CN107779266B - Method for directly transesterifying water-containing microalgae biomass based on microchannel reactor - Google Patents
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Abstract
A method for directly transesterifying water-containing microalgae biomass based on a microchannel reactor comprises the steps of suspending fresh microalgae biomass with the water content not higher than 95% by using a suspending agent, injecting the suspended fresh microalgae biomass into the microchannel reactor, and carrying out transesterification reaction between short-chain alcohol (C1-C4) and intracellular grease by using sulfuric acid or hydrochloric acid as a catalyst to prepare fatty acid alcohol esters (fat acid alkyl esters). The method has the advantages that the micro-channel reactor is used for carrying out the transesterification of the water-containing microalgae biomass, the sample does not need to be dried and the grease extraction treatment, the sample pretreatment process is greatly simplified, and the method has the characteristics of quick reaction and easy realization of high flux. The method has important significance for the rapid analysis and detection of fatty acid components and the screening of oil-producing algae strains in the process of microalgae culture.
Description
Technical Field
The invention relates to a transesterification method, in particular to a method for directly transesterifying hydrous microalgae biomass by using a microchannel reactor under acid catalysis.
Background
The transesterification reaction is an indispensable process in the analysis of fatty acids of oils and fats based on gas chromatography. The laboratory establishes an acid-catalyzed direct transesterification technology of the aqueous microalgae biomass, and the reaction time is 1 hour (Bioresource technology,176(0), 284-287.); im and the like establish a method for directly transesterifying the microalgae biomass containing water by using a cosolvent chloroform,
the reaction was continued for 1.5 hours to achieve a yield of 91.1% (Bioresource Technology,152, 534-537.). However, although the above techniques shorten the transesterification reaction time, they still cannot meet the requirement of rapidly determining the change of fatty acid components in the process of culturing microalgae. For the existing microalgae oil fatty acid analysis technology based on gas chromatography, due to mass transfer limitation of transesterification reaction, direct transesterification of water-containing microalgae biomass is still the rate-limiting step in the whole analysis process.
Due to the miniaturized characteristic size of the microchannel reactor, compared with the traditional reactor, the microchannel reactor has the advantages of large specific surface area, high mass and heat transfer efficiency and easy parallel amplification to realize high flux. The reaction rate of the conventional acid catalysis transesterification reaction is mainly limited by the mass transfer rate between two-phase reactants, and the conversion efficiency needs to be improved by prolonging the reaction time, so that the problem of low efficiency of the conventional acid catalysis transesterification can be solved by using a microchannel reactor with large specific surface area and high mass transfer efficiency for transesterification, and the required reaction time is shortened. In published Chinese patents CN 101148409A and CN 1861751A, and in academic literature published by various Research groups, microchannel reactors have been used for transesterification reactions to shorten the transesterification time (Chemical Engineering Science,104, 610-. However, in the above techniques, liquid oil is used as a raw material, and when the liquid oil is applied to fatty acid component analysis of a microalgae sample, an oil extraction process is still required, and the problem of long time consumption in fatty acid component analysis of microalgae is not solved.
In conclusion, the existing direct transesterification technology for the hydrous microalgae biomass and the transesterification technology based on the microchannel reactor have advantages and disadvantages, and if the advantages of the existing direct transesterification technology for the hydrous microalgae biomass and the transesterification technology based on the microchannel reactor can be combined, the transesterification operation efficiency of the hydrous microalgae biomass can be greatly improved, and the timeliness of microalgae biomass detection and the efficiency of subsequent processing can be further improved. However, in the prior art system, the microchannel reactor has small channel size, and the distribution of the water-containing biomass in the alcohol solution is not uniform, which causes the problems of reaction channel blockage or uneven sample reaction and the like, so that the transesterification of the water-containing microalgae biomass in the direct microreactor has not been successfully reported. Through analyzing the difficulties, the breakthrough core is to solve the problem of uniform distribution of the water-containing microalgae biomass in the reaction system. The invention introduces the inert medium polyethylene glycol with certain viscosity and density as the suspending agent for the first time, successfully realizes the uniform and stable dispersion of the water-containing microalgae biomass in a liquid system, and further completes the subsequent transesterification reaction.
Usually, microalgae cells obtained after primary dewatering of microalgae culture fluid by different harvesting processes such as centrifugation are called algal mud (science and technology in food industry, 36(4), 199-. Microalgae colonies generally refer to macroscopic colonies of microalgae cells grown on solid media (aquatic biologies report, 37(3), 547-552).
