CN109865494B - Mixed feed liquid continuous neutralization layering system after chlorination hydrolysis - Google Patents
Mixed feed liquid continuous neutralization layering system after chlorination hydrolysis Download PDFInfo
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- CN109865494B CN109865494B CN201910143295.0A CN201910143295A CN109865494B CN 109865494 B CN109865494 B CN 109865494B CN 201910143295 A CN201910143295 A CN 201910143295A CN 109865494 B CN109865494 B CN 109865494B
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- 239000007788 liquid Substances 0.000 title claims abstract description 25
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 18
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 16
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 15
- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 13
- 238000003860 storage Methods 0.000 claims abstract description 30
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 4
- 229940093503 ethyl maltol Drugs 0.000 description 4
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a mixed feed liquid continuous neutralization layering system after chlorination hydrolysis, which comprises a storage kettle, a first reactor, a first alkali liquid storage tank, a second reactor, a second alkali liquid storage tank, a first metering pump, a second metering pump, a third metering pump, a layering device, a detection device and a control device.
Description
Technical Field
The invention relates to the technical field of ethyl maltol preparation, in particular to a mixed feed liquid continuous neutralization layering system after chlorination and hydrolysis.
Background
The ethyl maltol production process is divided into a Grignard working section, a chlorination working section, a sublimation working section and a crystallization working section. In the traditional chlorination section of ethyl maltol production process, firstly, a 54% -56% methanol aqueous solution is fed into a chlorination kettle by a circulating pump, and furfuryl alcohol (kg) and methanol (L) 1 are added dropwise into the chlorination kettle: 1. and (3) introducing chlorine into the reaction kettle, and feeding the materials into the hydrolysis kettle by using a circulating pump after the reaction is finished. And (3) evaporating methanol in a hydrolysis kettle and then carrying out hydrolysis reaction. After 3 hours of hydrolysis, it is necessary to perform neutralization to a pH of 2.5 to 3.0 and then to perform delamination. Because the materials in the reaction kettle are too little after the methanol is recovered in the early stage of the reaction kettle, and the manhole of the reaction kettle needs to be opened manually to detect the pH data. After the pH reaches the standard, the asphalt, the black oil layer and the water layer are required to be separated manually at rest. This step requires a large amount of skilled labor and is easily exposed to flammable and toxic gases. And the utilization rate of the equipment is low, which is not beneficial to the continuous production. Uncontrollable factors exist in the manual process, which results in low product yield.
Disclosure of Invention
It is necessary to provide a continuous neutralization layering system for mixed liquor after chlorination and hydrolysis.
The mixed feed liquid continuous neutralization layering system after chlorination hydrolysis comprises a storage kettle, a first reactor, a first alkali liquid storage tank, a second reactor, a second alkali liquid storage tank, a first metering pump, a second metering pump, a third metering pump, a layering device, a detection device and a control device, wherein the inlet of the storage kettle is connected with the chlorination hydrolysis kettle through a pipeline, the outlet of the storage kettle is connected with the inlet of the third metering pump, the outlet of the third metering pump is connected with the inlet of the first reactor through a first pipeline, the outlet of the first reactor is connected with the inlet of the second reactor through a second pipeline, the outlet of the second reactor is connected with the layering device through a pipeline, the layering device is sequentially provided with a gas phase outlet, a water phase outlet, an oil layer outlet and a bottom layer outlet from top to bottom for respectively discharging gas, a water layer, an oil layer and a bottom layer, the outlet of the first alkali liquor storage tank is connected with the first metering pump, the outlet of the first metering pump is connected with the first pipeline, the outlet of the second alkali liquor storage tank is connected with the second metering pump, the outlet of the second metering pump is connected with the second pipeline, the detection device comprises a first pH detector and a second pH detector, the first pH detector is arranged at the outlet of the first reactor and is used for detecting the pH value of mixed feed liquor flowing out of the outlet of the first reactor, the second pH detector is arranged at the outlet of the second reactor and is used for detecting the pH value of mixed feed liquor flowing out of the outlet of the second reactor and providing the pH value to the control device, a processor is arranged in the control device and is connected with the first metering pump, the second metering pump and the third metering pump, and the processor receives the pH value and processes the pH value and according to the processing result, the first metering pump, the second metering pump is controlled to control the amount of lye fed to the first and second reactors.
