CN104593159B - Using the method for complex solid Catalyst Production biodiesel - Google Patents
Using the method for complex solid Catalyst Production biodiesel Download PDFInfo
- Publication number
- CN104593159B CN104593159B CN201510059776.5A CN201510059776A CN104593159B CN 104593159 B CN104593159 B CN 104593159B CN 201510059776 A CN201510059776 A CN 201510059776A CN 104593159 B CN104593159 B CN 104593159B
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- Prior art keywords
- biodiesel
- esterification
- solid catalyst
- catalyst production
- complex solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003225 biodiesel Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000011949 solid catalyst Substances 0.000 title claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 84
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000032050 esterification Effects 0.000 claims abstract description 24
- 238000005886 esterification reaction Methods 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000005809 transesterification reaction Methods 0.000 claims abstract description 17
- 150000001768 cations Chemical class 0.000 claims abstract description 15
- 235000011187 glycerol Nutrition 0.000 claims abstract description 14
- 239000002699 waste material Substances 0.000 claims abstract description 14
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 6
- 238000004062 sedimentation Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 4
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims abstract description 3
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 claims abstract description 3
- 150000002148 esters Chemical class 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000004519 grease Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 claims description 4
- 238000011069 regeneration method Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000012066 reaction slurry Substances 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 7
- 238000001816 cooling Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 102000004882 Lipase Human genes 0.000 description 1
- 108090001060 Lipase Proteins 0.000 description 1
- 239000004367 Lipase Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- 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 present invention relates to a kind of method using complex solid Catalyst Production biodiesel, it is characterized in that, waste oil is obtained to qualified absolute oil after pretreatment, qualified absolute oil is passed through in slurry bubble esterification destilling tower, under the catalysis of esterification resin cation esterification is carried out with the first methanol gas, free fatty and the first methanol gas generation fatty acid methyl ester and water in qualified absolute oil, first coarse biodiesel is subjected to transesterification under the catalysis of fatty biology enzyme with the second methanol gas, glyceric acid three ester and the second methanol gas generation fatty acid methyl ester and water in first coarse biodiesel, obtain the second coarse biodiesel, second coarse biodiesel is subjected to sedimentation separation, obtain coarse biodiesel finished product and glycerine.Simple to operate using the above method, catalyst activity is high, it is not necessary to often more catalyst changeout, productivity effect is not interfered with, very with practical value.
Description
Technical field
The present invention relates to energy field, the more particularly to production method of biodiesel, in particular to one kind uses composite solid
The method that body catalyst produces biodiesel.
Background technology
High acid value waste oil produces biodiesel, domestic at present generally using liquid soda acid as catalyst, as a result deposits
It is difficult to separate in product, washing process produces the waste water for polluting environment again, the problems such as equipment corrosion is serious, and energy consumption is higher.Adopt
With the solid catalyst for being easy to separation, the trial of such as biology enzyme or ion exchange resin, it is multiple to run into its regeneration operation
It is miscellaneous.Receptor 1 activity influences, it is necessary to which frequent more catalyst changeout, influences production efficiency and economic benefit.
So a kind of simple to operate, catalyst activity is high, it is not necessary to which often being produced from waste oil for more catalyst changeout is given birth to
The method of thing diesel oil is that very have practical value.
The content of the invention
The invention aims to overcome it is above-mentioned in the prior art the shortcomings that, there is provided a kind of simple to operate, catalyst is lived
Property it is high, it is not necessary to the often method using complex solid Catalyst Production biodiesel of more catalyst changeout.
To achieve these goals, the invention provides a kind of side using complex solid Catalyst Production biodiesel
Method, its feature is, comprises the following steps：
Step (1)：Waste oil is obtained to qualified absolute oil after pretreatment, described qualified absolute oil is passed through slurry bubble
In esterification-destilling tower, esterification, described qualified absolute oil are carried out with the first methanol gas under the catalysis of esterification resin cation
In free fatty and described first methanol gas generation fatty acid methyl ester and water, its reaction equation such as formula (I),
Obtain the first coarse biodiesel；
Step (2)：The first described coarse biodiesel is turned under the catalysis of fatty biology enzyme with the second methanol gas
Esterification, glyceric acid three ester in the first described coarse biodiesel and described the second methanol gas generation fatty acid methyl ester and
Water, its reaction equation such as formula (II), obtains the second coarse biodiesel,
The second described coarse biodiesel is carried out sedimentation separation by step (3), obtains coarse biodiesel finished product and glycerine.