According to the invention, the water-containing microalgae biomass is uniformly dispersed in the reaction system by using the specific suspending agent, so that the problem of pipeline blockage in the process of directly performing transesterification on the water-containing microalgae biomass by using the microchannel reactor is solved, and the steps of sample drying and grease extraction are omitted. Moreover, by introducing the microchannel reactor technology, the mass transfer efficiency in the reaction process is greatly increased, the transesterification reaction rate is increased, and the microalgae fatty acid component analysis process is simplified. It is expected that the method can be applied to fatty acid component analysis of different biological grease samples, such as oleaginous yeast and the like, by properly modifying the rapid transesterification technology of the microchannel reactor, and provides a feasible method for fatty acid component analysis in the formation process of complex biological samples by adopting trace sample detection, thereby having important significance to related production and research.
Disclosure of Invention
The invention aims to provide a method for rapidly transesterifying water-containing microalgae biomass by using a microchannel reactor, which solves the problems of complicated analysis process of fatty acid components, low reaction efficiency, long consumed time and the like of the prior transesterification technology.
A method for carrying out rapid transesterification on water-containing microalgae biomass by using a microchannel reactor comprises the steps of firstly, re-suspending the water-containing microalgae biomass by using a pre-prepared alcoholic solution I (acid-short chain alcoholic solution), then adding a solution II (0.5g/mL-1.0g/mL suspending agent-short chain alcohol), wherein the adding amount is 1-4 times of the volume of the solution I, and uniformly mixing. And injecting the uniformly mixed sample into the microchannel reactor by using a metering pump to start reaction, and controlling the reaction temperature and the reaction time.
Wherein, the microchannel reactor is a corrosion-resistant capillary microchannel reactor with the inner diameter of 0.2 mm-1.0 mm. The short-chain alcohol is generally understood to be an alcohol with 1-4 carbon atoms, and comprises methanol, ethanol, propanol, isopropanol, butanol or isobutanol, wherein methanol or ethanol is preferred. The acid is sulfuric acid or hydrochloric acid, the dosage of the acid is 1-10% of the volume of the short-chain alcohol, the acid is purchased from commercial products, and the common specifications are 95-98% of sulfuric acid and 36-38% of hydrochloric acid. The transesterification reaction temperature is 70-110 ℃, and the reaction time is 5-30 min. The suspending agent should have a relatively high density or viscosity, and be compatible with short-chain alcohol, and the average molecular weight of the polyethylene glycol series compound which does not react with other substances in a transesterification system is between 1000-10000; the water-containing microalgae biomass is fresh microalgae biomass with the water content not higher than 95% obtained by centrifuging or filtering a microalgae culture solution to remove water, the water-containing microalgae biomass refers to microalgae biomass with the mass water content of 5-95%, specifically is algae mud obtained by concentrating the microalgae culture solution, and can also be one or two of microalgae colonies obtained by plate culture. The microalgae is unicellular algae selected from one or more of green algae, golden algae, and diatom. The invention realizes the direct transesterification of the water-containing microalgae biomass in the microchannel reactor for the first time, omits the steps of raw material drying and grease extraction compared with the traditional intermittent transesterification method, and greatly enhances the mixing degree of heterogeneous reactants due to the characteristic of high mass and heat transfer efficiency of the microchannel reactor, thereby having higher reaction efficiency. And secondly, compared with the traditional method, the method has the advantages of simple steps, high reaction speed and low sample consumption, is convenient to integrate and couple with gas chromatography analysis, realizes one-step analysis of fatty acid components of the microalgae biomass, has important significance for realizing online analysis of fatty acid components of trace biological samples, has important application value in aspects of fatty acid metabolic analysis and the like in microalgae cells particularly in the process of culturing microalgae, and cannot be realized by the traditional intermittent transesterification method.
Drawings
FIG. 1 is the thin-layer chromatography results of direct transesterification efficiency in a micro-channel reactor for aqueous microalgae biomass at different reaction temperatures, wherein (A), (B), (C) and (D) are the thin-layer chromatography results of the standard and the products obtained in examples 1, 2 and 3, respectively.
