CN115608298A - Reactor is used in preparation of temperature adjustable ethylene carbonate - Google Patents
Reactor is used in preparation of temperature adjustable ethylene carbonate Download PDFInfo
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- CN115608298A CN115608298A CN202211254228.4A CN202211254228A CN115608298A CN 115608298 A CN115608298 A CN 115608298A CN 202211254228 A CN202211254228 A CN 202211254228A CN 115608298 A CN115608298 A CN 115608298A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
- C07D317/38—Ethylene carbonate
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a temperature-adjustable reactor for preparing ethylene carbonate, which comprises a reaction assembly and a temperature adjusting assembly; for the preparation process of the ethylene carbonate, the high-temperature reaction in the reaction stage and the cooling and cooling reaction in the later stage are fused together, namely, the high-temperature heating reaction is realized through the high-temperature control structure firstly, and then the reaction is carried out through the low-temperature control structure when the temperature needs to be reduced in the later stage or the reaction is carried out at a lower temperature.
Description
Technical Field
The invention relates to a temperature-adjustable reactor for preparing ethylene carbonate, in particular to a technology for realizing accurate and rapid control of the temperature of intermediate reaction.
Background
The ethylene carbonate is used as electrolyte for producing lithium battery and capacitor in electronic industry, as stabilizer for plastic foaming agent and synthetic lubricating oil, excellent solvent and organic synthetic intermediate, excellent solvent for polyacrylonitrile and polyvinyl chloride, as hydroxyethylation agent and chemical material for organic synthesis, water glass slurry and fiber finishing agent.
The synthesis of ethylene carbonate is diversified, and the prior art patent document CN113999198A (application No. CN 202111500880.5) discloses a synthesis method of ethylene carbonate, wherein the core reaction step refers to "step 5", and the reaction solution is heated to 105 ℃ and kept refluxing for 5h to complete condensation reaction, so as to obtain orange solution. And 6, cooling the orange solution to below 50 ℃. And 7, carrying out reduced pressure distillation on the orange solution, collecting excessive hexamethyldisilazane, ethylene glycol and 75-80 ℃/1.03kPa of fraction, wherein the fraction is N-trimethylsilylimidazole, the yield is 92%, and the content is 98% through liquid phase detection. And step 8, stirring and dissolving the triphosgene and the dichloromethane, wherein the mass ratio of the triphosgene to the dichloromethane is 5.94: and 100, stirring to be completely dissolved to obtain a solution II, wherein in the process, N-trimethylsilylimidazole and triphosgene generate trimethylchlorosilane and ethylene carbonate under the action of dichloromethane and at the temperature of 20 ℃. And 9, cooling the solution to below 20 ℃ in an ice bath mode.
Therefore, in the reaction process, the temperature of the reaction needs to be changed repeatedly, namely, a plurality of temperature ranges including 105 ℃, 75-80 ℃ and below 20 ℃ are wide in span, in practical production, 10L, 20L or 50L of glass containers or plastic containers are generally adopted for carrying out chemical reactions, heating higher than 100 ℃ is generally carried out by electric heating or medium oil heating, cooling is generally required below 30 ℃, cooling is generally carried out by cooling water or other coolants, and therefore the temperature control modes of the two temperature controls are different, although the temperature control of different types of reaction vessels can be realized by transferring materials, the workload is increased undoubtedly, a plurality of reaction containers need to be used, inconvenience is caused, more resources are occupied, and danger is caused to frequent transferring and operating of the glass containers.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for reducing the problem of frequent material transfer in a synthesis reaction, namely, the number of containers occupied by materials is reduced as much as possible, and rapid temperature control change is realized.
