CN103451243A - Method for preparing chemicals from algae through hydrothermal conversion - Google Patents

Method for preparing chemicals from algae through hydrothermal conversion Download PDF

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CN103451243A
CN103451243A CN2013104054472A CN201310405447A CN103451243A CN 103451243 A CN103451243 A CN 103451243A CN 2013104054472 A CN2013104054472 A CN 2013104054472A CN 201310405447 A CN201310405447 A CN 201310405447A CN 103451243 A CN103451243 A CN 103451243A
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algae
micro
solution
culture
hydrothermal
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孙予罕
魏伟
汪靓
赵权宇
孔令照
刘子玉
王慧
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Shanghai Advanced Research Institute of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E50/10—Biofuels, e.g. bio-diesel

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Abstract

The invention discloses a method for preparing chemicals from algae through hydrothermal conversion. The method comprises the following steps of 1) putting microalgae into a photoreactor, regulating the components of a culture medium and forming a culture solution through cultivation; 2) pretreating the culture solution to obtain a treated solution; 3) putting the treated solution into a hydrothermal reaction kettle and carrying out a hydrothermal catalytic coupling hydrogenation reaction to obtain liquid-phase products containing chemicals. The method provided by the invention realizes the conversion of the chemical industrial raw materials from non-renewability to renewability; as a result, the production of bulk chemicals on the petroleum resources is avoided, the carbon balance of the process is realized, the emission of CO2 is reduced greatly, and the production of other high-value-added products is realized; besides, the culture process of microalgae is simple and the yield of the microalgae is high; consequently, the method has wide application prospect.

