CN102093213A - Esterification reactor and esterification reaction method based on solid catalyst - Google Patents
Esterification reactor and esterification reaction method based on solid catalyst Download PDFInfo
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- CN102093213A CN102093213A CN2010105889165A CN201010588916A CN102093213A CN 102093213 A CN102093213 A CN 102093213A CN 2010105889165 A CN2010105889165 A CN 2010105889165A CN 201010588916 A CN201010588916 A CN 201010588916A CN 102093213 A CN102093213 A CN 102093213A
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- 239000011949 solid catalyst Substances 0.000 title claims abstract description 49
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 34
- 230000032050 esterification Effects 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 190
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 19
- 229930195729 fatty acid Natural products 0.000 claims abstract description 19
- 239000000194 fatty acid Substances 0.000 claims abstract description 19
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 7
- 230000008676 import Effects 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- 230000004044 response Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 25
- 230000000694 effects Effects 0.000 abstract description 15
- 238000011084 recovery Methods 0.000 abstract description 8
- 150000004668 long chain fatty acids Chemical class 0.000 abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 4
- 239000007795 chemical reaction product Substances 0.000 abstract description 3
- 239000012043 crude product Substances 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 239000000203 mixture Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 5
- 150000002646 long chain fatty acid esters Chemical class 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000002638 heterogeneous catalyst Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 239000002815 homogeneous catalyst Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 Fatty acid ester Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
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- 239000002893 slag Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention relates to an esterification reactor based on a solid catalyst and a long-chain fatty acid esterification method using the same. The esterification reactor comprises a reaction tube, a feed pump, a circulating pump and a solid-liquid separator, wherein the outlet of the feed pump is connected to the bottom end of the reaction tube, so that the feed pump can send reaction raw materials and a reaction liquid part from a reaction chamber into the reaction chamber; the inlet of the circulating pump is connected with the reaction chamber, so that the circulating pump can be used for selectively outputting reaction products in multiple positions in the height direction of the reaction chamber; and the inlet of the solid-liquid separator is connected with the outlet of the circulating pump, so that the solid-liquid separator can be used for separating the reaction products from the circulating pump into the reaction liquid part and a solid catalyst-enriched slurry part. The light phase outlet of the solid-liquid separator is used as a crude product outlet and connected to the feed pump, so that the reaction liquid part flows back to the reaction chamber; and the heavy phase outlet of the solid-liquid separator is used as a solid catalyst recovery outlet and connected to the bottom end of the reactor, so that the slurry part flows back to the reaction chamber. The invention can greatly enhance the catalyst separation effect, reduce the circulating pump abrasion caused by the catalyst and enhance the esterification efficiency of the fatty acid.
Description
Technical field
The present invention relates to a kind of esterification device and esterifying reaction method based on solid catalyst.
Background technology
Fatty acid ester, for example long chain fatty acid ester can synthesize through esterification under the effect of an acidic catalyst by lipid acid acid and alcohols.Industrial catalyzer commonly used is that solubilized such as sulfuric acid, Phenylsulfonic acid maybe can be dispersed in organic acid or the mineral acid in the reaction solution at present, is called homogeneous catalyst.Homogeneous catalyst and reaction raw materials to contact effect good, so catalytic efficiency is higher; Be difficult to from reaction system Separation and Recovery and reused yet finish the back an acidic catalyst, can only discharge with waste water usually in reaction.For this reason, people have developed multiple solid acid catalyst and have been used for esterification, and these catalyzer are insoluble to reaction solution in reaction process, be called heterogeneous catalyst.Heterogeneous catalyst after reaction is finished, be easy to by filter, mechanical separation means Separation and Recovery such as centrifugal or sedimentation, and can be recycled and reused for subsequent reactions, therefore can economize on resources and reduce pollution.Usually need meet the following conditions in the industrial esterification of heterogeneous catalyst catalysis long chain acid of utilizing: (1) longer chain fatty acid obtains well to contact with alcohol.Because longer chain fatty acid and the bigger polarity difference of alcohol existence, and often can not dissolve each other, therefore needing comparatively, intensive stirs the mixed contact of strengthening the two that acts on; (2) higher temperature of reaction.Within the specific limits, temperature raises and helps the carrying out of esterification, so reactive system need remain under the higher temperature of reaction; (3) reaction solution contacts with the good of catalyzer.In order to improve the effect that contacts of heterogeneous catalyst and reaction solution, adopt usually to strengthen and stir, increase specific surface area of catalyst, increase catalyst levels means such as (solid-to-liquid ratios); (4) rational solid catalyst Separation and Recovery and recycling method; (5) pure consumption is higher than the stoichiometric quantity number.Alcohol excess makes molecular balance trend towards generating long chain fatty acid ester, makes reaction more thorough.
