CN117288003A - Device and method for improving heat exchange efficiency of chlorination reaction heat exchanger in maltol production - Google Patents
Device and method for improving heat exchange efficiency of chlorination reaction heat exchanger in maltol production Download PDFInfo
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- CN117288003A CN117288003A CN202311405456.1A CN202311405456A CN117288003A CN 117288003 A CN117288003 A CN 117288003A CN 202311405456 A CN202311405456 A CN 202311405456A CN 117288003 A CN117288003 A CN 117288003A
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- heat exchanger
- thin film
- control valve
- reaction
- refrigerant
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- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 27
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229940043353 maltol Drugs 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000003507 refrigerant Substances 0.000 claims abstract description 57
- 238000001704 evaporation Methods 0.000 claims abstract description 51
- 239000010409 thin film Substances 0.000 claims abstract description 49
- 230000008020 evaporation Effects 0.000 claims abstract description 44
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 33
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 102
- 238000006243 chemical reaction Methods 0.000 claims description 68
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 20
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 17
- 239000000460 chlorine Substances 0.000 claims description 17
- 229910052801 chlorine Inorganic materials 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 7
- 208000012839 conversion disease Diseases 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 229940093503 ethyl maltol Drugs 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- NGGPLHHTRNJSDT-UHFFFAOYSA-N methylmaltol Natural products COC1=C(C)OC=CC1=O NGGPLHHTRNJSDT-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 235000014101 wine Nutrition 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B39/00—Evaporators; Condensers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
- F25B9/08—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point using ejectors
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F27/00—Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention provides a device and a method for improving heat exchange efficiency of a chlorination reaction heat exchanger in maltol production, and belongs to the technical field of maltol production. According to the invention, a horizontal thin film evaporation heat exchanger is adopted to replace a traditional heat exchanger, refrigerant liquid ammonia or freon is injected and evaporated, and evaporated gas carries tiny refrigerant liquid drops to move upwards in the rising process, and the liquid drops contact the wall surface of a heat exchange tube to form efficient evaporation, so that a large heat exchange coefficient can be achieved, efficient heat transfer is realized, and the reaction conversion rate and the product yield are improved; and the bottom of the heat exchanger has almost no liquid storage, so that a small filling amount can be achieved, and the safety risk is reduced.
Description
Technical Field
The invention belongs to the technical field of maltol production, and particularly relates to a method for improving the heat exchange efficiency of a chlorination reaction heat exchanger and reducing the chlorination reaction risk in maltol production.
Background
The maltol is also called methyl maltol, has special aroma of burnt cream hard candy, is a broad-spectrum aroma synergist, has the functions of enhancing aroma, fixing aroma and sweetening, can be prepared into edible essence, cosmetic essence and the like, and is widely applied to various industries at present, such as industries of food, beverage, wine brewing, cosmetics, pharmacy and the like.
In recent years, the application field of maltol is continuously widened, the dosage requirement is also continuously increased, and various manufacturers are researching how to improve the production efficiency of maltol. The current production process of maltol is divided into a Grignard working section, a chlorination working section, a sublimation working section, a crystallization working section and a drying working section. The chlorination working section is an instant reaction process, ensures the timely transfer of reaction heat, shortens the reaction time, and is a key point for reducing the occurrence of byproducts and improving the product yield.
Patent CN111454238A discloses a production process of a methyl/ethyl maltol chlorination section, by arranging a pipeline reactor with a specific structure, a precooled methanol aqueous solution is pumped in from an inner pipe feed inlet of the pipeline reactor, then chlorine is introduced through a chlorine introducing pipe, and simultaneously an alpha-furanol solution is pumped in the feed inlet of the inner pipe, materials in the inner pipe of the pipeline reactor are in a turbulent flow state through a mixed flow plate and a turbulent flow device, the contact surface between the materials is continuously updated, the gas-liquid mixing is enhanced, the chlorination reaction efficiency is effectively improved, the side reaction of the chlorination reaction is reduced, and the yield of maltol/ethyl maltol is improved.
