CN112126528A - Preparation method of biodiesel - Google Patents
Preparation method of biodiesel Download PDFInfo
- Publication number
- CN112126528A CN112126528A CN202011012992.1A CN202011012992A CN112126528A CN 112126528 A CN112126528 A CN 112126528A CN 202011012992 A CN202011012992 A CN 202011012992A CN 112126528 A CN112126528 A CN 112126528A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- biodiesel
- fatty acid
- long
- chain fatty
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003225 biodiesel Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 150000004668 long chain fatty acids Chemical class 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000011282 treatment Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims description 16
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 9
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 9
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 9
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000005642 Oleic acid Substances 0.000 claims description 9
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 9
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 9
- 235000021314 Palmitic acid Nutrition 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 150000002148 esters Chemical class 0.000 description 6
- 239000011964 heteropoly acid Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 5
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 description 5
- 229940073769 methyl oleate Drugs 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 4
- 235000021588 free fatty acids Nutrition 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- BEKZXQKGTDVSKX-UHFFFAOYSA-N propyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCCC BEKZXQKGTDVSKX-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/003—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with alcohols
-
- 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
- C10L1/026—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only for compression ignition
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of biodiesel, which comprises the following steps: the method comprises the steps of taking Anderson type polyoxometallate as a catalyst, taking long-chain fatty acid and short-chain alcohol as raw materials, reacting for 4-24 hours at the temperature of 60-150 ℃, and carrying out post-treatment to obtain the biodiesel. Compared with the prior art, the invention takes long-chain fatty acid as a raw material, adds excessive short-chain alcohol, heats, stirs and mixes evenly at a certain temperature, finally adds catalyst polyoxometallate, and fully reacts for a period of time to obtain the product. The method adopts polyoxometallate as a catalyst, has high catalytic activity, good selectivity, recyclability, mild required reaction conditions, simple preparation method, economy and environmental friendliness, and has popularization and utilization values.
Description
Technical Field
The invention belongs to the technical field of biodiesel, and relates to a preparation method of biodiesel.
Background
The rapid development of modern economy is promoted by the large investment of fossil energy. Meanwhile, the increasing consumption of fossil fuels has also caused serious energy crisis and environmental problems, and the development and utilization of biofuels have been receiving attention. Biodiesel has received much attention because of its clean, non-toxic, renewable, and high cetane, high flash point fuel properties.
The components of the biodiesel on the market are mainly fatty acid methyl ester, and can be obtained by carrying out base catalytic reaction on animal and vegetable oil and methanol, but the production scale of the biodiesel is continuously increased, the production cost of the biodiesel is always increased, and problems related to influences on grain safety, land change and the like are also caused. In order to avoid such problems, the main solution is to use inexpensive raw materials with high FFA (free fatty acid) content including acidic oils, edible oils and waste oils. However, these feedstocks are not suitable for direct alkaline catalysis processes because they form soaps and complicate the purification process.
The acid catalysis method is a simple method for preparing biodiesel through esterification reaction of FFA (mainly comprising oleic acid, palmitic acid, linoleic acid, stearic acid and the like) and short-chain alcohol. Conventional acid catalysts are predominantly liquid mineral acids, e.g. H2SO4HCl and H3PO4And the like, although the catalyst has good catalytic activity for the esterification reaction of FFA, the catalyst has the disadvantages of environmental unfriendliness, serious environmental pollution caused by waste acid, troublesome post-treatment process and serious corrosion to equipment.
Disclosure of Invention
The invention aims to provide a preparation method of biodiesel, which utilizes Anderson type polyoxometallate to replace strong corrosive acid as a catalyst and has the characteristics of economy, environmental protection, greenness and high efficiency.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of biodiesel comprises the following steps: the biodiesel is prepared by taking Anderson type polyoxometallate as a catalyst, taking long-chain fatty acid and short-chain alcohol as raw materials, reacting for 4-24 hours at the temperature of 60-150 ℃, and carrying out post-treatment.
Furthermore, the central atom of the Anderson type polyoxometallate is Cu, Al, Fe, Co, Cr or Ni.
Further, the long-chain fatty acid is hexadecanoic acid or oleic acid. The long chain fatty acids are selected to be saturated or unsaturated.
Further, the short-chain alcohol is C1-C4 fatty alcohol (namely methanol, ethanol, propanol and butanol).
Furthermore, the molar ratio of the catalyst to the long-chain fatty acid is 1 (50-1000).
Furthermore, the molar ratio of the long-chain fatty acid to the short-chain alcohol is 1 (1-20).
Further, the post-treatment comprises catalyst removal, extraction and product purification.
Further, the catalyst in the reaction system was removed by filtration.
Further, extraction was performed by adding an aqueous sodium carbonate solution to obtain an organic phase.
