CN104357098A - Method and system for producing biodiesel - Google Patents
Method and system for producing biodiesel Download PDFInfo
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- CN104357098A CN104357098A CN201410538021.9A CN201410538021A CN104357098A CN 104357098 A CN104357098 A CN 104357098A CN 201410538021 A CN201410538021 A CN 201410538021A CN 104357098 A CN104357098 A CN 104357098A
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000003225 biodiesel Substances 0.000 title claims abstract description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 465
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- 238000010438 heat treatment Methods 0.000 claims abstract description 84
- 238000005809 transesterification reaction Methods 0.000 claims abstract description 42
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 33
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000376 reactant Substances 0.000 claims abstract description 19
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims description 108
- 238000001704 evaporation Methods 0.000 claims description 65
- 230000008020 evaporation Effects 0.000 claims description 65
- 238000000926 separation method Methods 0.000 claims description 39
- 239000011949 solid catalyst Substances 0.000 claims description 31
- 239000002551 biofuel Substances 0.000 claims description 30
- 238000011084 recovery Methods 0.000 claims description 30
- 238000012546 transfer Methods 0.000 claims description 30
- 238000001914 filtration Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 20
- 235000011187 glycerol Nutrition 0.000 claims description 13
- 230000003197 catalytic effect Effects 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000839 emulsion Substances 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
- 239000000203 mixture Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 4
- 239000007787 solid Substances 0.000 abstract 3
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000000047 product Substances 0.000 description 10
- 230000004044 response Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 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
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect 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
- 239000002244 precipitate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material 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 method and a system for producing biodiesel, and belongs to the technical field of methods for producing the biodiesel and system device structures for producing the biodiesel with the methods. The method comprises steps as follows: a powdery solid contact agent, triglyceride and methyl alcohol are mixed for circulation and have the catalytic reaction by means of a microwave heating mechanism, and the purpose of transesterification can be rapidly achieved; the heating temperature is directly increased after transesterification, so that methyl alcohol is steamed out, separated, condensed by a heat exchanger and recycled; and reactants are directly moved out of the reaction system after methyl alcohol is moved out, and the biodiesel, glycerinum and the powdery solid contact agent can be directly separated out. With the adoption of the method and the system for producing the biodiesel, the transesterification reaction efficiency of the solid contact agent is improved, the procedure for removing the contact agent through washing is omitted, the production cost is reduced, and a production process meeting requirements of energy conservation, emission reduction and environment protection is achieved.
Description
Technical field
The present invention relates to a kind of method and system producing biofuel, belong to the technical field of the method and system apparatus structure of production chemical product, belong to the technical field of the system apparatus arrangements of method and the Using such method manufacturing biofuel manufacturing biofuel specifically.
Background technology
Traditional biological diesel oil mainly uses liquid alkali catalyst (catalyst also claims catalyzer) to react in the majority, generally uses sodium hydroxide (NaOH) to be main.Its response procedures as shown in Figure 1, triglyceride, methyl alcohol and catalyst is utilized to carry out catalysis transesterification reaction, due to generally comparatively high temps and pressure must be had when reacting, and then have people to apply ultrasound or microwave to accelerate katalysis, accelerate transesterification speed, and its product can remain sodium hydroxide (NaOH) catalyst, must first carry out removing sodium hydroxide (NaOH) catalyst, Pollution risk and processing cost and medicament will be increased thus, more causing a large amount of waste water to affect environment, is not perfect transesterification system.
Though have many-sided research in solid-state catalyst transesterification, often catalyst must be fixed on porous support, allow reactant (triglyceride and methyl alcohol) flow through solid-state catalyst and react.It acquires a certain degree of difficulty because porous material is coated to catalyst, and porous material is often easy causes obstruction because of greasy dirt, and reduce reaction table area, cause reaction passivation, transesterification rate is deteriorated.Thirdly must reactivate when catalyst passivation, the polynary reuse of its material not easily, activation has suitable difficulty, easy formation waste, be not a kind of good using forestland, market application is few, and its response procedures as shown in Figure 2, its unique benefit is that reaction after product directly can be separated use, does not clean generation wastewater problem.
Both different catalyst reaction patterns aforementioned are desirable all not to the utmost, although biofuel transesterification is not a new technology, still can not escape this two patterns, its space that is greatly improved to the research of its response procedures.
Using ultrasonic technology and microwave technique application are proposed in prior art CN 1896183, CN 101029243, CN 1935947, CN 1013072468 in the production process of biofuel, wherein ultrasonic technology is in order to increase emulsion dispersion effect, but also increases equipment cost and energy loss.
How improving reaction efficiency, reduction production cost and equipment build cost, are suitable important topics, more can meet 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 and provide a kind of method and system producing biofuel, to realize improving reaction efficiency, reduction production cost and equipment build cost, more can meet energy-saving, emission-reducing, environment friendly measure, reach the object of cleaner production dreamboat.
