CN108893134B - Method for preparing biofuel oil by catalytic cracking of high-acid-value waste oil - Google Patents
Method for preparing biofuel oil by catalytic cracking of high-acid-value waste oil Download PDFInfo
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- CN108893134B CN108893134B CN201810880556.2A CN201810880556A CN108893134B CN 108893134 B CN108893134 B CN 108893134B CN 201810880556 A CN201810880556 A CN 201810880556A CN 108893134 B CN108893134 B CN 108893134B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
- C10G3/44—Catalytic treatment characterised by the catalyst used
- C10G3/48—Catalytic treatment characterised by the catalyst used further characterised by the catalyst support
- C10G3/49—Catalytic treatment characterised by the catalyst used further characterised by the catalyst support containing crystalline aluminosilicates, e.g. molecular sieves
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
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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
Abstract
A method for preparing biofuel by catalytically cracking high-acid-value waste oil is characterized in that a mesoporous molecular sieve catalyst loaded with composite metal oxide is used for catalytically cracking the high-acid-value waste oil to prepare the biofuel, the method is characterized in that the mesoporous molecular sieve loaded with alkaline earth metal oxide and lanthanum oxide in situ is used as the catalyst, the mass ratio of the waste oil to the catalyst is 5:1-100:1, the mass ratio of the loaded alkaline earth metal oxide to the lanthanum oxide to the mesoporous molecular sieve SBA-15 is 1:1:10-1:30:200, the reaction temperature is 650 ℃, the reaction time is 1.0-6.0h, the hydrocarbon-rich biofuel is prepared, and the catalyst is recycled and reused. Compared with the prior art: 1. the catalyst has good catalytic performance and outstanding shape-selective catalytic capability. 2. The catalyst is easy to recover and can be recycled, and after the catalyst is recycled for 10 times, the yield of the biofuel is still more than 85%.
Description
Technical Field
A method for preparing biofuel oil by catalytic cracking of waste oil, namely a novel method for preparing biofuel oil by catalytic cracking of high-acid-value waste oil by a mesoporous molecular sieve catalyst loaded with composite metal oxide.
Background
The increasing decrease of petroleum resources leads to energy shortage and sharp rise of petroleum price, people pay more and more attention to the substitute of petroleum fuel, and the bio-fuel oil is a petroleum fuel oil energy substitute which is attracted attention in recent years. The biofuel oil has combustion performance equivalent to that of petroleum fuel, is environment friendly and has resource regeneration, and is one of ideal fuel for replacing petroleum fuel oil. At present, the biofuel oil is mainly prepared by taking grease as a raw material and catalyzing ester exchange reaction by using an alkaline catalyst, and the process has the defects that: the obtained biofuel has poor low-temperature fluidity and stability, low heat value and difficulty in refining glycerin by-products. In addition, the high acid value waste oil contains more carboxylic acid acidic substances, so that before the base catalysis transesterification reaction, the esterification reaction treatment is carried out by adopting an acidic catalyst, and the purposes of utilizing carboxylic acid in the raw oil and fat and reducing the acid value of the raw oil are achieved. Otherwise, the acidic substance in the raw oil can directly react with the alkali catalyst in the process of the ester exchange reaction catalyzed by the alkali catalyst, so that on one hand, the consumption of the alkali catalyst is increased, and on the other hand, the generated carboxylate has the performance of an anionic surfactant, so that the reaction mixture is emulsified when being subjected to post-treatment water washing operation, and oil-water phase separation is difficult to realize. Therefore, the preparation of the bio-fuel oil by the ester exchange reaction of the waste oil with high acid value belongs to an environment-friendly process. Compared with the ester exchange technology, the method has the advantages of direct catalytic cracking of the grease, one-step directional preparation of the high-quality biomass fuel oil, low production cost, simplified process, no generation of glycerin byproducts, less discharge of three wastes and the like. However, the raw materials of the current catalytic pyrolysis oil mostly adopt high-quality raw oil such as rubber seed oil, soybean oil and rapeseed oil, and the bio-fuel oil prepared by adopting high-acid-value waste oil as the raw material through the pyrolysis reaction has the defects of complex components, high content of acidic substances and the like, so that the prepared bio-fuel oil has the problems of low yield, high acid value, low heat value and the like. Therefore, the bio-fuel oil is prepared by catalytically cracking the waste oil by the mesoporous molecular sieve loaded with the composite metal oxide.
Disclosure of Invention
The invention aims to replace the traditional production process of producing the biofuel by using the catalyst and develop the production process of preparing the biofuel by directly catalyzing and cracking the waste oil and fat by the catalyst under the high-temperature reaction.
