CN104357098B - Produce the method and system of biodiesel - Google Patents
Produce the method and system of biodiesel Download PDFInfo
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- CN104357098B CN104357098B CN201410538021.9A CN201410538021A CN104357098B CN 104357098 B CN104357098 B CN 104357098B CN 201410538021 A CN201410538021 A CN 201410538021A CN 104357098 B CN104357098 B CN 104357098B
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- 239000003225 biodiesel Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 432
- 239000003054 catalyst Substances 0.000 claims abstract description 137
- 238000010438 heat treatment Methods 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- 238000005809 transesterification reaction Methods 0.000 claims abstract description 41
- 238000000926 separation method Methods 0.000 claims abstract description 34
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims abstract description 29
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000376 reactant Substances 0.000 claims abstract description 17
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 14
- 235000011187 glycerol Nutrition 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims description 74
- 238000001704 evaporation Methods 0.000 claims description 60
- 230000008020 evaporation Effects 0.000 claims description 60
- 238000011084 recovery Methods 0.000 claims description 30
- 238000012546 transfer Methods 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 24
- 230000004044 response Effects 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 20
- 238000012545 processing Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 238000013517 stratification Methods 0.000 claims description 4
- 210000002421 cell wall Anatomy 0.000 claims description 3
- 230000001351 cycling effect Effects 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002283 diesel fuel Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000010828 elution Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000000047 product Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003626 triacylglycerols Chemical class 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- BGOFCVIGEYGEOF-UJPOAAIJSA-N helicin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=CC=C1C=O BGOFCVIGEYGEOF-UJPOAAIJSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a kind of method and system that produce biodiesel, belong to the technical field of manufacturing the method for biodiesel and the system and device structure of Using such method manufacturing biodiesel. The present invention utilizes the solid-state catalyst of powdery and triglyceride and methyl alcohol mixing circulation, mat heating using microwave mechanism carries out catalytic reaction, can reach fast transesterification target, directly improves heating-up temperature after its transesterification, allow methyl alcohol steam separation, reclaim use through heat exchanger condensation. After methyl alcohol shifts out, reactant directly shifts out reaction system, can directly isolate the solid-state catalyst of biodiesel, glycerine and powdery. The present invention not only improves solid-state catalyst transesterification reaction efficiency, and exempts water elution except catalyst program, reduces production costs, and builds and meets energy-saving, emission-reducing, environment friendly production technology.
Description
Technical field
The present invention relates to a kind of method and system that produce biodiesel, belong to the method and system dress of production chemical productThe technical field of interposed structure, belongs to specifically and manufactures the method for biodiesel and Using such method and manufacture biodieselThe technical field of system and device structure.
Background technology
Traditional biological diesel oil is mainly to use liquid alkali catalyst (catalyst also claims catalyst) to react in the majority, generally uses hydrogen-oxygenIt is main changing sodium (NaOH). Its response procedures as shown in Figure 1, utilizes triglyceride, methyl alcohol and catalyst to carry out catalysis transesterification reaction,Owing to generally time must having higher temperature and pressure in reaction, and then there is people to apply ultrasonic or microwave accelerates catalytic action,Accelerate transesterification speed, and its product can remain NaOH (NaOH) catalyst, must first remove NaOH (NaOH)Catalyst, will increase pollution risk and processing cost and medicament thus, more cause a large amount of waste water to affect environment, not be perfect transesterificationSystem.
Though have many-sided research in solid-state catalyst transesterification, often catalyst must be fixed on porous carrier, allow reactionThing (triglyceride and methyl alcohol) the solid-state catalyst of flowing through reacts. It acquires a certain degree of difficulty because of porous material coating catalyst, and manyHole material, often easily because greasy dirt causes obstruction, reduces reaction table area, causes reaction passivation, transesterification rate variation. Secondly exist againWhen catalyst passivation, must reactivate, the polynary reuse of its material is difficult for, and activation has suitable difficulty, easily forms discarded object, is notA kind of good use pattern, market application is few, and as shown in Figure 2, its unique benefit is that reaction afterproduct can be straight to its response proceduresConnect and separate use, do not clean generation wastewater problem.
Aforementioned both different catalyst reaction patterns are all desirable not to the utmost, although biodiesel transesterification is not a new technology,Its response procedures research still can not escaped to this two patterns, its space that is greatly improved.
Application is proposed super in prior art CN1896183, CN101029243, CN1935947, CN1013072468Technology of acoustic wave and microwave technology are applied in the production process of biodiesel, and wherein ultrasonic technology is in order to increase emulsion dispersion effectReally, but also increase equipment cost and energy loss.
How improving reaction efficiency, reduce production costs and equipment builds cost, is a suitable important topic, more can accord withClose energy-saving, emission-reducing, environment friendly measure, reach cleaner production dreamboat.
Summary of the invention
The present invention is directed to the deficiencies in the prior art a kind of method and system that produce biodiesel are provided, to realize raisingReaction efficiency, reduces production costs and equipment builds cost, more can meet energy-saving, emission-reducing, environment friendly measure, reaches cleaner production idealThe object of target.