Can adopt three class reactors to implement heterogeneous esterification reaction at present.One, tank reactor.Utilize mechanical stirring to strengthen contacting of lipid acid and alcohol, and make the solid catalyst suspended dispersed in reaction solution; Utilize external whizzer or filter Separation and Recovery solid catalyst.Its two, fixed-bed reactor.Solid catalyst is filled in forms porous fixed bed in the reaction tubes, contact with catalyzer when reaction solution is flowed through the space of fixed bed, discharge and directly and catalyst separating from the fixed bed outlet subsequently.Its three, fluidized-bed reactor.Reaction solution forms turbulent flow in reactor under the driving of recycle pump, drive the solid catalyst particle suspended dispersed, thereby each is well contacted mutually; After reaction finishes, the circulation of stopped reaction liquid, solid catalyst and reaction solution are by settlement separate, and after reaction solution was discharged, solid catalyst was reusable.
In the esterification of catalysis of solid catalyst longer chain fatty acid, fluidized-bed reactor has certain advantage with respect to other two class.With respect to tank reactor, (1) does not have mechanical stirring mechanism, and the equipment good seal performance can be born higher temperature and pressure; (2) reactor wall surface-area is big, and the heat transfer efficiency height need not to be provided with the coiled pipe heat exchange, keeps in repair easy; (3) larger ratio of height to diameter reactor itself has catalyst sedimentation Separation and Recovery ability, in theory whizzer or filter separating catalyst can be set again.With respect to fixed-bed reactor, (1) bed pressure drop is little, need not to equip high-pressure pump; (2) longer chain fatty acid and alcohol obtain continuing to mix, and contact effective; (3) catalyst particle size and aperture there is not strict restriction; (4) catalyzer is changed conveniently.Yet still there is bigger limitation in conventional fluidized-bed reactor, is difficult to directly apply to the industrial production of long chain fatty acid ester.Its major cause is: (1) solid catalyst is subjected to the intensive fluid shearing in reaction process, and collision mutually between the particle, causes the broken or wearing and tearing of granules of catalyst, forms small catalyst fines.These catalyst fineses are difficult to not only need the longer settling time by the complete Separation and Recovery of standing sedimentation, and can mix wherein when the reaction solution discharging, cause greater loss; (2) a large amount of solid catalysts are suspended in the reaction solution, and the recycle pump of flowing through repeatedly causes lasting wearing and tearing to circulating pump impeller and spiral case, causes the recycle pump life-span significantly to descend; (3) solid content must be controlled in the normal range of operation of recycle pump, causes catalyst levels to be subjected to very big restriction, can't improve reaction efficiency by significantly improving solid-to-liquid ratio.
Summary of the invention
At the limitation that above-mentioned all kinds of reactors exist, the present invention proposes a kind of circulating fluid bed reaction unit with two-stage isolating construction.
Apparatus of the present invention are a kind of esterification devices based on solid catalyst, comprising: reaction tubes defines reaction chamber; Fresh feed pump, its outlet is connected to the reaction tubes bottom, is used for partly sending reaction raw materials and/or from the reaction solution of reaction chamber into reaction chamber; Recycle pump, its import is connected with reaction chamber, and is connected to selectively a plurality of positions on the reaction chamber short transverse with reaction mass output-response chamber; And solid-liquid separator, its import is connected with outlet of circulating pump, and being used in the future, the reaction mass of self-circulating pump is separated into described reaction solution part and the slurry part that is rich in solid catalyst.Wherein, the thick products export of the light phase export of solid-liquid separator conduct, and be connected to the fresh feed pump inlet so that described reaction solution part can be back to reaction chamber; And the heavy out of solid-liquid separator exports as reclaiming solid catalyst, and is connected to the reactor bottom so that described slurry part can be back to reaction chamber.