The invention provides a temperature-adjustable reactor for preparing ethylene carbonate, which comprises a reaction assembly and a temperature adjusting assembly;
the reaction assembly is provided with a support frame, a clamping piece, a stirring structure and a reaction container, wherein the clamping piece is arranged in the middle of the support frame, and the stirring structure is arranged at the top of the support frame;
the temperature adjusting assembly is provided with a moving vehicle, a rotating part, a high-temperature control structure and a low-temperature control structure, the rotating part is arranged on the moving vehicle, the high-temperature control structure and the low-temperature control structure are arranged on the rotating part, the high-temperature control structure is provided with a first clamping part and a first heating plate, an electric heating wire or a heating conduit is arranged in the first heating plate, and heat conducting oil is arranged in the heating conduit; the low-temperature control structure is provided with a second clamping piece and a second heating plate, a cooling guide pipe is arranged in the second heating plate, and a refrigerant medium is arranged in the cooling guide pipe.
The beneficial effect of above-mentioned scheme does: for the preparation process of the ethylene carbonate, the high-temperature reaction in the reaction stage and the cooling and cooling reaction in the later stage are combined together, namely, the high-temperature heating reaction is realized through the high-temperature control structure firstly, and then the temperature is reduced in the later stage or the reaction is carried out at a lower temperature, the reaction is carried out through the low-temperature control structure, the technical scheme can reduce the repeated transfer of materials and the frequent replacement and use of reaction containers, so that the reaction operation concentrated in a relatively fixed area is realized, the workload is reduced, and the reaction process is very suitable for a chemical laboratory test and a chemical pilot test, namely, the reaction with the reaction volume of below 20L, such as 5L and 500 ML.
One preferable scheme is that the stirring structure comprises an extension plate, a stirring motor and a stirring rod, the stirring motor is arranged on the upper side of the stirring extension plate, the stirring motor is connected with the stirring rod, and the bottom of the stirring rod is detachably arranged in the reaction vessel;
the reaction vessel is provided with a plurality of feed inlets, and sealing plugs are arranged on the feed inlets;
the bottom of the reaction container is provided with a discharge hole, and an outlet valve is arranged on the discharge hole;
the fraction collector is provided with a collecting bottle, and the upper inlet of the collecting bottle is connected with the gas outlet of the reaction vessel through a condensing pipe; the bottom of the collecting bottle is provided with a feed opening, the feed opening is provided with a feed valve, the feed opening is connected with the feed opening of the reaction vessel through a guide pipe, and the feed opening is provided with a feed valve.
The beneficial effect of above-mentioned scheme does: the required reaction materials can be conveniently added into the reaction container through the arrangement of the feed inlet, and the materials of the reaction container are conveniently transferred away through the discharge hole at the bottom when required. According to the characteristics of the reaction, fraction collection is required in the reaction, and the fraction collection can be realized through condensation of a condensation tank in the prior art, and preferably, the reaction container can be provided for negative pressure environment for condensation, and the corresponding required fraction can be collected after condensation.
The fraction to be subjected to the secondary reaction may be reversely transferred to the reaction vessel. The transfer may be manually assisted or may be automated.
Preferably, the first clamping member and the second clamping member have a mounting plate, a driving motor, a driving sector gear, a driven sector gear, a first driving rod, a second driving rod, a first bending rod, a second bending rod, a first stabilizing rod and a second stabilizing rod, the driving motor is arranged at the bottom of the mounting plate and connected with the driving sector gear, the driving sector gear is meshed with the driven sector gear, the driving sector gear is connected with a first circular plate at the inner end of the first driving rod, the first circular plate is rotatably arranged on the mounting plate, the outer end of the first driving rod is hinged at the inner end of the first bending rod, the middle part of the first bending rod is hinged on the first stabilizing rod, and the inner end of the first stabilizing rod is hinged on the mounting plate; the outer end of the first bending rod is provided with the first heating plate;
the inner end of the second driving rod is arranged on a second circular plate, the second circular plate is rotatably arranged on the mounting plate, the outer end of the second driving rod is hinged to the inner end of a second bending rod, the middle part of the second bending rod is hinged to the second stabilizing rod, and the inner end of the second stabilizing rod is hinged to the mounting plate; the outer end of the second bending rod is provided with the second heating plate, and the first heating plate and the second heating plate form the first heating plate; the first clamping piece and the second clamping piece are identical in structure.