It is preferred that described pretreatment comprises the following steps：
Step (1.1)：After solid impurity and moisture therein is removed after described waste oil filtering, after adding flocculant
Refiningly cook, the grease refiningly cooked；
Step (1.2)：After the described precipitation of grease refiningly cooked filtering, described qualified absolute oil is obtained.
It is preferred that described esterification resin cation is large aperture resin cation.Resin particle Pore Diameter Specific Surface accumulates
45m2/ more than g.
It is preferred that the first described methanol gas is to be passed through from bottom to top in described slurry bubble esterification-destilling tower, and from
It is recovered above described slurry bubble esterification-destilling tower.
It is preferred that described transesterification occurs in transesterification kettle stirred reactor.
It is preferred that described qualified absolute oil Han Shui≤0.5%, acid value ＞ 100.
It is preferred that described slurry bubble esterification-destilling tower temperature is at 70 DEG C~75 DEG C, 0.2~0.3MPa of pressure, slurry
Solid content 25~30%, described reaction time of esterification are 4 hours.
It is preferred that described transesterification temperature is 35 DEG C -40 DEG C, reaction slurry solid-to-liquid ratio 15~20%, pH value=
7, the described transesterification time is 2.5 hours.
It is preferred that described fatty biology enzyme is fixed on the resin of large aperture.
Using the method using complex solid Catalyst Production biodiesel of the present invention, it uses segment arrangement cation
Resin and the biology enzyme being fixed on resin, different courses of reaction is completed in different equipment, is especially esterified cation
Resin is arranged in slurry bubble esterification-destilling tower and carries out esterification, there is many special point of gas caps on tower tray, prevents solid phase
Spill, gas passes through.Per the special switch of tower fuel-economizing, it is easy to solid phase smoothly to discharge and add if necessary.It is esterified cation
Resin is the catalyst of high acid value waste oil esterification, in the slurry bubble column of esterification-distillation, is passed through methanol gas, free acid quilt
The moisture generated while esterification is taken out of (from bottom to top) one by one by the methanol gas of excess, esterification obtain it is not only fast but also thoroughly,
The moisture generated during this is taken out of by methanol gas and accelerates reaction speed, and the regeneration and replacing of resin are in situation about not stopping production
Under be carried out continuously.Enter immediately after the suitably cooling of the reaction solution of esterification and adjustment pH value and turn by catalyst of solid biologic enzyme
Continuous transesterification is carried out in esterifying kettle, a kind of biology in high activity high life (above cycle half a year) is used in kettle
Enzyme.Generate and pay in this biodiesel and produced glycerine (glycerine also generated in the lump while generating biodiesel), pass through
Plain sedimentation separates, and just obtains coarse biodiesel and glycerine.Zonal cooling is smoothed out producing biodiesel like this.Separate work
Make very simple, without washing, by-product glycerin quality is up to food-grade.
Brief description of the drawings
Fig. 1 is process chart of the embodiment of the present invention using the method for complex solid Catalyst Production biodiesel.
Embodiment
In order to be more clearly understood that the technology contents of the present invention, the specific implementation method of the present invention is made into one below
Walk explanation.
