluidity in the reactor; meanwhile, polymer fluid is distributed and heated on the liquid-holding heat exchange plate in a film mode, small molecules easily penetrate through a gas-liquid two-phase interface to enter a gas phase and flow out of the tackifying reactor from a gas phase outlet, and therefore the small molecules are escaped. After the micromolecules in the polymer fluid flowing through the liquid-holding heat exchange plate are removed, the viscosity is further increased, and the aim of tackifying or removing micromolecule monomers is further fulfilled. Finally, after passing through the liquid-holding heating plate, the polymer fluid further flows into the material outlet of the tackifying reactor by means of gravity flow.
Further, the gas phase outlet is connected with a condenser, and the condenser is connected with a vacuum pump for controlling the operation pressure of the tackifying reactor. The gas phase outlet is a channel for small molecules to flow out of the tackifying reactor and is an important channel for adjusting the internal pressure of the tackifying reactor, the gas phase outlet is connected with a condenser, the condenser is connected with a vacuum pump, and the condenser is used for condensing and collecting the small molecule vacuum pump and is used for controlling the operating pressure of the whole tackifying reactor.
Further, the high-efficiency heat exchanger and the tackifying reactor are connected through a flange or welded together.
Further, the bottom of the fluid distributor is of a porous structure or a slit structure, and the material flow is driven by pressure, extruded through the pores or slits and flows downwards in the form of filiform strands or strip-shaped sheets under the action of gravity.
Optionally, the size of the openings of the fluid distributor is 0.5-10mm, and the specific size of the openings is determined according to the viscosity of the fluid.
Optionally, the slit width of the fluid distributor is 0.1-8mm, and the length is 5mm or more, which is smaller than the inner diameter of the shell.
Further, hold liquid hot plate and all fix at shells inner wall, and to the slope of casing middle part, inclination (indicate to hold the contained angle of liquid hot plate and vertical direction) is 0 ~ 75 (not including 0 °). The inclination angle of the liquid-holding heat exchange plate is determined according to the viscosity parameter of the reactant, and the layer number of the liquid-holding heat exchange plate is determined by the residence time required by the reaction.
Furthermore, an inner insert used for forcibly mixing and shearing materials is arranged inside the heat exchange tube, the inner insert is a metal framework which is arranged in a reciprocating and interweaving mode or a metal element which is arranged in a spiral mode, the metal framework or the metal element is tightly contacted with the inner wall of the heat exchange tube, the projection surface of the metal framework or the metal element is the same as the inner diameter of the heat exchange tube, and the metal framework or the metal element is fixed in the heat exchange tube, so that the materials are continuously sheared, mixed and heat transferred in a flowing state.
When passing through the high-efficiency heat exchanger, the high-viscosity polymer fluid is continuously sheared and continuously peeled from the wall of the heat exchange tube under the flow guide effect of the inner plug-in unit, and the polymer fluid is continuously updated on the inner wall of the heat exchange tube, so that the high-efficiency heat transfer of the high-viscosity polymer fluid is realized.
Furthermore, temperature detection elements are arranged on the upper portion and the lower portion of the shell.
Further, the shell is in a heat exchange type or a heat preservation type without a jacket, a full jacket, a partial jacket or a companion pipe.
As mentioned above, the reactor for continuously tackifying polymer of the utility model has the following beneficial effects:
the utility model discloses a polymer continuous tackifying reactor can carry out the continuous tackifying of high viscosity polymer fluid material and micromolecule or volatile component desorption reaction, and this reactor can heat or the concurrent heating to the polymer, makes the polymer keep good mobility in the reactor, is particularly useful for handling the system that contains the little molecular weight ratio great; the reactor is of a vertical structure, most of the material flows in the reactor through gravity flow and flows in the form of falling strips or thin films, so that the gas-liquid mass transfer specific surface area is large, the mass transfer resistance is low, and small molecules can be removed more thoroughly. Therefore, the reactor has simple structure, is easy to amplify, can be easily amplified to a single production line, achieves the output of tens of thousands of tons or even tens of thousands of tons, and breaks the bottleneck of the traditional horizontal squirrel cage or disc reactor.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The present invention can also be implemented or applied through other different specific embodiments, and various details in the present specification can be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention.