For reaching described object, technical scheme of the present invention is:
One produces biodiesel process, it is characterized in that comprising the following steps:
(201) raw material prepares: prepare triglyceride, methyl alcohol and catalyst; Wherein the mol ratio of triglyceride and methyl alcohol is 1:1-1:20, and the weight ratio of catalyst and triglyceride is 0.5:100-10:100, and this catalyst is less than 75 μm microminiaturization pulverized solid catalyst;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed with pulverized solid catalyst out-phase, pulverized solid catalyst is due to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and more can fully mix through circulating of recycle pump, increase out-phase Contact area and time, and be easy to reclaim pulverized solid catalyst;
(203) microwave heating catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulate and pass in and out microwave reactor and carry out heatable catalytic transesterification reaction, increase homogeneous heating between out-phase, accelerate transesterification reaction, microwave frequency used is 2450MHz, temperature is set as 30-80 DEG C, and the circulating reaction time is 5-30 minute;
(204) unnecessary methyl alcohol is steamed: after having reacted, application and transesterification reaction same microwave heating catalyticreactor steam unnecessary methyl alcohol, temperature is set as 65-100 DEG C, time is 5-20 minute, methyl alcohol vaporator rate is accelerated in cyclical operation, not only reclaims methyl alcohol and also extends the reaction times and make transesterification reaction more complete;
(205) filtration is shifted out: after reaction, pulverized solid catalyst can reach through solid-state catalyst strainer and directly catch catalyst fast to carry out reuse;
(206) stratification: form upper strata biofuel and lower floor's glycerine of separation after leaving standstill through catching product liquid after pulverized solid catalyst, time of repose is 0.5-2 hour;
(207) biofuel finished product is generated.
Recyclable the returning in former processing procedure raw material preparation step (201) of the methyl alcohol that this step (204) steams uses.
Recyclable the returning in former processing procedure raw material preparation step (201) of pulverized solid catalyst that this step (205) directly catches through solid-state catalyst strainer uses.
Based on the described system producing biodiesel process, comprising:
Microwave heating catalyticreactor, controls in order to the microwave energy and temperature providing circulating reaction thing, methanol stripper;
Continuity reactive evaporation device, the storage area of coming in and going out microwave heating catalyticreactor in order to provide reactant and methyl alcohol evaporation remove space;
Circulation transport control system device, in order to provide reactant pan feeding, mixing, circulation and methanol eddy conveying;
Methanol Recovery condensing works, in order to provide Evaporation of methanol condensation to carry out refluxing or reclaiming;
Standing separation device, to have reacted and the standing separation of after product is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst strainer, in order to provide the recovery of having reacted rear pulverized solid catalyst;
Described microwave heating catalyticreactor to be tightly connected with described continuity reactive evaporation device and described circulation transport control system device conducting respectively by pipeline;
Described Methanol Recovery condensing works to be tightly connected with described continuity reactive evaporation device and described circulation transport control system device conducting respectively by pipeline;
Described solid-state catalyst strainer is connected conducting with described circulation transport control system device and described standing separation device respectively by pipeline.
This microwave heating catalyticreactor main body is a column microwave reaction chamber; This microwave reaction chamber uprightly arrange and for hollow, sealing rigid structure, bottom is provided with microwave reaction entrance, top be provided with microwave reaction outlet; This microwave reaction entrance to be tightly connected conducting by pipeline and this circulation transport control system device; The outlet of this microwave reaction to be tightly connected conducting by pipeline and this continuity reactive evaporation device; The transesterification circulation line of curl is provided with in this microwave reaction chamber; A plurality of microwave heating catalyticreactor drive unit is evenly provided with outside this microwave reaction chamber; One end of this transesterification circulation line is connected conducting with this microwave reaction inlet seal; 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 uprightly arranges and is the rigid structure of hollow, sealing, and cone bottom is provided with reaction cycle outlet, and cone top part is provided with methanol vapor outlet, evaporation reactor inlet and be connected with the emergency vent of Safety control valve; This emergency vent being connected with Safety control valve is between the outlet of this methanol vapor and this evaporation reactor inlet; This evaporation reactor inlet to be tightly connected conducting by pipeline and this microwave heating catalyticreactor; The outlet of this reaction cycle to be tightly connected conducting by pipeline and this circulation transport control system device; The outlet of this methanol vapor to be tightly connected conducting by pipeline and this Methanol Recovery condensing works; The outer wall of this evaporation reactive tank bottom is connected with reactive evaporation thermometer.