For reaching described object, technical scheme of the present invention is:
A kind of method for preparing biodiesel that produces, is characterized in that comprising the following steps:
(201) raw material is prepared: prepare triglyceride, methyl alcohol and catalyst; The wherein mol ratio of triglyceride and methyl alcoholFor 1:1-1:20, the weight ratio of catalyst and triglyceride is 0.5:100-10:100, and this catalyst is the following microminiaturization powder of 75 μ mThe solid-state catalyst of shape;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed with the solid-state catalyst out-phase of powdery, and powdery is solid-stateCatalyst is due to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and circulating through circulating pumpMore can fully mix, increase out-phase Contact area and time, and be easy to reclaim the solid-state catalyst of powdery;
(203) heating using microwave catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulation turnover microwave reactor carry outHeatable catalytic transesterification reaction, increases homogeneous heating between out-phase, accelerates transesterification reaction, and microwave frequency used is 2450MHz, temperature settingBe decided to be 30-80 DEG C, the circular response time is 5-30 minute;
(204) steam unnecessary methyl alcohol: after having reacted, application steams with the same heating using microwave catalytic reactor of transesterification reactionUnnecessary methyl alcohol, Temperature Setting is 65-100 DEG C, and the time is 5-20 minute, and methyl alcohol evaporation rate is accelerated in cycling, not only reclaimsMethyl alcohol also extends the reaction time makes transesterification reaction more complete;
(205) shift out filtration: after reaction, the solid-state catalyst of powdery can reach fast and directly catch through solid-state catalyst filterCatch catalyst to carry out reuse;
(206) stratification: product liquid forms the biological bavin in the upper strata separating after leaving standstill after catching the solid-state catalyst of powderyOil and lower floor's glycerine, time of repose is 0.5-2 hour;
(207) generate biodiesel finished product.
Recyclable the returning in former processing procedure raw material preparation process (201) of methyl alcohol that this step (204) steams used.
The solid-state catalyst of powdery that this step (205) directly catches through solid-state catalyst filter is recyclable returns former processing procedureIn raw material preparation process (201), use.
Based on a system for described product method for preparing biodiesel, comprising:
Heating using microwave catalytic reactor, in order to provide microwave energy and the temperature control of circular response thing, methanol stripper;
Continuity reactive evaporation device, in order to provide storage area and the methyl alcohol that reactant is come in and gone out heating using microwave catalytic reactor to steamSend out and remove space;
Circulation transport control system device, in order to provide reactant pan feeding, mixing, circulation and methanol eddy to carry;
Methanol Recovery condensing unit, in order to provide evaporation methanol condensed to reflux or to reclaim;
Standing separation device, has reacted and the standing separation of afterproduct is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst filter, in order to provide the recovery of having reacted the solid-state catalyst of rear powdery;
Described heating using microwave catalytic reactor by pipeline respectively with described continuity reactive evaporation device and described followingThe conducting that is tightly connected of ring transport control system device;
Described Methanol Recovery condensing unit by pipeline respectively with described continuity reactive evaporation device and described circulationThe conducting that is tightly connected of transport control system device;
Described solid-state catalyst filter by pipeline respectively with described circulation transport control system device and describedStanding separation device connects conducting.
This heating using microwave catalytic reactor main body is a column microwave reaction chamber; During this microwave reaction chamber uprightly arranges and isEmpty, to seal rigid structure, bottom is provided with microwave reaction entrance, and top is provided with microwave reaction outlet; This microwave reaction entersMouthful by the conducting that is tightly connected of pipeline and this circulation transport control system device; This microwave reaction exports by pipeline and this continuityThe conducting that is tightly connected of reactive evaporation device; In this microwave reaction chamber, be provided with the transesterification circulation line of curl; This microwave reactionOutside chamber, be evenly provided with a plurality of heating using microwave catalytic reactor drive units; One end of this transesterification circulation line and this microwave are anti-Answer inlet seal to connect conducting; This microwave reaction exit is provided with heatable catalytic temperature control module.
This continuity reactive evaporation device main body is a gyroscope-like or taper evaporation reactive tank; This evaporation reactive tank is upright arrange andFor the rigid structure of hollow, sealing, cone bottom is provided with reaction cycle outlet, and cone top part is provided with methanol vapor outlet, evaporationReactor inlet and the emergency vent that is connected with Safety control valve; This emergency vent that is connected with Safety control valve is positioned at thisBetween methanol vapor outlet and this evaporation reactor inlet; This evaporation reactor inlet is anti-by pipeline and this heating using microwave catalysisAnswer the device conducting that is tightly connected; The outlet of this reaction cycle is by the conducting that is tightly connected of pipeline and this circulation transport control system device;The outlet of this methanol vapor is by the conducting that is tightly connected of pipeline and this Methanol Recovery condensing unit; The outer wall of this evaporation reactive tank bottomBe connected with reactive evaporation thermometer.
