CN106799220A - The exploitation and its application in catalyzed transesterification of sunflower stalk ash solid catalyst - Google Patents
The exploitation and its application in catalyzed transesterification of sunflower stalk ash solid catalyst Download PDFInfo
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- CN106799220A CN106799220A CN201710104647.2A CN201710104647A CN106799220A CN 106799220 A CN106799220 A CN 106799220A CN 201710104647 A CN201710104647 A CN 201710104647A CN 106799220 A CN106799220 A CN 106799220A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
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- 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
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- 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
- C11C3/10—Ester interchange
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- 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
- C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
- C10L2290/12—Regeneration of a solvent, catalyst, adsorbent or any other component used to treat or prepare a fuel
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- 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
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Abstract
The present invention relates to field of biodiesel oil, the exploitation and its application in catalyzed transesterification of specifically a kind of sunflower stalk ash solid catalyst, the development approach comprises the following steps；It is S1, predrying：The advance sunflower stalk ash collected is dried into water removal；S2, high-temperature calcination：Pre-dried sunflower stalk ash is placed in Muffle furnace, temperature one and the time one of calcining is set, high-temperature calcination is carried out；S3, hydration：To distilled water is added in the sunflower stalk ash after high-temperature calcination, dried after being uniformly mixed；S4, low-temperature activation：Sunflower stalk ash after hydration is placed in Muffle furnace, temperature two and the time two of calcining is set, low-temperature activation is carried out；It is S5, mechanical-moulded：Preserved being placed in drier after the sunflower stalk ash mechanical lapping after low-temperature activation.The beneficial effects of the invention are as follows：1st, catalyst low raw-material cost, environmentally friendly and renewable；2nd, catalyst preparation technology is simple, and biodiesel production rate is high.
Description
Technical field
The present invention relates to field of biodiesel oil, the exploitation of specifically a kind of sunflower stalk ash solid catalyst and its in catalysis
Application in ester exchange reaction.
Background technology
There is biodiesel renewable, biodegradable, nontoxic, carbon to neutralize, advantages of environment protection, and can reduce
Greenhouse gas emission, while reduce the dependence to the fossil fuel of increasingly depleted, thus countries in the world are promoting it to be used for bavin
In oil turbine.Biodiesel is that under catalyst action, the purpose that animal and plant grease is obtained with methyl alcohol ester exchange reaction is produced
Thing, accessory substance is glycerine.
Widely used homogeneous catalyst in current biodiesel synthesis, future is expected to be substituted by solid catalyst.With it is equal
Phase catalyst is compared, and solid catalyst to be had easily reclaim and the simple advantage of postprocessing working procedures.Wherein, with the compound of potassium element
For solid base catalyst prepared by active component is the focus of current research.Researcher is developed such as K2O/Ti-HMS、KF/
CuAl-LDOs、K2CO3/Al2O3Etc. a series of such catalyst, but these catalyst are subject to catalyst raw material sources and preparation
The limitation of cost, it is impossible to meet the requirement of industrialized production.Therefore, in order to adapt to industrial wanting for biodiesel catalyst
Ask, it is necessary to start with from catalyst raw material angle, exploitation is a kind of efficiently, cheap, the extensive solid catalyst of raw material sources.
