CN105861021A - Method for preparing biodiesel from marine microalgae - Google Patents
Method for preparing biodiesel from marine microalgae Download PDFInfo
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- CN105861021A CN105861021A CN201610381550.1A CN201610381550A CN105861021A CN 105861021 A CN105861021 A CN 105861021A CN 201610381550 A CN201610381550 A CN 201610381550A CN 105861021 A CN105861021 A CN 105861021A
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- Prior art keywords
- methanol
- base material
- marine microalgae
- preparing biodiesel
- method preparing
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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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
- C10G2300/1014—Biomass of vegetal origin
-
- 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
Abstract
The invention provides a method for preparing biodiesel from marine microalgae, comprising the steps of: cleaning Phaeodactylum tricornutum, carrying out plate-and-frame filter pressing to remove water, adding the wet Phaeodactylum tricornutum into water, adding cellulase, protease and sodium citrate, mixing the materials, carrying out enzymolysis at 45-55 DEG C for 2-5h, carrying out enzyme deactivation, regulating the pH value of the obtained enzymolysis liquid to 9.0-10.0, adding an equal volume of chloroform-methanol, carrying out extraction, adding the organic phase to mixed liquid of concentrated sulfuric acid, tetrahydrofuran and methanol, standing after shaker oscillation, washing and centrifuging the obtained ester phase with petroleum ether-95v/v%ethanol to obtain an oil phase and concentrating the oil phase. The preparation method has the advantages of high yield of biodiesel, good quality, simple production process and low cost and can be widely popularized.
Description
Technical field
The invention belongs to bioenergy technical field, be specifically related to a kind of method preparing biodiesel for base material with marine microalgae.
Background technology
Biodiesel, refers to water plant oils and fatss such as oil crop, wild oil crop and engineering microalgaes, and animal oil
Methyl ester that fat, biodiesel etc. are made by trans-esterification processes for raw oil or ethyl ester fuel.As alternative petrochemical industry bavin
The clean biometric fuel of oil, the serviceability of biodiesel is substantially suitable with petrifaction diesel with existing, and it is special to have good environment
Property and biodegradable, have vast potential for future development.
The selection of glyceride stock depends mainly on cost of material and the popularity in its source.According to statistics, biodiesel is prepared as
This is cost of material, and therefore using cheap raw material and raising conversion ratio thus reducing cost is that can biodiesel practical
Crucial.Oilseed plant is due to shortcomings such as the area that occupies cultivated land, growth cycle length, climate impacts, and can not become biological bavin
The permanent plan of oil raw oil material supply.Marine microalgae is Organic substance and the main provider of energy in marine ecology system, with
Other raw materials are compared, and have the advantages that photosynthetic efficiency is high, adaptive capacity to environment is strong, growth cycle is short, biological yield is high.
Easily supporting due to microalgae and easily receive, the biomass energies such as colony is numerous, institute's fatty acids are huge, and therefore microalgae is new bio bavin
Oil one of raw material oil sources, is also one of the trend of future biological diesel oil development.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide a kind of side preparing biodiesel with marine microalgae for base material
Method, gained yield of biodiesel is high, quality is good.
A kind of method preparing biodiesel for base material with marine microalgae, comprises the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in water 5～10 parts, add cellulase 0.01～
0.05 part, proteinase-10 .03～0.07 part, sodium citrate 0.04～0.08 part, mixing, 45～55 DEG C of enzymolysis 2～5h, enzyme denaturing,
Obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 9.0～10.0, adds isopyknic chloroform-methanol, extraction,
Take organic facies；
Step 4, adds the concentrated sulphuric acid of 2～4 times of volumes, oxolane, the mixed liquor of methanol by step 2 gained organic facies,
Stand after shaking table concussion 4～8h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 2～5 times of volumes, centrifugal, obtains oil phase,
Concentrate, to obtain final product.
Further, in step 1, enzymolysis process need to be carried out in nitrogen atmosphere.
Further, in the chloroform-methanol of step 3, chloroform, the volume ratio of methanol are 1:1.
Further, concentrated sulphuric acid in the mixed liquor of the concentrated sulphuric acid of step 4, oxolane, methanol, oxolane, methanol
Volume ratio is 1:1:1.
Further, in step 4, the condition of shaking table concussion is 40～60 DEG C, 200～500rpm.
Further, in the petroleum ether-95v/v% ethanol of step 5, petroleum ether, the volume ratio of 95v/v% ethanol are 1:2.