This circulation transport control system device comprises pan feeding control valve, heating using microwave catalytic reactor transfer valve, and microwave addsHeat catalysis device return valve, leaves standstill transfer valve, circular response valve, circulating pump and methanol eddy valve;
Described circulating pump connects this standing transfer valve of conducting by pipeline, and this standing transfer valve connects conducting by pipelineThis solid-state catalyst filter;
Described circulating pump connects respectively this pan feeding control valve of conducting and methanol eddy valve by pipeline; This methanol eddy valveConnect this Methanol Recovery condensing unit of conducting by pipeline;
Described pan feeding control valve connects conducting methyl alcohol, the input port of triglyceride and catalyst;
Described circulating pump connects this circular response valve of conducting by pipeline; This circular response valve connects conducting by pipelineThis continuity reactive evaporation device;
Described circulating pump connects respectively this heating using microwave catalytic reactor return valve of conducting by pipeline and this microwave addsHeat catalysis device transfer valve; This heating using microwave catalytic reactor transfer valve by pipeline respectively with this heating using microwave catalytic reactionDevice is connected conducting with this heating using microwave catalytic reactor return valve; The company of this heating using microwave catalytic reactor return valve connecting lineContact connects at this heating using microwave catalytic reactor between the connecting line of this heating using microwave catalytic reactor transfer valve; This is micro-Ripple heatable catalytic reactor transfer valve connects conducting outlet.
This Methanol Recovery condensing unit comprises methanol eddy outlet, Methanol Recovery valve, and methyl alcohol heat-exchange device and methyl alcohol steamGas intake; One end of this methyl alcohol heat-exchange device connects conducting this methanol vapor intake is set, and the other end connects conducting and establishesPut this methanol eddy outlet; This methanol vapor intake is connected conducting with this continuity reactive evaporation device; This methanol eddy outlet is logicalThe connecting line that is provided with the threeway mouth of pipe in the middle of crossing connects this circulation transport control system device of conducting; This Methanol Recovery valve one endBe connected conducting with the described threeway mouth of pipe, the other end connects conducting methyl alcohol delivery outlet.
This standing separation device main body is a gyroscope-like standing separation groove; This standing separation groove uprightly arranges and is hollow, closeThe rigid structure of envelope; Top-shaped bottom is connected conducting by pipeline with glycerine outlet valve; Top-shaped middle part arranges biological bavinThis biodiesel outlet of oil export is connected conducting by pipeline with biodiesel outlet valve; The cell wall of this standing separation groove is provided withLayering indicating window; This top-shaped top of standing separation groove arranges and leaves standstill liquid entrance; This standing liquid entrance is solid by pipeline and thisState catalyst filter connects conducting.
This solid-state catalyst filter comprises solid-state catalyst output-controlling device, catalyst outlet, and catalyst filtering module, is filtered intoMouth and filtering outlet; This catalyst filtering module is upright setting, and top is provided with filtering outlet, and bottom is provided with catalyst outlet,Side is provided with filtration entrance; This filtering outlet is connected conducting by pipeline with this standing separation device; This filtration entrance is by pipeRoad is connected conducting with this circulation transport control system; This catalyst exports by one of pipeline and this solid-state catalyst output-controlling deviceEnd connects conducting; The other end of this solid-state catalyst output-controlling device connects the solid-state catalyst delivery outlet of conducting.
Adopt technical scheme of the present invention first owing to having simplified the production routine of biodiesel, improve transesterification reaction effectRate, the solid-state catalyst of application powdery reaction transesterification, gets rid of original solid-state catalyst carrier facility, allows the solid-state catalyst one of reactant and powderyAnd circulation, except can maintain the large advantage of the solid-state catalyst contact area of powdery, also can allow more simplification of consersion unit. Build and liquid stateCatalyst same reaction mode, allows solid-state catalyst directly mix directly reaction with reactant, increases reaction time and area, improves anti-Answer efficiency, get rid of only reaction disappearance on carrier of solid-state catalyst.
Its two, built high efficiency, share multi-functional heating using microwave module, utilize heating using microwave and catalytic anti-Should, improve transesterification efficiency, see through microwave and vibrate and can improve transesterification effect at a high speed, at more applied microwave heating Quick of reaction back segmentHigh-temperature allows unnecessary methyl alcohol directly in reactive tank, steam and to remove, and sees through circulating-heating mode and reaches reaction and fast eliminating methyl alcoholObject, reduces energy loss and shortens the processing procedure time, allows transesterification and methanol removal can share same group of heater, reaches equipment letterChange and shorten the effect of processing procedure.
Its three, with the reaction of the solid-state catalyst of powdery, exempt back segment catalyst and reclaim and discharge of wastewater object, product and catalystApply simple and easy Shen and fall pattern direct layering, upper strata is biodiesel, and lower floor is glycerine, and sediment is catalyst, or catalyst also can be firstSee through filter and take out the solid-state catalyst of powdery. Catalyst can repeatedly use, also can direct activation, there is no carrier impurity, and can be lightEasily recycling utilization, reaches energy-saving and emission-reduction cleaning operation target.
In sum, technical scheme of the present invention is owing to further having improved original blind spot, and application microminiaturization catalyst, mixesIn reactant, not only can mix with reactant circulation, and can increase transesterification reaction, more have to flow to heating using microwave with reactant and urgeChange device, can see through the catalysis of the direct-type higher-order of oscillation and heating, more can add fast response, make reaction more thorough, and then shorten while reactionBetween, setting up solid-state catalyst has the same fast reaction effect of liquid catalyst, and has solid-state catalyst system capable environmental protection advantage, can effectively changeKind production routine, enhances productivity.
Brief description of the drawings
Fig. 1 is conventional liquid soda acid catalyst transesterification schematic flow sheet;
Fig. 2 is conventional solid-state catalyst transesterification schematic flow sheet;
Fig. 3 is that the present invention innovates the schematic flow sheet that produces method for preparing biodiesel;
Fig. 4 is that the present invention innovates the system architecture schematic diagram that produces biodiesel.