In preferred reaction unit, described solid-liquid separator is a wet cyclone.
In preferred reaction unit, the aspect ratio of described reaction tubes is 6-18.
In preferred reaction unit, also comprise the inhaling type jet mixer that stretches into reaction chamber from the reaction tubes bottom, its import links to each other with the charging pump outlet, and the reaction solution part of reaction raw materials and backflow is spurted into the reaction chamber bottom through this inhaling type jet mixer.
Another aspect of the present invention, a kind of longer chain fatty acid esterification method is provided, it uses esterification device of the present invention, wherein, during the reaction mass circulating reaction, reaction mass is turbulence state at the reaction chamber hypomere, feasible longer chain fatty acid and alcohol and solid catalyst particle thorough mixing as reaction raw materials; Basically be laminar flow regime at the reaction chamber epimere, make solid catalyst particle wherein keep lower content because of part is settled down to the below turbulent area; And the material level that recycles of reaction chamber is put and is arranged on the laminar flow regime district.
Esterification device of the present invention owing to adopt the tubular reactor with larger ratio of height to diameter, when the reaction tubes hypomere forms turbulent area, can remain at epimere and be beneficial to the settled disengaging zone of solid catalyst; In addition, be arranged on outside equipment for separating liquid from solid to further separating through settled reaction mass.Such design not only can significantly improve the separating effect of catalyzer, and can reduce the wearing and tearing of catalyzer to recycle pump.The strong mixing that forms also can effectively promote longer chain fatty acid esterification efficient through refluxing.
Description of drawings
Fig. 1 is the synoptic diagram of the esterification device of the present invention's one preferred implementation; And
Fig. 2 shows the suction melange effect and the cycling stream effect of inhaling type jet mixer shown in Figure 1.
Embodiment
Below, introduce reaction unit primary structure feature of the present invention and advantage thereof respectively by embodiment.
Fig. 1 is the synoptic diagram of the esterification device of the present invention's one preferred implementation.In the reaction unit, carry order, be followed successively by fresh feed pump 1, inhaling type injector 2, reaction tubes 4, lift discharge nozzle 5, recycle pump 3 and wet cyclone 6 by feed liquid.Above each several part connects by pipeline by diagram, and valve regulated flow and pressure can be set.
The light phase export of wet cyclone is that upper outlet is connected to fresh feed pump, and when reaction finishes as thick products export; The heavy out of wet cyclone promptly is exported to the catalyzer backflow opening for feed of reaction tubes bottom down, also can reclaim catalyzer from this outlet.
Fresh feed pump is common liquid delivery pump, for example can select to have more high-lift impeller pump.It is used for the input of reaction raw materials (for example, longer chain fatty acid, alcohol); In reaction process, also accept fluid from the cyclone separator upper outlet, make and pump material acquisition higher momentum, be beneficial to the thorough mixing of reaction chamber bottom material.
Longer chain fatty acid and pure molecular polarity difference are big, and the degree of dissolving each other is low.Therefore in reaction process, the alcohol that has neither part nor lot in reaction can be lower because of density, and tend to be diffused into reaction tubes top.And flow in the reaction tubes upper body is laminar flow, for alcohol has been created good condition to the diffusion on reaction tubes top.Therefore in reaction process, reaction tubes top has higher pure content.When the top liquid phase through recycle pump again behind wet cyclone, gently mutually in pure content will further rise.When therefore gently importing (preferably, through the inhaling type jet mixer) by fresh feed pump, pure content is higher in the input fluid.Local high " alcohol oil rate " (being the ratio of the mole number of pure molecule and fatty acid molecule) that forms in the reaction chamber bottom thus is very beneficial for the carrying out of esterification and the raising of lipid acid utilization ratio.