Tables 1, 2, 3 and 4 show the fatty acid compositions obtained by transesterification of the golden, nannochloropsis, and chlorella vulgaris obtained in examples 1, 2, 3 and 4, respectively, with a microchannel reactor, wherein BR and MR are the results of transesterification in a conventional flask and transesterification in a microchannel reactor, respectively, to obtain the fatty acid compositions, -10%, and + 10% is the variation range of ± 10% based on the results obtained after transesterification in a conventional flask. For fatty acid components with relative content of more than 10% obtained by micro-reactor transesterification, the fatty acid relative content is within +/-10% variation range of traditional flask transesterification, namely, the fatty acid component result obtained by the micro-reactor transesterification method is considered to be consistent with the traditional flask transesterification result.
Detailed Description
The invention firstly provides a method for directly transesterifying water-containing microalgae biomass based on a microchannel reactor, which directly transesterifies the water-containing microalgae biomass with the water content of not more than 95 percent in the microchannel reactor, omits the steps of raw material drying and oil extraction, and accelerates the speed of the transesterification reaction.
The process and results of the present invention are illustrated by the following specific examples. It should be understood that these examples are only intended to illustrate the present invention and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The microchannel reactor of the present invention can be obtained by directly purchasing commercial products or processing the products by the same processing method as conventional products, and will not be described in detail herein.
Example 1:
resuspending 30mg of aqueous microalgae biomass (with mass water content of 90%) obtained by centrifuging the equilateral sarcandra glabra culture fluid by using 1mL of a pre-prepared sulfuric acid-methanol solution with volume concentration of 6%, adding 2mL of a 0.8g/mL polyethylene glycol methanol solution with average molecular weight of 4000, mixing uniformly, injecting into a microchannel reactor by using an injection pump, keeping the reaction time for 20min, and reacting at the temperature of 90 ℃. After the reaction, an outlet sample was collected, and the treated sample was subjected to product analysis using gas chromatography (qualitative by standard comparison or mass spectrometry), and the composition of the obtained fatty acids is shown in table 1. By comparing the results obtained by the direct transesterification in the microchannel reactor with the transesterification in the conventional flask, the fatty acid components and relative contents obtained by the method disclosed by the invention are within a range of +/-10% credible variation based on the transesterification in the conventional flask. And the traditional flask transesterification method needs at least 1h, but the method only needs 20min of reaction, thereby greatly accelerating the analysis speed of the microalgae fatty acid. In addition, as can be seen from the results of thin layer chromatography in fig. 1(90 ℃), the major lipid substances (phospholipid PC, triglyceride TAG) contained in the microalgae biomass were converted into Fatty Acid Methyl Ester (FAME) after the reaction in the microchannel reactor, which indicates that the conversion rate obtained by the method is high.
Example 2:
using 1mL of 6% pre-prepared sulfuric acid-methanol solution to re-suspend 100mg of aqueous microalgae biomass (with mass water content of 80%) obtained from the centrifugal nannochloropsis oculata culture solution, adding 3mL of 0.8g/mL polyethylene glycol methanol solution with the average molecular weight of 4000, mixing uniformly, injecting into a microchannel reactor by using an injection pump, keeping for 15min, and reacting at 100 ℃. After the reaction was completed, the outlet-treated sample was subjected to product analysis using gas chromatography, and the composition of the obtained fatty acid was shown in table 2. As shown in FIG. 1(100 ℃ C.) for the results of thin layer chromatography, the major reactant components (phospholipid PC, triglyceride TAG) in the sample were completely converted into Fatty Acid Methyl Ester (FAME) after passing through the microchannel reactor, and the conversion rate was close to 100%.
Example 3:
the procedure is as in example 1, 100mg of aqueous microalgae biomass (with a mass water content of 80%) obtained from the culture solution of nannochloropsis oculata is resuspended in 2mL of a pre-prepared 4% sulfuric acid-methanol solution, 4mL of a 0.7g/mL polyethylene glycol methanol solution is added, the average molecular weight of polyethylene glycol is 6000, after mixing, the mixture is injected into a microchannel reactor by using an injection pump, the retention time is 30min, and the reaction temperature is 80 ℃. After the reaction was completed, the outlet-treated sample was subjected to product analysis using gas chromatography, and the composition of the obtained fatty acid was shown in Table 3. As can be seen from the results of thin layer chromatography in FIG. 1(80 ℃ C.), most of the major reactant components (phospholipid PC, triglyceride TAG) in the sample were converted into Fatty Acid Methyl Ester (FAME) after passing through the microchannel reactor, and some of the reactants were not converted.