The invention provides a working method of a temperature-adjustable reactor for preparing ethylene carbonate, which comprises the following steps:
s1, filtering reaction liquid of ethylene glycol and N' N-carbonyl diimidazole to obtain a first filtrate, adding imidazole powder, filtering again to obtain a second filtrate, adding hexamethyldisilazane into the second filtrate, stirring, adding a catalyst, and heating to obtain reaction liquid;
s2: adding the reaction solution into a reaction container, then keeping the temperature at 105 ℃ and keeping refluxing for 5h to obtain an orange reaction solution, and heating the orange reaction solution through a high-temperature control structure in the heating process to keep the temperature in the reaction container at 105 ℃;
s3: after the reaction is finished, switching the high-temperature control structure and the low-temperature control structure, namely, turning the high-temperature control structure and the low-temperature control structure through the rotation of the rotating piece so as to enable the second heating plate of the low-temperature control structure to be attached to the outer wall of the reaction vessel, and then cooling through the refrigerant medium in the cooling guide pipe; the temperature is kept below 50 ℃;
s4: rotating the first heating plate or the second heating plate to heat, distilling out fraction N-trimethylsilylimidazole, and opening the bottom of the reaction container to discharge residual reaction liquid in the reaction container;
s5: adding fraction N-trimethylsilylimidazole into a reaction container in a reverse direction, adding triphosgene and dichloromethane into the reaction container, stirring until the triphosgene and the dichloromethane are dissolved to obtain a solution II, and forming ethylene carbonate at the temperature of below 20 ℃; namely, the temperature of the reaction vessel is controlled to be kept below 20 ℃ through a cooling conduit in the low-temperature control structure.
The invention provides a working method of a temperature-adjustable reactor for preparing ethylene carbonate, which comprises the following steps: the stirring rod is driven by the stirring motor to stir in the reaction vessel, and the liquid in the reaction vessel is selectively discharged from the discharge port under the control of an outlet valve at the bottom of the reaction vessel;
the reaction liquid in the reaction vessel collects the distillate into a collecting bottle in a distillation mode, and the distillate in the collecting bottle is reversely transferred into the reaction vessel through a cylinder feed opening.
The working method of the temperature-adjustable reactor for preparing the ethylene carbonate provided by the invention comprises the following steps:
the driving motor provides power to drive the fan-shaped teeth to rotate, and when the fan-shaped teeth are driven to rotate, the first driving rod is driven to drive the first bending rod to move, so that the first heating plate forms clamping action or unfolding action, and the first heating plate is close to the reaction container to form temperature control when the clamping action is implemented; meanwhile, the driving fan-shaped teeth drive the driven fan-shaped teeth to move, and the driven fan-shaped teeth drive the second driving rod and the second bending rod to move, so that the second heating plate is close to or far away from the reaction container, and the temperature of the reaction container is controlled;
and the high-temperature control structure and the low-temperature control structure selectively perform temperature control on the reaction vessel through the rotating action of the rotating member.
Drawings
FIG. 1 is a schematic structural diagram of a temperature-adjustable reactor for preparing ethylene carbonate according to the present invention in plan view;
FIG. 2 is a schematic diagram of a temperature-tunable ethylene carbonate production reactor according to the present invention;
FIG. 3 is a schematic diagram of a reactor for preparing ethylene carbonate with adjustable temperature according to the present invention;
FIG. 4 is a schematic view of a partial structure of a temperature-adjustable reactor for preparing ethylene carbonate according to the present invention;
FIG. 5 is a schematic structural diagram of a temperature-adjustable reactor temperature adjustment assembly for ethylene carbonate production according to the present invention;
FIG. 6 is a schematic diagram of a portion of a temperature-adjustable reactor for preparing ethylene carbonate according to the present invention.