The invention realizes the continuous production of the neutralization of the ethyl maltol chloride solution by a continuous automatic process, simplifies the problem of difficult operation of the existing workers, and improves the product yield. And DCS on-line control and monitoring are adopted, so that the influence of human factors on the product yield is reduced, the production cost is reduced, the equipment utilization rate of the front working section is improved, the production environment is improved, and the method is safe and environment-friendly.
Drawings
Fig. 1 is a schematic structural diagram of the continuous neutralization layering system of the mixed liquor after chlorination hydrolysis.
Fig. 2 is a schematic view of the internal structure of the first reactor.
Fig. 3 is an enlarged view of a portion of the mixer of fig. 2.
Figure 4 is a schematic diagram of another embodiment of the mixer in figure 2.
Fig. 5 is a functional block diagram of the controller.
In the figure: the storage tank 10, the first reactor 20, the first pipe 21, the second pipe 22, the pipe body 23, the mixing section 231, the reaction section 232, the outflow section 233, the mixer 234, the inner pipe 2341, the first inlet section 23411, the first pressurizing section 23412, the first spouting section 23413, the outer pipe 2342, the second inlet section 23421, the second pressurizing section 23422, the second spouting section 23423, the jacket layer 24, the first lye tank 30, the second reactor 40, the second lye tank 50, the first metering pump 60, the second metering pump 70, the third metering pump 80, the layering device 90, the tower body 91, the gas phase outlet 92, the water phase outlet 93, the oil layer outlet 94, the bottom layer outlet 95, the upper expanding section 96, the lower expanding section 97, the first pH meter 101, the second pH meter 102, the first temperature detector 103, the second temperature detector 104, and the control device 110.
Detailed Description
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Referring to fig. 1 to 5, the embodiment of the invention provides a continuous neutralization layering system for mixed feed liquid after chlorination and hydrolysis, which comprises a storage kettle 10, a first reactor 20, a first alkali liquor storage tank 30, a second reactor 40, a second alkali liquor storage tank 50, a first metering pump 60, a second metering pump 70, a third metering pump 80, a layering device 90, a detection device and a control device 110, wherein an inlet of the storage kettle 10 is connected with the chlorination and hydrolysis kettle through a pipeline, an outlet of the storage kettle 10 is connected with an inlet of the third metering pump 80, an outlet of the third metering pump 80 is connected with an inlet of the first reactor 20 through a first pipeline 21, an outlet of the first reactor 20 is connected with an inlet of the second reactor 40 through a second pipeline 22, an outlet of the second reactor 40 is connected with the layering device 90 through a pipeline, the layering device 90 is sequentially provided with a gas phase outlet 92, a water phase outlet 93, an oil layer outlet 94 and a bottom layer outlet 95 from top to bottom, for discharging gas, water layer, oil layer, bottom layer respectively, the export of first lye storage tank 30 is connected with first measuring pump 60, the export of first measuring pump 60 is connected with first pipeline 21, the export of second lye storage tank 50 is connected with second measuring pump 70, the export of second measuring pump 70 is connected with second pipeline 22, the detection device includes first pH detector 101 and second pH detector 102, first pH detector 101 sets up in the export of first reactor 20 for detecting the pH value of mixed feed liquid that flows out of the export of first reactor 20, second pH detector 102 sets up in the export of second reactor 40 for detecting the pH value of mixed feed liquid that flows out of the export of second reactor 40, and provide the pH value to controlling means 110, controlling means 110 is inside sets up the treater, the treater sets up with first measuring pump 60, the second metering pump 70 and the third metering pump 80 are connected, and the processor receives and processes the pH value and controls the first metering pump 60 and the second metering pump 70 according to the processing result, thereby controlling the amount of the alkali lye added into the first reactor 20 and the second reactor 40.