It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the invention in a schematic manner, and only the components related to the invention are shown in the drawings instead of the actual implementation of the invention, the shapes, the amounts and the proportions of the components may be changed arbitrarily according to the number, the shapes and the sizes of the components in the actual implementation, and the layout of the components may be more complicated. The structure, ratio, size and the like shown in the drawings attached to the present specification are only used for matching with the content disclosed in the specification, so as to be known and read by people familiar with the technology, and are not used for limiting the limit conditions which can be implemented by the present invention, so that the present invention does not have the substantial significance in the technology, and any structure modification, ratio relationship change or size adjustment should still fall within the scope which can be covered by the technical content disclosed by the present invention without affecting the efficacy which can be produced by the present invention and the purpose which can be achieved by the present invention. Meanwhile, the terms such as "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for convenience of description, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof may be made without substantial technical changes, and the present invention is also regarded as the scope of the present invention.
Description of reference numerals:
the device comprises a shell 101, a fluid distributor 102, a liquid holding heating plate 103, a gas phase outlet 104, a cylinder 201, a heat exchange pipe 202, a material inlet 30, a material outlet 40, a heating medium inlet and outlet 50 and a temperature detection element 60.
The specific implementation process is as follows:
as shown in figure 1, the utility model discloses a polymer is tackifying reactor in succession includes vertical casing 101, and the top of casing 101 is equipped with high-efficient heat exchanger, passes through flange joint between high-efficient heat exchanger and the tackifying reactor, perhaps welds together. The high-efficiency heat exchanger is a tube type heat exchanger, the tube type heat exchanger comprises a vertical tube body 201, a material inlet 30 is formed in the top of the tube body 201, a plurality of heat exchange tubes 202 which are vertically arranged and communicated with the material inlet 30 are arranged in the tube body 201, and the lower ends of the heat exchange tubes 202 are communicated with the inside of a shell 101 of the viscosity increasing reactor; the upper part and the lower part of the side wall of the cylinder 201 are respectively provided with a heating medium inlet and outlet 50 communicated with the inside of the cylinder 201. The shell 101 is internally provided with a fluid distributor 102 and a plurality of layers of liquid holding heating plates 103 which are arranged in a staggered manner from top to bottom in sequence, the liquid holding heating plates 103 are obliquely arranged, the liquid holding heating plates 103 are heat exchange plates which are communicated with heating media, concretely, the liquid holding heating plates 103 are composed of upper and lower double-layer plates, a flow channel for cold and hot media to flow is arranged between the two plates, and the cold and hot media flow between the two plates according to a preset channel, so that the liquid holding heating plates 103 maintain constant temperature and provide heat for materials in contact with the liquid holding heating plates 103; the upper part and the lower part of the side wall of the shell 101 are respectively provided with a heating medium inlet and outlet 50 communicated with the inner pipeline of the liquid-holding heat exchange plate, the position of the heating medium inlet and outlet 50 positioned at the upper part of the side wall of the shell 101 is higher than the liquid-holding heating plate 103 positioned at the top, and the position of the heating medium inlet and outlet 50 positioned at the lower part of the side wall of the shell 101 is lower than the liquid-holding heating plate 103 positioned at the bottom; the upper part of the side wall of the shell 101 is provided with a gas phase outlet 104, the position of the gas phase outlet 104 on the side wall of the shell 101 is lower than the fluid distributor 102 and higher than the uppermost liquid holding heating plate 103, the bottom of the shell 101 is provided with a material outlet 40, and the material outlet 40 can be connected with a conveying pump, a screw extruder or other equipment with a conveying function.
The working mode of the reactor is as follows:
high-viscosity polymer fluid enters the heat exchange tube 202 from the material inlet 30, is heated by the high-efficiency heat exchanger and then enters the fluid distributor 102 of the tackifying reactor, then falls on the liquid-holding heat exchange plate, and flows along the inclined direction of the liquid-holding heat exchange plate under the action of gravity, so that the polymer is continuously heated on the liquid-holding heat exchange plate to supplement heat brought by the gasification of small molecular substances after entering the tackifying reactor, thereby ensuring that the high molecular polymer keeps good fluidity in the reactor, meanwhile, the polymer fluid is distributed and heated on the liquid-holding heat exchange plate in a film form, small molecules easily pass through a gas-liquid two-phase interface to enter a gas phase, and flow out of the tackifying reactor from the gas-phase outlet 104, and thus the escape of the small molecules is completed. After the micromolecules in the polymer fluid flowing through the liquid-holding heat exchange plate are removed, the viscosity is further increased, and the aim of tackifying or removing micromolecule monomers is further fulfilled. Finally, after passing through the liquid-holding heating plate 103, the polymer fluid further flows by gravity flow into the material outlet 40 of the tackifying reactor.
