CN108855030B - Composite solid base catalyst and application of composite solid base catalyst in preparation of biodiesel by catalyzing ester exchange - Google Patents
Composite solid base catalyst and application of composite solid base catalyst in preparation of biodiesel by catalyzing ester exchange Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- 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
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Abstract
The invention discloses a composite solid base catalyst and application thereof in preparing biodiesel by catalytic ester exchange, wherein the catalyst is prepared by loading an active component A and an active component B in aluminum oxide, zirconium dioxide or magnesium oxide, wherein the active component A is Na, K or Cs, and the active component B is any one or more than two of Ba, Ca, Ce and La; the loading capacity of the active component A is 4-12% and the loading capacity of the active component B is 0.1-1% by weight of the carrier. The catalyst has the advantages of simple preparation process, low cost, low requirements on acid value and water content in raw materials for preparing the biodiesel by ester exchange, less saponification byproducts, simple product post-treatment process and long service life of the catalyst.
Description
Technical Field
The invention belongs to the technical field of biodiesel preparation, and particularly relates to a composite solid base biodiesel catalyst.
Background
The biodiesel is fatty acid methyl ester or ethyl ester prepared from vegetable oil (such as rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, etc.), animal oil (such as fish oil, lard, beef tallow, mutton fat, etc.), waste oil or microbial oil by transesterification with methanol or ethanol. Compared with petroleum diesel, the biodiesel has the characteristics of good combustion performance, good low-temperature starting performance, excellent lubricating performance, almost no sulfur and arene, biodegradability, wide raw material source, renewability and the like, and is a typical 'green energy'. The biodiesel can be used as a clean liquid fuel for replacing petroleum diesel, and has great potential and wide market prospect.
In the traditional production of biodiesel, concentrated sulfuric acid, benzenesulfonic acid, phosphoric acid, sodium methoxide, sodium hydroxide, potassium hydroxide and other homogeneous acid-base catalysts are often adopted for production. The biodiesel conversion rate of the catalysts is high, but the subsequent treatment needs water washing to remove the residual catalyst in the product, so that a large amount of waste water is generated on one hand, and the loss of the biodiesel product is caused on the other hand. The heterogeneous catalyst can simplify the separation process of the product and has the characteristic of reutilization. Heterogeneous catalysts for the chemical preparation of biodiesel include solid acid catalysts and solid base catalysts. The solid acid catalyst has good adaptability to raw oil with high free fatty acid content, but needs higher reaction temperature and longer reaction time. The solid base catalyst has high reaction activity and mild reaction conditions, but requires low acid value and water content in the raw materials.
Disclosure of Invention
Aiming at the defects of the solid base catalyst, the invention provides the composite solid base catalyst which is suitable for the ester exchange reaction of various animal and vegetable oils (natural oils such as rapeseed oil, soybean oil, recycled cooking oil, inferior oil after oil processing and the like) with the acid value of 2-10, and has the advantages of less catalyst consumption and high catalytic efficiency.
The composite solid base catalyst used for solving the technical problems is prepared by taking any one of alumina, zirconium dioxide and magnesium oxide as a carrier and loading an active component A and an active component B, wherein the active component A is any one of Na, K and Cs, and the active component B is any one or more than two of Ba, Ca, Ce and La; the loading capacity of the active component A is 4-12% and the loading capacity of the active component B is 0.1-1% by weight of the carrier.
The composite solid base catalyst further preferably takes alumina as a carrier, the active component A is K, and the active component B is Ba and Ca or Ba and La; based on the carrier, the loading capacity of K is 4-5%, the loading capacity of Ba is 0.3-0.4%, and the loading capacity of Ca or La is 0.1%.
The composite solid base catalyst further preferably comprises an active component A of Cs and an active component B of Ba and/or La; calculated by the carrier, the loading capacity of Cs is 4-6%, when the active component B is Ba, the loading capacity of Ba is 0.5-0.6%, when the active component B is La, the loading capacity of La is 0.2-0.3%, when the active component B is Ba and La, the loading capacity of Ba is 0.1-0.2%, and the loading capacity of La is 0.1-0.2%.
The composite solid base catalyst further preferably takes zirconium oxide as a carrier, an active component A is Na, and an active component B is Ce; the loading capacity of Na is 8-9% and the loading capacity of Ce is 0.1-0.2% based on the carrier.
The composite solid base catalyst further preferably comprises an active component A of K or Na and an active component B of Ba and Ce; based on the carrier, the loading capacity of K or Na is 5-7%, the loading capacity of Ba is 0.2-0.3%, and the loading capacity of Ce is 0.1-0.2%.