This circulation transport control system device comprises pan feeding control valve, microwave heating catalyticreactor transfer valve, microwave heating catalyticreactor reverse flow valve, leaves standstill transfer valve, circulating reaction valve, recycle pump and methanol eddy valve;
Described recycle pump connects this standing transfer valve of conducting by pipeline, and this standing transfer valve connects this solid-state catalyst strainer of conducting by pipeline;
Described recycle pump connects this pan feeding control valve of conducting and methanol eddy valve respectively by pipeline; This methanol eddy valve connects this Methanol Recovery condensing works of conducting by pipeline;
Described pan feeding control valve connects conducting methyl alcohol, the input aperture of triglyceride and catalyst;
Described recycle pump connects this circulating reaction valve of conducting by pipeline; This circulating reaction valve connects this continuity reactive evaporation device of conducting by pipeline;
Described recycle pump connects this microwave heating catalyticreactor reverse flow valve of conducting and this microwave heating catalyticreactor transfer valve respectively by pipeline; This microwave heating catalyticreactor transfer valve is connected conducting with this microwave heating catalyticreactor and this microwave heating catalyticreactor reverse flow valve respectively by pipeline; The tie point of this microwave heating catalyticreactor reverse flow valve connecting pipeline connects between the connecting pipeline of this microwave heating catalyticreactor transfer valve at this microwave heating catalyticreactor; This microwave heating catalyticreactor transfer valve connects conducting relief outlet.
This Methanol Recovery condensing works comprises methanol eddy outlet, Methanol Recovery valve, methyl alcohol heat exchanger and methanol vapor intake; One end of this methyl alcohol heat exchanger connects conducting and arranges this methanol vapor intake, and the other end connects conducting and arranges the outlet of this methanol eddy; This methanol vapor intake is connected conducting with this continuity reactive evaporation device; The connecting pipeline that the outlet of this methanol eddy is provided with the threeway mouth of pipe by centre connects this circulation transport control system device of conducting; This Methanol Recovery valve one end is connected conducting with the described threeway mouth of pipe, and the other end connects conducting methyl alcohol delivery port.
This standing separation device main body is a gyroscope-like standing separation groove; This standing separation groove uprightly arrange and for hollow, sealing rigid structure; Top-shaped bottom is connected conducting by pipeline with glycerol outlet valve; Top-shaped middle part arrange biofuel export this biofuel outlet be connected conducting by pipeline with biofuel outlet valve; The cell wall of this standing separation groove is provided with layering indicating window; This top-shaped top of standing separation groove arranges standing liquid entrance; This standing liquid entrance is connected conducting by the solid-state catalyst strainer of pipeline and this.
This solid-state catalyst strainer comprises solid-state catalyst output-controlling device, and catalyst exports, catalyst filtration module, filters entrance and filtering outlet; This catalyst filtration module is upright setting, and top is provided with filtering outlet, and bottom is provided with catalyst outlet, and side is provided with filtration entrance; This filtering outlet is connected conducting by pipeline with this standing separation device; This filtration entrance is connected conducting by pipeline with this circulation transport control system; The outlet of this catalyst is connected conducting by one end of the solid-state catalyst output-controlling device of pipeline and this; The other end of this solid-state catalyst output-controlling device connects the solid-state catalyst delivery port of conducting.
Adopt technical scheme of the present invention first owing to simplifying the production sequence of biofuel, improve transesterification reaction efficiency, application pulverized solid catalyst reaction transesterification, get rid of original solid-state catalyst carrier facility, reactant and pulverized solid catalyst is allowed to circulate in the lump, except the large advantage of pulverized solid catalyst contact area can be maintained, conversion unit more simplification also can be allowed.Build and liquid catalyst same reaction mode, allow solid-state catalyst directly with reactant mixing direct reaction, increase reaction times and area, improve reaction efficiency, get rid of solid-state catalyst and only react on carrier and lack.
They are two years old, build high-level efficiency, share multi-functional microwave heating module, utilize microwave heating and catalytic reaction, improve transesterification efficiency, vibrate at a high speed through microwave and can improve transesterification effect, after the reaction section more applied microwave heating Quick high-temperature allow unnecessary methyl alcohol directly steam in reactive tank to remove, reaction and fast eliminating methyl alcohol object is reached through circulating-heating mode, reduce energy loss and shorten processing time, allow transesterification and methanol removal can share same group of well heater, reach the effect that equipment simplifies and shortens processing procedure.
Its three, with the reaction of pulverized solid catalyst, exempt back segment catalyst and reclaim and discharge of wastewater object, reaction product and catalyst are applied simple and easy Shen and are fallen pattern direct layering, and upper strata is biodiesel, and lower floor is glycerine, precipitate is catalyst, or catalyst also first can take out pulverized solid catalyst through filtration unit.Catalyst can repeatedly use, also can direct activation, does not have carrier impurity, can recycling utilization easily, reaches energy-saving and emission-reduction cleaning operation target.