In the present invention, a two-stage pH adjustment mode is set, when the pH value detected by the first pH meter 101 at the outlet of the first reactor 20 meets the process requirement, the second metering pump 70 does not act, and the second reactor 40 serves as the secondary mixer 234 to perform secondary mixing on the mixed material liquid, and then sends the mixed material liquid to the layering device 90; when the pH value detected by the first pH meter 101 does not meet the process requirement, the second metering pump 70 is operated, and the alkaline solution is added to the second reactor 40, so that the pH value of the mixed solution is secondarily adjusted, so that when the first metering pump 60 is operated, the amount of the alkaline solution added is large, as a coarse adjustment, and the amount of the alkaline solution added is small, as a fine adjustment, the second metering pump 70 is operated, so that the pH value of the alkaline solution entering the layering device 90 meets the process requirement.
Examples of online control of lye addition by the processor may be: the method comprises the steps that a first pH reference value and a second pH reference value are stored in advance in a processor, the pH value of mixed feed liquid flowing out of an outlet of a first reactor 20, namely, a first pH value, the pH value of mixed feed liquid flowing out of an outlet of a second reactor 40, namely, a second pH value, the processor compares the received first pH value with the first pH reference value, when the first pH value is lower than the first pH reference value, the processor sends an action signal to a second metering pump 70, the second metering pump 70 acts, alkali liquid is added into a second pipeline 22, and after the second reactor 40 reacts, a second pH detector 102 continuously monitors the second pH value; when the first pH value is not lower than the first pH reference value, it indicates that the process requirement is met, the processor does not send an action signal to the second metering pump 70, the second metering pump 70 does not act, and the second reactor 40 serves as a secondary reactor to perform secondary mixing reaction on the mixed material liquid.
Further, the first reactor 20 and the second reactor 40 have the same structure, the first reactor 20 includes a pipe body 23 and a jacket layer 24, the pipe body 23 includes a mixing section 231, a reaction section 232, and an outflow section 233 that are sequentially disposed, the front end of the mixing section 231 is provided with an inlet to be connected with the first pipe 21, the rear end is provided with an outlet to be connected with the second pipe 22, the jacket layer 24 surrounds the outer wall of the pipe body 23, a space for circulating water to flow is reserved in the jacket layer 24, a circulating water inlet and a circulating water outlet are respectively disposed at two ends of the jacket layer 24, an alkali liquor inlet is disposed on the side wall of the front end of the mixing section 231 to be communicated with the mixing section 231, and a pH value detecting port is disposed on the side wall of the outflow section 233 for inserting the first pH meter 101.
Further, the detecting device further includes a first temperature detector 103 and a second temperature detector 104, and a temperature measuring port is further formed on a side wall of the reaction section 232 of the first reactor 20 for inserting the first temperature detector 103 to detect the temperature inside the first reaction section 232, and a temperature measuring port is further formed on a side wall of the reaction section 232 of the second reactor 40 for inserting the second temperature detector 104 to detect the temperature inside the second reaction section 232.
Further, still set up the blender 234 inside mixing section 231, the blender 234 includes coaxial nested inner tube 2341 and outer tube 2342, inner tube 2341 includes first entering section 23411, first pressure applying section 23412, first blowout section 23413 that sets gradually, first entering section 23411 is constant diameter body 23, the front end and the first pipeline 21 of first entering section 23411 are connected, the rear end and the front end of first pressure applying section 23412 of first entering section 23411 are connected, the rear end and the front end of first blowout section 23413 of first pressure applying section 23412 are connected, the rear end of first pressure applying section 23412 is from the necking down body 23 of front-to-back, outer tube 2342 includes second entering section 2352, second pressure applying section 23422, second blowout section 23423 that sets gradually, second entering section 23421 is constant diameter body 23, the front end and the second pipeline 22 of second entering section 23421 are connected, the rear end and the front end of second entering section 23422 of second entering section 2324 are connected with the front end of second blowout section 2335, the rear end of second pressure applying section 2352 is opened, the front end and the rear end of second blowout section 2352 is opened, the front end of second pressure applying section is opened to the front end of second opening section is opened, the front end of second pressure applying section 2352 is opened, the front end is opened to the front end is opened, the front end is opened to open to the front section is opened.
The arrangement of the first pressure applying section 23412 in the mixer 234, in conjunction with the third metering pump 80, allows the feed liquid entering the mixing section 231 of the first reactor 20 to be pressurized, and by the time the reaction section 232 is entered, a vortex mixing has been established in the mixing section 231, allowing the feed liquid to be thoroughly mixed with the lye.