Therefore, carrying out numerous studies work both at home and abroad, the calcium of various biomass castoff such as preparations such as fish scale, shell class is found
Based solid alkali catalyst, but there is not been reported to prepare kalium group solid base catalyst with biomass castoff.China is agriculture big
State, can all produce substantial amounts of biomass castoff, wherein agricultural crop straw to occupy significant proportion every year.With the day of haze problem
Beneficial serious, the treatment of agricultural crop straw is also increasingly paid attention to by the Chinese government.Wherein, it is with agricultural crop straw combustion power generation
The effective way that stalk original place is burned is solved, related industry is fast-developing.However, obtained by agricultural crop straw combustion power generation
Plant ash, be not yet utilized effectively.The plant ash constituent content that different burning plants are obtained has very big difference.Difference is planted
Potassium oxide and calcium oxide weight/mass percentage composition (Shen Qirong, Tan Jinfang, Qian Xiaoqing soil fertilizer science general surveys in thing plant ash
[M] Beijing：Higher Education Publishing House, 2001.228.), as shown in table 1：
Calcium oxide and potassium oxide content in the different plant plait wood ashes of table 1
As shown in Table 1, in different plant plait wood ashes, the potassium oxide content highest in sunflower stalk ash, and with higher
The calcium oxide of content.Additionally, sunflower has plantation in China's multiple province, such as Inner Mongolia Autonomous Region, Xinjiang Uygur is autonomous
Area, Heilungkiang etc., about 1,300,000 hectares of cultivated area (Zhao Guixing, Zhong Peng, Chen Xia, wait China sunflower industry development present situation and
Countermeasure [J] agriculture projects, 2011,1 (2)：42-45.), thus source widely.Therefore, sunflower stalk ash is a preferable class
The raw material for preparing biodiesel solid base catalyst.
The content of the invention
An object of the present invention is to provide a kind of development approach of sunflower solid catalyst.
Another object of the present invention is application of the sunflower solid catalyst in catalyzed transesterification.
The invention provides following technical scheme：
A kind of development approach of sunflower stalk ash solid catalyst, the development approach comprises the following steps；
It is S1, predrying：The advance sunflower stalk ash collected is dried into water removal；
S2, high-temperature calcination：Pre-dried sunflower stalk ash is placed in Muffle furnace, temperature one and the time of calcining is set
One, carry out high-temperature calcination；
S3, hydration：To distilled water is added in the sunflower stalk ash after high-temperature calcination, dried after being uniformly mixed；
S4, low-temperature activation：Sunflower stalk ash after hydration is placed in Muffle furnace, temperature two and the time of calcining is set
Two, carry out low-temperature activation；
It is S5, mechanical-moulded：Preserved being placed in drier after the sunflower stalk ash mechanical lapping after low-temperature activation.
Preferably, described pre-drying step is that sunflower stalk ash is placed in heated-air circulation oven, at 80-110 DEG C
5-7h is dried, to remove moisture of the absorption in sunflower stalk ash.
Preferably, described high-temperature calcination be will be predrying after sunflower stalk ash be positioned in Muffle furnace, in 800-
1100 DEG C of calcining 2-5h.
Preferably, described hydration is according to mass ratio 3-6 by the sunflower stalk ash after distilled water, high-temperature calcination：1 mixes
Close, stirring at normal temperature 1-3h, stand 5-9h, 100-120 DEG C dries 4-8h.
Preferably, described low-temperature activation is will to be hydrated dried sunflower stalk ash to be placed in Muffle furnace, in 600-
700 DEG C of calcining 2-4h.
Preferably, it is described it is mechanical-moulded be that the sunflower stalk ash mechanical grinding after low-temperature activation is clayed into power, Ran Houli
It is positioned over drier memory storage.
Preferably, the sunflower be selected from a kind of in large and small three road eyebrow, dirty oil certain herbaceous plants with big flowers, U.S. certain herbaceous plants with big flowers and Hei Bei or they
Mixture.
A kind of application of the sunflower stalk ash solid catalyst in catalyzed transesterification, by grease and methyl alcohol according to mole
Compare 12-16:1 is added in reactor, after being well mixed, the catalyst of the oil quality fraction 5-7% is added, in 60-70
Stirring reaction 3.5-5h under DEG C temperature conditionss, stops stirring, and suction filtration takes filtrate and reclaims catalyst, and filtrate is placed on into point liquid leaks
6-8h is stood in bucket, is divided into two-layer, upper strata is biodiesel phase, separated that biodiesel is mutually depressurized goes out residual methanol i.e.
Can obtain biodiesel.
Preferably, the grease is selected from any one in vegetable oil, animal tallow and waste oil.