Detailed Description
The first embodiment:
as shown in fig. 1 to 3, the present invention provides a temperature-adjustable reactor for preparing ethylene carbonate, which comprises a reaction assembly 10 and a temperature adjustment assembly 60;
the reaction assembly 10 is provided with a support frame 20, a clamping piece 30, a stirring structure 40 and a reaction container 50, wherein the clamping piece 30 is arranged in the middle of the support frame 20, and the stirring structure 40 is arranged at the top of the support frame 20;
the temperature adjusting assembly 60 comprises a moving vehicle 61, a rotating part 70, a high temperature control structure 80 and a low temperature control structure 90, wherein the rotating part 70 is arranged on the moving vehicle 61, the high temperature control structure 80 and the low temperature control structure 90 are arranged on the rotating part 70, the high temperature control structure 80 comprises a first clamping part 100 and a first heating plate 101, an electric heating wire or a heating conduit is arranged in the first heating plate 101, and heat conducting oil is arranged in the heating conduit; low temperature control structure 90 has second clamping piece 110 and second heating plate 111, have the cooling pipe in the second heating plate 111, have refrigerant medium in the cooling pipe.
The invention provides a working method of a temperature-adjustable reactor for preparing ethylene carbonate, which comprises the following steps:
s1, filtering reaction liquid of ethylene glycol and N' N-carbonyl diimidazole to obtain a first filtrate, adding imidazole powder, filtering again to obtain a second filtrate, adding hexamethyldisilazane into the second filtrate, stirring, adding a catalyst, and heating to obtain reaction liquid; this step is obtained in the manner of the prior art;
s2: adding the reaction solution into a reaction container 50, then keeping the temperature at 105 ℃ and keeping the reflux for 5h to obtain an orange reaction solution, and heating the orange reaction solution through a high-temperature control structure 80 in the heating process to keep the temperature in the reaction container 50 at 105 ℃;
s3: after the reaction is finished, the high temperature control structure 80 and the low temperature control structure 90 are switched, that is, the high temperature control structure 80 and the low temperature control structure 90 are turned by the rotation of the rotating member 70, so that the second heating plate 111 of the low temperature control structure 90 is attached to the outer wall of the reaction vessel 50, and then the cooling is finished by the cooling medium in the cooling conduit; the temperature is kept below 50 ℃; at this stage, the temperature in the low-temperature control structure 90 may be normal temperature or may be reduced by introducing a normal-temperature liquid medium;
s4: at this time, fraction N-trimethylsilylimidazole is distilled off, the fractions are collected in collection bottles, and if there are a plurality of fractions, they are collected in collection bottles, respectively, and then an opening (discharge port) 52 at the bottom of the reaction vessel 50 is opened to allow the residual reaction liquid inside the reaction vessel to be discharged;
s5: adding fraction N-trimethylsilylimidazole into a reaction container reversely, adding triphosgene and dichloromethane into the reaction container, stirring until the triphosgene and the dichloromethane are dissolved to obtain a solution II, and forming ethylene carbonate at the temperature of below 20 ℃; namely, the temperature of the reaction vessel is controlled to be kept below 20 ℃ through a cooling conduit in the low-temperature control structure.
The second embodiment:
as shown in fig. 3 and 4, the stirring structure 40 includes an extension plate 41, a stirring motor 42 and a stirring rod 43, the stirring motor 42 is disposed on the upper side of the extension plate 41, the stirring motor 42 is connected to the stirring rod 43, and the bottom of the stirring rod 43 is detachably disposed in the reaction vessel 50;
the reaction vessel 50 is provided with a plurality of feed inlets 51, and a sealing plug is arranged on each feed inlet 51;
the bottom of the reaction vessel 50 is provided with a discharge port 52, and an outlet valve is arranged on the discharge port 52;
the distillation device also comprises a fraction collector 120, wherein the fraction collector 120 is provided with a collecting bottle 121, and an upper inlet 122 of the collecting bottle 121 is connected with the gas outlet 53 of the reaction vessel 50 through a condensing pipe 125; the bottom of the collecting bottle 121 is provided with a feed opening 123, the feed opening 123 is provided with a feed valve, the feed opening 123 is connected with the feed opening 51 of the reaction vessel 50 through a guide pipe 124, and the feed opening 123 is provided with a feed valve.