The fresh feed pump outputting material enters reaction chamber through the inhaling type jet mixer, and can obtaining more, intensive mixes.In the middle part of the inhaling type jet mixer places at the bottom of the reaction tubes.Fluid from fresh feed pump has higher energy, and flow velocity sharply rises during by jet hole, and static pressure descends, and the reaction solution outer to suction port causes suction, and make it to be inhaled into the back and mix rapidly with the injection fluid, and through discharging behind mixing tube and the diffuser tube.The longer chain fatty acid and the solid catalyst that have larger proportion in the inhalant liquid, and have the alcohol of larger proportion in the liquid phase of jet orifice ejection, the two obtains intense mixing in jet mixer, obtain good contact effect.Because near the fluid the suction port is constantly sucked jet mixer, and constantly obtain to replenish, therefore, help improving overall mixed effect at the outside local circulation stream that forms of mixing tank from the jet mixer outlet.Fig. 2 shows the suction melange effect and the cycling stream effect of inhaling type jet mixer.
In addition, injector is preferably designed as and makes the injection fluid and suck the fluidic volume ratio is 6-20: 1, and this helps the local higher zone of pure ratio that forms in reactor, and reaction is carried out to the direction that helps esterification.
Reactor adopts reaction tubes, because its bigger aspect ratio helps keeping different flow states at different sections, as turbulence state or laminar flow regime.This reaction tubes hypomere can form the mixing zone, and rate of flow of fluid is high and flow to confusion, and its liquid phase flow form is a turbulent flow, and wherein each composition obtains strong and mixing that continue; This reaction tubes epimere can form the disengaging zone, and rate of flow of fluid is low and main body is upwards mobile, and its liquid phase flow form is a laminar flow, and most of solid catalyst sinks to entering the mixing zone under settlement action, and most of unreacted alcohol is enriched to the upper strata because of density is lower.The reaction tubes wall is a heat-transfer surface, is used to improve or keeps the interior temperature of reaction of reaction tubes.Preferably, the aspect ratio of reaction tubes is 6: 1 to 18: 1.Reaction tubes shown in Figure 1 is isometrical pipe, but the present invention is not limited to this, can be adapter bonnet also, keeps strong blended turbulence state or laminar flow regime as long as help at different sections.
The lift discharge nozzle is the pipe that reaction chamber is stretched at autoreaction pipe top, and liftable is regulated the position of the mouth of pipe in reaction tubes.The fall way discharge port that Fig. 1 specifically illustrates is in the discharging position after reaction finishes.In reaction process, the discharging mouth of pipe is positioned at top, laminar region, with the low reaction mass of output catalyst granule content, is preferably located in and goes up the following 1-10cm of liquid level in the reaction tubes.After reaction was finished, the discharging mouth of pipe was positioned at place, catalyst deposit layer top, reaction tubes bottom, for example, under the situation of using the inhaling type jet mixer, the discharging mouth of pipe can be located at the above 1-10cm of inhaling type jet mixer suction port.
Recycle pump is accepted the reaction-ure fluid from the lift discharge nozzle, makes it obtain higher momentum, thereby obtain high flow velocities in wet cyclone.Because fluid is from the lower laminar region output of solid catalysis agent content, so the less damage that is subjected to solid catalyst of recycle pump conversely, has only less solid catalyst particle to be broken into fine powder because of pump delivery in the reaction process.
Wet cyclone is used for the high efficiency separation of solid catalyst and reaction solution, has far above settlement separate separating factor.In reaction process, accept the fluid of self-circulating pump, with wherein residual solid catalyst particle and liquid phase separation, and make it respectively from outlet and upper outlet are discharged down.After reaction is finished, accept the fluid of self-circulating pump, wherein residual solid catalyst is separated with reaction product, obtain light phase at upper outlet, discharge as crude product; Exporting the acquisition heavy phase down, wherein contain a large amount of solid catalyst particles, be back to the reaction tubes bottom.Because wet cyclone separating factor height, therefore when solid catalyst because of wearing and tearing and collision generation during than small-particle, still can be with most granules of catalyst Separation and Recovery.For thoroughly reclaiming the solid catalyst particle in the crude product fluid, the 1-2 level of can further connecting cyclone separator.