The beneficial effects of the invention are as follows：
The performance of the biodiesel that present specification embodiment is obtained, as shown in table 2：
The performance of the biodiesel of table 2
Knowable to the result of present specification embodiment and table 2, the raw material for producing catalyst is sunflower stalk ash, its source
Extensively, it is cheap, and be a kind of environmentally friendly, pollution-free, reproducible resource；And China's sunflower planting is mainly distributed on
Relatively backward west area, catalyst is prepared using sunflower stalk ash, can provide machine for the vast remote districts development in western part
Meeting, promotes the development of local economy；Meanwhile, the simple production process of catalyst is rich in potassium and calcium constituent, catalyst in catalyst
Active high, the yield of biodiesel is high, and the biodiesel obtained by catalysis has excellent performance, its density, kinematic viscosity, acid
Value, mechanical admixture, pour point, flash-point and copper corrosion test have reached national standard.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the SEM photograph of sunflower stalk ash；
Fig. 2 is the SEM photograph of sunflower stalk ash solid catalyst.
Specific embodiment
With the sunflower stalk burning generation in the Tacheng Prefecture of Xinjiang Uygur Autonomous Regions Kazak Autonomous Prefecture of Ili to day
Certain herbaceous plants with big flowers stalk ash is catalyst raw material.
Embodiment 1
A kind of preparation method of sunflower stalk ash solid catalyst, in accordance with the following steps, first places sunflower stalk ash
5h is dried at 80 DEG C in heated-air circulation oven, to remove wetting moisture and capillary moisture of the absorption in sunflower stalk ash；
Sunflower stalk ash after will be predrying is positioned in Muffle furnace, and 2h is calcined at 850 DEG C；After by distilled water, high-temperature calcination to day
Certain herbaceous plants with big flowers stalk ash is according to mass ratio 3:1 mixing, stirring at normal temperature 1.5h stands 6h, and 110 DEG C dry 7h；Then will be hydrated it is dried to
Day certain herbaceous plants with big flowers stalk ash is secondary to be placed in Muffle furnace, and 2h are calcined at 650 DEG C；By the sunflower stalk ash mechanical grinding grinds after low-temperature activation
End, is positioned over drier memory storage immediately after.
A kind of application of sunflower stalk ash solid catalyst in catalyzed transesterification, comprises the following steps, first will
Grease and methyl alcohol are according to mol ratio 14:1 is added in reactor, after being well mixed, adds urging for the oil quality fraction 5%
Agent, the stirring reaction 3.5h under 70 DEG C of temperature conditionss stops stirring, and suction filtration takes filtrate and reclaims catalyst, and filtrate is placed on
6h is stood in separatory funnel, is divided into two-layer, upper strata is biodiesel phase, separated that biodiesel is mutually depressurized goes out to remain first
Alcohol is that can obtain biodiesel, and biodiesel production rate is 85.61%.
Embodiment 2
A kind of preparation method of sunflower stalk ash solid catalyst, in accordance with the following steps, first places sunflower stalk ash
6h is dried at 100 DEG C in heated-air circulation oven, to remove wetting moisture and capillary moisture of the absorption in sunflower stalk ash；
Sunflower stalk ash after will be predrying is positioned in Muffle furnace, and 3h is calcined at 800 DEG C；After by distilled water, high-temperature calcination to day
Certain herbaceous plants with big flowers stalk ash is according to mass ratio 4:1 mixing, stirring at normal temperature 1h stands 8h, and 120 DEG C dry 6h；Then will be hydrated dried to day
Certain herbaceous plants with big flowers stalk ash is secondary to be placed in Muffle furnace, and 3h is calcined at 600 DEG C；By the sunflower stalk ash mechanical grinding grinds after low-temperature activation
End, is positioned over drier memory storage immediately after.