Based on the above, the invention relates to a method for preparing biofuel oil by catalytic cracking of high acid value waste oil, namely a mesoporous molecular sieve catalyst loaded with composite metal oxide for catalytic cracking of high acid value waste oilThe novel method for preparing the biofuel oil from the acid value waste oil is characterized in that mesoporous molecular sieve loaded with alkaline earth metal oxide and lanthanum oxide in situ is used as a catalyst, the mass ratio of the waste oil to the catalyst is 5:1-100:1, the mass ratio of the loaded alkaline earth metal oxide, the loaded lanthanum oxide to the mesoporous molecular sieve SBA-15 is 1:1:10-1:30:200, the reaction temperature is 300-650 ℃, the reaction time is 1.0-6.0h, the hydrocarbon-rich biofuel oil is prepared, and the catalyst is recycled, wherein the mesoporous molecular sieve loaded with the composite metal oxide is MgO/La/mesoporous molecular sieve2O3-SBA-15、CaO/La2O3-SBA-15、BaO/La2O3-SBA-15 or SrO/La2O3-SBA-15, wherein the acid value of the waste oil is 8-42mgKOH g-1Waste oil and fat with high acid value.
The invention is characterized in that the reaction conditions are that the mass ratio of the waste oil and the catalyst is 15:1-45:1, the mass ratio of the supported alkaline earth metal oxide to the lanthanum oxide to the mesoporous molecular sieve SBA-15 is 1:5:50-1:15:150, the reaction temperature is 380-480 ℃, and the reaction time is 1.0-2.5 h.
The invention solves the technical problem by the following technical scheme:
uses a load type mesoporous molecular sieve MgO/La2O3The catalytic cracking acid value of the catalyst SBA-15 is 40mgKOH g-1The waste oil and fat are used as an example to explain a specific technical scheme.
Preparation of the catalyst: MgO/La2O3The synthesis of the-SBA-15 catalyst adopts P123 as a template agent, tetraethoxysilane TEOS as a silicon source and magnesium chloride MgCl2And lanthanum chloride LaCl3Inorganic salt, hydrochloric acid and deionized water which are needed for synthesis, wherein the molar ratio of the raw materials is 1TEOS:0.02P123:0.1MgCl2:0.1LaCl3:6HCl:192H2And O. The specific synthesis steps are as follows: 20g P123 and calculated amount of MgCl2And LaCl3Dissolved in 150g of deionized water and 600g of 2mol/L HCl, 42.5g of TEOS were added with stirring at 40 ℃ and stirred for 24h at 40 ℃. Then the mixed solution is transferred to a 1000mL crystallization kettle and crystallized for 48h at 100 ℃. Then, the crystallized mixed solution is transferred into a three-neck flask, and the temperature is reducedThe solvent was evaporated to dryness under reduced pressure to obtain a white precipitate. Finally, roasting at 550 ℃ for 6h to obtain MgO and La2O3And SBA-15 with the mass ratio of 1:8:50 molecular sieve MgO/La2O3SBA-15 catalyst 4.0 g.
Preparing the biofuel oil by catalytic cracking of the waste oil: an acid value of 35 mgKOH. g-120g of waste oil and fat, MgO and La2O3SBA-15 weight ratio of MgO/La of catalyst to SBA-15 is 1:8:502O3SBA-150.8 g was charged into a reaction flask equipped with a thermocouple and reacted at 430 ℃ for 1.5 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture such as the catalyst remaining in the reaction vessel after the reaction is washed with dichloroethane, filtered, dried, and the catalyst is recovered and recovered. The conversion rate of the waste oil is 100 percent, the yield of the biofuel is 88.3 percent, and the acid value of the biofuel is 8mgKOH g-1And the content of the aliphatic hydrocarbon of C6-C17 in the obtained biofuel is 78.6 percent.
Compared with the traditional reaction, the invention is characterized in that:
1. the catalyst has good catalytic performance and outstanding shape-selective catalytic capability.
2. The catalyst is easy to recover and can be recycled, and after the catalyst is recycled for 10 times, the yield of the biofuel is still more than 85%.
Detailed description of the invention
The process of the present invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1: an acid value of 35 mgKOH. g-120g of waste oil and fat, MgO and La2O3SBA-15 weight ratio of MgO/La of catalyst to SBA-15 is 1:8:502O3SBA-150.8 g was charged into a reaction flask equipped with a thermocouple and reacted at 430 ℃ for 1.5 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; remains after the reactionThe mixture of the catalyst and the like in the reactor was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 100 percent, the yield of the biofuel is 88.3 percent, and the acid value of the biofuel is 8mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 78.6 percent.
