CN100586568C - Preparation method for solid base catalyst for biological diesel oil synthesis - Google Patents
Preparation method for solid base catalyst for biological diesel oil synthesis Download PDFInfo
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- CN100586568C CN100586568C CN200710171903A CN200710171903A CN100586568C CN 100586568 C CN100586568 C CN 100586568C CN 200710171903 A CN200710171903 A CN 200710171903A CN 200710171903 A CN200710171903 A CN 200710171903A CN 100586568 C CN100586568 C CN 100586568C
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- 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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The invention discloses a solid base catalyst for synthesizing biodiesel, a preparation method and use thereof. The method of the invention has the advantages of simple technique, rich raw materials,low catalyst production cost and the prepared catalyst has high catalytic efficiency, good reproducibility and environmental protection.
Description
Technical field
The present invention relates to green, field of renewable energy technology, specifically be meant a kind of efficient, cheap solid base catalyst, preparation method and its usage that catalysis fatty glyceride and methyl alcohol carry out the ester exchange reaction biodiesel synthesis that be used for.
Background technology
At present, biodiesel oil preparing process mainly contains direct mixing method, mini-emulsion process, high-temperature cracking method and ester-interchange method.Mini-emulsion process is that vegetable and animals oils, solvent and micro-emulsifier are mixed, and makes the method for the low micro emulsion body of more former vegetable and animals oils viscosity.Though the biodiesel of this method preparation can reduce the animals and plants oil viscosity, Cetane number is not high, and problem such as carbon deposit and lubricant pollution is difficult to solve in the burning.Direct mixing method is plant and mineral diesel directly to be mixed carry out combustion method, and the viscosity of this type fuel is too high and be eliminated.The high-temperature cracking method process is simple, does not have pollutant to produce, and shortcoming is at high temperature to carry out, and needs catalyst, the cracking apparatus costliness, and the difficult control of the extent of reaction, output is not high yet.
Industrial production biodiesel mainly adopts ester-interchange method.Ester-interchange method is ester exchange reaction to be taken place for vegetable and animals oils and various short chain alcohol obtain less fatty acid ester of molecular weight and glycerine under catalyst action.The fatty acid ester that these molecular weight are less can be directly as diesel fuel because viscosity is lower.The ester-interchange method that is used to prepare biodiesel at present can be divided into homogeneous catalysis ester-interchange method, enzymatic ester method, overcritical ester-interchange method and heterogeneous catalysis ester-interchange method substantially.
The homogeneous catalysis method is present the most frequently used method, and the catalyst of employing is generally hydrogen-oxygen sodium or potassium hydroxide, and advantage is less demanding to reaction condition, and reaction efficiency is better.But shortcoming is that the saponification side reaction takes place easily, and product is difficult to separate, and catalyst can not reuse, and particularly needs washing in subtractive process, thereby produces more sewage, and environmental pollution is big.Enzymatic and overcritical synthetic method require high to reaction condition, cost is big, also have very big distance with production application at present.In fact the heterogeneous catalysis ester-interchange method is exactly the method that adopts catalysis of solid catalyst.Adopt the main advantage of solid catalyst to be, catalyst separation is easy, and post processing is simple, and environmental pollution is little.
Be used for the synthetic solid catalyst of biodiesel and mainly be divided into solid acid and the big class of solid base, the solid acid catalyst is generally relatively good to the catalytic effect that adopts low-carbon alcohols and aliphatic acid biodiesel synthesis, but poor for the catalytic effect that adopts low-carbon alcohols and fatty glyceride biodiesel synthesis.Because the main composition of vegetable and animals oils is a fatty glyceride, have only and just contain the part free fatty in the discarded vegetable and animals oils, so the solid acid catalyst generally only is used in and utilizes in the pre-treatment of waste oils and fats when preparing biodiesel raw material.And the solid alkali catalyst is better to the effect of catalysis low-carbon alcohols and fatty glyceride biodiesel synthesis, so the solid alkali catalyst is the emphasis of developing at present.