Further, in step 5, centrifugal condition is 4 DEG C, 10000～12000rpm, 10～15min.
The preparation method yield of biodiesel of the present invention is high, quality is good, and production technology is simple, cost is simple, can be widely popularized.
Detailed description of the invention
Embodiment 1
A kind of method preparing biodiesel for base material with marine microalgae, comprises the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in 5 parts of water, add cellulase 0.01 part,
Proteinase-10 .03 part, sodium citrate 0.04 part, mixing, 45 DEG C of enzymolysis 5h, enzyme denaturing, obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 9.0, adds isopyknic chloroform-methanol, extraction, takes organic
Phase；
Step 4, adds the concentrated sulphuric acid of 2 times of volumes, oxolane, the mixed liquor of methanol, shaking table by step 2 gained organic facies
Stand after concussion 4h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 2 times of volumes, centrifugal, obtains oil phase, dense
Contracting, to obtain final product.
Wherein, in step 1, enzymolysis process need to be carried out in nitrogen atmosphere；In chloroform-methanol, chloroform, the volume ratio of methanol are 1:
1；Concentrated sulphuric acid, oxolane, methanol mixed liquor in concentrated sulphuric acid, oxolane, the volume ratio of methanol be 1:1:1；Step
In rapid 4, the condition of shaking table concussion is 40 DEG C, 500rpm；Petroleum ether, the body of 95v/v% ethanol in petroleum ether-95v/v% ethanol
Long-pending ratio is 1:2；In step 5, centrifugal condition is 4 DEG C, 10000rpm, 15min.
The yield of the present embodiment biodiesel is the 17.8% of wet algae weight, and acid number is 0.75mgKOH/g.
Embodiment 2
A kind of method preparing biodiesel for base material with marine microalgae, comprises the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in 8 parts of water, add cellulase 0.03 part,
Proteinase-10 .06 part, sodium citrate 0.07 part, mixing, 50 DEG C of enzymolysis 5h, enzyme denaturing, obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 9.5, adds isopyknic chloroform-methanol, extraction, takes organic
Phase；
Step 4, adds the concentrated sulphuric acid of 3 times of volumes, oxolane, the mixed liquor of methanol, shaking table by step 2 gained organic facies
Stand after concussion 4h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 2 times of volumes, centrifugal, obtains oil phase, dense
Contracting, to obtain final product.
Wherein, in step 1, enzymolysis process need to be carried out in nitrogen atmosphere；In chloroform-methanol, chloroform, the volume ratio of methanol are 1:
1；Concentrated sulphuric acid, oxolane, methanol mixed liquor in concentrated sulphuric acid, oxolane, the volume ratio of methanol be 1:1:1；Step
In rapid 4, the condition of shaking table concussion is 50 DEG C, 300rpm；Petroleum ether, the body of 95v/v% ethanol in petroleum ether-95v/v% ethanol
Long-pending ratio is 1:2；In step 5, centrifugal condition is 4 DEG C, 12000rpm, 10min.
The yield of the present embodiment biodiesel is the 16.9% of wet algae weight, and acid number is 0.79mgKOH/g.
Embodiment 3
A kind of method preparing biodiesel for base material with marine microalgae, comprises the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in 6 parts of water, add cellulase 0.04 part,
Proteinase-10 .05 part, sodium citrate 0.07 part, mixing, 45 DEG C of enzymolysis 2h, enzyme denaturing, obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 10.0, adds isopyknic chloroform-methanol, extraction, takes organic
Phase；
Step 4, adds the concentrated sulphuric acid of 3 times of volumes, oxolane, the mixed liquor of methanol, shaking table by step 2 gained organic facies
Stand after concussion 4h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 4 times of volumes, centrifugal, obtains oil phase, dense
Contracting, to obtain final product.
Wherein, in step 1, enzymolysis process need to be carried out in nitrogen atmosphere；In chloroform-methanol, chloroform, the volume ratio of methanol are 1:
1；Concentrated sulphuric acid, oxolane, methanol mixed liquor in concentrated sulphuric acid, oxolane, the volume ratio of methanol be 1:1:1；Step
In rapid 4, the condition of shaking table concussion is 40 DEG C, 500rpm；Petroleum ether, the body of 95v/v% ethanol in petroleum ether-95v/v% ethanol
Long-pending ratio is 1:2；In step 5, centrifugal condition is 4 DEG C, 10000rpm, 15min.
The yield of the present embodiment biodiesel is the 17.1% of wet algae weight, and acid number is 0.81mgKOH/g.