Patent CN108383816a discloses a method for exchanging heat in the chlorination reaction of maltol, comprising the following steps: (1) Introducing aqueous methanol solution into the chlorination kettle, starting a chlorination circulating pump to enable the aqueous methanol solution to circularly flow in the chlorination kettle and the plate exchanger, changing the refrigerant of the plate exchanger into liquid ammonia, controlling the pressure of a liquid ammonia storage tank to be 1.0-1.5Mp, opening a plate-exchange liquid ammonia inlet valve to introduce the liquid ammonia, and controlling the gas phase pressure of a liquid ammonia outlet of the plate exchanger to be 0.3Mpa; (2) When the temperature of the methanol solution in the chlorination kettle is reduced to-15 ℃, starting to dropwise add furfuryl alcohol and introducing chlorine, and regulating an ammonia adding valve and the ammonia gas phase pressure to control the kettle temperature to be not higher than-8 ℃; (3) When all furfuryl alcohol in the overhead tank is dripped, the reaction in the chlorination kettle is finished, the ammonia adding valve is closed, and the material is discharged from the bottom of the chlorination kettle. The method uses liquid ammonia as a refrigerant directly, so that an intermediate link of freezing the calcium chloride aqueous solution is omitted, heat loss is reduced, and the risk of environment pollution caused by salt water leakage is eliminated.
Certain progress has been made in regulating and controlling the process conditions of the chlorination section to increase the production efficiency. However, in the production, the chlorination reaction needs to be carried out at a low temperature, the reaction temperature is controlled to be less than-8 ℃, the heat exchanger commonly used at present uses a lower-temperature refrigerant to exchange heat and remove the reaction heat, the heat exchange is carried out on the calcium chloride aqueous solution through liquid ammonia, the gasification of the liquid ammonia is utilized to absorb heat, the calcium chloride cold brine is prepared, and then the calcium chloride cold brine is utilized to take away the chlorination reaction heat through a plate heat exchanger or a tube array heat exchanger. The chlorination reaction is a strong exothermic reaction, the reaction heat is relatively large, the heat exchange effect of the traditional heat exchanger is low, the reaction heat cannot be removed in time, the reaction overtemperature phenomenon can occur, the chlorination reaction needs to be stopped at the moment, and the temperature is high, so that the number of side reaction products is large, and the yield of the products is reduced. Secondly, the traditional heat exchanger liquid-phase refrigerant flows and washes, so that the heat exchanger is easy to leak, and the safety risk is high.
Disclosure of Invention
The invention aims to solve the problems of low heat exchange efficiency and high reaction risk of a chlorination reaction heat exchanger in the production of maltol, and provides a method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a device for improving the heat exchange efficiency of a chlorination reaction heat exchanger in the production of maltol comprises a mixing reaction tank, a circulating pump, a horizontal thin film evaporation heat exchanger, a reaction mixer, a refrigerant control valve, a furfuryl alcohol control valve and a chlorine control valve.
The bottom of the mixing reaction tank is connected with the inlet of the circulating pump through a flange, the three-way pipeline is connected with the furfuryl alcohol control valve (furfuryl alcohol comes from a furfuryl alcohol elevated tank) on the pipeline connected with the inlet of the mixing reaction tank and the inlet of the circulating pump, and the outlet of the circulating pump is connected with the reaction mixer in the sealing head of the horizontal thin film evaporator through the flange and the pipeline. The material reacted in the mixing reactor is cooled by the horizontal film evaporator and then connected with the mixing reaction tank by the flange and the pipeline, the reaction material circulates in the mixing reaction tank, and the reacted material is pumped to the next section by the circulating pump. Refrigerant enters the horizontal thin film evaporator through a refrigerant control valve, and the refrigerant control valve is associated with the pressure of the horizontal thin film evaporator and the temperature of the reaction materials. The refrigerant comes from the refrigeration section, passes through the thin film evaporator and returns to the refrigeration section.
Further, the reactants furfuryl alcohol and chlorine in the chlorination reaction process are fed through a reaction mixer.
A method for improving the heat exchange efficiency of a chlorination reaction heat exchanger in the production of maltol is realized by the device.
The method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol comprises the following steps:
firstly, pumping a methanol aqueous solution into a mixing reaction tank, starting stirring, and starting a circulating pump to circulate;
step two, opening a refrigerant control valve, and enabling the refrigerant to enter the horizontal thin film evaporation heat exchanger, evaporate after contacting the wall surface of the horizontal thin film evaporation heat exchanger, and cool;
and thirdly, opening a furfuryl alcohol control valve and a chlorine control valve, and introducing reactant furfuryl alcohol and chlorine into the reaction mixer to complete the reaction in the horizontal thin film evaporation heat exchanger.
Further, in the first step, the mass fraction of the methanol water solution is 40% -70%.
In the second step, the refrigerant is liquid ammonia or freon.