At present, solid bases catalyst type is many, as loaded catalyst, strong-base anion-exchange resin, the various metal oxide that is insoluble to low-carbon alcohols or hydroxide or the like.But these catalyst exist or price is higher, complicated process of preparation, or problem such as catalytic effect is not good.
Directly adopt calcium carbonate, calcium oxide, calcium hydroxide to report more as the synthetic alkali solid catalyst of biodiesel, advantage is that the raw material sources of preparation catalyst are abundant, cheap, but sixty-four dollar question is that catalytic effect is poor excessively under the synthesis under normal pressure condition, in order to improve the conversion ratio of biodiesel, just need to adopt and prolong the reaction time or adopt reaction condition (Te Xu Gong Open 2001-271090, Te Xu Gong Open 2004-35873 such as high temperature, high pressure), so practicality is poor.
Summary of the invention
The purpose of this invention is to provide a kind of solid base catalyst that utilizes methyl alcohol and vegetable and animals oils biodiesel synthesis.
Purpose of the present invention also provides a kind of preparation method who utilizes the solid base catalyst of methyl alcohol and vegetable and animals oils biodiesel synthesis, and this catalyst manufacture craft is simple, and cost of material is cheap, and the reclaiming utilization is convenient, excellent catalytic effect.
Another object of the present invention provides the purposes of above-mentioned solid base catalyst, and this catalyst is used for methyl alcohol and vegetable and animals oils biodiesel synthesis.
Solid base catalyst of the present invention is by high-temperature calcination calcium carbonate, calcium oxide hydrogen or calcium oxide, directly cools off the calcium oxide solid base catalyst that calcium methoxide is contained on the surface that makes with methyl alcohol or methanol steam then.
The preparation method of solid base catalyst of the present invention may further comprise the steps:
1. calcium carbonate, calcium oxide or calcium hydroxide were calcined 0.5-4 hour in 600-1000 ℃ high temperature furnace.
With calcined calcium carbonate or calcium oxide, calcium hydroxide directly takes out or cool to 400-950 ℃ of taking-up in high temperature furnace naturally.
3. the calcined material of taking out in the step 2 is put into the methanol liquid cool to room temperature with the methanol liquid cast or with calcined material, obtain the catalyst of the present invention's preparation.Also the calcined material in the step 2 directly can be put into the closed container that is full of methanol steam together with the container of splendid attire calcined material and naturally cool to room temperature, obtain the catalyst of the present invention's preparation.Make closed container be full of the measure of methanol steam, can adopt and in closed container, put into methanol liquid in advance, several different methods such as vacuumize then.
4. the catalyst seal packing that step 3 is obtained is preserved, or is directly used in methyl alcohol or methyl alcohol and the reaction of vegetable and animals oils biodiesel synthesis.
Experiment shows, according to the solid base catalyst of above step preparation methyl alcohol and fatty glyceride being carried out ester exchange is that fatty acid methyl ester (biodiesel) has very high catalytic efficiency.The high reason of solid base catalyst catalytic efficiency for understanding fully that the present invention prepares has detected its composition with infrared spectrum, as shown in Figure 1.And compared the diffractive features of common calcium oxide and catalyst of the present invention by X-ray scattering detector, as shown in Figure 2.The solid base catalyst of the present invention's preparation has the calcium methoxide feature.This solid base catalyst catalytic efficiency that may be the present invention prepares is higher than the major reason of ordinary calcium carbonate, calcium oxide, calcium hydroxide far away.
Advantage of the present invention is:
1. adopt the catalyst efficient height of this method preparation, be equivalent to the calcium methoxide for preparing by calcium metal in the document Leader.
2. the equipment of the process route of preparation catalyst and use is simple, abundant raw material and cheap, and the Catalyst Production cost is low.
3. Zhi Bei catalyst is renewable, and renovation process is simple.
4. Zhi Bei catalyst without any pollution, is the environmental type catalyst to environment.
Description of drawings
Fig. 1 is the infrared spectrogram of solid catalyst of the present invention.