The preparation method of the composite solid base catalyst comprises the following steps: according to the composition of the catalyst, firstly, dipping a carrier and a soluble salt water solution of an active component A for 10-20 hours by an isometric dipping method, and drying; and then, impregnating the compound of the carrier and the active component A by using a soluble salt water solution of the active component B for 5-10 hours, drying, and roasting at 400-600 ℃ for 4-6 hours to obtain the composite solid base catalyst.
The invention discloses an application of a composite solid base catalyst in preparing biodiesel by catalyzing ester exchange of waste oil, which comprises the following steps: adding a catalyst accounting for 5-15% of the mass of the waste oil with the acid value of 2-10 mgKOH/g, heating to 50-60 ℃, introducing gasified methanol, continuously heating to 80-100 ℃, and reacting for 1-3 hours.
The waste oil is any one of waste oil, hogwash oil and acidified oil.
The invention discloses an application of a composite solid base catalyst in preparing biodiesel by catalyzing ester exchange of waste oil, which comprises the following steps: adding a catalyst accounting for 5-15% of the mass of the waste oil with the acid value of 2-10 mgKOH/g, heating to 50-60 ℃, introducing gasified methanol, continuously heating to 80-100 ℃, and reacting for 1-3 hours.
The waste oil is swill-cooked dirty oil, acidified oil, etc.
The catalyst has low cost and simple preparation process, has low requirements on acid value and water content in raw materials when being used for biodiesel transesterification, and has few saponification byproducts; the product post-treatment process is simple, and the service life of the catalyst is long.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to these examples.
Example 1 using alumina as a carrier, 8.5g of alumina was impregnated with 11mL of a 3.1% by mass aqueous solution of sodium hexametaphosphate for 6 hours in accordance with the loading of Na and 0.6% by mass of Ba (both based on the carrier) by an impregnation method, and after the impregnation was completed, the mixture was dried at 105 ℃ for 2 hours, and then impregnated with 10.5mL of a 0.5% by mass aqueous solution of barium chloride for 8 hours, and after the impregnation was completed, the mixture was dried at 105 ℃ for 6 hours, and then calcined at 500 ℃ for 4 hours, thereby obtaining a 4% Na-0.6% Ba/alumina catalyst.
Example 2
Using magnesium oxide as a carrier, adopting an impregnation method, impregnating 12.1g of magnesium oxide with 10.6mL of 5.8% by mass sodium hexametaphosphate aqueous solution for 5 hours according to the Na loading amount of 5%, the Ba loading amount of 0.3% and the Ce loading amount of 0.1% (based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, then impregnating with 1.9mL of 2% by mass barium chloride and 6.6mL of 0.2% by mass cerium sulfate aqueous solution for 10 hours, drying at 80 ℃ for 10 hours after the impregnation is finished, and then roasting at 550 ℃ for 3 hours to obtain the 5% Na-0.3% Ba-0.1% Ce/magnesium oxide catalyst.
Example 3
Zirconium dioxide is used as a carrier, an impregnation method is adopted, according to the loading capacity of K being 8 percent and the loading capacity of Ce being 0.1 percent (both based on the carrier), 10.6g of zirconium dioxide is impregnated with 8.6mL of 10 percent aqueous solution of potassium carbonate by mass fraction for 10 hours, after the impregnation is finished, the zirconium dioxide is dried at 105 ℃ for 3 hours, then is impregnated with 5.5mL of 0.2 percent aqueous solution of cerium sulfate by mass fraction for 10 hours, after the impregnation is finished, the zirconium dioxide is dried at 80 ℃ for 12 hours, and then is roasted at 550 ℃ for 4 hours, so that the 8 percent Na-0.1 percent Ce/zirconium dioxide catalyst.
Example 4
Using alumina as a carrier, adopting an impregnation method, impregnating 12.7g of alumina with 12.9mL of 5% by mass potassium carbonate aqueous solution for 10 hours according to the loading of K, the loading of Ba of 0.4% and the loading of Ca of 0.1% (based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, impregnating with 5.1mL of 1% by mass barium chloride aqueous solution and 6.4mL of 0.2% by mass calcium chloride aqueous solution for 6 hours, drying at 105 ℃ for 6 hours after the impregnation is finished, and then roasting at 500 ℃ for 4.5 hours to obtain the 5% K-0.4% Ba-0.1% Ca/alumina catalyst.
Example 5
Using magnesium oxide as a carrier, adopting an impregnation method, impregnating 9.6g of magnesium oxide with 10mL of 10% by mass potassium carbonate aqueous solution at 10% by mass for 12 hours according to the loading of K and the loading of La of 0.3% (both based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, impregnating with 6mL of 0.5% by mass lanthanum sulfate aqueous solution for 6 hours, drying at 80 ℃ for 6 hours after the impregnation is finished, and roasting at 500 ℃ for 5 hours to obtain the 10% K-0.3% La/magnesium oxide catalyst.