Example 4:
resuspending 100mg of aqueous microalgae biomass (with mass water content of 90%) obtained by centrifuging phaeodactylum tricornutum culture solution by using 1mL of 6% pre-prepared sulfuric acid-methanol solution, adding 4mL of 0.6g/mL polyethylene glycol methanol solution with average molecular weight of 8000, mixing uniformly, injecting into a microchannel reactor by using an injection pump, keeping for 15min, and reacting at 100 ℃. After the reaction was completed, the outlet-treated sample was subjected to product analysis using gas chromatography, and the composition of the obtained fatty acid was shown in Table 4.
Example 5:
the procedure is as in example 1, 50mg of chlorella algae colonies (mass water content 75%) collected from the plate are resuspended in 1mL of a pre-prepared 6% sulfuric acid-methanol solution, 2mL of a 1g/mL polyethylene glycol methanol solution is added, the average molecular weight of polyethylene glycol is 3500, after mixing, the mixture is injected into a microchannel reactor by using a syringe pump, the retention time is 30min, and the reaction temperature is 90 ℃. After the reaction was completed, the outlet-treated sample was subjected to product analysis using gas chromatography, and the composition of the obtained fatty acid was shown in Table 5.
TABLE 1 ingredient list of fatty acids obtained by transesterification in Microchannel reactor of Zhanjiang Coccomys
| Name of component | BR | -10％ | +10％ | MR |
| C14:0 | 13.3±0 | 11.9 | 14.6 | 13.2±0.2 |
| C16:0 | 7.8±0 | 7.0 | 8.5 | 7.4±0.2 |
| C16:1n7 | 5.7±0 | 5.1 | 6.3 | 5.4±0 |
| C16:2n4 | 1.1±0.2 | 1.0 | 1.3 | 1.1±0 |
| C18:1n9 | 10.6±0.1 | 9.6 | 11.7 | 10±0.1 |
| C18:1n7 | 0.9±0.1 | 0.8 | 1.0 | 0.8±0.1 |
| C18:2n6 | 3.4±0 | 3.1 | 3.8 | 3.4±0 |
| C18:3n3 | 9.8±0 | 8.8 | 10.8 | 9.9±0 |
| C18:4n3 | 32.6±0 | 29.3 | 35.9 | 33.8±0.3 |
| C18:5n3 | 3.5±0.1 | 3.1 | 3.8 | 3.7±0 |
| C22:6n3 | 11.3±0 | 10.1 | 12.4 | 11.2±0 |
Description of the drawings: the component names are shorthand notations for fatty acids. Taking C16:1n7 as an example, wherein "C16" indicates that the number of carbon atoms of the fatty acid molecule is 16, the number after the colon (: 1) indicates that the fatty acid molecule has one carbon-carbon double bond, and the number after n "7" indicates the lower of two carbon atom numbers of double bond bonding (counting from the methyl end, the other end is the carboxyl end).
TABLE 2 Table of fatty acid compositions obtained by transesterification in a Nannochloropsis microchannel reactor
| Name of component | BR | -10％ | +10％ | MR |
| C14:0 | 7.2±0 | 6.5 | 8.0 | 7.4±0.2 |
| C16:0 | 33.6±0 | 30.2 | 37.0 | 33.5±0.1 |
| C16:1n7 | 23.1±0.1 | 20.8 | 25.4 | 23.2±0.1 |
| C18:1n9 | 11±0 | 9.9 | 12.1 | 10.7±0 |
| C18:2n6 | 2.6±0 | 2.4 | 2.9 | 2.6±0.1 |
| C20:4n6 | 5.4±0 | 4.8 | 5.9 | 5.3±0 |
| C20:5n3 | 17.1±0.1 | 15.3 | 18.8 | 17.2±0 |
TABLE 3 Table of fatty acid compositions obtained by transesterification in a Nannochloropsis microchannel reactor
TABLE 4 Table of fatty acid compositions obtained by transesterification in Phaeodactylum tricornutum microchannel reactor
| Name of component | BR | -10％ | +10％ | MR |
| C14:0 | 7.1±0 | 6.4 | 7.8 | 7.2±0.1 |
| C16:0 | 15±0.1 | 13.5 | 16.5 | 15.2±0 |
| C16:1n7 | 33.3±0 | 29.9 | 36.6 | 33±0.1 |
| C16:2n4 | 4.1±0 | 3.7 | 4.5 | 4.2±0 |
| C16:3n4 | 5.7±0.1 | 5.1 | 6.3 | 6.1±0.1 |
| C18:1n9 | 5±0.1 | 4.5 | 5.5 | 4.7±0.1 |
| C18:1n7 | 1.2±0.1 | 1.1 | 1.3 | 1.3±0 |
| C20:4n6 | 1.7±0.1 | 1.5 | 1.8 | 1.7±0 |
| C20:5n3 | 27±0.1 | 24.3 | 29.7 | 26.8±0.1 |
TABLE 5 list of fatty acid components obtained by transesterification in Chlorella plate clone algal colony micro-channel reactor
| Name of component | BR | -10％ | +10％ | MR |
| C16:0 | 23.5 | 21.1 | 25.8 | 24.6 |
| C16:1n9 | 0.8 | 0.8 | 0.9 | 0.9 |
| C16:1n7 | 2.5 | 2.2 | 2.7 | 2.6 |
| C16:1n3 | 4.8 | 4.3 | 5.3 | 4.7 |
| C16:3n4 | 11.3 | 10.2 | 12.5 | 10.4 |