Fig. 2 is the X-ray scattering comparison diagram of solid catalyst of the present invention and common calcium oxide.
Among Fig. 2, A is a solid catalyst of the present invention, and B is a calcium oxide reagent.
The specific embodiment
Followingly in conjunction with the embodiments the present invention is described in further detail, but can not limit content of the present invention.
Embodiment 1
Take by weighing CaO10g, (NH
4)
2CO
325g in the 800ml beaker, adds 200ml water, adds emulsifying agent (tween) 2g, puts into the cold bath cooling, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes is carried out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 900 ℃, calcining was burnt 2 hours, was cooled to 650 ℃, took out the back and made catalyst with the absolute methanol cooling.
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for above-mentioned catalyst of 1g and 21.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, catalyst separation is gone out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 97.3%.
Take by weighing calcium carbonate reagent (analyzing pure) 3g and be warming up to 900 ℃ in high temperature resistance furnace in crucible, calcining was burnt 2 hours, was cooled to 650 ℃, took out the back and made catalyst with the absolute methanol cooling.
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for above-mentioned catalyst of 1g and 21.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, catalyst separation is gone out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 95.6%.
Embodiment 3
Take by weighing Ca (Ac)
240g, (NH
4)
2CO
330g in the 800ml beaker, adds 300ml water, adds emulsifying agent (tween) 3g, puts into the cold bath cooling, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes carries out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 900 ℃, calcined 2 hours, be cooled to 500 ℃, take out the back and make catalyst with the absolute methanol cooling.
With 50g soybean oil (density is 0.92g/cm3), above-mentioned catalyst of 1g and 21.5ml methyl alcohol (density is 0.792g/cm3) mixed liquor is put into 250ml triangle ground flask, be placed on and be heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, react after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 93.5%.
Embodiment 4
Take by weighing Ca (Ac)
240g, (NH
4)
2CO
330g in the 800ml beaker, adds 300ml water, puts into the cold bath cooling, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes carries out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 950 ℃, calcined 3 hours, be cooled to 700 ℃, take out the back and make catalyst with the absolute methanol cooling.
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for above-mentioned solid catalyst of 1g and 20.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor moved to make catalyst separation in the centrifuge by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 98.4%.
Embodiment 5
Take by weighing Ca (Ac)
240g, (NH
4)
2CO
330g in the 800ml beaker, adds 300ml water, adds emulsifying agent (tween) 3g, puts into the cold bath cooling, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes carries out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 900 ℃, calcined 2 hours, after the taking-up, put into the surplus drier that methyl alcohol is arranged of lower floor, vacuumized 0.5 hour.
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for above-mentioned catalyst of 1g and 20.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 96.7%.
Embodiment 6
Take by weighing Ca (Ac)
240g, (NH
4)
2CO
330g in the 800ml beaker, adds 300ml water, adds emulsifying agent (tween) 3g, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes carries out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 900 ℃, calcination 2 hours is cooled to 650 ℃, takes out the back and makes catalyst with the absolute methanol cooling.
With the 50g rapeseed oil, (density is 0.792g/cm for above-mentioned catalyst of 1g and 21.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 97.4%.
Embodiment 7
Take by weighing Ca (Ac)
240g, (NH
4)
2CO
330g in the 800ml beaker, adds 300ml water, adds emulsifying agent (tween) 3g, puts into the cold bath cooling, and high-speed stirred is 1 hour simultaneously, generates CaCO
3The calcium carbonate that makes carries out suction filtration, then puts into oven drying, keep 105 ℃ 2 hours, wait to parch the back and grind in small, broken bitsly, put into drier and preserve stand-by.Take by weighing 1.786gCaCO
3In crucible, in high temperature resistance furnace, be warming up to 900 ℃, calcined 2 hours, be cooled to 650 ℃, take out the back and make catalyst with the absolute methanol cooling.