In sum, technical scheme of the present invention is owing to further improving original blind spot, application microminiaturization catalyst, be mixed in reactant, not only can with reactant circulation mixing, and can transesterification reaction be increased, more have with reactant flow to microwave heating catalyst converter, through the catalysis of direct type HF oscillation and heating, more can add fast response, make reaction more thorough, and then Reaction time shorten, setting up solid-state catalyst has the same rapid reaction effect of liquid catalyst, and has solid-state catalyst system capable environmental advantages, effectively can improve production sequence, enhance productivity.
Accompanying drawing explanation
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 producing biodiesel process;
Fig. 4 is that the present invention innovates the system architecture schematic diagram producing biofuel.
Number in the figure explanation
1. methyl alcohol 2. triglyceride
3. catalyst
5. biofuel 6. glycerine
10. microwave heating catalyticreactor
11. microwave heating catalyticreactor 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. microwave heating catalyticreactor transfer valve 34. microwave heating catalyticreactor reverse flow valves
35. leave standstill transfer valve 36. circulating reaction valve
37. recycle pump 38. methanol eddy valves
40. Methanol Recovery condensing workss
41. methanol eddies export 42. Methanol Recovery delivery valves
43. methyl alcohol heat exchanger 44. methanol vapor intakes
50. standing separation devices
51. biofuel outlet valve 52. glycerol outlet valves
53. layering indicating window 54. standing separation grooves
55. leave standstill liquid entrance
60. solid-state catalyst strainers
61. solid-state catalyst output-controlling device 62. catalyst outlets
63. catalyst filtration modules 64. filter entrance
65. filtering outlets
Embodiment
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, one produces biodiesel process, it is characterized in that comprising the following steps:
(201) raw material prepares: prepare triglyceride, methyl alcohol and catalyst; Wherein the mol ratio of triglyceride and methyl alcohol is 1:1-1:20, and 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, and the better weight ratio of this catalyst and triglyceride is 7:100; This catalyst is less than 75 μm microminiaturization pulverized solid catalyst;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed with pulverized solid catalyst out-phase, pulverized solid catalyst is due to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and more can fully mix through circulating of recycle pump, increase out-phase Contact area and time, and be easy to reclaim pulverized solid catalyst;
(203) microwave heating catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulate and pass in and out microwave reactor and carry out heatable catalytic transesterification reaction, increase homogeneous heating between out-phase, accelerate transesterification reaction, microwave frequency used is 2450MHz, temperature is set as 30-80 DEG C, and preferred temperature is set as 50 DEG C; The circulating reaction time is 5-30 minute, and preferably the circulating reaction time is 26 minutes;
(204) steam unnecessary methyl alcohol: after having reacted, application and transesterification reaction same microwave heating catalyticreactor steam unnecessary methyl alcohol, and temperature is set as 65-100 DEG C, and preferred temperature is set as 85 DEG C; Time is 5-20 minute, and the better time is 16 minutes; Methyl alcohol vaporator rate is accelerated in cyclical operation, not only reclaims methyl alcohol and also extends the reaction times and make transesterification reaction more complete; Recyclable the returning in former processing procedure raw material preparation step (201) of the methyl alcohol steamed uses.
(205) filtration is shifted out: after reaction, pulverized solid catalyst can reach through solid-state catalyst strainer and directly catch catalyst fast to carry out reuse; Recyclable the returning in former processing procedure raw material preparation step (201) of pulverized solid catalyst directly caught through solid-state catalyst strainer uses.
(206) stratification: form upper strata biofuel and lower floor's glycerine of separation after leaving standstill through catching product liquid after pulverized solid catalyst, time of repose is 0.5-2 hour;
(207) biofuel finished product is generated.
As shown in Figure 4, a kind of based on the above-mentioned system producing biodiesel process, comprising:
Microwave heating catalyticreactor 10, controls in order to the microwave energy and temperature providing circulating reaction thing, methanol stripper;
Continuity reactive evaporation device 20, the storage area of coming in and going out microwave heating catalyticreactor in order to provide reactant and methyl alcohol evaporation remove space;
Circulation transport control system device 30, in order to provide reactant pan feeding, mixing, circulation and methanol eddy conveying;
Methanol Recovery condensing works 40, in order to provide Evaporation of methanol condensation to carry out refluxing or reclaiming;
Standing separation device 50, to have reacted and the standing separation of after product is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst strainer 60, in order to provide the recovery of having reacted rear pulverized solid catalyst;
Described microwave heating catalyticreactor 10 to be tightly connected with described continuity reactive evaporation device 20 and described circulation transport control system device 30 conducting respectively by pipeline;
Described Methanol Recovery condensing works 40 to be tightly connected with described continuity reactive evaporation device 20 and described circulation transport control system device 30 conducting respectively by pipeline;
Described solid-state catalyst strainer 60 is connected conducting with described circulation transport control system device 30 and described standing separation device 50 respectively by pipeline.