Further, the product purification process comprises the following steps: anhydrous magnesium sulfate was added for drying, and then filtered and concentrated.
Polyoxometallate (POM) is also called heteropoly acid, is an ionic metal oxygen cluster compound, has the advantages of unique acidity, low temperature and high activity and the like, and various structures of the Polyoxometallate (POM) can be used for catalyzing the esterification reaction of long-chain fatty acid and short-chain alcohol in the invention.
In the invention, long-chain fatty acid (oleic acid or hexadecanoic acid) and short-chain alcohol are used as raw materials, and are heated, stirred and subjected to reflux reaction in the presence of a polyoxometallate catalyst to prepare a synthetic ester, namely the product can be used as biodiesel, and the chemical reaction formulas are respectively as follows:
compared with the prior art, the invention has the following characteristics:
1) the invention takes long-chain fatty acid as raw material, adds excessive short-chain alcohol (as reactant and solvent at the same time), heats, stirs and mixes evenly at a certain temperature, finally adds catalyst polyoxometallate, and fully reacts for a period of time to obtain the product. The method adopts polyoxometallate as a catalyst, has high catalytic activity, good selectivity, recyclability, mild required reaction conditions, simple preparation method, economy and environmental friendliness, and has popularization and utilization values.
2) The method adopts a one-pot method, has mild reaction conditions, simple and convenient operation, high product yield, environmental protection, great reduction of cost, reduction of the generation of three wastes and reduction of the environmental protection pressure, and is suitable for industrial mass production.
Drawings
FIG. 1 is a nuclear magnetic resonance hydrogen spectrum of methyl oleate prepared in example 11H NMR(CDCl3) A drawing;
FIG. 2 is a NMR hydrogen spectrum of propyl palmitate prepared in example 21H NMR(CDCl3) Figure (a).
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
2.82g (0.01mol) of oleic acid, 1.92g (0.06mol) of methanol and 1.0 mol% of Anderson type heteropoly acid with Al as a central metal atom are put into a dry reaction tube, the reaction temperature is controlled at 80 ℃, after the heat preservation reaction for 12h, the reaction is stopped, after standing for a period of time, a sample is prepared and subjected to GC-MS detection, the result shows that an obvious product peak is generated, and after treatment, separation and purification are carried out to obtain an ester product and a nuclear magnetic test is carried out, and the result is shown in figure 1. The yield of the product, methyl oleate, was 51%.
Example 2:
putting 2.56g (0.01mol) of hexadecanoic acid, 2.4g (0.04mol) of propanol and 1.5 mol% of Anderson type heteropoly acid taking Al as a central metal atom into a dry reaction tube, controlling the reaction temperature at 100 ℃, carrying out heat preservation reaction for 8h, stopping the reaction, standing for a period of time, preparing a sample, carrying out GC-MS detection, and obtaining an ester product through aftertreatment, separation and purification, and carrying out nuclear magnetic testing, wherein the result is shown in figure 2. The yield of the product propyl palmitate was 57%.
Example 3:
5.65g (0.02mol) of oleic acid, 3.2g (0.10mol) of methanol and 1.0 mol% of Anderson type heteropoly acid taking Fe as a central metal atom are put into a dry reaction tube, the reaction temperature is controlled at 80 ℃, the reaction is stopped after the heat preservation reaction for 6h, the reaction is stopped after the reaction is kept still for a period of time, a sample is prepared and subjected to GC-MS detection, and the result shows that an obvious product peak is produced, and the ester product is obtained through post-treatment, separation and purification and is subjected to nuclear magnetic testing. The yield of the product, methyl oleate, was 38%.
Example 4:
5.65g (0.02mol) of oleic acid, 3.2g (0.10mol) of methanol and 1.0 mol% of Anderson type heteropoly acid taking Cu as a central metal atom are put into a dry reaction tube, the reaction temperature is controlled at 80 ℃, the reaction is stopped after the heat preservation reaction for 8 hours, the reaction is stopped after the reaction is stood for a period of time, a sample is prepared and subjected to GC-MS detection, and the result shows that an obvious product peak is produced, and the ester product is obtained through post-treatment, separation and purification and is subjected to nuclear magnetic testing. The yield of the product, methyl oleate, was 42%.
Example 5:
5.65g (0.02mol) of oleic acid, 3.2g (0.10mol) of methanol and 1.0 mol% of Anderson type heteropoly acid taking Ni as a central metal atom are put into a dry reaction tube, the reaction temperature is controlled at 80 ℃, the reaction is stopped after the heat preservation reaction for 6 hours, the reaction is stopped after the reaction is stood for a period of time, a sample is prepared and is subjected to GC-MS detection, the result shows that an obvious product peak is generated, and the ester product is obtained through post-treatment, separation and purification and is subjected to nuclear magnetic testing. The yield of the product methyl oleate was 40%.