Example 6
Taking zirconium dioxide as a carrier, adopting an impregnation method, impregnating 11.6g of zirconium dioxide with 10mL of 7% potassium carbonate aqueous solution for 10 hours according to the loading of K, 0.1% of Ce and 0.1% of Las (both based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, impregnating with 5.8mL of 0.2% cerium sulfate aqueous solution and 5.8mL of 0.2% lanthanum sulfate aqueous solution for 8 hours, drying at 80 ℃ for 8 hours after the impregnation is finished, and then roasting at 500 ℃ for 4 hours to obtain the 6% K-0.1% Ce-0.1% La/zirconium dioxide catalyst.
Example 7
By taking alumina as a carrier, adopting an impregnation method, according to the loading capacity of K of 7 percent, the loading capacity of Ce of 0.1 percent and the loading capacity of Ba of 0.2 percent (calculated by the carrier), impregnating 8.7g of alumina with 12mL of 5 percent aqueous solution of potassium carbonate by mass fraction for 12 hours, drying at 105 ℃ for 2 hours after the impregnation is finished, then impregnating with 4.4mL of 0.2 percent cerium sulfate by mass fraction and 3.5mL of 0.5 percent aqueous solution of barium chloride by mass fraction for 5 hours, drying at 80 ℃ for 6 hours after the impregnation is finished, and then roasting at 500 ℃ for 5 hours to obtain the catalyst of 7 percent K-0.1 percent Ce-0.2 percent Ba/alumina.
Example 8
Using zirconium dioxide as a carrier, adopting an impregnation method, impregnating 10.5g of zirconium dioxide with 8.5mL of 5% aqueous solution of potassium carbonate by mass fraction for 10 hours according to the loading capacity of K being 4%, the loading capacity of Ce being 0.1% and the loading capacity of La being 0.1% (based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, then impregnating with 5.3mL of 0.2% cerium sulfate by mass fraction and 5.3mL of 0.2% aqueous solution of lanthanum sulfate by mass fraction for 6 hours, drying at 80 ℃ for 5 hours after the impregnation is finished, and then roasting at 500 ℃ for 5 hours to obtain the 4% K-0.1% Ce-0.1% La/zirconium dioxide catalyst.
Example 9
Using alumina as a carrier, adopting an impregnation method, impregnating 13.6g of alumina with 11mL of 5% by mass potassium carbonate aqueous solution for 10 hours according to the loading capacity of K, the loading capacity of Ba of 0.3% and La0.1% (all based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, impregnating with 4.8mL of 1% by mass barium chloride and 6.8mL of 0.2% by mass lanthanum sulfate aqueous solution for 6 hours, drying at 80 ℃ for 6 hours after the impregnation is finished, and then roasting at 500 ℃ for 5 hours to obtain the 4% K-0.3% Ba-0.1% La/alumina catalyst.
Example 10
Taking zirconium dioxide as a carrier, adopting an impregnation method, according to the loading capacity of K being 8% and the loading capacity of La being 0.2% (both based on the carrier), impregnating 11.4g of zirconium dioxide with 9.2mL of 10% potassium carbonate aqueous solution by mass fraction for 10 hours, drying at 105 ℃ for 2 hours after the impregnation is finished, then impregnating with 11.5mL of 0.2% lanthanum sulfate aqueous solution by mass fraction for 6 hours, drying at 80 ℃ for 6 hours after the impregnation is finished, and then roasting at 500 ℃ for 5 hours to obtain the 8% K-0.2% La/zirconium dioxide catalyst.
Example 11
By taking alumina as a carrier and adopting an impregnation method, according to the loading capacity of Cs of 6 percent and the loading capacity of Ba of 0.5 percent (both based on the carrier), the alumina is impregnated with 12.5mL of aqueous solution of cesium carbonate with the mass fraction of 5 percent for 8 hours, the alumina is dried at 105 ℃ for 2 hours after the impregnation is finished, then is impregnated with 10.3mL of aqueous solution of barium chloride with the mass fraction of 0.5 percent for 6 hours, the alumina is dried at 105 ℃ for 6 hours after the impregnation is finished, and then is roasted at 550 ℃ for 4 hours, so that the Ba/alumina catalyst with the mass fraction of 6 percent to 0.5 percent of Cs is obtained.