Fig. 1 is process chart of the embodiment of the present invention using the method for complex solid Catalyst Production biodiesel.Such as
Shown in Fig. 1,
Waste oil is pre-processed, after solid impurity and moisture therein are removed after waste oil is filtered, adds flocculation
Refiningly cooked after agent, the grease refiningly cooked, after precipitation filtering, obtain qualified absolute oil, the grease Han Shui of the qualified absolute oil≤
0.5%, acid value ＞ 100, under conditions of above-mentioned technique reaches stable state, to the diameters of Ф 311, the slurry of built-in three bubbling column plates
Bubbling esterification-destilling tower, tower top charge door continuously inject the waste oil fat raw material of acid value 100 with 0.450L/min flow.Simultaneously
Continuously it is passed through methanol gas from bottom of towe, flow 0.420L/min, temperature is 72 DEG C in now slurry bubble esterification-destilling tower, pressure
For 0.25MPa, slurry fluid solid content is 30%, and methanol vapor phase, which is fed, certain degree of superheat, and the pressure in tower by coupling therewith
Methanol distillation column control, reaction time 4 hours.Be employed as the esterification resin cation of catalyst for large aperture sun from
Subtree fat.It can successively obtain being esterified coarse biodiesel (the first coarse biodiesel) 0.456L/ from bottom of towe after stable state is operated
Min (wherein aqueous 0.6%, free acid 1.0%), excessive methanol reclaims methanol by the methanol distillation column above destilling tower
Measure as 23.5L/min (99.8% concentration), releasing moisture content 0.1kg/min.
Above-mentioned coarse biodiesel, which passes through, is cooled to 35~40 DEG C, continuously enters Ф 500 transesterification kettle stirred reactor, its
Middle resin filling immobilized lipase biology enzyme (Israel's import) carries out transesterification solid-to-liquid ratio 20% or so, is adjusted with buffer
PH=7 or so is saved, adds quantity of methyl alcohol 0.024L/min, transesterification 2~2.5 hours time., transesterification temperature is 35 DEG C,
Transesterification coarse biodiesel (the second coarse biodiesel) 0.445L/min is obtained, sedimentation separates 18 grams/min of glycerine, obtains coarse biometric
For diesel oil finished product to the total yield about 97.7% of effective waste oil, the utilization rate of material is preferable.
Using the method using complex solid Catalyst Production biodiesel of the present invention, it uses segment arrangement cation
Resin and the biology enzyme being fixed on resin, different courses of reaction is completed in different equipment, is especially esterified cation
Resin is arranged in slurry bubble esterification-destilling tower and carries out esterification, there is many special point of gas caps on tower tray, prevents solid phase
Spill, gas passes through.Per the special switch of tower fuel-economizing, it is easy to solid phase smoothly to discharge and add if necessary.It is esterified cation
Resin is the catalyst of high acid value waste oil esterification, in the slurry bubble column of esterification-distillation, is passed through methanol gas, free acid quilt
The moisture generated while esterification is taken out of (from bottom to top) one by one by the methanol gas of excess, esterification obtain it is not only fast but also thoroughly,
The moisture generated during this is taken out of by methanol gas and accelerates reaction speed, and the regeneration and replacing of resin are in situation about not stopping production
Under be carried out continuously.Enter immediately after the suitably cooling of the reaction solution of esterification and adjustment pH value and turn by catalyst of solid biologic enzyme
Continuous transesterification is carried out in esterifying kettle, a kind of biology in high activity high life (above cycle half a year) is used in kettle
Enzyme.Generate and pay in this biodiesel and produced glycerine (glycerine also generated in the lump while generating biodiesel), pass through
Plain sedimentation separates, and just obtains coarse biodiesel and glycerine.Zonal cooling is smoothed out producing biodiesel like this.Separate work
Make very simple, without washing, by-product glycerin quality is up to food-grade.
Ingenious arrangement on present invention process, brings out the best in each other, just right with its respective deficiency that each advantage is kept away, special
Independently developed novel device slurry bubble esterification-destilling tower is not employed as esterification main equipment, simplifies operating process and significantly
Thing damage is reduced, biodiesel oil product and catalyst and byproduct glycerine easily separate, and without the pollution of wash water, equipment is without corruption
Erosion, operates relatively low, the energy saving of the cost of overhaul, and the expense of two kinds of catalyst presses current effect and life-span projection, biology per ton
Consumed cost is less than 100 yuan to diesel oil on a catalyst, therefore this technique can claim green, the high acid value of processing of economical rationality
Waste oil produces biodiesel new technology.
In this description, the present invention is described with reference to its specific embodiment.But it is clear that it can still make
Various modifications and alterations are without departing from the spirit and scope of the present invention.Therefore, specification is considered as illustrative rather than limit
Property processed.