Example 6:
the preparation method of the biodiesel comprises the following steps: the biodiesel is obtained by taking Anderson type polyoxometallate as a catalyst, taking long-chain fatty acid and short-chain alcohol as raw materials, reacting for 24 hours at the temperature of 60 ℃, and carrying out post-treatment.
Wherein, the central atom of the Anderson type polyoxometallate is Cu or Al. The long chain fatty acid is palmitic acid. The short-chain alcohol is methanol or ethanol.
The molar ratio of catalyst to long chain fatty acid is 1:50, and the molar ratio of long chain fatty acid to short chain alcohol is 1: 20.
The post-treatment comprises catalyst removal, extraction and product purification. The catalyst in the reaction system was removed by filtration. The organic phase was obtained by extraction with aqueous sodium carbonate solution. The purification process of the product is as follows: anhydrous magnesium sulfate was added for drying, and then filtered and concentrated.
Example 7:
the preparation method of the biodiesel comprises the following steps: the biodiesel is obtained by reacting 4 hours at 150 ℃ by taking Anderson type polyoxometallate as a catalyst and long-chain fatty acid and short-chain alcohol as raw materials and carrying out post-treatment.
Wherein, the central atom of the Anderson type polyoxometallate is Fe or Co. The long chain fatty acid is oleic acid. The short-chain alcohol is n-propanol.
The molar ratio of the catalyst to the long-chain fatty acid is 1:1000, and the molar ratio of the long-chain fatty acid to the short-chain alcohol is 1: 1.
The post-treatment comprises catalyst removal, extraction and product purification. The catalyst in the reaction system was removed by filtration. The organic phase was obtained by extraction with aqueous sodium carbonate solution. The purification process of the product is as follows: anhydrous magnesium sulfate was added for drying, and then filtered and concentrated.
Example 8:
the preparation method of the biodiesel comprises the following steps: the biodiesel is obtained by taking Anderson type polyoxometallate as a catalyst, taking long-chain fatty acid and short-chain alcohol as raw materials, reacting for 12 hours at 110 ℃, and carrying out post-treatment.
Wherein, the central atom of the Anderson type polyoxometallate is Cr or Ni. The long chain fatty acid is palmitic acid. The short-chain alcohol is butanol.
The molar ratio of catalyst to long chain fatty acid is 1:600 and the molar ratio of long chain fatty acid to short chain alcohol is 1: 8.
The post-treatment comprises catalyst removal, extraction and product purification. The catalyst in the reaction system was removed by filtration. The organic phase was obtained by extraction with aqueous sodium carbonate solution. The purification process of the product is as follows: anhydrous magnesium sulfate was added for drying, and then filtered and concentrated.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of biodiesel is characterized by comprising the following steps: the biodiesel is prepared by taking Anderson type polyoxometallate as a catalyst, taking long-chain fatty acid and short-chain alcohol as raw materials, reacting for 4-24 hours at the temperature of 60-150 ℃, and carrying out post-treatment.
2. The method of claim 1, wherein the central atom of the Anderson polyoxometallate is Cu, Al, Fe, Co, Cr or Ni.
3. The method of claim 1, wherein the long chain fatty acid is palmitic acid or oleic acid.
4. The method for preparing biodiesel according to claim 1, wherein the short-chain alcohol is a C1-C4 fatty alcohol.
5. The preparation method of biodiesel according to claim 1, wherein the molar ratio of the catalyst to the long-chain fatty acid is 1 (50-1000).
6. The preparation method of biodiesel according to claim 1, wherein the molar ratio of the long-chain fatty acid to the short-chain alcohol is 1 (1-20).
7. The method of claim 1, wherein the post-treatment comprises catalyst removal, extraction and product purification.
8. The method according to claim 7, wherein the catalyst in the reaction system is removed by filtration.
9. The method of claim 7, wherein the organic phase is obtained by adding aqueous sodium carbonate solution for extraction.