More than be the preferred implementation of apparatus of the present invention, it can do following change, still can obtain similar effects.
For example, wet cyclone can substitute with other solid-liquid separating equipment, as the whizzer of continuous discharging slag.The lift discharge nozzle can adjust the structure that material level puts with other and replace, and for example, can a plurality of discharge ports be set at reaction tubes tube wall different heights place.
Below the concise and to the point process of utilizing esterification device of the present invention to implement longer chain fatty acid esterification reaction of describing.But should be understood that though device of the present invention develops at the longer chain fatty acid esterification, it is equally applicable to other esterification based on solid catalyst.
With fresh feed pump reaction raw materials (longer chain fatty acid and alcohol) is sent in the reaction tubes, with in the new adding reaction tubes or the solid catalyst particle that retains mix.
Treat that liquid level rises to reaction tubes top predetermined height, the beginning cyclical operation: to wet cyclone, reaction mass is separated into described reaction solution part and is rich in the slurry part of solid catalyst the ON cycle pump from liquid level below discharging pump; The reaction solution part is back to reaction chamber through the fresh feed pump inlet, and the slurry part directly is back to reaction chamber, thereby forms the reactant outer circulation.
During the circulating reaction, reaction mass is turbulence state at the reaction chamber hypomere, feasible longer chain fatty acid and alcohol and solid catalyst particle thorough mixing as reaction raw materials; Basically be laminar flow regime at the reaction chamber epimere, make solid catalyst particle wherein keep lower content because of part is settled down to the below turbulent area; And the material level that recycles of reaction chamber is put and is arranged on the laminar flow regime district.Wherein recycling material level puts and is preferably disposed on the following 1-10cm of reaction chamber liquid level place.
After reaction finishes, after treating that solid catalyst particle is settled down to the reaction tubes bottom, locate as the discharging position by the top with the solid catalyst particle settled layer, export the lower reaction solution of solid catalysis agent content to described equipment for separating liquid from solid with recycle pump, through further exporting as thick product after the solid-liquid separation.The granules of catalyst and the isolating granules of catalyst of wet cyclone that are settled down to reaction chamber bottom are recyclable, or reside in reaction chamber and treat down the batch reaction use.
In sum, esterification device of the present invention is when implementing esterification, and have the following advantages: (1) catalyst separation is effective. Have two-stage solid catalyst separating mechanism (Disengagement zone in the reaction tube and cyclone hydraulic separators), even still have good separation organic efficiency for the small catalyst granules because of wearing and tearing or collision generation, thereby reduced catalyst loss. (2) degree of wear of reduction pump. Solid catalyst is before entering circulating pump and feed pump, and major part obtains separating, the wearing and tearing of pump are significantly descended, and the consumption of catalyst in whole reaction system, be not subjected to the restriction of pump work performance. (3) mixed effective. In suction-type jet mixer inside, LCFA, alcohol and solid catalyst are mixed strongly, and in suction-type blender outside, have also consisted of the circular flow of main body, have improved overall mixed effect. (4) reaction efficiency height. Can form the zone of high pure ratio in the part, be conducive to the esterification of LCFA. With respect to the popular response device, can reduce the initial alcohol consumption, thereby save the energy consumption of reclaiming alcohol. (5) flexible operation. Discharging mouth of pipe liftable is regulated, can regulate targetedly for the different phase of course of reaction or the variation of feed composition, thus the stability of maintenance reaction effect. (6) reaction starts fast. After reaction finished, the catalyst mud that outlet is flowed out under the cyclone separator contained a certain amount of reactant liquor, wherein contains a large amount of long-chain fatty acid esters. Because long-chain fatty acid ester all has good dissolving power to LCFA and alcohol, therefore can starting stage of next time reaction as a kind of cosolvent, significantly reduce the interfacial tension of LCFA and alcohol, thereby improve the contact effect of two kinds of reactants, and then improve initial reaction efficient. In addition, it is good that this reactor still possesses the HTHP performance, simple in structure, easy maintenance, heat transfer efficiency advantages of higher.