In the second step, the refrigerant enters the horizontal thin film evaporation heat exchanger through injection and is evaporated, the refrigerant is immediately evaporated after contacting the wall surface of the horizontal thin film evaporation heat exchanger, no liquid refrigerant exists, a large heat exchange coefficient can be achieved, and efficient heat transfer is achieved. The refrigerant charge is small, and the refrigerant immediately rises and evaporates after entering the evaporator, so that the bottom almost has no liquid storage, the small charge can be achieved, and the safety risk is reduced.
In the second step, the injection amount of the refrigerant is controlled by a refrigerant control valve according to the pressure in the horizontal thin film evaporation heat exchanger and the material temperature.
Preferably, the pressure in the horizontal thin film evaporation heat exchanger is 0.05-0.15MPa, the temperature is-18 ℃ to-10 ℃, further preferably 0.08-0.11MPa, and the temperature is-15 ℃ to-12 ℃;
still more preferably, the pressure is 0.05-0.1MPa and the temperature is-18 ℃ to-13 ℃.
Further preferably, the pressure in the horizontal thin film evaporation heat exchanger is 0.10MPa and the temperature is-13 ℃.
Further, in the third step, the charging ratio of the furfuryl alcohol and the chlorine is 1:1.05-1.25 (molar ratio).
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the horizontal thin film evaporation heat exchanger to replace the traditional heat exchanger, the refrigerant (liquid ammonia or freon) is injected and evaporated, the evaporated gas entrains tiny refrigerant drops to move upwards in the rising process, and the drops contact the wall surface of the heat exchange tube to form high-efficiency evaporation, thereby achieving a large heat exchange coefficient and realizing high-efficiency heat transfer. The refrigerant charge is small, and the refrigerant immediately rises and evaporates after entering the evaporator, so that the bottom almost has no liquid storage, the small charge can be achieved, and the safety risk is reduced.
2. According to the invention, the mixer is arranged at the inlet of the main pipe of the heat exchanger, the reaction furfuryl alcohol is input from the inlet of the pump, the chlorine is input from the inlet of the heat exchanger, the materials are mixed in the mixer and then enter the heat exchanger for reaction, the reaction heat is removed in time, and the reaction conversion rate and the product yield are improved.
3. The shell side of the horizontal thin film evaporator has no liquid phase flow, and avoids abrasion caused by scouring and vibration of liquid phase refrigerant to the heat exchange tube, so that the service life of the thin film evaporator is longer than that of a conventional heat exchanger.
4. And controlling the temperature and the evaporating pressure of reactants in the horizontal thin film evaporating heat exchanger, and further improving the reaction conversion rate and the product yield.
Drawings
FIG. 1 is a schematic diagram showing the structure of a device for improving the heat exchange efficiency of a chlorination reaction heat exchanger in the production of maltol in example 1 of the present disclosure; in the figure: 1 is a mixing reaction tank, 2 is a circulating pump, 3 is a horizontal thin film evaporation heat exchanger, 4 is a reaction mixer, 5 is a refrigerant control valve, 6 is a furfuryl alcohol control valve, and 7 is a chlorine control valve.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way. The following is merely exemplary of the scope of the invention as claimed and many variations and modifications of the invention will be apparent to those skilled in the art in light of the disclosure, which are intended to be within the scope of the invention as claimed.
The invention is further illustrated by means of the following specific examples. The various chemical reagents used in the examples of the present invention were obtained by conventional commercial means unless otherwise specified.
Example 1
Referring to fig. 1, the device for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the maltol production comprises a mixing reaction tank 1, a circulating pump 2, a horizontal thin film evaporation heat exchanger 3, a reaction mixer 4, a refrigerant control valve 5, a furfuryl alcohol control valve 6 and a chlorine control valve 7. The bottom of the mixing reaction tank 1 is sequentially connected with a circulating pump 2, a reaction mixer 4 and a horizontal thin film evaporation heat exchanger 3 through pipelines;
a furfuryl alcohol control valve 6 is arranged between the pipelines communicated with the mixing reaction tank 1 and the circulating pump 2;
a chlorine control valve 7 is arranged between the pipeline communicated with the circulating pump 2 and the reaction mixer 4;
the bottom of the horizontal thin film evaporation heat exchanger 3 is connected with a refrigerant control valve 5, and the refrigerant enters the horizontal thin film evaporation heat exchanger 3 after passing through the refrigerant control valve 5.