A kind of application of sunflower stalk ash solid catalyst in catalyzed transesterification, comprises the following steps, first will
Grease and methyl alcohol are according to mol ratio 12:1 is added in reactor, after being well mixed, adds urging for the oil quality fraction 6%
Agent, the stirring reaction 4h under 65 DEG C of temperature conditionss stops stirring, and suction filtration takes filtrate and reclaim catalyst, and filtrate is placed on point
7h is stood in liquid funnel, is divided into two-layer, upper strata is biodiesel phase, separated that biodiesel is mutually depressurized goes out residual methanol
Biodiesel is can obtain, biodiesel production rate is 83.95%.
Embodiment 3
A kind of preparation method of sunflower stalk ash solid catalyst, in accordance with the following steps, first places sunflower stalk ash
5h is dried at 105 DEG C in heated-air circulation oven, to remove wetting moisture and capillary moisture of the absorption in sunflower stalk ash；
Sunflower stalk ash after will be predrying is positioned in Muffle furnace, and 4h is calcined at 900 DEG C；After by distilled water, high-temperature calcination to day
Certain herbaceous plants with big flowers stalk ash is according to mass ratio 5:1 mixing, stirring at normal temperature 2h stands 5h, and 110 DEG C dry 4h；Then will be hydrated dried to day
Certain herbaceous plants with big flowers stalk ash is secondary to be placed in Muffle furnace, and 2h is calcined at 700 DEG C；By the sunflower stalk ash mechanical grinding grinds after low-temperature activation
End, is positioned over drier memory storage immediately after.
A kind of application of sunflower stalk ash solid catalyst in catalyzed transesterification, comprises the following steps, first will
Grease and methyl alcohol are according to mol ratio 12:1 is added in reactor, after being well mixed, adds urging for the oil quality fraction 5%
Agent, the stirring reaction 4.5h under 65 DEG C of temperature conditionss stops stirring, and suction filtration takes filtrate and reclaims catalyst, and filtrate is placed on
6h is stood in separatory funnel, is divided into two-layer, upper strata is biodiesel phase, separated that biodiesel is mutually depressurized goes out to remain first
Alcohol is that can obtain biodiesel, and biodiesel production rate is 85.35%.
Embodiment 4
A kind of preparation method of sunflower stalk ash solid catalyst, in accordance with the following steps, first places sunflower stalk ash
7h is dried at 110 DEG C in heated-air circulation oven, to remove wetting moisture and capillary moisture of the absorption in sunflower stalk ash；
Sunflower stalk ash after will be predrying is positioned in Muffle furnace, and 5h is calcined at 1100 DEG C；After by distilled water, high-temperature calcination to day
Certain herbaceous plants with big flowers stalk ash is according to mass ratio 6:1 mixing, stirring at normal temperature 3h stands 9h, and 100 DEG C dry 8h；Then will be hydrated dried to day
Certain herbaceous plants with big flowers stalk ash is secondary to be placed in Muffle furnace, and 4h is calcined at 600 DEG C；By the sunflower stalk ash mechanical grinding grinds after low-temperature activation
End, is positioned over drier memory storage immediately after.
A kind of application of sunflower stalk ash solid catalyst in catalyzed transesterification, comprises the following steps, first will
Grease and methyl alcohol are according to mol ratio 16:1 is added in reactor, after being well mixed, adds urging for the oil quality fraction 7%
Agent, the stirring reaction 5h under 60 DEG C of temperature conditionss stops stirring, and suction filtration takes filtrate and reclaim catalyst, and filtrate is placed on point
8h is stood in liquid funnel, is divided into two-layer, upper strata is biodiesel phase, separated that biodiesel is mutually depressurized goes out residual methanol
Biodiesel is can obtain, biodiesel production rate is 82.07%.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, although with reference to foregoing reality
Apply example to be described in detail the present invention, for a person skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic.It is all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (9)
1. the development approach of a kind of sunflower stalk ash solid catalyst, it is characterised in that the development approach comprises the following steps；
It is S1, predrying：The advance sunflower stalk ash collected is dried into water removal；
S2, high-temperature calcination：Pre-dried sunflower stalk ash is placed in Muffle furnace, temperature one and the time one of calcining is set,
Carry out high-temperature calcination；
S3, hydration：To distilled water is added in the sunflower stalk ash after high-temperature calcination, dried after being uniformly mixed；
S4, low-temperature activation：Sunflower stalk ash after hydration is placed in Muffle furnace, temperature two and the time two of calcining is set,
Carry out low-temperature activation；
It is S5, mechanical-moulded：Preserved being placed in drier after the sunflower stalk ash mechanical lapping after low-temperature activation.