Number in the figure explanation
1. methyl alcohol 2. triglycerides
3. catalyst
5. biodiesel 6. glycerine
10. heating using microwave catalytic reactor
11. heating using microwave catalytic reactor drive unit 12. heatable catalytic temperature control modules
13. microwave reaction chamber 14. microwave reaction entrances
15. microwave reactions export 16. transesterification circulation lines
20. continuity reactive evaporation devices
21. Safety control valve 22. reactive evaporation thermometers
23. methanol vapor export 24. reaction cycle outlets
25. evaporation reactive tanks 26. evaporate reactor inlet
30. circulation transport control systems
31. pan feeding control valves
33. heating using microwave catalytic reactor transfer valve 34. heating using microwave catalytic reactor return valves
35. leave standstill transfer valve 36. circular response valves
37. circulating pump 38. methanol eddy valves
40. Methanol Recovery condensing units
41. methanol eddies export 42. Methanol Recovery delivery valves
43. methyl alcohol heat-exchange device 44. methanol vapor intakes
50. standing separation devices
51. biodiesel outlet valve 52. glycerine outlet valves
53. layering indicating window 54. standing separation grooves
55. leave standstill liquid entrance
60. solid-state catalyst filters
61. solid-state catalyst output-controlling device 62. catalyst outlets
63. catalyst filtering modules 64. filter entrance
65. filtering outlets
Detailed description of the invention
Below in conjunction with accompanying drawing, method and system structure of the present invention is described in detail as follows.
As shown in Figure 3, a kind of method for preparing biodiesel that produces, is characterized in that comprising the following steps:
(201) raw material is prepared: prepare triglyceride, methyl alcohol and catalyst; The wherein mol ratio of triglyceride and methyl alcoholFor 1:1-1:20, the better mol ratio of this triglyceride and methyl alcohol is 1:9; The weight ratio of catalyst and triglyceride is 0.5:100-10:100, the better weight ratio of this catalyst and triglyceride is 7:100; This catalyst is that the following microminiaturization powdery of 75 μ m is solidState catalyst;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed with the solid-state catalyst out-phase of powdery, and powdery is solid-stateCatalyst is due to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and circulating through circulating pumpMore can fully mix, increase out-phase Contact area and time, and be easy to reclaim the solid-state catalyst of powdery;
(203) heating using microwave catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulation turnover microwave reactor carry outHeatable catalytic transesterification reaction, increases homogeneous heating between out-phase, accelerates transesterification reaction, and microwave frequency used is 2450MHz, temperature settingBe decided to be 30-80 DEG C, preferred temperature is set as 50 DEG C; The circular response time is 5-30 minute, and preferably the circular response time is 26Minute;
(204) steam unnecessary methyl alcohol: after having reacted, application steams with the same heating using microwave catalytic reactor of transesterification reactionUnnecessary methyl alcohol, Temperature Setting is 65-100 DEG C, preferred temperature is set as 85 DEG C; Time is 5-20 minute, and the better time is 16 pointsClock; Methyl alcohol evaporation rate is accelerated in cycling, not only reclaims methyl alcohol and also extends the reaction time and make transesterification reaction more complete; SteamRecyclable the returning in former processing procedure raw material preparation process (201) of methyl alcohol used.
(205) shift out filtration: after reaction, the solid-state catalyst of powdery can reach fast and directly catch through solid-state catalyst filterCatch catalyst to carry out reuse; The solid-state catalyst of powdery that directly catches through solid-state catalyst filter is recyclable, and to return former processing procedure formerIn material preparation process (201), use.
(206) stratification: product liquid forms the biological bavin in the upper strata separating after leaving standstill after catching the solid-state catalyst of powderyOil and lower floor's glycerine, time of repose is 0.5-2 hour;
(207) generate biodiesel finished product.
As shown in Figure 4, a kind of system based on above-mentioned product method for preparing biodiesel, comprising:
Heating using microwave catalytic reactor 10, in order to provide microwave energy and the temperature control of circular response thing, methanol stripper;
Continuity reactive evaporation device 20, in order to the storage area and the methyl alcohol that provide reactant to come in and go out heating using microwave catalytic reactorEvaporation removes space;
Circulation transport control system device 30, in order to provide reactant pan feeding, mixing, circulation and methanol eddy to carry;
Methanol Recovery condensing unit 40, in order to provide evaporation methanol condensed to reflux or to reclaim;
Standing separation device 50, has reacted and the standing separation of afterproduct is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst filter 60, in order to provide the recovery of having reacted the solid-state catalyst of rear powdery;
Described heating using microwave catalytic reactor 10 by pipeline respectively with described continuity reactive evaporation device 20 and described inCirculation transport control system device 30 conducting that is tightly connected;
Described Methanol Recovery condensing unit 40 by pipeline respectively with described continuity reactive evaporation device 20 and describedCirculation transport control system device 30 conducting that is tightly connected;
Described solid-state catalyst filter 60 by pipeline respectively with described circulation transport control system device 30 and instituteThe standing separation device 50 of stating connects conducting.