Example 2
The method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol comprises the following steps:
firstly, pumping 60% methanol aqueous solution by mass fraction into a mixing reaction tank 1, starting stirring, and starting a circulating pump 2 to circulate;
step two, opening a refrigerant control valve 5, enabling liquid ammonia of a refrigerant to enter the horizontal thin film evaporation heat exchanger 3, evaporating after contacting the wall surface of the horizontal thin film evaporation heat exchanger 3, and cooling; the injection quantity of the refrigerant is controlled by a refrigerant control valve 5 according to the pressure in the horizontal thin film evaporation heat exchanger 3 and the material temperature, wherein the pressure is 0.1MPa, and the material temperature is-13 ℃;
and thirdly, opening a furfuryl alcohol control valve 6 and a chlorine control valve 7, and introducing reactant furfuryl alcohol and chlorine into the reaction mixer 4, wherein the furfuryl alcohol introducing amount is 100kg/h, and the chlorine introducing amount is 120kg/h, so that the reaction is completed in the horizontal thin film evaporation heat exchanger 3.
After the reaction was completed, the conversion of the chlorination reaction was 84.5%, and the yield of the product was 77.06%.
Example 3
The method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol comprises the following steps:
firstly, pumping 60% methanol aqueous solution by mass fraction into a mixing reaction tank 1, starting stirring, and starting a circulating pump 2 to circulate;
step two, opening a refrigerant control valve 5, enabling liquid ammonia of a refrigerant to enter the horizontal thin film evaporation heat exchanger 3, evaporating after contacting the wall surface of the horizontal thin film evaporation heat exchanger 3, and cooling; the injection quantity of the refrigerant is controlled by a refrigerant control valve 5 according to the pressure in the horizontal thin film evaporation heat exchanger 3 and the material temperature, wherein the pressure is 0.05MPa, and the temperature is-18 ℃;
and thirdly, opening a furfuryl alcohol control valve 6 and a chlorine control valve 7, and introducing reactant furfuryl alcohol and chlorine into the reaction mixer 4, wherein the furfuryl alcohol inlet amount is 120kg/h, and the chlorine inlet amount is 150kg/h, so that the reaction is completed in the horizontal thin film evaporation heat exchanger 3.
After the reaction was completed, the conversion of the chlorination reaction was 80%, and the yield of the product was 72.19%.
Example 4
The method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol comprises the following steps:
firstly, pumping 60% methanol aqueous solution by mass fraction into a mixing reaction tank 1, starting stirring, and starting a circulating pump 2 to circulate;
step two, opening a refrigerant control valve 5, enabling liquid ammonia of a refrigerant to enter the horizontal thin film evaporation heat exchanger 3, evaporating after contacting the wall surface of the horizontal thin film evaporation heat exchanger 3, and cooling; the injection quantity of the refrigerant is controlled by a refrigerant control valve 5 according to the pressure in the horizontal thin film evaporation heat exchanger 3 and the material temperature, wherein the pressure is 0.14MPa, and the temperature is-10 ℃;
and thirdly, opening a furfuryl alcohol control valve 6 and a chlorine control valve 7, and introducing reactant furfuryl alcohol and chlorine into the reaction mixer 4, wherein the furfuryl alcohol inlet amount is 120kg/h, and the chlorine inlet amount is 150kg/h, so that the reaction is completed in the horizontal thin film evaporation heat exchanger 3.
After the reaction was completed, the conversion of the chlorination reaction was found to be 74.3%, and the yield of the product was found to be 66.1%.
Example 5
The method for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol comprises the following steps:
firstly, pumping 60% methanol aqueous solution by mass fraction into a mixing reaction tank 1, starting stirring, and starting a circulating pump 2 to circulate;
step two, opening a refrigerant control valve 5, enabling liquid ammonia of a refrigerant to enter the horizontal thin film evaporation heat exchanger 3, evaporating after contacting the wall surface of the horizontal thin film evaporation heat exchanger 3, and cooling; the injection quantity of the refrigerant is controlled by a refrigerant control valve 5 according to the pressure in the horizontal thin film evaporation heat exchanger 3 and the material temperature, wherein the pressure is 0.3MPa, and the temperature is-18 ℃;
and thirdly, opening a furfuryl alcohol control valve 6 and a chlorine control valve 7, and introducing reactant furfuryl alcohol and chlorine into the reaction mixer 4, wherein the furfuryl alcohol inlet amount is 120kg/h, and the chlorine inlet amount is 150kg/h, so that the reaction is completed in the horizontal thin film evaporation heat exchanger 3.