As shown in fig. 6, in a preferred embodiment, the height of the collecting bottle 121 is higher than the feed inlet 51, so that the materials in the collecting bottle 121 can be more conveniently discharged into the reaction vessel through the pipeline for subsequent reaction in a cooling environment, that is, the process is performed: adding fraction N-trimethylsilylimidazole into a reaction container reversely, adding triphosgene and dichloromethane into the reaction container, stirring until the triphosgene and the dichloromethane are dissolved to obtain a solution II, and forming ethylene carbonate at the temperature of below 20 ℃; namely, the temperature of the reaction vessel is controlled by a cooling conduit in the low-temperature control structure so as to be kept below 20 ℃,
the invention provides a working method of a temperature-adjustable reactor for preparing ethylene carbonate, which comprises the following steps: the stirring rod 43 is driven by the stirring motor 42 to stir in the reaction vessel 50, and the outlet valve at the bottom of the reaction vessel 50 is controlled to selectively discharge the liquid in the reaction vessel 50 through the discharge port 52;
the reaction liquid in the reaction vessel 50 is distilled to collect the fraction in the collection bottle 121, and the fraction in the collection bottle 121 is reversely transferred to the reaction vessel 50 through the feed opening 123.
The third embodiment:
as shown in fig. 5, the first clamp 100 and the second clamp 110 have a mounting plate 151, a driving motor 152, a driving sector gear 153, a driven sector gear 154, a first driving lever 155, a second driving lever 156, a first bent lever 157, a second bent lever 158, a first stabilizer bar 159, and a second stabilizer bar 161, the driving motor 152 is disposed at the bottom of the mounting plate 151, the driving motor 152 is connected to the driving sector gear 153, the driving sector gear 153 is engaged with the driven sector gear 154, the driving sector gear 153 is connected to a first circular plate 162 at the inner end of the first driving lever 155, the first circular plate 162 is rotatably disposed on the mounting plate 151, the driving motor 152 is connected to a first circular plate 162, the outer end of the first driving lever 155 is hinged to the inner end of the first bent lever 157, the middle portion of the first bent lever 157 is hinged to the first stabilizer bar 159, and the inner end of the first stabilizer bar 159 is hinged to the mounting plate 151; the outer end of the first bending rod 157 is provided with the first heating plate 101;
the inner end of the second driving lever 156 is on a second circular plate 163, the second circular plate 163 is rotatably disposed on the mounting plate 151, the outer end of the second driving lever 156 is hinged at the inner end of a second bent lever 158, the middle part of the second bent lever 158 is hinged at the second stabilizer bar 161, and the inner end of the second stabilizer bar 161 is hinged at the mounting plate 151; the outer end of the second bending rod 158 is provided with the second heating plate 111, and the first heating plate 101 and the second heating plate 111 form the heating unit for heating or cooling the reaction container; the first clamping member 100 and the second clamping member 110 have the same structure.
The working method of the temperature-adjustable reactor for preparing the ethylene carbonate provided by the invention comprises the following steps:
the driving motor 152 provides power to rotate the first circular plate 162 and the driving sector gear 153, and when the driving sector gear 153 rotates, the driving shaft 155 drives the first bending rod 157 to move, so that the first heating plate 101 forms a clamping action or an unfolding action, and when the clamping action is performed, the first heating plate 101 is close to the reaction vessel 50 to form temperature control; meanwhile, the driving sector-shaped teeth 153 drive the driven sector-shaped teeth 154 to move, and the driven sector-shaped teeth 154 enable the second driving rod 156 and the second bending rod 158 to move, so that the second heating plate 111 is close to or far away from the reaction vessel 50, thereby performing temperature control on the reaction vessel 50;
and the high temperature control structure 80 and the low temperature control structure 90 are selectively temperature-controlled with respect to the reaction vessel 50 by the rotating action of the rotary 70.
It should be noted that the synthesis and production method of ethylene carbonate of the present invention adopts the technology mentioned in patent document CN113999198A (application No. CN 202111500880.5), and the reaction steps and procedures not described in detail in the present invention can adopt the technical content in the document, and can also adopt other technologies similar to the present step in the prior art in an auxiliary way.
