CN111548335A - Methyl/ethyl maltol chlorination section production facility - Google Patents
Methyl/ethyl maltol chlorination section production facility Download PDFInfo
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- CN111548335A CN111548335A CN202010422678.4A CN202010422678A CN111548335A CN 111548335 A CN111548335 A CN 111548335A CN 202010422678 A CN202010422678 A CN 202010422678A CN 111548335 A CN111548335 A CN 111548335A
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- 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
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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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/002—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out in foam, aerosol or bubbles
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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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2405—Stationary reactors without moving elements inside provoking a turbulent flow of the reactants, such as in cyclones, or having a high Reynolds-number
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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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
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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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- 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
- C07D309/32—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
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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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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Abstract
The invention discloses methyl/ethyl maltol chlorination section production equipment which is characterized by comprising a first pipeline reactor and a second pipeline reactor which are arranged in series, wherein a flow mixing device and a turbulence device are sequentially arranged in the first pipeline reactor, the turbulence device is arranged in the second pipeline reactor, a chlorine through pipe is arranged on the first pipeline reactor at a position close to a feed inlet, a chlorine supplementing pipe is arranged on the second pipeline reactor at a position close to the feed inlet, materials in an inner pipe of the pipeline reactor are in a turbulent flow state through the flow mixing plate and the turbulence device, the contact surface between the materials is constantly updated, 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.
Description
Technical Field
The invention relates to the technical field of production of flavor and essence, in particular to methyl/ethyl maltol chlorination section production equipment.
Background
Maltol, also known as methyl maltol, white needle crystals or white crystalline powder, has a melting point of 162 ℃ and 164 ℃, is a natural compound emitting aroma and is widely found in foods such as soybeans, coffee, bread, caramel and the like. Ethyl maltol, white needle crystals or white crystalline powder, with a melting point of 89-93 ℃, has a lasting caramel and fruit aroma per se, and dilute solutions have a relatively sweet fruit aroma. The ethyl maltol is a maltol homolog, has stronger aroma and stronger volatility due to slight change of the molecular structure, is a good aroma synergist for tobacco, food, beverage, essence, fruit wine, daily cosmetics and the like, has obvious effects on improving and enhancing the aroma of the food, plays a role in sweetening sweet foods and can prolong the storage period of the food.
At present, a synthetic route taking furfural as a raw material is often adopted in industrial production to prepare methyl/ethyl maltol, and the synthetic route has the advantages of simple production process, low production cost, less three wastes, easily-reached conditions and the like. The process comprises the steps of firstly preparing a Grignard reagent by using halogenated hydrocarbon and magnesium as main raw materials, then reacting furfural with the Grignard reagent to synthesize alpha-furan alkanol, and finally obtaining maltol and ethyl maltol through a series of oxidation reactions.
At present, chlorination reaction in methyl/ethyl maltol production is always single-kettle intermittent reaction, artificial subjective control error is the main reason of low conversion rate, intense chlorination reaction is also the main reason of side reaction in a kettle for 6 hours, the chlorination conversion rate can only reach 68%, the generation of by-product asphalt causes the increase of by-product waste asphalt in the later working section, the average amount of the single-kettle waste asphalt is 45kg, and the difficulty in solid waste treatment is increased. Chinese patent ZL201610750579.2 discloses a maltol pipeline chlorination reaction method, wherein a pipeline made of Hastelloy is arranged as a reactor, methanol, chlorine and furfuryl alcohol react through the pipeline, the reacted materials enter a collection transfer tank from an outlet of the pipeline, and the reaction materials collected by the transfer tank are hydrolyzed and sublimated to obtain a maltol crude product. The method breaks through the traditional reaction mode, combines the characteristics of violent chlorination reaction and instantaneous completion, changes the prior kettle-type full-mixed flow reaction into plug flow distribution reaction in a pipeline, can ensure the completion of the chlorination reaction, reduces the probability of further chlorination into byproducts, improves the yield of the workshop section by 5 percent, and reduces the solid waste generated by the rear workshop section. However, in order to make the reaction materials fully contact with each other, the method needs to be provided with the filler made of hastelloy materials, and the reaction materials need to stay in the filler region for 15 to 25 seconds, and in the actual production, corrugated plates made of hastelloy materials are overlapped together, and then the overlapped corrugated plates are cut into a cylinder shape and placed into a reaction pipeline.
Disclosure of Invention
Aiming at the problems that the reaction conversion rate of the chlorination section is low, the number of byproducts is large in the existing methyl/ethyl maltol production, and the effect of fully contacting reaction materials is not ideal due to the fact that the reaction time of the existing maltol pipeline chlorination reaction method is simply prolonged, the invention provides methyl/ethyl maltol chlorination section production equipment which is capable of shortening the reaction time, effectively reducing the side reaction of the chlorination reaction in the methyl/ethyl maltol production and improving the conversion rate of the chlorination reaction in the methyl/ethyl maltol production.