After the reaction was completed, the conversion of the chlorination reaction was found to be 76%, and the yield of the product was found to be 69.3%.
Comparative example 1
Prepared by the method disclosed in example 2 of CN108383816a, the specific procedure is as follows:
pumping 50% aqueous methanol solution 3500L into a chlorination kettle, opening a circulating pump to enable the aqueous methanol solution to continuously circulate in the chlorination kettle and a plate exchanger, changing a refrigerant into liquid ammonia, controlling the pressure of a liquid ammonia storage tank to be 1.0-1.5Mp, opening an ammonia adding valve to introduce the liquid ammonia, directly vaporizing and absorbing the liquid ammonia in the plate exchanger by utilizing the vaporization and heat absorption principle of the liquid ammonia, directly cooling reaction materials, controlling the gas phase pressure of an ammonia outlet to be 0.3Mpa, regulating the introducing amount of the liquid ammonia through the ammonia adding valve, enabling the temperature of the chlorination kettle to be not higher than-12 ℃, starting to dropwise add furfuryl alcohol after the temperature of the aqueous methanol solution in the chlorination kettle is reduced to-15 ℃, enabling the furfuryl alcohol dropwise adding speed to be 100kg/h, introducing chlorine gas simultaneously, ending the reaction after 5 hours, and discharging the solution from the bottom of the chlorination kettle.
After the reaction was completed, the conversion of the chlorination reaction was found to be 64%, and the yield of the product was found to be 57.72%.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. The device for improving the heat exchange efficiency of the chlorination reaction heat exchanger in the production of maltol is characterized by comprising a mixing reaction tank (1), a circulating pump (2), a horizontal thin film evaporation heat exchanger (3), a reaction mixer (4), a refrigerant control valve (5), a furfuryl alcohol control valve (6) and a chlorine control valve (7);
the bottom of the mixing reaction tank (1) is sequentially connected with a circulating pump (2), a reaction mixer (4) and a horizontal thin film evaporation heat exchanger (3) through pipelines;
a furfuryl alcohol control valve (6) is arranged between the pipeline communicated with the mixing reaction tank (1) and the circulating pump (2);
a chlorine control valve (7) is arranged between the pipeline communicated with the circulating pump (2) and the reaction mixer (4);
the bottom of the horizontal thin film evaporation heat exchanger (3) is connected with a refrigerant control valve (5), and the refrigerant enters the horizontal thin film evaporation heat exchanger (3) after passing through the refrigerant control valve (5).
2. The apparatus according to claim 1, characterized in that the reactants furfuryl alcohol and chlorine during the chlorination reaction are fed through the reaction mixer (4).
3. A method for improving the heat exchange efficiency of a chlorination reaction heat exchanger in the production of maltol, which is realized by the device of claim 1 or 2.
4. A method according to claim 3, comprising the steps of:
firstly, pumping a methanol aqueous solution into a mixing reaction tank (1), starting stirring, and starting a circulating pump (2) to circulate;
step two, opening a refrigerant control valve (5), enabling the refrigerant to enter the horizontal thin film evaporation heat exchanger (3), evaporating after contacting the wall surface of the horizontal thin film evaporation heat exchanger (3), and cooling;
and thirdly, opening a furfuryl alcohol control valve (6) and a chlorine control valve (7), and introducing reactant furfuryl alcohol and chlorine into the reaction mixer (4) to complete the reaction in the horizontal thin film evaporation heat exchanger (3).
5. The method according to claim 4, wherein in the first step, the mass fraction of the aqueous methanol solution is 50 to 70%.
6. The method according to claim 4, wherein in the second step, the refrigerant is liquid ammonia or freon.
7. The method according to claim 4, wherein in the second step, the injection amount of the refrigerant is controlled by a refrigerant control valve (5) according to the pressure in the horizontal thin film evaporation heat exchanger (3) and the material temperature.
8. The method according to claim 4, characterized in that the pressure in the horizontal thin film evaporation heat exchanger (3) is 0.05-0.15MPa and the temperature is-18 ℃ to-10 ℃.
9. A method according to claim 8, characterized in that the pressure in the horizontal thin film evaporation heat exchanger (3) is 0.1MPa and the temperature is-13 ℃.
10. The method according to claim 4, wherein in the third step, the furfuryl alcohol and chlorine gas are introduced in a molar ratio of 1:1.1-1.25.
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