The clamping member may be a mechanical gripper in the prior art, as long as the clamping action can be formed, for example, a hydraulic gripper of a handling robot for gripping heavy objects in CN202111560974.1, or a mechanical gripper structure in CN202121220627.x may be adopted.
Preferably, the first bending rod 157 and the second bending rod 158 have mounting screw holes thereon, and the first heating plate and the second heating plate also have a plurality of sets of protruding pieces arranged in the height direction, and the protruding pieces have mounting screw holes thereon, and then the heights of the first heating plate and the second heating plate can be adjusted, that is, the first heating plate and the second heating plate are fastened with fasteners of different heights with the first heating plate through the protruding pieces, so that the heating plate (also called as a cooling plate when cooling) can be heated or cooled to different heights, and thus, the change of different heights is formed, that is, the contact height of the heating plate to the reaction vessel is changed, and thus, the temperature control of different temperatures or different levels is convenient to use.
The heating plate also comprises an external device, namely, when the liquid medium is supplied to the pipeline in the heating plate, the low-temperature liquid medium is needed, and in this time, the liquid can be circularly supplied to the pipeline through the refrigerant.
In addition, rotating structure can be installed to the both sides of rotating member, and rotating structure and high temperature control structure or low temperature control structural connection just so can be so that the temperature control structure realizes the upset, and rotating structure is the motor for example, namely makes the whole especially hot plate upset of temperature control structure and realize handstanding, namely makes originally be in the hot plate that upwards places can handstand the motion.
For some cases, an opening is not formed in the bottom of the reaction container, when residual materials in the reaction container need to be transferred, the stirring structure is firstly moved away from the reactor, then the reaction container is clamped through the clamping structures of the high-temperature control structure and the low-temperature control structure, namely, the clamping and fixing effects are achieved, then the clamping piece on the supporting frame is loosened, then the reaction container is moved to the corresponding position through the rotation effect, namely, the rotation of the rotating piece, and then the reaction container is turned over, so that the opening in the top of the reaction container faces downwards, the materials are poured into the recovery container, and then the reaction container is moved to the original position to perform subsequent processes. Such a process is very practical for reaction vessels without a bottom opening, especially for glass reaction vessels. In addition, the first heating plate and the second heating plate can be used for temperature control and clamping and overturning movement, and the two purposes are achieved.
The inner walls of the interlayers of the first heating plate and the second heating plate of the high-temperature control structure and the low-temperature control structure are provided with pipelines, circulating media are introduced into the pipelines, liquid media are introduced into the pipelines through external equipment such as heating equipment or refrigeration equipment, meanwhile, two groups of independent pipelines are arranged in the high-temperature control structure, the main pipeline and the auxiliary pipeline occupy a main part, the auxiliary pipeline occupies a small amount of part, the main pipeline is used for heating and introducing heat media, the auxiliary pipeline can be selectively spliced or connected with a cooling pipeline in the low-temperature control structure to introduce the low-temperature media into the high-temperature control structure, because under some conditions, the temperature in a reaction container is obviously higher than a set temperature, for example, when the temperature exceeds 10 ℃, the cold media can be introduced due to insensitivity of temperature control, the overhigh problem of timely slight adjustment can not be solved, and the temperature of the reaction container can be reduced through the temperature reduction of the auxiliary pipeline, so as to maintain a reasonable temperature range.
In further preferred embodiment, the pipeline arrangement of the inlayer of the first hot plate of high temperature control structure and second hot plate is the multiunit, and the pipeline of multiunit is independent setting, and the height of different groups is located different height position, then keep apart through the removable panel between two sets of adjacent pipelines, be provided with a plurality of removable panels on the direction of height of first hot plate and second hot plate, removable panel is parallel with the bottom plate, can dismantle the side of the hot plate in board and the drawing perpendicular, then can play the isolation effect through removable panel when two hot plates are close to. To different container height or size, select different capacity, that is to say can dismantle or install the board of dismantling, just so can obtain the structure of not using capacity or degree of depth, then be used for reaction vessel's heating control, only need in this time to the pipeline of reaction vessel's parcel heat can, and then different heating are organized to the pipeline of the below of the board of dismantling of reaction vessel's bottom, can the energy saving like this.