Claims (8)
- A kind of 1. method using complex solid Catalyst Production biodiesel, it is characterised in that comprise the following steps：Step (1)：Waste oil is obtained to qualified absolute oil after pretreatment, described qualified absolute oil is passed through slurry bubble ester In change-destilling tower, esterification is carried out with the first methanol gas under the catalysis of esterification resin cation, in described qualified absolute oil Free fatty and described first methanol gas generation fatty acid methyl ester and water, the first described methanol gas is leads to from bottom to top Enter in described slurry bubble esterification-destilling tower, free fatty is esterified while the moisture of generation is by the methanol gas of excess Taken out of above described slurry bubble esterification-destilling tower, realize the regeneration that resin cation is esterified in continuous production, its is anti- Ying Shiru formulas (I),Obtain the first coarse biodiesel；Step (2)：PH and second is adjusted by the first described coarse biodiesel under the catalysis of fatty biology enzyme and with buffer Methanol carries out transesterification, the fat of glyceric acid three in the first described coarse biodiesel and described the second methanol generation fat Sour methyl esters and glycerine, its reaction equation such as formula (II), obtain the second coarse biodiesel,The second described coarse biodiesel is carried out sedimentation separation by step (3), obtains coarse biodiesel finished product and glycerine.
- 2. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Pretreatment comprise the following steps：Step (1.1)：After solid impurity and moisture therein is removed after described waste oil filtering, refined after adding flocculant Boil, the grease refiningly cooked；Step (1.2)：After the described precipitation of grease refiningly cooked filtering, described qualified absolute oil is obtained.
- 3. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Esterification resin cation be large aperture resin cation.
- 4. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Transesterification occur in transesterification kettle stirred reactor.
- 5. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Qualified absolute oil Han Shui≤0.5%, acid value ＞ 100.
- 6. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Slurry bubble esterification-destilling tower temperature at 70 DEG C~75 DEG C, 0.2~0.3MPa of pressure, slurry solid content 25~30% is described Reaction time of esterification be 4 hours.
- 7. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Transesterification temperature be 35 DEG C -40 DEG C, reaction slurry solid-to-liquid ratio 15~20%, pH value=7, during described transesterification Between be 2.5 hours.
- 8. the method according to claim 1 using complex solid Catalyst Production biodiesel, it is characterised in that described Fatty biology enzyme be fixed on the resin of large aperture.
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| CN201510059776.5A CN104593159B (en) | 2015-02-05 | 2015-02-05 | Using the method for complex solid Catalyst Production biodiesel |
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| CN110093212A (en) * | 2019-04-23 | 2019-08-06 | 龙岩卓越新能源股份有限公司 | A kind of method of waste oil continuous esterification production |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816645A (en) * | 2012-09-14 | 2012-12-12 | 天津工业大学 | Continuous preparation method of biodiesel |
| CN103160379A (en) * | 2011-12-09 | 2013-06-19 | 深圳市贝壳能源科技有限公司 | Method for producing biodiesel by virtue of high-acid-value oil raw material |
| CN103242914A (en) * | 2013-05-30 | 2013-08-14 | 广州市特种承压设备检测研究院 | Method for rapidly producing biodiesel from kitchen garbage and produced biodiesel |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160379A (en) * | 2011-12-09 | 2013-06-19 | 深圳市贝壳能源科技有限公司 | Method for producing biodiesel by virtue of high-acid-value oil raw material |
| CN102816645A (en) * | 2012-09-14 | 2012-12-12 | 天津工业大学 | Continuous preparation method of biodiesel |
| CN103242914A (en) * | 2013-05-30 | 2013-08-14 | 广州市特种承压设备检测研究院 | Method for rapidly producing biodiesel from kitchen garbage and produced biodiesel |
Non-Patent Citations (1)
| Title |
|---|
| 固定化洋葱假胞菌G63脂肪酶转酯化大豆油合成生物柴油;郭道义等;《中国油脂》;20080430;第33卷(第4期);54页摘要，左栏第1段，右栏第1，2段 * |
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