Further, the gas phase outlet 104 is connected to a condenser (not shown) connected to a vacuum pump (not shown) for controlling the operation pressure of the tackifying reactor. The gas phase outlet 104 is a channel for small molecules to flow out of the tackifying reactor and is an important channel for adjusting the internal pressure of the tackifying reactor, the gas phase outlet 104 is connected with a condenser, the condenser is connected with a vacuum pump, the condenser is used for condensing and collecting the small molecules, and the vacuum pump is used for controlling the operating pressure of the whole tackifying reactor.
As shown in fig. 2, the fluid distributor 102 is a barrel structure with a porous structure or slit structure at the bottom and an open top, and the fluid is driven by pressure to be extruded through the pores or slits and flows downward in the form of filiform strands or ribbon-shaped sheets under the action of gravity.
Specifically, the opening size of the fluid distributor 102 is 0.5-10mm, and the specific opening size is determined according to the viscosity of the fluid; the slit width of the fluid distributor 102 is 0.1-8mm, the length is 5mm or more, and is smaller than the inner diameter of the housing 101.
Furthermore, liquid holding heating plate 103 is fixed on the inner wall of casing 101, and inclines to the middle part of casing 101, and inclination angle (indicating the contained angle of liquid holding heating plate 103 and vertical direction) is 0 ~ 75 (excluding 0 °). The inclination angle of the liquid-holding heat exchange plate is determined according to the viscosity parameter of the reactant, and the layer number of the liquid-holding heat exchange plate is determined by the residence time required by the reaction.
Further, the heat exchange tube 202 is internally provided with an insert for forced mixing and shearing of the material, which is a metal skeleton arranged in a reciprocating interlaced manner or a metal element arranged in a spiral shape, and the metal skeleton or the metal element is in close contact with the inner wall of the heat exchange tube 202, has a projection plane identical to the inner diameter of the heat exchange tube 202, and is fixed (e.g., welded) in the heat exchange tube 200, thereby continuously shearing, mixing and transferring heat of the material in a flowing state.
When passing through the high-efficiency heat exchanger, the high-viscosity polymer fluid is continuously sheared and continuously peeled off from the tube wall of the heat exchange tube 202 under the flow guiding action of the inner plug-in unit, and the polymer fluid is continuously updated on the inner wall of the heat exchange tube 202, so that the high-efficiency heat transfer of the high-viscosity polymer fluid is realized.
Further, the upper part and the lower part of the shell 101 are both provided with the temperature detecting elements 60, the temperature detecting elements 60 positioned at the upper part of the shell 101 are lower than the fluid distributor 102 and are as high as the gas phase outlet 104, and the temperature detecting elements 60 positioned at the lower part of the shell 101 are arranged at the material outlet 40.
Further, the housing 101 provides a channel for the flow of reactants and products, and also provides space and support for the liquid-holding heating plate 103, and is also a place for reaction. The shell 101 can be in the form of heat exchange type or heat preservation type without a jacket, a full jacket, a partial jacket or a pipe.
The continuous polymer tackifying reactor of the present invention is applied to practical production. It should be understood that the following examples are only for further illustration of the present invention, and should not be construed as limiting the scope of the present invention, and that the modifications and adjustments made by those skilled in the art according to the above-mentioned contents of the present invention are not essential to the present invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Based on the scheme, the continuous polymer tackifying reactor is designed and manufactured, and the main parameters are as follows: the diameter of the shell 101 is 400mm, and the height is 6000 mm; the bottom of the fluid distributor 102 is of an open pore structure, and the diameter of the open pore is 2 mm; the number of the liquid holding heating plates 103 is 4, and the liquid holding heat exchange plates form an angle of 45 degrees with the horizontal direction; the length of the heat exchange tube 202 is 1500mm, and the diameter of the cylinder 201 is 300 mm. The design temperature is 300 ℃ and the design pressure is-0.1 MPa.
Feeding the pre-condensed polyethylene terephthalate (PET) melt into a tackifying reactor at a flow rate of 15kg/h, controlling the temperature in the reactor at 240 ℃ and the reaction pressure at-0.099 MPa, and staying in the reactor for 30min to obtain the tackified PET melt. The intrinsic viscosity of the polymer before and after the reaction was measured, the intrinsic viscosity of the PET before entering the reactor was 0.4dL/g, and after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.3 dL/g.