This microwave heating catalyticreactor 10 is have microwave heating catalyticreactor 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, and utilize recycle pump 37 to introduce reaction.This microwave heating catalyticreactor 10 main body is a column microwave reaction chamber 13; This microwave reaction chamber 13 uprightly arranges and be the rigid structure of hollow, sealing, and bottom is provided with microwave reaction entrance 14, and top is provided with microwave reaction and exports 15; This microwave reaction entrance 14 to be tightly connected conducting by pipeline and this circulation transport control system device 30; This microwave reaction outlet 15 to be tightly connected conducting by pipeline and this continuity reactive evaporation device 20; The transesterification circulation line 16 of curl is provided with in this microwave reaction chamber 13; This transesterification circulation line 16 is apply nonmetal and can build by heatproof more than 100 DEG C materials, and object to allow microwave penetration, allows reactant heat and catalysis.This microwave reaction chamber 13 is outer is evenly provided with a plurality of microwave heating catalyticreactor drive unit 11; Be arranged on microwave heating catalyticreactor drive unit 11 outside this microwave reaction chamber 13 to arrange in even annular and also can arrange in wrong annular between evenly; One end of this transesterification circulation line 16 and this microwave reaction entrance 14 are tightly connected conducting; 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 providing reactant to come in and go out microwave heating catalyticreactor 10 and methyl alcohol evaporation remove space; This continuity reactive evaporation device 20 is by evaporation reactive tank 25, evaporation reactor chamber entrance 26, Safety control valve 21, reactive evaporation thermometer 22, and methanol vapor outlet 23 and reaction cycle outlet 24 combine.This continuity reactive evaporation device 20 main body is a gyroscope-like or taper evaporation reactive tank 25; This evaporation reactive tank 25 uprightly arranges and be the rigid structure of hollow, sealing, and cone bottom is provided with reaction cycle outlet 24, and cone top part is provided with methanol vapor outlet 23, evaporation reactor inlet 26 and be connected with the emergency vent of Safety control valve 21; This emergency vent being connected with Safety control valve 21 is between this methanol vapor outlet 23 and this evaporation reactor inlet 26; This evaporation reactor inlet 26 to be tightly connected conducting by pipeline and this microwave heating catalyticreactor 10; This reaction cycle outlet 24 to be tightly connected conducting by pipeline and this circulation transport control system device 30; This methanol vapor outlet 23 to be tightly connected conducting by pipeline and this Methanol Recovery condensing works 40; The outer wall of this evaporation reactive tank 25 bottom is connected with reactive evaporation thermometer 22.
This circulation transport control system device 30 comprises pan feeding control valve 31, microwave heating catalyticreactor transfer valve 33, microwave heating catalyticreactor reverse flow valve 34, leaves standstill transfer valve 35, circulating reaction valve 36, recycle pump 37 and methanol eddy valve 38;
Described recycle pump 37 connects this standing transfer valve 35 of conducting by pipeline, and this standing transfer valve 35 connects this solid-state catalyst strainer 60 of conducting by pipeline;
Described recycle pump 37 connects this pan feeding control valve 31 of conducting and methanol eddy valve 38 respectively by pipeline; This methanol eddy valve 38 connects this Methanol Recovery condensing works 40 of conducting by pipeline;
Described pan feeding control valve 31 connects conducting methyl alcohol, the input aperture of triglyceride and catalyst;
Described recycle pump 37 connects this circulating reaction valve 36 of conducting by pipeline; This circulating reaction valve 36 connects this continuity reactive evaporation device 20 of conducting by pipeline;
Described recycle pump 37 connects conducting this microwave heating catalyticreactor reverse flow valve 34 and this microwave heating catalyticreactor transfer valve 33 respectively by pipeline; This microwave heating catalyticreactor transfer valve 33 is connected conducting with this microwave heating catalyticreactor 10 and this microwave heating catalyticreactor reverse flow valve 34 respectively by pipeline; The tie point of this microwave heating catalyticreactor reverse flow valve 34 connecting pipeline connects between the connecting pipeline of this microwave heating catalyticreactor transfer valve 33 at this microwave heating catalyticreactor 10; This microwave heating catalyticreactor transfer valve 33 connects conducting relief outlet.
This Methanol Recovery condensing works 40 comprises methanol eddy outlet 41, Methanol Recovery valve 42, methyl alcohol heat exchanger 43 and methanol vapor intake 44; One end of this methyl alcohol heat exchanger 43 connects conducting and arranges this methanol vapor intake 44, and the other end connects conducting and arranges this methanol eddy outlet 41; This methanol vapor intake 44 is connected conducting with this continuity reactive evaporation device 20; This methanol eddy outlet 41 connects this circulation transport control system device 30 of conducting by the middle connecting pipeline being provided with the threeway mouth of pipe; 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 port.