First hot plate 101 and second hot plate 111 have semicircle curved surface and bottom plate in the drawing, and can dismantle the board and then carry out detachably and connect on the not co-altitude position of semicircle curved surface, and can dismantle the board and be parallel with the bottom plate, just so can make the not pipe group of co-altitude keep apart and arrange, the equal independent control of heating medium of each pipe group, mutual noninterference.
Claims (6)
1. A reactor for preparing ethylene carbonate with adjustable temperature is characterized by comprising:
the reaction assembly is provided with a support frame, a clamping piece, a stirring structure and a reaction container, wherein the clamping piece is arranged in the middle of the support frame, and the stirring structure is arranged at the top of the support frame;
the temperature adjusting assembly is provided with a moving vehicle, a rotating part, a high-temperature control structure and a low-temperature control structure, the rotating part is arranged on the moving vehicle, the high-temperature control structure and the low-temperature control structure are arranged on the rotating part, the high-temperature control structure is provided with a first clamping part and a first heating plate, an electric heating wire or a heating conduit is arranged in the first heating plate, and heat conducting oil is arranged in the heating conduit; the low-temperature control structure is provided with a second clamping piece and a second heating plate, a cooling guide pipe is arranged in the second heating plate, and a refrigerant medium is arranged in the cooling guide pipe.
2. The temperature-adjustable reactor for preparing ethylene carbonate according to claim 1, wherein the stirring structure comprises an extension plate, a stirring motor and a stirring rod, the stirring motor is arranged on the upper side of the extension plate, the stirring motor is connected with the stirring rod, and the bottom of the stirring rod is detachably arranged in the reaction vessel;
the reaction vessel is provided with a plurality of feed inlets, and sealing plugs are arranged on the feed inlets;
the bottom of the reaction container is provided with a discharge hole, and an outlet valve is arranged on the discharge hole;
the fraction collector is provided with a collecting bottle, and the upper inlet of the collecting bottle is connected with the gas outlet of the reaction vessel through a condensing pipe; the bottom of the collecting bottle is provided with a feed opening, the feed opening is provided with a feed valve, the feed opening is connected with the feed opening of the reaction vessel through a guide pipe, and the feed opening is provided with a feed valve.
3. The reactor for preparing ethylene carbonate with adjustable temperature according to claim 1, wherein the first clamping member and the second clamping member have a mounting plate, a driving motor, a driving sector gear, a driven sector gear, a first driving rod, a second driving rod, a first bending rod, a second bending rod, a first stabilizing rod and a second stabilizing rod, the driving motor is arranged at the bottom of the mounting plate and is connected with the driving sector gear, the driving sector gear is meshed with the driven sector gear, the driving sector gear is connected to a first circular plate at the inner end of the first driving rod, the first circular plate is rotatably arranged on the mounting plate, the outer end of the first driving rod is hinged at the inner end of the first bending rod, the middle part of the first bending rod is hinged at the first stabilizing rod, and the inner end of the first bending rod is hinged at the mounting plate; the outer end of the first bending rod is provided with the first heating plate;
the inner end of the second driving rod is arranged on a second circular plate, the second circular plate is rotatably arranged on the mounting plate, the outer end of the second driving rod is hinged to the inner end of a second bending rod, the middle part of the second bending rod is hinged to the second stabilizing rod, and the inner end of the second stabilizing rod is hinged to the mounting plate; the outer end of the second bending rod is provided with the second heating plate, and the first heating plate and the second heating plate form the first heating plate; the first clamping piece and the second clamping piece are identical in structure.