In order to achieve the purpose, the invention adopts the technical scheme that:
a methyl/ethyl maltol chlorination section production facility which is characterized in that: comprises a first pipeline reactor and a second pipeline reactor, wherein a discharge port of the first pipeline reactor is connected with a feed port of the second pipeline reactor through a pipeline, a flow mixing device and a turbulent device are sequentially arranged in the first pipeline reactor along the material flowing direction, wherein the flow mixing device comprises a first flow mixing plate and a second flow mixing plate, a turbulent flow device is arranged in the second pipeline reactor, a chlorine pipe is arranged on the first pipeline reactor and close to the feed inlet, the whole chlorine pipe is L-shaped, the top end of the chlorine introducing pipe is connected with the liquid chlorine buffer tank through an electromagnetic valve, the outlet of the chlorine introducing pipe is positioned on the axis of the inner pipe and points to the discharge hole of the inner pipe, and the chlorine introducing pipe is positioned between the first mixed flow plate and the second mixed flow plate, and a chlorine supplementing pipe is arranged on the second pipeline reactor and is close to the feed inlet, and the structure of the chlorine supplementing pipe is the same as that of the chlorine introducing pipe.
The pipeline reactor through the series arrangement replaces traditional cauldron formula reactor, and pipeline reactor compares in reation kettle specific surface area big, more does benefit to the exchange of reaction heat, and not only reaction rate is fast, and heat dispersion is superior moreover, controls reaction temperature more easily. The flow state of the material is adjusted through the mixed flow device and the turbulent flow device inside the pipeline reactor, so that the contact surface between the chlorine and the liquid material is continuously updated, the chlorination reaction efficiency is effectively improved, the chlorination reaction time is shortened, and the side reaction is reduced.
Furthermore, the first pipeline reactor and the second pipeline reactor also comprise a jacket, and a refrigerant inlet and a refrigerant outlet are arranged on the jacket. The chlorination reaction has higher requirement on temperature, and the temperature of materials in the pipeline reactor is adjusted by arranging the jacket, so that the requirement of the chlorination reaction on the temperature is ensured.
Furthermore, the outlet ends of the chlorine introducing pipe and the chlorine supplementing pipe are provided with fixing frames, the end parts of the fixing frames are provided with a material distribution device, the material distribution device is a conical thin plate, and round through holes are uniformly formed in the thin plate. Through setting up feed divider, when chlorine got into the inner tube through leading to the chlorine pipe, feed divider can smash great bubble for the contact surface increase of chlorine and material, through the combination with the mixed flow board, make fully contact between chlorine and the material.
Furthermore, the first mixed flow plate and the second mixed flow plate are obliquely fixed on the inner wall of the first pipeline reactor, the middle parts of the first mixed flow plate and the second mixed flow plate are provided with flow passing through holes, and the outer diameters of the first mixed flow plate and the second mixed flow plate are the same as the inner diameter of the first pipeline reactor. Through setting up the mixed flow board, when the material stream was through the mixed flow board, some material passed through the through-hole that overflows on the mixed flow board, and another part is then blockked and then passes through the clearance between mixed flow board and the inner tube for the flow state of material changes, increases the mixed degree. After the methanol aqueous solution and the alpha-furan alkanol solution enter the feeding hole, the flow state of the material in the inner tube is changed through the first mixed flow plate, so that the methanol aqueous solution and the alpha-furan alkanol solution are fully mixed, and the chlorine and the liquid material are preliminarily mixed through further mixed flow of the second mixed flow plate.
Furthermore, the turbulence device is a concentric reducer with a large head and a small head, and the small head of the reducer points to the discharge hole of the inner pipe. Through setting up the torrent device for reaction material is the torrent state, makes further mixing between chlorine and the liquid material, makes the contact surface between the material constantly update, effectively improves chlorination reaction efficiency, reduces chlorination reaction's side reaction.
Furthermore, the chlorine introducing pipe and the chlorine supplementing pipe are both provided with flow regulating valves. Through flow control valve, the chlorine flux of chlorine pipe and chlorine supplementing pipe is controlled to control the chlorine proportion through chlorine pipe and chlorine supplementing pipe, make the reaction more complete, further restrain the production of side reaction, thereby improve the productivity of maltol/ethyl maltol.
Furthermore, temperature sensors are arranged on the inner walls of the first pipeline reactor and the second pipeline reactor. The internal temperature of the pipeline reactor is monitored in real time through the temperature sensor, the measurement result is fed back to the control center, and the control center controls the refrigerant, so that the internal temperature of the pipeline reactor is adjusted, and the chlorination reaction is ensured to be carried out smoothly.