This heating using microwave catalytic reactor 10 is to have heating using microwave catalytic reactor drive unit 11, microwave reaction chamber 13,Heatable catalytic temperature control module 12, microwave reaction entrance 14, microwave reaction outlet 15 and transesterification circulation line 16 are formed by combining, profitIntroduce and react with circulating pump 37. These heating using microwave catalytic reactor 10 main bodys are a column microwave reaction chamber 13; This microwave reactionChamber 13 uprightly arranges and is the rigid structure of hollow, sealing, and bottom is provided with microwave reaction entrance 14, and it is anti-that top is provided with microwaveShould export 15; This microwave reaction entrance 14 is by the conducting that is tightly connected of pipeline and this circulation transport control system device 30; This is micro-Ripple reaction outlet 15 is by the conducting that is tightly connected of pipeline and this continuity reactive evaporation device 20; In this microwave reaction chamber 13, be provided with intoSpiral helicine transesterification circulation line 16; This transesterification circulation line 16 is apply nonmetal and can build by the more than 100 DEG C material of heatproof,Object is to allow microwave penetration, allows reactant heat and catalysis. This microwave reaction chamber 13 is outer to be evenly provided with a plurality of microwaves and to addHeat catalysis device drive unit 11; The heating using microwave catalytic reactor drive unit 11 being arranged on outside this microwave reaction chamber 13 canBe the setting of even annular also can be evenly between wrong annular arrange; One end of this transesterification circulation line 16 and this microwave reaction entrance 14Conducting is tightly connected; This microwave reaction exports 15 places and is provided with heatable catalytic temperature control module 12.
This continuity reactive evaporation device 20: the storage area and the methyl alcohol that provide reactant to come in and go out heating using microwave catalytic reactor 10Evaporation removes space; This continuity reactive evaporation device 20 is by evaporation reactive tank 25, evaporation reactor chamber entrance 26, Safety control valve21, reactive evaporation thermometer 22, methanol vapor outlet 23 and reaction cycle outlet 24 combine. This continuity reactive evaporation device 20Main body is a gyroscope-like or taper evaporation reactive tank 25; The upright rigidity knot that arranges and be hollow, sealing of this evaporation reactive tank 25Structure, cone bottom is provided with reaction cycle outlet 24, and cone top part is provided with methanol vapor outlet 23, evaporates reactor inlet 26 and connectsBe connected to the emergency vent of Safety control valve 21; This emergency vent that is connected with Safety control valve 21 is positioned at this methanol vapor and goes outBetween mouth 23 and this evaporation reactor inlet 26; This evaporation reactor inlet 26 is by pipeline and this heating using microwave catalytic reactor10 conductings that are tightly connected; This reaction cycle outlet 24 is tightly connected and is led by pipeline and this circulation transport control system device 30Logical; The outlet 23 of this methanol vapor is by the conducting that is tightly connected of pipeline and this Methanol Recovery condensing unit 40; This evaporation reactive tank 25The outer wall of bottom is connected with reactive evaporation thermometer 22.
This circulation transport control system device 30 comprises pan feeding control valve 31, heating using microwave catalytic reactor transfer valve 33,Heating using microwave catalytic reactor return valve 34, leaves standstill transfer valve 35, circular response valve 36, circulating pump 37 and methanol eddy valve 38;
Described circulating pump 37 connects this standing transfer valve 35 of conducting by pipeline, and this standing transfer valve 35 connects by pipelineConnect this solid-state catalyst filter 60 of conducting;
Described circulating pump 37 connects respectively this pan feeding control valve 31 of conducting and methanol eddy valve 38 by pipeline; This methyl alcoholReturn valve 38 connects this Methanol Recovery condensing unit 40 of conducting by pipeline;
Described pan feeding control valve 31 connects conducting methyl alcohol, the input port of triglyceride and catalyst;
Described circulating pump 37 connects this circular response valve 36 of conducting by pipeline; This circular response valve 36 connects by pipelineConnect this continuity reactive evaporation device 20 of conducting;
It is micro-with this that described circulating pump 37 connects respectively this heating using microwave catalytic reactor return valve 34 of conducting by pipelineRipple heatable catalytic reactor transfer valve 33; This heating using microwave catalytic reactor transfer valve 33 by pipeline respectively with this heating using microwaveCatalytic reactor 10 is connected conducting with this heating using microwave catalytic reactor return valve 34; This heating using microwave catalytic reactor return valveThe tie point of 34 connecting lines is positioned at this heating using microwave catalytic reactor 10 and connects this heating using microwave catalytic reactor transfer valve 33Connecting line between; This heating using microwave catalytic reactor transfer valve 33 connects conducting outlet.
This Methanol Recovery condensing unit 40 comprises methanol eddy outlet 41, Methanol Recovery valve 42, methyl alcohol heat-exchange device 43And methanol vapor intake 44; One end of this methyl alcohol heat-exchange device 43 connects conducting this methanol vapor intake 44 is set, anotherOne end connects conducting this methanol eddy outlet 41 is set; This methanol vapor intake 44 is connected and leads with this continuity reactive evaporation device 20Logical; The connecting line that this methanol eddy outlet 41 is provided with the threeway mouth of pipe by centre connects this circulation transport control system of conductingDevice 30; These Methanol Recovery valve 42 one end are connected conducting with the described threeway mouth of pipe, and the other end connects conducting methyl alcohol delivery outlet.