4. The reactor for preparing ethylene carbonate with adjustable temperature according to claim 1, which is characterized by comprising the following steps:
s1, filtering reaction liquid of ethylene glycol and N' N-carbonyl diimidazole to obtain a first filtrate, adding imidazole powder, filtering again to obtain a second filtrate, adding hexamethyldisilazane into the second filtrate, stirring, adding a catalyst, and heating to obtain reaction liquid;
s2: adding the reaction solution into a reaction container, then keeping the temperature at 105 ℃ and keeping the reflux for 5h to obtain an orange reaction solution, and heating the orange reaction solution through a high-temperature control structure in the heating process to keep the temperature in the reaction container at 105 ℃;
s3: after the reaction is finished, switching the high-temperature control structure and the low-temperature control structure, namely, turning the high-temperature control structure and the low-temperature control structure through the rotation action of the rotating piece so that the second heating plate of the low-temperature control structure is attached to the outer wall of the reaction container, and then cooling is finished through the cooling medium in the cooling guide pipe; the temperature is kept below 50 ℃;
s4: rotating the first heating plate or the second heating plate to heat, distilling out fraction N-trimethylsilylimidazole, and opening the bottom of the reaction container to discharge residual reaction liquid in the reaction container;
s5: adding fraction N-trimethylsilylimidazole into a reaction container in a reverse direction, adding triphosgene and dichloromethane into the reaction container, stirring until the triphosgene and the dichloromethane are dissolved to obtain a solution II, and forming ethylene carbonate at the temperature of below 20 ℃; namely, the temperature of the reaction vessel is controlled to be kept below 20 ℃ through a cooling conduit in the low-temperature control structure.
5. The temperature-adjustable reactor for preparing ethylene carbonate according to claim 4, wherein the stirring rod is driven by the stirring motor to stir in the reaction vessel, and the outlet valve at the bottom of the reaction vessel is controlled to selectively discharge the liquid in the reaction vessel;
the reaction liquid in the reaction container collects the fraction into a collecting bottle in a distillation mode, and the fraction in the collecting bottle is reversely transferred into the reaction container through a cylinder feed opening.
6. The reactor for preparing ethylene carbonate with adjustable temperature as claimed in claim 4, wherein the driving motor provides power to drive the sector gear to rotate, and when the sector gear is driven to rotate, the first driving rod is driven to drive the first bending rod to move, so that the first heating plate forms a clamping action or an unfolding action, and when the clamping action is implemented, the first heating plate is close to the reaction container to form temperature control; meanwhile, the driving fan-shaped teeth drive the driven fan-shaped teeth to move, and the driven fan-shaped teeth drive the second driving rod and the second bending rod to move, so that the second heating plate is close to or far away from the reaction container, and the temperature of the reaction container is controlled;
and the high-temperature control structure and the low-temperature control structure selectively perform temperature control on the reaction vessel through the rotating action of the rotating member.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211254228.4A CN115608298A (en) | 2022-10-13 | 2022-10-13 | Reactor is used in preparation of temperature adjustable ethylene carbonate |
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| CN202211254228.4A CN115608298A (en) | 2022-10-13 | 2022-10-13 | Reactor is used in preparation of temperature adjustable ethylene carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116422244A (en) * | 2023-06-13 | 2023-07-14 | 山东瑞诚化工设备有限公司 | High-efficient safe type continuous hydrogenation equipment |
| CN117531469A (en) * | 2023-10-16 | 2024-02-09 | 南雄市沃太化工有限公司 | Waterproof polyurethane acrylate composite material and preparation device thereof |
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2022
- 2022-10-13 CN CN202211254228.4A patent/CN115608298A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116422244A (en) * | 2023-06-13 | 2023-07-14 | 山东瑞诚化工设备有限公司 | High-efficient safe type continuous hydrogenation equipment |
| CN116422244B (en) * | 2023-06-13 | 2023-10-10 | 山东瑞诚化工设备有限公司 | High-efficient safe type continuous hydrogenation equipment |
| CN117531469A (en) * | 2023-10-16 | 2024-02-09 | 南雄市沃太化工有限公司 | Waterproof polyurethane acrylate composite material and preparation device thereof |
| CN117531469B (en) * | 2023-10-16 | 2024-06-11 | 南雄市沃太化工有限公司 | Waterproof polyurethane acrylate composite material and preparation device thereof |
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