Example 2
By using the tackifying reactor described in embodiment 1, a fluid material of polybutylene terephthalate adipate (PBAT) which has been subjected to pre-polycondensation is fed into the tackifying reactor at a flow rate of 10kg/h, the temperature in the reactor is controlled at 245 ℃ and the reaction pressure is-0.099 MPa, a tackifying reaction is carried out, and the fluid material stays in the reactor for 45min, so that a tackified PBAT melt is obtained. The intrinsic viscosity of the polymer before and after the reaction was measured, the intrinsic viscosity of the PBAT before entering the reactor was 0.8dL/g, and after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.5 dL/g.
Example 3
The method comprises the steps of utilizing the tackifying reactor described in embodiment 1, feeding polymerized polylactic acid (PLA) fluid material into the tackifying reactor at a flow rate of 15kg/h, controlling the reaction temperature at 210 ℃ and the reaction pressure at-0.098 MPa, performing tackifying and devolatilization to remove lactide monomers which are not completely reacted, and staying in the reactor for 30min to obtain polylactic acid after tackifying and devolatilization. The intrinsic viscosity of the polymer before and after the reaction was measured, and the intrinsic viscosity of the polylactic acid before entering the reactor was 1.3dL/g, and after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.5 dL/g.
Example 4
By using the tackifying reactor described in embodiment 1, polymerized polybutylene succinate (PBS) fluid material is fed into the tackifying reactor at a flow rate of 15kg/h, the reaction temperature is controlled at 235 ℃, the reaction pressure is-0.099 MPa, and tackifying and devolatilization are performed to remove small molecular substances generated in the polymerization process, including water, butanediol and tetrahydrofuran generated by side reactions. The reaction solution is kept in the reactor for 30min to obtain the tackified and devolatilized PBS. The intrinsic viscosity of the polymer before and after the reaction was measured, and the intrinsic viscosity of PBS before entering the reactor was 0.7dL/g, and after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.3 dL/g.
Example 5
The open pore form of the fluid distributor 102 of the tackifying reactor described in example 1 was modified to a slit structure with the dimensions: the width of the slit is 1mm, and the length of the slit is 5 mm; other configurations and parameters of the device are unchanged.
Feeding a prepolycondensation polybutylene terephthalate adipate (PBAT) melt material into a tackifying reactor at a flow rate of 10kg/h, controlling the temperature in the reactor at 245 ℃ and the reaction pressure at-0.099 MPa, carrying out tackifying reaction, and staying in the reactor for 45min to obtain the tackified PBAT melt. The intrinsic viscosity of the polymer before and after the reaction was measured, the intrinsic viscosity of the PBAT before entering the reactor was 0.8dL/g, and after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.4 dL/g.
Comparative example 1
The method comprises the steps of adopting a traditional horizontal squirrel cage reactor, enabling a pre-condensed polyethylene terephthalate (PET) melt to enter a tackifying reactor at a flow rate of 15kg/h, controlling the temperature in the reactor at 240 ℃ and the reaction pressure at-0.099 MPa, and staying in the reactor for 30min to obtain the tackified PET melt. The intrinsic viscosity of the polymer before and after the reaction was measured and the intrinsic viscosity of the PET before entering the reactor was 0.4dL/g, after passing through the tackifying reactor, the intrinsic viscosity was increased to 1.0 dL/g.
Comparative example 2
The method comprises the steps of adopting a traditional horizontal disc reactor, enabling a pre-condensed polyethylene terephthalate (PET) melt to enter a tackifying reactor at a flow rate of 15kg/h, controlling the temperature in the reactor at 240 ℃ and the reaction pressure at-0.099 MPa, and staying in the reactor for 30min to obtain the tackified PET melt. The intrinsic viscosity of the polymer before and after the reaction was measured and the intrinsic viscosity of the PET before entering the reactor was 0.4dL/g, after passing through the tackifying reactor, the intrinsic viscosity was increased to 0.9 dL/g.
Compared with the traditional horizontal squirrel cage or disc reactor, the tackifying reactor of the utility model can accelerate the speed of removing small molecules and effectively improve the viscosity of the polymer; moreover, the tackifying reactor has simple structure and easy amplification, can easily realize the series connection of a plurality of reactors, amplify the output of a single production line, realize ten-thousand tons or even dozens of thousand tons, and break the bottleneck of the traditional horizontal squirrel cage or disc reactor.
The above embodiments are merely illustrative of the principles and effects of the present invention, and are not to be construed as limiting the invention. It will be apparent to those skilled in the art that modifications and variations can be made to the above-described embodiments without departing from the spirit and scope of the invention, and it is intended that all equivalent modifications and variations be covered by the appended claims without departing from the spirit and scope of the invention.