This standing separation device 50; Provide and reacted and the standing separation of afterproduct is reclaimed in methyl alcohol evaporation; This standing separationDevice 50 is by biodiesel outlet valve 51, glycerine outlet valve 52, stratification indicating window 53, standing separation groove 54 and standing liquid(drawing) entrance 55 grades are combined into. These standing separation device 50 main bodys are a gyroscope-like standing separation groove 54; This standing separation groove 54Upright arrange and be the rigid structure of hollow, sealing; Top-shaped bottom is connected conducting by pipeline with glycerine outlet valve 52; TopThe middle part of spiral arranges biodiesel and exports the outlet of this biodiesel and be connected conducting by pipeline with biodiesel outlet valve 51; ShouldThe cell wall of standing separation groove 54 is provided with layering indicating window 53; This top-shaped top of standing separation groove 54 arranges and leaves standstill liquid entrance55; This standing liquid entrance 55 is connected conducting by the solid-state catalyst filter 60 of pipeline and this.
This solid-state catalyst filter 60 comprises solid-state catalyst output-controlling device 61, catalyst outlet 62, catalyst filtering module63, filter entrance 64 and filtering outlet 65; This catalyst filtering module 63 is upright setting, and top is provided with filtering outlet 65, the endEnd is provided with catalyst outlet 62, and side is provided with and filters entrance 64; This filtering outlet 65 is by pipeline and this standing separation device 50Connect conducting; This filtration entrance 64 is connected conducting by pipeline with this circulation transport control system 30; This catalyst outlet 62 is passed throughPipeline is connected conducting with one end of this solid-state catalyst output-controlling device 61; The other end of this solid-state catalyst output-controlling device 61Connect the solid-state catalyst delivery outlet of conducting.
The present invention implement time first by methyl alcohol 1, triglyceride 2 and catalyst 3, according to triglyceride and methyl alcohol moleThan being 1:1-1:20, the weight ratio of catalyst and triglyceride is that 0.5:100-10:100 ratio is mixed, and catalyst is below 75 μ mThe solid-state catalyst of microminiaturization powdery, utilizes circulating pump 37 and pan feeding control valve 31 to introduce and flows to heating using microwave catalytic reactor transfer valve33, enter heating using microwave catalytic reactor 10, through microwave reaction entrance 14, microwave reaction chamber 13 is to microwave reaction outlet 15, streamEvaporation reactor inlet 26 to continuity reactive evaporation device 20 flows into, and is stored in evaporation reactive tank 25, completes charging program, closesPan feeding control valve 31.
Enter heatable catalytic response procedures, ON cycle reactive valve 36, allows reactant (methyl alcohol 1+ triglyceride 2+ catalyst3) see through circulating pump 37 and flow to heating using microwave catalytic reactor 10, formation circulates. Further open heating using microwave catalysis anti-Answer device drive unit 11 to carry out heatable catalytic, microwave frequency used is 2450MHz, and Temperature Setting is 30-80 DEG C, and the reaction time is5-30min, allows reactant vibration form directly heating and catalysis transesterification reaction, and it utilizes heatable catalytic temperature control module 12, allows itBe controlled at best catalytic reaction temperature. And methyl alcohol 1 has evaporation situation in this temperature, application Methanol Recovery condensing unit 40, willMethanol vapor condensation, further applies methanol eddy valve 38 methanol liquid is drawn back into entering in reactant again, after completing reaction,Entering methyl alcohol steams except program.
Enter methyl alcohol and steam except program, further heatable catalytic temperature control module 12 is heightened to the above temperature of methyl alcohol boiling point, temperatureDegree is set as 65-100 DEG C, and the time is 5-20min, allows unnecessary methanol gasifying and shifting out fast, imports through methanol vapor outlet 23Methanol Recovery condensing unit 40, further applies methyl alcohol heat-exchange device 43, by methanol condensed, closes methanol eddy valve 38, opensOpen Methanol Recovery delivery valve 42 and draw unnecessary methyl alcohol, can be back in processing procedure, after methyl alcohol steams, close Methanol Recovery delivery valve42, close heating using microwave catalytic reactor drive unit 11, enter the reactant program that shifts out.
Enter the reactant program that shifts out, open and leave standstill transfer valve 35 in advance, further close heating using microwave catalytic reactionDevice transfer valve 33, further opens heating using microwave catalytic reactor return valve 34, utilizes circulating pump 37 gravitation, further will ownReactant moves to solid-state catalyst filter 60, and application catalyst filtering module 63 is placed in standing separation device 50 front ends and leaves standstill input35, valve leaches solid-state powdery catalyst, sees through solid-state catalyst output-controlling device 61 and draws through catalyst outlet 62, can reachDirectly catch catalyst. Can flow in the standing separation groove 54 of standing separation device 50 by product liquid, treat cleaning reaction systemReaction product is closed all control valves and circulating pump 37, completes response procedures. The program of leaving standstill, time of repose is that 0.5-2 is littleTime, product can form the biodiesel 5 on upper strata, and lower floor's glycerine 6 can be seen hierarchical scenario by layering indicating window 53, andBiodiesel 5 can be drawn with biodiesel outlet valve 51, and glycerine and catalyst can be drawn with glycerine outlet valve 52, and catches solidState catalyst can return processing procedure again and use, and reaches easily the target of production biodiesel.