When the mixed liquor enters the inner pipe 2341 along the first entering section 23411 of the inner pipe 2341 and passes through the first pressing section 23412, the liquor has larger pressure due to the reduction of space, and is further sprayed out from the first spraying section 23413 to form siphon vortex, so that the alkali liquor entering the outer pipe 2342 is siphoned and sucked by the liquor, and the siphon suction forms the power for the alkali liquor naturally entering the mixer 234, and a separate power source is not required to be arranged for the first alkali liquor storage tank 30.
As another way of understanding, the end of the first conduit 21 may also be regarded as the first entry section 23411 of the mixing section 231. The diameter of the tube 23 of the first reactor 20 and the second reactor 40 is 57-89mm and the length is 2500mm.
The reaction section 232 is provided with packing inside the tube body 23 to form a reaction space having a suitable resistance.
Further, the mixer 234 is obliquely disposed inside the inner pipe 2341 of the mixing section 231, the mixer 234 is near the bottom of the inner pipe 2341, and the outlet direction of the mixer 234 is inclined upward.
The outlet of the mixer 234 is obliquely arranged, so that the sprayed mixed material is sprayed obliquely upwards, and then forms larger vortex and mixed flow force when being sprayed obliquely upwards and being impacted by the inner wall of the inner tube 2341 and the wall of the reaction section 232 in the process of falling downwards freely and being sprayed obliquely upwards, thereby being beneficial to further mixing; and the mixer 234 is arranged near the bottom of the inner pipe 2341, so that the space for lifting up the mixed material sprayed out from the outlet of the mixer 234 is larger, and the space inside the inner pipe 2341 is fully utilized.
Further, a stirring paddle is provided inside the storage tank 10, and a jacket layer 24 is provided on the outer wall of the storage tank 10.
Further, the layering device 90 includes a vertically arranged tower body 91, an upper expansion section 96 arranged at the upper part of the tower body 91, and a lower expansion section 97 arranged at the lower part of the tower body 91, wherein the inner diameters of the upper expansion section 96 and the lower expansion section 97 are larger than the inner diameter of the tower body 91, an inlet is further arranged on the side wall of the tower body 91, a gas phase outlet 92, a water phase outlet 93, an oil layer outlet 94 and a bottom layer outlet 95 are arranged on the side wall of the upper expansion section 96, and the inlet is arranged at the middle upper part of the tower body 91.
The inner diameters of the upper expansion section 96 and the lower expansion section 97 are larger than the inner diameter of the tower body 91, so that the change of the inner space from small to large is formed, the space is enlarged while the mixed material liquid is layered naturally according to different specific gravities, so that the volume drop is formed during layering, and the separation of materials with different specific gravities is facilitated.
The modules or units in the device of the embodiment of the invention can be combined, divided and deleted according to actual needs.
The foregoing disclosure is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the scope of the invention, as it is understood by those skilled in the art that all or part of the above-described embodiments may be practiced with equivalents thereof, which fall within the scope of the invention as defined by the appended claims.