Claims (9)
1. the esterification device based on solid catalyst is characterized in that, comprising:
Reaction tubes defines reaction chamber;
Fresh feed pump, its outlet is connected to the reaction tubes bottom, is used for partly sending reaction raw materials and/or from the reaction solution of reaction chamber into reaction chamber;
Recycle pump, its import is connected with reaction chamber, and is connected to selectively a plurality of positions on the reaction chamber short transverse with reaction mass output-response chamber; And
Solid-liquid separator, its import is connected with outlet of circulating pump, and the reaction mass that is used for the self-circulating pump in future is separated into described reaction solution part and the slurry part that is rich in solid catalyst,
Wherein, the thick products export of the light phase export of solid-liquid separator conduct, and be connected to the fresh feed pump inlet so that described reaction solution part can be back to reaction chamber; And the heavy out of solid-liquid separator exports as reclaiming solid catalyst, and is connected to the reactor bottom so that described slurry part can be back to reaction chamber.
2. according to the reaction unit of claim 1, it is characterized in that described solid-liquid separator is a wet cyclone.
3. reaction unit according to claim 1 and 2 is characterized in that, the aspect ratio of described reaction tubes is 6-18.
4. reaction unit according to claim 1 and 2, it is characterized in that, also comprise the inhaling type jet mixer that stretches into reaction chamber from the reaction tubes bottom, its import links to each other with the charging pump outlet, and the reaction solution part of reaction raw materials and backflow is spurted into the reaction chamber bottom through this inhaling type jet mixer.
5. reaction unit according to claim 4 is characterized in that the size of described inhaling type jet mixer is set to, and during reaction can form turbulent area and form the laminar region basically at the reaction chamber epimere at the reaction chamber hypomere.
6. reaction unit according to claim 4 is characterized in that, it is 6-20 with sucking the fluidic volume ratio that described inhaling type jet mixer is designed to spray fluid.
7. reaction unit according to claim 1 and 2 is characterized in that, recycle pump links to each other with reaction chamber via the adjustable discharge nozzle that stretches into reaction chamber, this adjustable discharge nozzle get that material level puts can be in reaction chamber short transverse adjusted; Perhaps, recycle pump is connected with reaction chamber via a plurality of discharge ports that are arranged on the reaction tubes different heights, makes that selectively a plurality of positions on the reaction chamber short transverse are with reaction mass output-response chamber.
8. the esterification process of a longer chain fatty acid, it uses each described esterification device of claim 1-7, wherein, during the reaction mass circulating reaction, reaction mass is turbulence state at the reaction chamber hypomere, feasible longer chain fatty acid and alcohol and solid catalyst particle thorough mixing as reaction raw materials; Basically be laminar flow regime at the reaction chamber epimere, make solid catalyst particle wherein keep lower content because of part is settled down to the below turbulent area; And the material level that recycles of reaction chamber is put and is arranged on the laminar flow regime district.
9. esterification process according to claim 8, wherein, the described material level that recycles is put and is arranged on the following 1-10cm of reaction chamber liquid level place; After reaction finishes, after treating that solid catalyst particle is settled down to the reaction tubes bottom, locate as the discharging position by the top with the solid catalyst particle settled layer, export the lower reaction solution of solid catalysis agent content to described equipment for separating liquid from solid with recycle pump, through further exporting as thick product after the solid-liquid separation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108704586A (en) * | 2018-05-16 | 2018-10-26 | 浙江工业大学 | A kind of liquid-solid reactor |
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| WO2004098760A1 (en) * | 2003-05-08 | 2004-11-18 | China Petroleum & Chemical Corporation | An apparatus for reaction or separation and continuous esterification method using the apparatus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704586A (en) * | 2018-05-16 | 2018-10-26 | 浙江工业大学 | A kind of liquid-solid reactor |
| CN108704586B (en) * | 2018-05-16 | 2020-03-17 | 浙江工业大学 | Liquid-solid reactor |
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