Embodiment 4
A kind of method preparing biodiesel for base material with marine microalgae, comprises the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in 10 parts of water, add cellulase 0.05 part,
Proteinase-10 .07 part, sodium citrate 0.08 part, mixing, 55 DEG C of enzymolysis 2h, enzyme denaturing, obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 10.0, adds isopyknic chloroform-methanol, extraction, takes organic
Phase；
Step 4, adds the concentrated sulphuric acid of 4 times of volumes, oxolane, the mixed liquor of methanol, shaking table by step 2 gained organic facies
Stand after concussion 4h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 5 times of volumes, centrifugal, obtains oil phase, dense
Contracting, to obtain final product.
Wherein, in step 1, enzymolysis process need to be carried out in nitrogen atmosphere；In chloroform-methanol, chloroform, the volume ratio of methanol are 1:
1；Concentrated sulphuric acid, oxolane, methanol mixed liquor in concentrated sulphuric acid, oxolane, the volume ratio of methanol be 1:1:1；Step
In rapid 4, the condition of shaking table concussion is 40 DEG C, 500rpm；Petroleum ether, the body of 95v/v% ethanol in petroleum ether-95v/v% ethanol
Long-pending ratio is 1:2；In step 5, centrifugal condition is 4 DEG C, 10000rpm, 15min.
The yield of the present embodiment biodiesel is the 18.4% of wet algae weight, and acid number is 0.73mgKOH/g.
Claims (7)
1. the method preparing biodiesel for base material with marine microalgae, it is characterised in that: comprise the following steps:
Step 1, takes Phaeodactylum and cleans, remove moisture removal through filter press, obtain wet algae；
Step 2, in parts by weight, takes 1 part of the wet algae of step 1 gained and adds in water 5～10 parts, add cellulase 0.01～
0.05 part, proteinase-10 .03～0.07 part, sodium citrate 0.04～0.08 part, mixing, 45～55 DEG C of enzymolysis 2～5h, enzyme denaturing,
Obtain enzymolysis solution；
Step 3, by step 2 gained enzymolysis solution pH regulator to 9.0～10.0, adds isopyknic chloroform-methanol, extraction,
Take organic facies；
Step 4, adds the concentrated sulphuric acid of 2～4 times of volumes, oxolane, the mixed liquor of methanol by step 2 gained organic facies,
Stand after shaking table concussion 4～8h, obtain upper strata ester phase；
Step 5, by step 4 gained ester mutually by the petroleum ether-95v/v% washing with alcohol of 2～5 times of volumes, centrifugal, obtains oil phase,
Concentrate, to obtain final product.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
In 1, enzymolysis process need to be carried out in nitrogen atmosphere.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
In the chloroform-methanol of 3, chloroform, the volume ratio of methanol are 1:1.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
The concentrated sulphuric acid of 4, oxolane, methanol mixed liquor in concentrated sulphuric acid, oxolane, the volume ratio of methanol be 1:1:1.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
In 4, the condition of shaking table concussion is 40～60 DEG C, 200～500rpm.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
In the petroleum ether-95v/v% ethanol of 5, petroleum ether, the volume ratio of 95v/v% ethanol are 1:2.
The method preparing biodiesel for base material with marine microalgae the most according to claim 1, it is characterised in that: step
In 5, centrifugal condition is 4 DEG C, 10000～12000rpm, 10～15min.
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| CN201610381550.1A CN105861021A (en) | 2016-06-01 | 2016-06-01 | Method for preparing biodiesel from marine microalgae |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381217A (en) * | 2016-11-30 | 2017-02-08 | 广西东奇能源技术有限公司 | Preparation method of biological fuel with high combustion value |
| CN107603744A (en) * | 2017-10-23 | 2018-01-19 | 无锡超科食品有限公司 | A kind of fatty method in extraction powdered oil |
| CN109337940A (en) * | 2018-11-28 | 2019-02-15 | 北京大学 | The method for being catalyzed wet chlorella preparation biodiesel using two step enzyme methods |
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| CN106381217A (en) * | 2016-11-30 | 2017-02-08 | 广西东奇能源技术有限公司 | Preparation method of biological fuel with high combustion value |
| CN107603744A (en) * | 2017-10-23 | 2018-01-19 | 无锡超科食品有限公司 | A kind of fatty method in extraction powdered oil |
| CN109337940A (en) * | 2018-11-28 | 2019-02-15 | 北京大学 | The method for being catalyzed wet chlorella preparation biodiesel using two step enzyme methods |
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Application publication date: 20160817 |