2. the development approach of a kind of sunflower stalk ash solid catalyst according to claim 1, it is characterised in that described
Pre-drying step is that sunflower stalk ash is placed in heated-air circulation oven, and 5-7h is dried at 80-110 DEG C, is existed with removing absorption
Moisture in sunflower stalk ash.
3. the development approach of a kind of sunflower stalk ash solid catalyst according to claim 1, it is characterised in that described
High-temperature calcination be will be predrying after sunflower stalk ash be positioned in Muffle furnace, 800-1100 DEG C calcine 2-5h.
4. the development approach of a kind of sunflower stalk ash solid catalyst according to claim 1, it is characterised in that described
Hydration is according to mass ratio 3-6 by the sunflower stalk ash after distilled water, high-temperature calcination：1 mixing, stirring at normal temperature 1-3h stands 5-
9h, 100-120 DEG C dries 4-8h.
5. the development approach of a kind of sunflower stalk ash solid catalyst according to claim 1, it is characterised in that described
Low-temperature activation is will to be hydrated dried sunflower stalk ash to be placed in Muffle furnace, and 2-4h is calcined at 600-700 DEG C.
6. the development approach of a kind of sunflower stalk ash solid catalyst according to claim 1, it is characterised in that described
Mechanical-moulded is that the sunflower stalk ash mechanical grinding after low-temperature activation is clayed into power, and drier memory storage is positioned over immediately after.
7. a kind of development approach of sunflower stalk ash solid catalyst according to any one of claim 1 to 6, its feature
It is that the sunflower is selected from a kind of or their mixture in large and small three road eyebrow, dirty oil certain herbaceous plants with big flowers, U.S. certain herbaceous plants with big flowers and Hei Bei.
8. a kind of application of catalyst according to any one of claim 1 to 6 in ester exchange reaction, its feature exists
In by grease and methyl alcohol according to mol ratio 12-16:1 is added in reactor, after being well mixed, adds the oil quality point
The catalyst of number 5-7%, the stirring reaction 3.5-5h under 60-70 DEG C of temperature conditionss stops stirring, and suction filtration takes filtrate and recovery is urged
Agent, filtrate is placed in separatory funnel and stands 6-8h, is divided into two-layer, and upper strata is biodiesel phase, by biodiesel phase
Vacuum distillation is isolated residual methanol and can obtain biodiesel.
9. application of the catalyst according to claim 8 in ester exchange reaction, it is characterised in that the grease is selected from plants
Any one in thing oil, animal tallow and waste oil.
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Cited By (2)
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| CN111068721A (en) * | 2019-12-26 | 2020-04-28 | 山东大学 | Biomass ash solid base catalyst and preparation method and application thereof |
| CN113308277A (en) * | 2021-05-27 | 2021-08-27 | 内蒙古工业大学 | Application of sunflower straw ash in catalyzing steam gasification of medium-low-rank coal |
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|---|---|---|---|---|
| CN111068721A (en) * | 2019-12-26 | 2020-04-28 | 山东大学 | Biomass ash solid base catalyst and preparation method and application thereof |
| CN111068721B (en) * | 2019-12-26 | 2021-02-02 | 山东大学 | Biomass ash solid base catalyst and preparation method and application thereof |
| CN113308277A (en) * | 2021-05-27 | 2021-08-27 | 内蒙古工业大学 | Application of sunflower straw ash in catalyzing steam gasification of medium-low-rank coal |
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