This standing separation device 50; There is provided and to have reacted and the standing separation of after product is reclaimed in methyl alcohol evaporation; This standing separation device 50 is by biofuel outlet valve 51, glycerol outlet valve 52, stratification indicating window 53, and standing separation groove 54 and standing liquid (drawing) entrance 55 etc. are combined into.This standing separation device 50 main body is a gyroscope-like standing separation groove 54; This standing separation groove 54 uprightly arranges and is the rigid structure of hollow, sealing; Top-shaped bottom is connected conducting by pipeline with glycerol outlet valve 52; Top-shaped middle part arrange biofuel export this biofuel outlet be connected conducting by pipeline with biofuel outlet valve 51; The cell wall of this standing separation groove 54 is provided with layering indicating window 53; This top-shaped top of standing separation groove 54 arranges standing liquid entrance 55; This standing liquid entrance 55 is connected conducting by the solid-state catalyst strainer 60 of pipeline and this.
This solid-state catalyst strainer 60 comprises solid-state catalyst output-controlling device 61, catalyst outlet 62, and catalyst filtration module 63, filters entrance 64 and filtering outlet 65; This catalyst filtration 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 with and filters entrance 64; This filtering outlet 65 is connected conducting by pipeline with this standing separation device 50; This filtration entrance 64 is connected conducting by pipeline with this circulation transport control system 30; This catalyst outlet 62 is connected conducting by one end of the solid-state catalyst output-controlling device 61 of pipeline and this; The other end of this solid-state catalyst output-controlling device 61 connects the solid-state catalyst delivery port of conducting.
The present invention implement time first by methyl alcohol 1, triglyceride 2 and catalyst 3, mol ratio according to triglyceride and methyl alcohol is 1:1-1:20, the weight ratio of catalyst and triglyceride is the mixing of 0.5:100-10:100 ratio, catalyst is less than 75 μm microminiaturization pulverized solid catalyst, utilize recycle pump 37 and pan feeding control valve 31 to introduce and flow to microwave heating catalyticreactor transfer valve 33, enter microwave heating catalyticreactor 10, through microwave reaction entrance 14, microwave reaction chamber 13 is to microwave reaction outlet 15, the evaporation reactor inlet 26 flowing to continuity reactive evaporation device 20 flows into, be stored in evaporation reactive tank 25, complete feeding schedule, close pan feeding control valve 31.
Enter heatable catalytic response procedures, ON cycle threshold of the reaction 36, allow reactant (methyl alcohol 1+ triglyceride 2+ catalyst 3) flow to microwave heating catalyticreactor 10 through recycle pump 37, formation circulates.Further unlatching microwave heating catalyticreactor drive unit 11 carries out heatable catalytic, microwave frequency used is 2450MHz, temperature is set as 30-80 DEG C, reaction times is 5-30min, allow reactant vibrate and form direct heating and catalysis transesterification reaction, it utilizes heatable catalytic temperature control module 12, allows it control in best catalyzed reaction temperature.And methyl alcohol 1 has evaporation issues in this temperature, application Methanol Recovery condensing works 40, by methanol vapor condensation, methanol liquid leads back and enters in reactant by application methanol eddy valve 38 more further, after reaction to be done, enters methyl alcohol and steams except program.
Entering methyl alcohol steams except program, further heatable catalytic temperature control module 12 is heightened the above temperature of methyl alcohol boiling point, temperature is set as 65-100 DEG C, time is 5-20min, allow unnecessary methanol gasifying and shifting out fast, Methanol Recovery condensing works 40 is imported through methanol vapor outlet 23, further application methyl alcohol heat exchanger 43, by methanol condensed, close methanol eddy valve 38, open Methanol Recovery delivery valve 42 and draw unnecessary methyl alcohol, can be back in processing procedure, Methanol Recovery delivery valve 42 is closed after methyl alcohol steams, close microwave heating catalyticreactor drive unit 11, enter and shift out reactant program.
Enter and shift out reactant program, then open in advance and leave standstill transfer valve 35, further closedown microwave heating catalyticreactor transfer valve 33, further unlatching microwave heating catalyticreactor reverse flow valve 34, utilize recycle pump 37 gravitation, further all reactants are moved to solid-state catalyst strainer 60, application catalyst filtration module 63, be placed between standing separation device 50 front end and standing transfer valve 35 and pulverized solid catalyst is leached, draw through catalyst outlet 62 through solid-state catalyst output-controlling device 61, can reach and directly catch catalyst.Then flow in the standing separation groove 54 of standing separation device 50 by product liquid, reactive system reaction product to be cleaned then closes all control valves and recycle pump 37, completes response procedures.The program of leaving standstill, time of repose is 0.5-2 hour, reaction product can form the biofuel 5 on upper strata, lower floor's glycerine 6, can see hierarchical scenario by layering indicating window 53, and biofuel 5 applicable biological diesel oil outlet valve 51 is drawn, and glycerine and catalyst can be drawn with glycerol outlet valve 52, and catch solid-state catalyst can return again processing procedure use, reach the target of production biofuel easily.