The invention has the advantages that:
(1) the pipeline reactor is adopted to replace the traditional kettle type reactor, the occupied area is small, the optimization of the layout of production equipment is facilitated, and the pipeline reactor is larger than the specific surface area of the reaction kettle, is more beneficial to the exchange of reaction heat and is easier to control the reaction temperature.
(2) The end part of the chlorine introducing pipe is provided with the material distributing device, when chlorine enters the inner pipe through the chlorine introducing pipe, the material distributing device can crush larger bubbles, so that the contact surface of the chlorine and the material is increased, and the chlorine and the material are fully contacted through combination with the mixed flow plate.
(3) Through setting up mixed flow plate and torrent device for the reaction material is the torrent state, makes further mixing between chlorine and the liquid material, makes the contact surface between the material constantly update, effectively improves chlorination reaction efficiency, reduces chlorination reaction's side reaction, thereby improves maltol/ethyl maltol's productivity.
Drawings
FIG. 1 is a schematic structural diagram of the present invention. The system comprises a first pipeline reactor 1, a second pipeline reactor 2, a turbulent flow device 3, a first mixed flow plate 4, a second mixed flow plate 5, a chlorine introducing pipe 6, a chlorine supplementing pipe 7, a jacket 8 and a material distributing device 9.
Detailed Description
Example 1
A methyl/ethyl maltol chlorination section production facility which is characterized in that: comprises a first pipeline reactor 1 and a second pipeline reactor 2, wherein the discharge hole of the first pipeline reactor is connected with the feed hole of the second pipeline reactor through a pipeline, a flow mixing device and a turbulent device 3 are sequentially arranged in the first pipeline reactor along the material flowing direction, wherein the flow mixing device comprises a first flow mixing plate 4 and a second flow mixing plate 5, a turbulent flow device 3 is arranged in the second pipeline reactor, a chlorine introducing pipe 6 is arranged on the first pipeline reactor and is close to the feed inlet, the whole chlorine introducing pipe is L-shaped, the top end of the chlorine introducing pipe is connected with the liquid chlorine buffer tank through an electromagnetic valve, the outlet of the chlorine introducing pipe is positioned on the axis of the inner pipe and points to the discharge hole of the inner pipe, and the chlorine introducing pipe is positioned between the first mixed flow plate and the second mixed flow plate, and a chlorine supplementing pipe 7 is arranged on the second pipeline reactor and close to the feed inlet, and the structure of the chlorine supplementing pipe is the same as that of the chlorine introducing pipe. The first pipeline reactor and the second pipeline reactor also comprise a jacket 8, and a refrigerant inlet and a refrigerant outlet are arranged on the jacket. The outlet ends of the chlorine introducing pipe and the chlorine supplementing pipe are provided with fixing frames, the end part of each fixing frame is provided with a material distributing device 9, each material distributing device is a conical thin plate, and round through holes are uniformly formed in the thin plates. The first mixed flow plate 5 and the second mixed flow plate 5 are obliquely fixed on the inner wall of the first pipeline reactor 1, flow passing through holes are formed in the middle of the first mixed flow plate and the middle of the second mixed flow plate, and the outer diameters of the first mixed flow plate and the second mixed flow plate are the same as the inner diameter of the first pipeline reactor. The turbulent device is a concentric reducer with big and small heads, and the small head of the reducer points to the discharge hole of the inner pipe. And flow regulating valves are arranged on the chlorine introducing pipe and the chlorine supplementing pipe. Temperature sensors are arranged on the inner walls of the first pipeline reactor and the second pipeline reactor.