Claims (3)
1. A mixed feed liquid continuous neutralization layering system after chlorination hydrolysis is characterized in that: comprises a storage kettle, a first reactor, a first alkali liquor storage tank, a second reactor, a second alkali liquor storage tank, a first metering pump, a second metering pump, a third metering pump, a layering device, a detection device and a control device, wherein the inlet of the storage kettle is connected with a chlorination hydrolysis kettle through a pipeline, the outlet of the storage kettle is connected with the inlet of the third metering pump, the outlet of the third metering pump is connected with the inlet of the first reactor through a first pipeline, the outlet of the first reactor is connected with the inlet of the second reactor through a second pipeline, the outlet of the second reactor is connected with the layering device through a pipeline, the layering device is sequentially provided with a gas phase outlet, a water phase outlet, an oil layer outlet and a bottom layer outlet from top to bottom for respectively discharging gas, a water layer, an oil layer and a bottom layer, the outlet of the first alkali liquor storage tank is connected with the first metering pump, the outlet of the first metering pump is connected with the first pipeline, the outlet of the second alkali liquid storage tank is connected with the second metering pump, the outlet of the second metering pump is connected with the second pipeline, the detection device comprises a first pH detector and a second pH detector, the first pH detector is arranged at the outlet of the first reactor and is used for detecting the pH value of mixed liquid flowing out of the outlet of the first reactor, the second pH detector is arranged at the outlet of the second reactor and is used for detecting the pH value of mixed liquid flowing out of the outlet of the second reactor and providing the pH value to the control device, a processor is arranged in the control device and is connected with the first metering pump, the second metering pump and the third metering pump, the processor receives the pH value and processes the pH value and controls the first metering pump and the second metering pump according to the processing result, thereby controlling the amount of lye added to the first reactor and the second reactor; the first reactor and the second reactor have the same structure, the first reactor comprises a pipe body and a jacket layer, the pipe body comprises a mixing section, a reaction section and an outflow section which are sequentially arranged, the front end of the mixing section is provided with an inlet and is connected with a first pipeline, the rear end of the mixing section is provided with an outlet and is connected with a second pipeline, the jacket layer surrounds the outer wall of the pipe body, a space for circulating water to flow is reserved in the jacket layer, a circulating water inlet and a circulating water outlet are respectively arranged at two ends of the jacket layer, an alkali liquor inlet is also arranged on the side wall of the front end of the mixing section and is communicated with the mixing section, and a pH value detection port is also arranged on the side wall of the outflow section for the first pH value detector to be inserted; the mixer is characterized in that a mixer is further arranged in the mixing section, the mixer comprises an inner pipe and an outer pipe which are coaxially nested, the inner pipe comprises a first inlet section, a first pressure applying section and a first spraying section which are sequentially arranged, the first inlet section is an equal-diameter pipe body, the front end of the first inlet section is connected with a first pipeline, the rear end of the first inlet section is connected with the front end of the first pressure applying section, the rear end of the first pressure applying section is connected with the front end of the first spraying section, the rear end of the first spraying section is open, the first pressure applying section is a necking pipe body from front to back, the outer pipe comprises a second inlet section, a second pressure applying section and a second spraying section which are sequentially arranged, the front end of the second inlet section is connected with a second pipeline, the rear end of the second inlet section is connected with the front end of the second pressure applying section, the rear end of the second spraying section is larger than the front end of the first spraying section, the rear end of the first spraying section is open, the first pressure applying section is arranged on the inner pipe, the second inlet section is arranged on the side wall of the mixer, the inner pipe is close to the bottom of the mixer, the first spraying section is arranged on the side wall of the mixer, the mixer is close to the rear side of the mixer, and the mixer is arranged on the side of the mixer; the layering device comprises a vertically arranged tower body, an upper expansion section arranged on the upper part of the tower body, and a lower expansion section arranged on the lower part of the tower body, wherein the inner diameters of the upper expansion section and the lower expansion section are larger than the inner diameter of the tower body, an inlet is further formed in the side wall of the tower body, a gas phase outlet, a water phase outlet, an oil layer outlet and a bottom layer outlet are formed in the side wall of the upper expansion section, and the inlet is formed in the middle upper part of the tower body.
2. The post-chlorination-hydrolysis mixed liquor continuous neutralization layering system of claim 1, wherein: the detection device further comprises a first temperature detector and a second temperature detector, a temperature measuring port is formed in the side wall of the reaction section of the first reactor for the first temperature detector to insert to detect the temperature inside the first reaction section, a temperature measuring port is formed in the side wall of the reaction section of the second reactor for the second temperature detector to insert to detect the temperature inside the second reaction section, and the diameters of the tube bodies of the first reactor and the second reactor are 57-89mm, and the lengths of the tube bodies of the first reactor and the second reactor are 2500mm.
3. The post-chlorination-hydrolysis mixed liquor continuous neutralization layering system of claim 1, wherein: the inside stirring rake that sets up of storage kettle sets up the jacket layer at the outer wall of storage kettle.
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| RU2681527C1 (en) * | 2016-12-30 | 2019-03-07 | Бейджинг Хуаши Юнайтед Энерджи Технолоджи энд Девелопмент Ко., Лтд. | Light petroleum products from heavy oil production method and device by the hydrogenation in the fluidized bed method |
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