Comparative example 1: an acid value of 35 mgKOH. g-120g of waste oil and fat, MgO and SBA-15 with the mass ratio of 1:50, MgO-SBA-150.8 g of catalyst are put into a reaction bottle with a thermocouple and react for 1.5h at 430 ℃. The air in the apparatus was removed with nitrogen before the reaction occurred. Cracked steam obtained in the reaction process flows into a collecting bottle after being condensed by cooling water, and non-condensable gas is collected by a vacuum air bag. After the reaction, the mixture remained in the reaction flask was washed with dichloroethane, filtered, dried and the catalyst was recovered. The conversion rate of the waste oil and fat is 74.7 percent, the yield of the biofuel is 62.5 percent, and the acid value of the biofuel is 14mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 76.3 percent.
Comparative example 2: an acid value of 35 mgKOH. g-120g of waste oil and fat of La2O3And SBA-15 by mass ratio of 8:50 catalyst La2O3SBA-150.8 g was charged into a reaction flask equipped with a thermocouple and reacted at 430 ℃ for 1.5 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 88.5 percent, the yield of the biofuel is 73.2 percent, and the acid value of the biofuel is 15mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 73.9 percent.
Comparative example 3: an acid value of 35 mgKOH. g-120g of waste oil and fat and 150.8 g of catalyst SBA are put into a reaction bottle with a thermocouple and reacted for 1.5h at 430 ℃. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. The cracked product obtained in the cracking process is collected, weighed and calculated after being condensed by cooling waterYield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil and fat is 42.3 percent, the yield of the biofuel is 31.0 percent, and the acid value of the biofuel is 22mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 60.8 percent.
Comparative example 4: an acid value of 35 mgKOH. g-120g of the waste oil and fat and 0.8g of MgO as a catalyst were put into a reaction flask equipped with a thermocouple and reacted at 430 ℃ for 1.5 hours. The air in the apparatus was removed with nitrogen before the reaction occurred. Cracked steam obtained in the reaction process flows into a collecting bottle after being condensed by cooling water, and non-condensable gas is collected by a vacuum air bag. After the reaction, the mixture remained in the reaction flask was washed with dichloroethane, filtered, dried and the catalyst was recovered. The conversion rate of the waste oil is 65.0 percent, the yield of the biofuel is 46.1 percent, and the acid value of the biofuel is 15mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 63.3 percent.
Comparative example 5: an acid value of 35 mgKOH. g-120g of waste oil and fat of (2), catalyst La2O30.8g was charged into a reaction flask equipped with a thermocouple and reacted at 430 ℃ for 1.5 hours. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil and fat is 68.8 percent, the yield of the biofuel is 51.9 percent, and the acid value of the biofuel is 17mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 62.0 percent.
Example 2: an acid value of 35 mgKOH. g-120g of waste oil and fat, MgO and La2O3SBA-15 is the catalyst MgO/La with the mass ratio of 1:1:102O3SBA-150.2 g was charged into a reaction flask equipped with a thermocouple and reacted at 300 ℃ for 6.0 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. CrackingCondensing the cracking product obtained in the process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 95.5 percent, the yield of the biofuel is 82.3 percent, and the acid value of the biofuel is 11mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 74.0 percent.
Example 3: an acid value of 16 mgKOH. g-120g of waste oil and fat, CaO and La2O3And SBA-15 weight ratio of 1:30:200 catalyst CaO/La2O3SBA-154 g was charged into a reaction flask equipped with a thermocouple and reacted at 650 ℃ for 1.0 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 100 percent, the yield of the biofuel is 87.2 percent, and the acid value of the biofuel is 9mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 79.2 percent.
Example 4: an acid value of 42 mgKOH. g-120g of waste oil and fat of BaO, La2O3SBA-15 and SBA-15 are in a mass ratio of 1:10:100, and the catalyst is BaO/La2O3SBA-152.0 g was charged into a reaction flask equipped with a thermocouple and reacted at 380 ℃ for 2.5 hours. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 82.3 percent, the yield of the biofuel is 75.5 percent, and the acid value of the biofuel is 13mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 76.4 percent.
Example 5: an acid value of 8 mgKOH. g-120g of waste oil and fat of SrO, La2O3SBA-15 weight ratio of the catalyst SrO/La of 1:15:702O3SBA-150.4 g was charged into a reaction flask equipped with a thermocouple and reacted at 480 ℃ for 4.0 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of waste oil is 96.7 percent, the yield of the biofuel is 84.2 percent, and the acid value of the biofuel is 3mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 78.6 percent.