Claims (9)
1. produce a system for method for preparing biodiesel, it is characterized in that comprising:
Heating using microwave catalytic reactor (10), in order to provide microwave energy and the temperature control of circular response thing, methanol stripper;
Continuity reactive evaporation device (20), in order to provide storage area and the methyl alcohol that reactant is come in and gone out heating using microwave catalytic reactor to steamSend out and remove space;
Circulation transport control system device (30), in order to provide reactant pan feeding, mixing, circulation and methanol eddy to carry;
Methanol Recovery condensing unit (40), in order to provide evaporation methanol condensed to reflux or to reclaim;
Standing separation device (50), has reacted and the standing separation of afterproduct is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst filter (60), in order to provide the recovery of having reacted the solid-state catalyst of rear powdery;
Described heating using microwave catalytic reactor (10) by pipeline respectively with described continuity reactive evaporation device (20) and described inCirculation transport control system device (30) conducting that is tightly connected;
Described Methanol Recovery condensing unit (40) by pipeline respectively with described continuity reactive evaporation device (20) and describedCirculation transport control system device (30) conducting that is tightly connected;
Described solid-state catalyst filter (60) by pipeline respectively with described circulation transport control system device (30) and instituteThe standing separation device (50) of stating connects conducting;
This circulation transport control system device (30) comprises pan feeding control valve (31), heating using microwave catalytic reactor transfer valve(33), heating using microwave catalytic reactor return valve (34), leaves standstill transfer valve (35), circular response valve (36), circulating pump (37) andMethanol eddy valve (38);
Described circulating pump (37) connects this standing transfer valve (35) of conducting by pipeline, and this standing transfer valve (35) passes through pipelineConnect this solid-state catalyst filter (60) of conducting;
Described circulating pump (37) connects respectively this pan feeding control valve (31) of conducting and methanol eddy valve (38) by pipeline; This firstAlcohol reflux valve (38) connects this Methanol Recovery condensing unit (40) of conducting by pipeline;
Described pan feeding control valve (31) connects conducting methyl alcohol, the input port of triglyceride and catalyst;
Described circulating pump (37) connects this circular response valve (36) of conducting by pipeline; This circular response valve (36) passes through pipelineConnect this continuity reactive evaporation device (20) of conducting;
Described circulating pump (37) connects respectively this heating using microwave catalytic reactor return valve (34) of conducting by pipeline and this is micro-Ripple heatable catalytic reactor transfer valve (33); This heating using microwave catalytic reactor transfer valve (33) by pipeline respectively with this microwaveHeatable catalytic reactor (10) is connected conducting with this heating using microwave catalytic reactor return valve (34); This heating using microwave catalytic reactionThe tie point of device return valve (34) connecting line is positioned at this heating using microwave catalytic reactor (10), and to connect this heating using microwave catalysis anti-Answer between the connecting line of device transfer valve (33); This heating using microwave catalytic reactor transfer valve (33) connects conducting outlet.
2. adopt a product method for preparing biodiesel for system as claimed in claim 1, it is characterized in that comprising the following steps:
(201) raw material is prepared: prepare triglyceride, methyl alcohol and catalyst; Wherein the mol ratio of triglyceride and methyl alcohol is 1:1-1:20, the weight ratio of catalyst and triglyceride is 0.5:100-10:100, this catalyst is that the following microminiaturization powdery of 75 μ m is solidState catalyst;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed to the solid-state catalyst of powdery with the solid-state catalyst out-phase of powderyDue to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and more can through circulating of circulating pumpFully mix, increase out-phase Contact area and time, and be easy to reclaim the solid-state catalyst of powdery;
(203) heating using microwave catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulation turnover microwave reactor heatCatalysis transesterification reaction, increases homogeneous heating between out-phase, accelerates transesterification reaction, and microwave frequency used is 2450MHz, and Temperature Setting is30-80 DEG C, the circular response time is 5-30 minute;
(204) steam unnecessary methyl alcohol: after having reacted, it is unnecessary that application and the same heating using microwave catalytic reactor of transesterification reaction steamMethyl alcohol, Temperature Setting is 65-100 DEG C, and the time is 5-20 minute, and methyl alcohol evaporation rate is accelerated in cycling, not only reclaims methyl alcoholAlso extending the reaction time makes transesterification reaction more complete;
(205) shift out filtration: after reaction the solid-state catalyst of powdery through solid-state catalyst filter reach directly catch fast catalyst withCarry out reuse;
(206) stratification: after catching powdery solid-state catalyst product liquid after leaving standstill, form the upper strata biodiesel that separates andLower floor's glycerine, time of repose is 0.5-2 hour;
(207) generate biodiesel finished product.
3. product method for preparing biodiesel as claimed in claim 2, is characterized in that the methyl alcohol that this step (204) steams is recyclableReturn in former processing procedure raw material preparation process (201) and use.
4. product method for preparing biodiesel as claimed in claim 2, is characterized in that this step (205) is through solid-state catalyst filtrationRecyclable the returning in former processing procedure raw material preparation process (201) of the solid-state catalyst of powdery that device directly catches used.