10. The method for preparing biodiesel according to claim 7, wherein the product purification process comprises: anhydrous magnesium sulfate was added for drying, and then filtered and concentrated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011012992.1A CN112126528A (en) | 2020-09-23 | 2020-09-23 | Preparation method of biodiesel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011012992.1A CN112126528A (en) | 2020-09-23 | 2020-09-23 | Preparation method of biodiesel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112126528A true CN112126528A (en) | 2020-12-25 |
Family
ID=73840597
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011012992.1A Pending CN112126528A (en) | 2020-09-23 | 2020-09-23 | Preparation method of biodiesel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112126528A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008122790A2 (en) * | 2007-04-05 | 2008-10-16 | University Of York | Heteropolyacid catalysts and biodiesel manufacturing methods using such catalysts |
| CN101294094A (en) * | 2007-04-29 | 2008-10-29 | 华中农业大学 | Method for preparing biological diesel oil by using nano-solid heteropoly acid, heteropolybase catalyst |
| CN104815690A (en) * | 2015-04-14 | 2015-08-05 | 贵州大学 | Multi-sulfonic acid funtionalized mesoporous polymeric solid acid catalyst and preparation method and application thereof |
| CN105754718A (en) * | 2016-04-26 | 2016-07-13 | 上海应用技术学院 | Method for preparing biodiesel |
| CN109647461A (en) * | 2018-12-12 | 2019-04-19 | 长春市梅丰科技有限公司 | The composite material of Keggin-type heteropoly acid or heteropolyacid salt and carbon molecular sieve, preparation method and application |
-
2020
- 2020-09-23 CN CN202011012992.1A patent/CN112126528A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008122790A2 (en) * | 2007-04-05 | 2008-10-16 | University Of York | Heteropolyacid catalysts and biodiesel manufacturing methods using such catalysts |
| CN101294094A (en) * | 2007-04-29 | 2008-10-29 | 华中农业大学 | Method for preparing biological diesel oil by using nano-solid heteropoly acid, heteropolybase catalyst |
| CN104815690A (en) * | 2015-04-14 | 2015-08-05 | 贵州大学 | Multi-sulfonic acid funtionalized mesoporous polymeric solid acid catalyst and preparation method and application thereof |
| CN105754718A (en) * | 2016-04-26 | 2016-07-13 | 上海应用技术学院 | Method for preparing biodiesel |
| CN109647461A (en) * | 2018-12-12 | 2019-04-19 | 长春市梅丰科技有限公司 | The composite material of Keggin-type heteropoly acid or heteropolyacid salt and carbon molecular sieve, preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| 刘悦冉: "SBA-15负载Anderson型杂多酸在氧化及酯化反应中的应用研究", 《中国优秀博硕士学问论文全文数据库 工程科技Ⅰ辑》 * |
| 舒庆等: "硅钨杂多酸制备、表征及催化油酸酯化反应合成生物柴油活性研究", 《有色金属科学与工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mansir et al. | Modified waste egg shell derived bifunctional catalyst for biodiesel production from high FFA waste cooking oil. A review | |
| CN101451072B (en) | Method for preparing biodiesel by sulfonic acid type ion liquid | |
| CN100569914C (en) | A kind of method of utilizing producing biodiesel from high acid number grease | |
| CN100335594C (en) | Method for preparing biological diesel oil | |
| CN101327437B (en) | Microwave-absorption type solid acid catalyst and use thereof in preparing biodiesel | |
| Yang et al. | Synthesis of biodiesel via transesterification of tung oil catalyzed by new Brönsted acidic ionic liquid | |
| CN101591574B (en) | Method for preparing biodiesel by zirconia solid base catalyst | |
| Qiuyun et al. | Solid acid used as highly efficient catalyst for esterification of free fatty acids with alcohols | |
| Kushwaha et al. | Esterification of oleic acid to biodiesel using biowaste‐based solid acid catalyst under microwave irradiation | |
| CN1810931A (en) | Microwave process to prepare biological diesel oil | |
| CN102188995B (en) | Catalyst prepared by utilizing paper mill black water and application of the catalyst in biodiesel preparation | |
| CN100523131C (en) | Esterification reaction technique of preparing biodiesel by waste oil | |
| CN101338215A (en) | Method for preparing biodiesel by catalyzing oil or fatty acid with solid | |
| CN101402873A (en) | Method for producing light biological diesel oil with seed oil of camphor | |
| CN101157868B (en) | Method for producing low freezing point biodiesel by employing waste animal and vegetable oil coupling and special device | |
| EP2917199B1 (en) | Process for manufacturing biofuels | |
| CN100365100C (en) | Method of preparing biological diesel oil by methanol critical low alkali process | |
| CN100526427C (en) | Method and catalyst for producing biological diesel oil by high-acid value grease | |
| CN100375780C (en) | Production of biological diesel oil with solid alkali | |
| CN112126528A (en) | Preparation method of biodiesel | |
| CN101148599B (en) | Method for preparing biological diesel oil from waste animals and plants grease with high acid value | |
| CN100548964C (en) | A kind of esterification process of lipid acid | |
| CN101225324B (en) | One-step method for preparing biodiesel by low-acid catalytic fatty or fatty acid | |
| CN102391914A (en) | Method for preparing biodiesel by catalysis of rare-earth oxide mesoporous material | |
| CN101067090B (en) | Solid catalysis for preparing biodiesel oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201225 |
|
| RJ01 | Rejection of invention patent application after publication |