Claims (10)
1. produce a biodiesel process, it is characterized in that comprising the following steps:
(201) raw material prepares: prepare triglyceride, methyl alcohol and catalyst; Wherein the mol ratio of triglyceride and methyl alcohol is 1:1-1:20, and the weight ratio of catalyst and triglyceride is 0.5:100-10:100, and this catalyst is less than 75 μm microminiaturization pulverized solid catalyst;
(202) mixed reactant program: triglyceride, methyl alcohol are mixed with pulverized solid catalyst out-phase, pulverized solid catalyst is due to microminiaturization increase and the emulsion dispersion effect of liquid triglyceride, methyl alcohol, and more can fully mix through circulating of recycle pump, increase out-phase Contact area and time, and be easy to reclaim pulverized solid catalyst;
(203) microwave heating catalysis transesterification reaction: triglyceride, methyl alcohol and catalyst circulate and pass in and out microwave reactor and carry out heatable catalytic transesterification reaction, increase homogeneous heating between out-phase, accelerate transesterification reaction, microwave frequency used is 2450MHz, temperature is set as 30-80 DEG C, and the circulating reaction time is 5-30 minute;
(204) unnecessary methyl alcohol is steamed: after having reacted, application and transesterification reaction same microwave heating catalyticreactor steam unnecessary methyl alcohol, temperature is set as 65-100 DEG C, time is 5-20 minute, methyl alcohol vaporator rate is accelerated in cyclical operation, not only reclaims methyl alcohol and also extends the reaction times and make transesterification reaction more complete;
(205) filtration is shifted out: after reaction, pulverized solid catalyst can reach through solid-state catalyst strainer and directly catch catalyst fast to carry out reuse;
(206) stratification: form upper strata biofuel and lower floor's glycerine of separation after leaving standstill through catching product liquid after pulverized solid catalyst, time of repose is 0.5-2 hour;
(207) biofuel finished product is generated.
2. produce biodiesel process as claimed in claim 1, it is characterized in that recyclable the returning in former processing procedure raw material preparation step (201) of methyl alcohol that this step (204) steams uses.
3. produce biodiesel process as claimed in claim 1, it is characterized in that recyclable the returning in former processing procedure raw material preparation step (201) of pulverized solid catalyst that this step (205) directly catches through solid-state catalyst strainer uses.
4., based on the system producing biodiesel process as described in as arbitrary in claim 1-3, it is characterized in that comprising:
Microwave heating catalyticreactor (10), controls in order to the microwave energy and temperature providing circulating reaction thing, methanol stripper;
Continuity reactive evaporation device (20), the storage area of coming in and going out microwave heating catalyticreactor in order to provide reactant and methyl alcohol evaporation remove space;
Circulation transport control system device (30), in order to provide reactant pan feeding, mixing, circulation and methanol eddy conveying;
Methanol Recovery condensing works (40), in order to provide Evaporation of methanol condensation to carry out refluxing or reclaiming;
Standing separation device (50), to have reacted and the standing separation of after product is reclaimed in methyl alcohol evaporation in order to provide;
Solid-state catalyst strainer (60), in order to provide the recovery of having reacted rear pulverized solid catalyst;
Described microwave heating catalyticreactor (10) to be tightly connected with described continuity reactive evaporation device (20) and described circulation transport control system device (30) conducting respectively by pipeline;
Described Methanol Recovery condensing works (40) to be tightly connected with described continuity reactive evaporation device (20) and described circulation transport control system device (30) conducting respectively by pipeline;
Described solid-state catalyst strainer (60) is connected conducting with described circulation transport control system device (30) and described standing separation device (50) respectively by pipeline.
5. system as claimed in claim 4, is characterized in that this microwave heating catalyticreactor (10) main body is a column microwave reaction chamber (13); This microwave reaction chamber (13) uprightly arranges and be the rigid structure of hollow, sealing, and bottom is provided with microwave reaction entrance (14), and top is provided with microwave reaction and exports (15); This microwave reaction entrance (14) to be tightly connected conducting by pipeline and this circulation transport control system device (30); This microwave reaction outlet (15) to be tightly connected conducting by pipeline and this continuity reactive evaporation device (20); The transesterification circulation line (16) of curl is provided with in this microwave reaction chamber (13); This microwave reaction chamber (13) is evenly provided with a plurality of microwave heating catalyticreactor drive unit (11) outward; One end of this transesterification circulation line (16) and this microwave reaction entrance (14) are tightly connected conducting; This microwave reaction outlet (15) place is provided with heatable catalytic temperature control module (12).