Example 12
Taking zirconium dioxide as a carrier, adopting an impregnation method, impregnating 11.5g of zirconium dioxide with 8.9mL of 8% cesium carbonate aqueous solution by mass fraction for 8 hours according to the loading of Cs and the loading of La of 0.2% (both based on the carrier), drying at 105 ℃ for 2 hours after the impregnation is finished, then impregnating with 11.5mL of 0.2% lanthanum sulfate aqueous solution by mass fraction for 5 hours, drying at 80 ℃ for 6 hours after the impregnation is finished, and roasting at 500 ℃ for 5 hours to obtain the 4% Cs-0.2% La/zirconium dioxide catalyst.
Example 13
By taking alumina as a carrier, adopting an impregnation method, according to the loading of Cs of 5 percent, the loading of Ba of 0.1 percent and the loading of La of 0.1 percent (calculated by the carrier), soaking 10.9g of alumina in 11mL of aqueous solution of cesium carbonate with the mass fraction of 5 percent for 8 hours, drying at 105 ℃ for 2 hours after the completion of the soaking, then soaking in 5.5mL of aqueous solution of lanthanum sulfate with the mass fraction of 0.2 percent and barium chloride with the mass fraction of 5.5mL of aqueous solution of barium chloride with the mass fraction of 0.2 percent for 5 hours, drying at 80 ℃ for 6 hours after the completion of the soaking, and then roasting at 500 ℃ for 5 hours to obtain the catalyst of 6 percent Cs-0.1 percent Ba-0.1 percent La/alumina.
In order to prove the beneficial effects of the invention, the inventor uses the composite solid base catalyst prepared in the embodiments 1-13 to catalyze the transesterification of the waste oil to prepare the biodiesel, and the specific experiment is as follows:
adding 8% of catalyst by mass into the hogwash oil with the acid value of 8.62mgKOH/g, heating to 60 ℃, introducing gasified methanol, continuously heating to 100 ℃, and reacting for 1.5 hours. The results are shown in Table 1.
TABLE 1 catalytic Effect of the catalyst of the invention
Claims (6)
1. The application of the composite solid base catalyst in preparing biodiesel by catalyzing waste oil transesterification comprises the following specific steps: adding a composite solid base catalyst with the mass of 5% -15% into waste oil with the acid value of 8.62-10 mgKOH/g, heating to 50-60 ℃, introducing gasified methanol, continuously heating to 80-100 ℃, and reacting for 1-3 hours; the composite solid base catalyst is prepared by taking any one of aluminum oxide, zirconium dioxide and magnesium oxide as a carrier, and loading an active component A and an active component B, wherein the active component A is any one of Na, K and Cs, and the active component B is any one or more than two of Ba, Ca, Ce and La; the loading capacity of the active component A is 4-12% and the loading capacity of the active component B is 0.1-1% by weight of the carrier.
2. The application of the composite solid base catalyst according to claim 1 in preparation of biodiesel by catalyzing transesterification of waste oil and fat, wherein the composite solid base catalyst comprises the following components in percentage by weight: the composite solid base catalyst takes alumina as a carrier, an active component A is K, and an active component B is Ba and Ca or Ba and La; based on the carrier, the loading capacity of K is 4-5%, the loading capacity of Ba is 0.3-0.4%, and the loading capacity of Ca or La is 0.1%.
3. The application of the composite solid base catalyst according to claim 1 in preparation of biodiesel by catalyzing transesterification of waste oil and fat, wherein the composite solid base catalyst comprises the following components in percentage by weight: the active component A is Cs, and the active component B is Ba and/or La; calculated by the carrier, the loading capacity of Cs is 4-6%, when the active component B is Ba, the loading capacity of Ba is 0.5-0.6%, when the active component B is La, the loading capacity of La is 0.2-0.3%, when the active component B is Ba and La, the loading capacity of Ba is 0.1-0.2%, and the loading capacity of La is 0.1-0.2%.
4. The application of the composite solid base catalyst according to claim 1 in preparation of biodiesel by catalyzing transesterification of waste oil and fat, wherein the composite solid base catalyst comprises the following components in percentage by weight: the composite solid base catalyst takes zirconium oxide as a carrier, an active component A is Na, and an active component B is Ce; the loading capacity of Na is 8-9% and the loading capacity of Ce is 0.1-0.2% based on the carrier.
5. The application of the composite solid base catalyst according to claim 1 in preparation of biodiesel by catalyzing transesterification of waste oil and fat, wherein the composite solid base catalyst comprises the following components in percentage by weight: the active component A is K or Na, and the active component B is Ba and Ce; based on the carrier, the loading capacity of K or Na is 5-7%, the loading capacity of Ba is 0.2-0.3%, and the loading capacity of Ce is 0.1-0.2%.
6. The application of the composite solid base catalyst according to claim 1 in preparation of biodiesel by catalyzing transesterification of waste oil and fat, wherein the composite solid base catalyst comprises the following components in percentage by weight: the waste oil is any one of waste oil, hogwash oil and acidified oil.
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