With the filtered fried waste oil of using of 50g, above-mentioned catalyst of 1g and 21.5ml methyl alcohol (density is 0.792g/cm3) mixed liquor is put into 250ml triangle ground flask, be placed on and be heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, react after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 97.3%.
Embodiment 8
With the catalyst of separating among the embodiment 4, add fresh soybean oil 50g (density is 0.92g/cm at every turn
3) and 21.5ml methyl alcohol (density is 0.792g/cm
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, catalyst separation is gone out.After using catalyst 10 times repeatedly by the aforesaid operations step, reactant liquor is poured in the separatory funnel, left standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 90.3%.
Embodiment 9
Catalyst oven dry with separating in the embodiment 4 places crucible, is warming up to 900 ℃ in high temperature resistance furnace, calcines 2 hours, is cooled to 650 ℃, takes out the back and makes catalyst with the absolute methanol cooling.
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for above-mentioned regenerated catalyst of 1g and 20.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 97.3%.
Comparative example:
(density is 0.92g/cm with the 50g soybean oil
3), (density is 0.792g/cm for 1g medicine calcium oxide (analyzing pure) and 20.5ml methyl alcohol
3) mixed liquor puts into 250ml triangle ground flask, is placed on and is heated with stirring to 67-68 ℃ on the constant temperature blender with magnetic force, reacts after 2 hours, stop to stir and heating.Reactant liquor is moved to centrifuge, will make catalyst separation by oneself and go out, pour into then in the separatory funnel, leave standstill, be divided into two-layer up and down.Behind upper strata water-bath distillation for removing methanol, recording conversion ratio is 14.3%.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (5)
1, a kind of preparation method who is used for the synthetic solid base catalyst of biodiesel is characterized in that: high-temperature calcination calcium carbonate, calcium oxide or calcium hydroxide; Above-mentioned calcined material is cooled to 400-950 ℃, then with methyl alcohol or in methanol steam cool to room temperature obtain the solid base catalyst that calcium methoxide is contained on the surface; Described calcining heat is 600-1000 ℃, and calcination time is 0.5-4 hour.
2, a kind of preparation method who is used for the synthetic solid base catalyst of biodiesel as claimed in claim 1, it is characterized in that: described calcium carbonate is natural whiting or synthetic calcium carbonate.
3, a kind of preparation method who is used for the synthetic solid base catalyst of biodiesel as claimed in claim 1, it is characterized in that: described calcining heat is 700-950 ℃.
4, a kind of preparation method who is used for the synthetic solid base catalyst of biodiesel as claimed in claim 1, it is characterized in that: described calcination time is 1-2 hour.
5, a kind of preparation method who is used for the synthetic solid base catalyst of biodiesel as claimed in claim 1 is characterized in that: the temperature of described calcined material before directly cooling off with methyl alcohol or methanol steam is 600-800 ℃.
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| CN101870893B (en) * | 2010-06-03 | 2013-05-22 | 濮阳市中油石化有限公司 | Diesel oil-saving catalyst and preparation method thereof |
| US9029583B2 (en) | 2011-02-14 | 2015-05-12 | Council Of Scientific & Industrial Research | Process for the preparation of fatty acid alkyl esters (biodiesel) from triglyceride oils using eco-friendly solid base catalysts |
| CN102430400B (en) * | 2011-09-05 | 2013-01-30 | 贵州大学 | Preparation method for natural calcium base porous solid alkaline catalyst for catalysis in interesterification |
| CN106345448B (en) * | 2016-08-26 | 2019-02-22 | 戴景明 | A kind of base catalyst preparing biodiesel |
| CN108863778A (en) * | 2018-07-24 | 2018-11-23 | 寿光诺盟化工有限公司 | A kind of preparation method of diallyl p phthalate |
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| Title |
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| 制备生物柴油酯交换催化剂的研究进展. 陈鸿庆等.广州化工，第34卷第4期. 2006 |
| 制备生物柴油酯交换催化剂的研究进展. 陈鸿庆等.广州化工，第34卷第4期. 2006 * |
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