6. system as claimed in claim 4, is characterized in that this continuity reactive evaporation device (20) main body is a gyroscope-like or taper evaporation reactive tank (25); This evaporation reactive tank (25) uprightly arranges and is the rigid structure of hollow, sealing, cone bottom is provided with reaction cycle outlet (24), cone top part is provided with methanol vapor outlet (23), evaporation reactor inlet (26) and be connected with the emergency vent of Safety control valve (21); This emergency vent being connected with Safety control valve (21) is positioned between this methanol vapor outlet (23) and this evaporation reactor inlet (26); This evaporation reactor inlet (26) to be tightly connected conducting by pipeline and this microwave heating catalyticreactor (10); This reaction cycle outlet (24) to be tightly connected conducting by pipeline and this circulation transport control system device (30); This methanol vapor outlet (23) to be tightly connected conducting by pipeline and this Methanol Recovery condensing works (40); The outer wall of this evaporation reactive tank (25) bottom is connected with reactive evaporation thermometer (22).
7. system as claimed in claim 4, it is characterized in that this circulation transport control system device (30) comprises pan feeding control valve (31), microwave heating catalyticreactor transfer valve (33), microwave heating catalyticreactor reverse flow valve (34), leave standstill transfer valve (35), circulating reaction valve (36), recycle pump (37) and methanol eddy valve (38);
Described recycle pump (37) connects this standing transfer valve (35) of conducting by pipeline, and this standing transfer valve (35) connects this solid-state catalyst strainer (60) of conducting by pipeline;
Described recycle pump (37) connects this pan feeding control valve (31) of conducting and methanol eddy valve (38) respectively by pipeline; This methanol eddy valve (38) connects this Methanol Recovery condensing works (40) of conducting by pipeline;
Described pan feeding control valve (31) connects conducting methyl alcohol, the input aperture of triglyceride and catalyst;
Described recycle pump (37) connects this circulating reaction valve (36) of conducting by pipeline; This circulating reaction valve (36) connects this continuity reactive evaporation device (20) of conducting by pipeline;
Described recycle pump (37) connects this microwave heating catalyticreactor reverse flow valve (34) of conducting and this microwave heating catalyticreactor transfer valve (33) respectively by pipeline; This microwave heating catalyticreactor transfer valve (33) is connected conducting with this microwave heating catalyticreactor (10) and this microwave heating catalyticreactor reverse flow valve (34) respectively by pipeline; The tie point of this microwave heating catalyticreactor reverse flow valve (34) connecting pipeline is positioned at this microwave heating catalyticreactor (10) and connects between the connecting pipeline of this microwave heating catalyticreactor transfer valve (33); This microwave heating catalyticreactor transfer valve (33) connects conducting relief outlet.
8. system as claimed in claim 4, it is characterized in that this Methanol Recovery condensing works (40) comprises methanol eddy outlet (41), Methanol Recovery valve (42), methyl alcohol heat exchanger (43) and methanol vapor intake (44); One end of this methyl alcohol heat exchanger (43) connects conducting and arranges this methanol vapor intake (44), and the other end connects conducting and arranges this methanol eddy outlet (41); This methanol vapor intake (44) is connected conducting with this continuity reactive evaporation device (20); This methanol eddy outlet (41) connects this circulation transport control system device (30) of conducting by the middle connecting pipeline being provided with the threeway mouth of pipe; 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 port.
9. system as claimed in claim 4, is characterized in that this standing separation device (50) main body is a gyroscope-like standing separation groove (54); This standing separation groove (54) uprightly arranges and is the rigid structure of hollow, sealing; Top-shaped bottom is connected conducting by pipeline with glycerol outlet valve (52); Top-shaped middle part arrange biofuel export this biofuel outlet be connected conducting by pipeline with biofuel outlet valve (51); The cell wall of this standing separation groove (54) is provided with layering indicating window (53); This standing separation groove (54) top-shaped top arranges standing liquid entrance (55); This standing liquid entrance (55) is connected conducting by the solid-state catalyst strainer (60) of pipeline and this.
10. system as claimed in claim 4, it is characterized in that this solid-state catalyst strainer (60) comprises solid-state catalyst output-controlling device (61), catalyst outlet (62), catalyst filtration module (63), filters entrance (64) and filtering outlet (65); This catalyst filtration 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 with and filters entrance (64); This filtering outlet (65) is connected conducting by pipeline with this standing separation device (50); This filtration entrance (64) is connected conducting by pipeline with this circulation transport control system (30); This catalyst outlet (62) is connected conducting by one end of the solid-state catalyst output-controlling device (61) of pipeline and this; The other end of this solid-state catalyst output-controlling device (61) connects the solid-state catalyst delivery port of conducting.
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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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| CN201410538021.9A CN104357098B (en) | 2014-10-13 | 2014-10-13 | Produce the method and system of biodiesel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659960A (en) * | 2017-04-01 | 2018-10-16 | 深圳华联世纪生物工程股份有限公司 | A kind of microwave legal system Biodiesel technological process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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2014
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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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659960A (en) * | 2017-04-01 | 2018-10-16 | 深圳华联世纪生物工程股份有限公司 | A kind of microwave legal system Biodiesel technological process |
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