5. the system as claimed in claim 1, is characterized in that this heating using microwave catalytic reactor (10) main body is that a column is micro-Ripple reaction chamber (13); This microwave reaction chamber (13) uprightly arranges and is the rigid structure of hollow, sealing, and it is anti-that bottom is provided with microwaveAnswer entrance (14), top is provided with microwave reaction outlet (15); This microwave reaction entrance (14) is carried by pipeline and this circulationControl system device (30) conducting that is tightly connected; This microwave reaction outlet (15) is by pipeline and this continuity reactive evaporation device (20)Conducting is tightly connected; In this microwave reaction chamber (13), be provided with the transesterification circulation line (16) of curl; This microwave reaction chamber(13) the outer a plurality of heating using microwave catalytic reactor drive units (11) that are evenly provided with; One end of this transesterification circulation line (16)With the conducting that is tightly connected of this microwave reaction entrance (14); This microwave reaction outlet (15) locates to be provided with heatable catalytic temperature control module(12)。
6. the system as claimed in claim 1, is characterized in that this continuity reactive evaporation device (20) main body is a gyroscope-like or coneShape evaporation reactive tank (25); This evaporation reactive tank (25) uprightly arranges and is the rigid structure of hollow, sealing, and cone bottom is provided withReaction cycle outlet (24), cone top part is provided with methanol vapor outlet (23), evaporates reactor inlet (26) and is connected with safetyThe emergency vent of control valve (21); This emergency vent that is connected with Safety control valve (21) is positioned at this methanol vapor outlet(23) and between this evaporation reactor inlet (26); This evaporation reactor inlet (26) is anti-by pipeline and this heating using microwave catalysisAnswer device (10) conducting that is tightly connected; This reaction cycle outlet (24) is close by pipeline and this circulation transport control system device (30)Envelope connects conducting; This methanol vapor outlet (23) is by the conducting that is tightly connected of pipeline and this Methanol Recovery condensing unit (40); ShouldThe outer wall of evaporation reactive tank (25) bottom is connected with reactive evaporation thermometer (22).
7. the system as claimed in claim 1, is characterized in that this Methanol Recovery condensing unit (40) comprises methanol eddy outlet(41), Methanol Recovery valve (42), methyl alcohol heat-exchange device (43) and methanol vapor intake (44); This methyl alcohol heat-exchange device(43) one end connects conducting this methanol vapor intake (44) is set, and the other end connects conducting this methanol eddy outlet is set(41); This methanol vapor intake (44) is connected conducting with this continuity reactive evaporation device (20); This methanol eddy outlet (41) is logicalThe connecting line that is provided with the threeway mouth of pipe in the middle of crossing connects this circulation transport control system device (30) of conducting; This Methanol Recovery valve(42) one end is connected conducting with the described threeway mouth of pipe, and the other end connects conducting methyl alcohol delivery outlet.
8. the system as claimed in claim 1, is characterized in that this standing separation device (50) main body is a gyroscope-like standing separationGroove (54); This standing separation groove (54) uprightly arranges and is the rigid structure of hollow, sealing; Top-shaped bottom by pipeline withGlycerine outlet valve (52) connects conducting; Top-shaped middle part arranges biodiesel and exports this biodiesel and export by pipeline and lifeThing diesel oil outlet valve (51) connects conducting; The cell wall of this standing separation groove (54) is provided with layering indicating window (53); This leaves standstill and dividesArrange from the top-shaped top of groove (54) and leave standstill liquid entrance (55); This standing liquid entrance (55) is by pipeline and this solid-state catalyst mistakeFilter (60) connects conducting.
9. the system as claimed in claim 1, is characterized in that this solid-state catalyst filter (60) comprises solid-state catalyst output controlDevice processed (61), catalyst outlet (62), catalyst filtering module (63), filters entrance (64) and filtering outlet (65); This catalyst mistakeFilter module (63) is upright setting, and top is provided with filtering outlet (65), and bottom is provided with catalyst outlet (62), and side is provided withFilter entrance (64); This filtering outlet (65) is connected conducting by pipeline with this standing separation device (50); This filtration entrance (64)Be connected conducting by pipeline with this circulation transport control system device (30); This catalyst outlet (62) is by pipeline and this solid-state touchingOne end of matchmaker's output-controlling device (61) connects conducting; It is solid that the other end of this solid-state catalyst output-controlling device (61) connects conductingState catalyst delivery outlet.
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| CN201410538021.9A CN104357098B (en) | 2014-10-13 | 2014-10-13 | Produce the method and system of biodiesel |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029243A (en) * | 2007-01-22 | 2007-09-05 | 湘潭大学 | Production of biological diesel oil |
| CN101058734A (en) * | 2007-05-31 | 2007-10-24 | 张付舜 | Device for industrially synthesizing biological diesel oil by microwave and method thereof |
| US20080173532A1 (en) * | 2007-01-24 | 2008-07-24 | Zhonghua John Zhu | Method and system for producing a hydrogen enriched fuel using microwave assisted methane decomposition on catalyst |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029243A (en) * | 2007-01-22 | 2007-09-05 | 湘潭大学 | Production of biological diesel oil |
| US20080173532A1 (en) * | 2007-01-24 | 2008-07-24 | Zhonghua John Zhu | Method and system for producing a hydrogen enriched fuel using microwave assisted methane decomposition on catalyst |
| CN101058734A (en) * | 2007-05-31 | 2007-10-24 | 张付舜 | Device for industrially synthesizing biological diesel oil by microwave and method thereof |
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