| C18:0 | 1.3 | 1.2 | 1.4 | 1.5 |
| C18:1n9 | 4.0 | 3.6 | 4.4 | 4.1 |
| C18:1n7 | 1.1 | 1.0 | 1.2 | 1.2 |
| C18:2n6 | 26.2 | 23.5 | 28.8 | 26.4 |
| C18:3n3 | 24.5 | 22.1 | 27.0 | 23.6 |
The method has the advantages that the micro-channel reactor is used for carrying out the transesterification of the water-containing microalgae biomass, the sample does not need to be dried and the grease extraction treatment, the sample pretreatment process is greatly simplified, and the method has the characteristics of quick reaction and easy realization of high flux. The method has important significance for the rapid analysis and detection of fatty acid components and the screening of oil-producing algae strains in the process of microalgae culture.
Claims (10)
1. The method for directly transesterifying the water-containing microalgae biomass based on the microchannel reactor is characterized by comprising the following steps of: suspending the water-containing microalgae biomass by using a suspending agent, injecting the water-containing microalgae biomass into a microchannel reactor, and carrying out transesterification reaction on short-chain alcohol with 1-4 carbon atoms in the microchannel reactor and lipid components in the water-containing microalgae biomass under an acid catalysis condition to prepare fatty acid short-chain alcohol ester; the suspending agent is polyethylene glycol with the average molecular weight of 1000-10000.
2. The method of claim 1, wherein:
the short-chain alcohol with the carbon atom number of 1-4 comprises one or more of methanol, ethanol, propanol, isopropanol, butanol and isobutanol.
3. The method of claim 2, wherein:
the short-chain alcohol comprises one or two of methanol or ethanol.
4. The method of claim 1, wherein:
the acid is one or two of sulfuric acid or hydrochloric acid, wherein the sulfuric acid is 95-98% of sulfuric acid by mass concentration, and the hydrochloric acid is 36-38% of hydrochloric acid by mass concentration.
5. A method according to claim 1, 2 or 3, characterized in that:
the method comprises the following specific steps: 1) preparing an acid short-chain alcohol solution I, wherein the acid dosage is 1-10% of the volume of the acid short-chain alcohol solution;
preparing 0.5g/mL-1.0g/mL suspending agent-short chain alcohol solution II;
2) after the water-containing microalgae biomass is re-dispersed by using the acid short-chain alcohol solution I, adding a suspending agent-short-chain alcohol solution II to uniformly suspend the dispersed microalgae biomass in a mixed system; wherein the dosage ratio of the water-containing microalgae biomass to the acid short-chain alcohol solution I to the suspending agent-short-chain alcohol solution II is 10-200 mg: 1mL of: 1-4 mL;
3) injecting the mixed system uniformly mixed in the step 2) into a micro-channel reactor by using a metering pump; the reaction time is 5min-30min, and the reaction temperature is 70-110 ℃.
6. The method according to claim 1 or 4, characterized in that:
the microchannel reactor is a capillary microchannel reactor with the inner diameter of 0.2 mm-1.0 mm, which is prepared from an acid corrosion resistant material.
7. The method of claim 6, wherein:
the acid corrosion resistant material is: polytetrafluoroethylene.
8. The method of claim 1, wherein: the water-containing microalgae biomass refers to microalgae biomass with the mass water content of 5-95%, specifically is algae mud obtained by concentrating microalgae culture solution, and can also be one or two of microalgae colonies obtained by plate culture.
9. The method according to claim 1 or 6, characterized in that: the microalgae is unicellular algae selected from one or more of green algae, golden algae, and diatom.
10. The method of claim 1, wherein: the suspending agent is polyethylene glycol with the average molecular weight of 1000-10000.
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