Example 6: an acid value of 42 mgKOH. g-120g of waste oil and fat of BaO, La2O3SBA-15 and SBA-15 are in a mass ratio of 1:10:100, and the catalyst is BaO/La2O3SBA-152.0 g was charged into a reaction flask equipped with a thermocouple and reacted at 400 ℃ for 5.0 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction was washed with dichloroethane, filtered, dried, and the catalyst was recovered. The conversion rate of the waste oil is 100 percent, the yield of the biofuel is 87.5 percent, and the acid value of the biofuel is 11mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 79.0 percent.
Example 7: an acid value of 40 mgKOH. g-120g of waste oil and fat, CaO and La2O3And SBA-15 weight ratio of 1:10:100 catalyst CaO/La2O3SBA-150.5 g was charged into a reaction flask equipped with a thermocouple and reacted at 450 ℃ for 2.0 h. Before the reactor is heated, the air in the device is replaced and exhausted by nitrogen. Condensing the cracking product obtained in the cracking process by cooling water, collecting, weighing and calculating the yield; collecting the non-condensable gas cracking products by using a vacuum air bag; the mixture of the catalyst and the like remaining in the reaction vessel after the reaction is washed with dichloroethane, filtered,Drying and recovering the catalyst. The conversion rate of the waste oil is 100 percent, the yield of the biofuel is 88.6 percent, and the acid value of the biofuel is 6mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 78.5 percent.
Example 8: CaO/La recovered in example 12O3SBA-15 is a catalyst and the cleavage reaction is carried out under the same conditions as in example 1. The results show that when the catalyst is repeatedly used for the 5 th time, the conversion rate of the waste oil is 100 percent, the yield of the biofuel is 87.6 percent, and the acid value of the biofuel is 7mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 78.5 percent; when the catalyst is repeatedly used for the 10 th time, the conversion rate of the waste oil is 100 percent, the yield of the biofuel is 86.5 percent, and the acid value of the biofuel is 8mgKOH g-1Wherein the content of C6-C17 aliphatic hydrocarbon in the biofuel is 76.8 percent.
Claims (2)
1. A method for preparing biofuel by catalytic cracking of high-acid-value waste oil is characterized in that a mesoporous molecular sieve catalyst loaded with composite metal oxide is used for preparing the biofuel by catalytic cracking of the high-acid-value waste oil, the method is characterized in that the mesoporous molecular sieve catalyst loaded with alkaline earth metal oxide and lanthanum oxide in situ is used as the catalyst, the mass ratio of the waste oil to the catalyst is 5:1-100:1, the mass ratio of the loaded alkaline earth metal oxide to the lanthanum oxide to the mesoporous molecular sieve SBA-15 is 1:1:10-1:30:200, the reaction temperature is 300 ℃. 650 ℃, the reaction time is 1.0-6.0h, the hydrocarbon-rich biofuel is prepared, and the catalyst is recycled and reused, and the mesoporous molecular sieve catalyst loaded with the composite metal oxide is MgO/La/mesoporous molecular sieve catalyst2O3-SBA-15、CaO/La2O3-SBA-15、BaO/La2O3-SBA-15 or SrO/La2O3-SBA-15, wherein the acid value of the waste oil is 8-42mgKOH g-1Waste oil and fat with high acid value.
2. The preparation method according to claim 1, wherein the mass ratio of the waste oil and the catalyst is 15:1-45:1, the mass ratio of the supported alkaline earth metal oxide, the lanthanum oxide and the mesoporous molecular sieve SBA-15 is 1:5:50-1:15:150, the reaction temperature is 380-.
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| CN101906312A (en) * | 2009-06-05 | 2010-12-08 | 北京瑞增兰宇新能源有限公司 | Method for preparing hydrocarbon fuel oil by mixing biomass oil and animal and vegetable oil |
| CN102936512A (en) * | 2012-10-07 | 2013-02-20 | 青岛科技大学 | Method for preparing liquid fuel oil through catalytic cracking of biological oil by using alkaline MCM-41 |
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| CN101906312A (en) * | 2009-06-05 | 2010-12-08 | 北京瑞增兰宇新能源有限公司 | Method for preparing hydrocarbon fuel oil by mixing biomass oil and animal and vegetable oil |
| CN102936512A (en) * | 2012-10-07 | 2013-02-20 | 青岛科技大学 | Method for preparing liquid fuel oil through catalytic cracking of biological oil by using alkaline MCM-41 |
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