Taking alpha-furan alkanol 165KG, 0L of soft water and 180L of methanol prepared in a Grignard reaction section, fully stirring and introducing a cooling medium, precooling to-20 ℃ to obtain an alpha-furan alkanol solution, pumping 1300L of recovered methanol aqueous solution into a solvent tank, precooling to-20 ℃, wherein the mass ratio of methanol to water in the methanol aqueous solution is 6:4, pumping the alpha-furan alkanol solution and the precooled methanol aqueous solution from a feed inlet of a first pipeline reactor, and simultaneously introducing chlorine gas through a chlorine introducing pipe and a chlorine supplementing pipe, wherein the flow ratio of the chlorine gas to the alpha-furan alkanol solution is 1 KG: 1.9L, controlling flow regulating valves on the chlorine introducing pipe and the chlorine supplementing pipe to enable the chlorine flux ratio of the chlorine introducing pipe to the chlorine supplementing pipe to be 8:1, controlling the temperature in the pipeline reactor to be below-6 ℃ by using a refrigerant in a jacket of the reactor, transferring a fully reacted material into a distillation tower from a discharge hole of a second pipeline reactor, heating for distillation to expel residual chlorine and recover methanol, recovering the recovered methanol, pumping the distilled material to a hydrolysis kettle, maintaining the temperature of the hydrolysis kettle to be 88 ℃, performing hydrolysis reaction, and after the hydrolysis rearrangement reaction is finished, enabling the conversion rate of a crude product to be 78.1%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A methyl/ethyl maltol chlorination section production facility which is characterized in that: comprises a first pipeline reactor (1) and a second pipeline reactor (2), wherein a discharge port of the first pipeline reactor is connected with a feed port of the second pipeline reactor through a pipeline, a mixed flow device and a turbulent flow device (3) are sequentially arranged in the first pipeline reactor along the material flowing direction, the mixed flow device comprises a first mixed flow plate (4) and a second mixed flow plate (5), the turbulent flow device (3) is arranged in the second pipeline reactor, a chlorine introducing pipe (6) is arranged on the first pipeline reactor and close to the feed port, the whole chlorine introducing pipe is L-shaped, the top end of the chlorine introducing pipe is connected with a liquid chlorine buffer tank through an electromagnetic valve, an outlet of the chlorine introducing pipe is positioned on the axis of an inner pipe, the outlet points to the discharge port of the inner pipe, the chlorine introducing pipe is positioned between the first mixed flow plate and the second mixed flow plate, and a chlorine supplementing pipe (7) is arranged on the second pipeline reactor and close to the feed port, the structure of the chlorine supplementing pipe is the same as that of the chlorine introducing pipe.
2. The methyl/ethyl maltol chlorination stage production facility as claimed in claim 1, wherein the first pipeline reactor and the second pipeline reactor further comprise a jacket (8), and the jacket is provided with a refrigerant inlet and a refrigerant outlet.
3. The methyl/ethyl maltol chlorination segment production equipment according to claim 1 or 2, wherein a fixing frame is arranged at the outlet ends of the chlorine introducing pipe and the chlorine supplementing pipe, a material distributing device (9) is arranged at the end part of the fixing frame, the material distributing device is a conical thin plate, and round through holes are uniformly formed in the thin plate.
4. The methyl/ethyl maltol chlorination stage production facility as claimed in claim 1, wherein the first mixed flow plate and the second mixed flow plate are fixed on the inner wall of the first pipeline reactor in an inclined manner, the middle parts of the first mixed flow plate and the second mixed flow plate are provided with flow passing through holes, and the outer diameters of the first mixed flow plate and the second mixed flow plate are the same as the inner diameter of the first pipeline reactor.
5. The methyl/ethyl maltol chlorination stage production facility as claimed in claim 1, wherein the turbulent device is a concentric reducer with large and small ends, and the small end of the reducer is directed to the outlet of the inner pipe.
6. The methyl/ethyl maltol chlorination stage production equipment according to claim 1, wherein the chlorine introducing pipe and the chlorine supplementing pipe are both provided with flow regulating valves.
7. The methyl/ethyl maltol chlorination stage production facility as claimed in claim 2, wherein the inner walls of the first pipeline reactor and the second pipeline reactor are provided with temperature sensors.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010422678.4A CN111548335B (en) | 2020-05-19 | 2020-05-19 | Methyl/ethyl maltol chlorination section production facility |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010422678.4A CN111548335B (en) | 2020-05-19 | 2020-05-19 | Methyl/ethyl maltol chlorination section production facility |
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| CN111548335A true CN111548335A (en) | 2020-08-18 |
| CN111548335B CN111548335B (en) | 2022-03-29 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183369A (en) * | 2011-12-28 | 2013-07-03 | 北京有色金属研究总院 | Apparatus and method for pipeline continuous carbonization of calcium and magnesium |
| CN106366061A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Maltol pipe chlorination reaction method |
| CN206778389U (en) * | 2017-05-25 | 2017-12-22 | 潍坊先达化工有限公司 | A kind of process units of 3 ethylmercapto group butyraldehyde |
| CN110252236A (en) * | 2019-07-08 | 2019-09-20 | 湖北仙粼化工有限公司 | A kind of diethanol monoisopropanolamine production multiple spot mixing reactor |
-
2020
- 2020-05-19 CN CN202010422678.4A patent/CN111548335B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183369A (en) * | 2011-12-28 | 2013-07-03 | 北京有色金属研究总院 | Apparatus and method for pipeline continuous carbonization of calcium and magnesium |
| CN106366061A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Maltol pipe chlorination reaction method |
| CN206778389U (en) * | 2017-05-25 | 2017-12-22 | 潍坊先达化工有限公司 | A kind of process units of 3 ethylmercapto group butyraldehyde |
| CN110252236A (en) * | 2019-07-08 | 2019-09-20 | 湖北仙粼化工有限公司 | A kind of diethanol monoisopropanolamine production multiple spot mixing reactor |
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