Description

Method by algae hydrothermal conversion Valuable Chemicals
Technical field
The present invention relates to a kind of method of chemical processed, particularly relate to a kind of by the method for algae hydrothermal conversion Valuable Chemicals.
Background technology
As everyone knows, the non-renewable fossil resource such as oil has formed the foundation stone of world today's fuel and chemical industry.But the problem of environmental pollution caused in the exhaustion day by day of fossil resource and use procedure, such as greenhouse CO 2gas purging, become two bottlenecks that restrict society and sustainable economic development.The dual problem of these resources and environments has greatly promoted people and has studied reproducible biomass resource.Because biomass have carbon balance and reproducible advantage, by Wood Adhesives from Biomass, be that energy chemical and large platform chemicals enjoy people to pay close attention to.Advanced industrial country makes one after another corresponding biomass and utilizes scheme, such as the U.S. expects the year two thousand thirty, from biomass, obtains the organic chemicals more than the liquid fuel and 25% more than 20%.From world wide, the bio-based product account for the petroleum chemicals total value from 2000 less than 1%, rise to 2008 6%, and annual with the speed increment higher than 30%, bio-based plastics is especially with 38% speed increment.The chemical industry that the biomass of take are raw material is the inexorable trend of Sustainable development.
Micro-algae is considered to produce the renewable raw materials of the tool prospect of biofuel and biorefinery because their long speed fast, can effectively consolidate carbon, do not occupy cultivated land and tap water, can accumulate in a large number in addition the potentiality of grease and carbohydrate.The existing family more than 150 in the whole world specializes in the company of micro-algae energy development at present, but there is no so far economically feasible micro-algae energy production system both at home and abroad.From to CO 2emission reduction effect on consider, the biofuel technique that the preparing biological diesel oil of take is end prod is to CO 2actual emission reduction effect enjoy query (T.Searching et al.Science319,1238-1240; 2008).
Producing large platform chemicals by Wood Adhesives from Biomass makes a breakthrough, the Zhang Tao researcher of Dalian Inst of Chemicophysics, Chinese Academy of Sciences successfully is applied to tungsten carbide catalyst cellulosic catalyzed conversion and prepares ethylene glycol, the ethylene glycol yield is opened great waves up to 61%(. and the wolfram varbide catalyse cellulose that nickel promotes directly transforms preparing ethylene glycol. Chinese basic science .2009,3:24-26), mean that the transition that ethylene glycol production is expected to break away from oil relies on, and adopt reproducible Biological resources production line.The low-carbon (LC) such as ethylene glycol, propylene glycol dibasic alcohol is very extensive in industrial application, can be used for producing trevira, frostproofer, lubricant, nonionogenic tenside etc.From the LCA (life cycle assessment) of product, the bio-based chemical transforms and compares biofuel to CO 2the reduction of discharging meaning will be more remarkable.With the energy utilization of micro-algae, compare, take micro-algae as the research that raw material transforms Valuable Chemicals still rare.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of by the method for algae hydrothermal conversion Valuable Chemicals.The method comprises that acquisition, the pre-treatment of algae liquid and the hydrothermal reaction coupling hydrocracking of high sugared micro-algae produce the steps such as low-carbon (LC) di-alcohols chemical, by adopting the high sugar post-directed training of reproducible micro-algal biomass of the present invention and chemical conversion, realizes CO 2green utilization to high-valued product, can effectively reduce discharging CO 2can obtain again the bulk chemical in non-petroleum base source, pass through micro-algal biomass petroleum replacing as basic material, realize a kind of bulk chemical production technique of carbon balance, and overcome a large amount of consumption and the consequent great amount of carbon dioxide emission problem of the Nonrenewable resources that fossil economy brings.
For solving the problems of the technologies described above, of the present invention by the method for algae hydrothermal conversion Valuable Chemicals, comprise step:
(1) micro-algae is put into to photoreactor, and the composition of regulation culture base, to reach the purpose that is conducive to the carbohydrate such as micro-algae accumulation starch, through cultivating, form nutrient solution;
(2) nutrient solution of step (1) are carried out to pre-treatment, obtain treatment solution (as the micro-algae dope after concentrated or other processing or containing micro-algae sugar moieties liquid);
(3) treatment solution of step (2) is put into to hydrothermal reaction kettle, carry out the reaction of hydro-thermal catalysis coupling hydro, obtain the liquid product containing chemical.In step (3), the sugar transformed in micro-algae by reaction orientation obtains chemical.
In described step (1), but micro-algae is the enduring high-concentration CO that screening obtains in agar plate or tubular reactor 2common fresh water or the micro-algae of seawater, comprising: one or more in chlorella, grid algae, spirulina, salt algae, chlamydomonas, Chlorococcum, micro-plan ball algae, four slit bamboo or chopped wood algaes;
Photoreactor comprises: air lift type, tubular type or flat photoreactor etc.
The formula of substratum is:
NaNO 30.2～1.0g/L, K 2hPO 40.02～0.06g/L, MgSO 47H 2o0.03～0.10g/L, CaCl 27H 2o0.02～0.06g/L, citric acid 0.003～0.006g/L, ironic citrate 0.003～0.007g/L, Na 2eDTA0.001～0.004g/L, micro-A5 solution 1ml and water.
Wherein, consisting of of micro-A5 solution: H 3bO 42.86g/L, MnCl 24H 2o1.81g/L, ZnSO 40.222g/L, Na 2moO 40.39g/L, CuSO 45H 2o0.079g/L, Co (NO 3) 26H 2o49.4g/L.
In step (1), culture condition is: CO 2concentration 1～15vol%(volume percent), 20～35 ℃ of culture temperature, the concentration of nutrient solution reaches the micro-algae/L of 2～10g/L(2～10g);
In described step (2), pre-treatment comprises: protein is separated or extracted to concentrated, sugar;
Wherein, concentrated method is: by separation method, nutrient solution is concentrated into to solid content 1～10wt%(mass percent) algae liquid, treat subsequent disposal; Separation method comprises: one or more in natural subsidence, flocculation sediment, filtration, centrifugal, air supporting;
The method that sugar is separated is: by nutrient solution directly or through above-mentioned concentrated after, add the dilute sulphuric acid of 5～20wt% to carry out heating hydrolysis, 90～160 ℃ of hydrolysis temperatures, hydrolysis time 0.5～5 hour, obtain sugary hydrolyzed solution, treats subsequent disposal;
Method for extracting proteins is: through the alkali extraction and acid precipitation method, the molten employing of alkali NaOH is adjusted to 10～11 by pH, and the heavy method of acid adopts HCl that pH is adjusted to 4～5, and the protein in stripping algae liquid obtains removing the algae liquid of protein (most of protein), treats subsequent disposal.
In described step (3), the condition of hydro-thermal catalysis coupling hydro reaction is:
200～300 ℃ of temperature, hydrogen pressure 2.0～10.0MPa, have high reactivity and optionally reacted under the catalyzer existence, and the proportion that catalyst levels accounts for reactant is 5.0～50%, reacts 0.5～8h.
Wherein, the active ingredient of catalyzer comprises: group VIII metal element or subgroup metallic element; The carrier of catalyzer comprises: one or more in gac (AC), diatomite, aluminum oxide, sial;
The group VIII metal element comprises: one or more in Ni, Ru, Rh, Pt;
The subgroup metallic element comprises: one or more in Cu, Zn, Cr, Mo, W.
In described step (3), chemical comprises: ethylene glycol, propylene glycol, butyleneglycol, methyl alcohol, ethanol or propyl alcohol.
In addition, described method also comprises: the liquid product to step (3) carries out further separating-purifying, to obtain refining chemical.
The present invention utilizes the micro-algae that contains a large amount of carbohydrate of cultivating under specified conditions, through simple pre-treatment, transforms to make by hydro-thermal shortening coupling reaction and take the chemical that the low-carbon (LC) dibasic alcohol such as ethylene glycol, propylene glycol are representative.Therefore, with traditional, take oil and compare as the technique of raw material production bulk chemical, of the present invention take micro-algae as the advantage of raw material production chemical as follows:
(1) realize the conversion of industrial chemicals from non-renewable to recyclability, break away from the dependence of the production of bulk chemical to petroleum resources;
(2) realize the carbon balance of technique, reduce discharging in a large number CO 2.For example, take that to produce ethylene glycol be example, the approach of the outer suitability for industrialized production ethylene glycol of Present Domestic be mainly take petroleum path as basic epoxyethane water legal.It is raw material that this production technique be take oil derived product ethene, directly carry out oxidizing reaction and generate oxyethane under catalyst action, after then oxyethane and water being mixed under the heating and pressurizing condition direct reaction, then pass through a series of separation means, remove by product, refining ethylene glycol.Adopt 1 ton of ethylene glycol of the every production of this production technique based on petroleum path, approximately need to consume 2.5 tons of crude oil, discharge CO 27.8 ton.Of the present inventionly take the ethylene glycol production technique that micro-algae is raw material and approximately can reduce discharging CO 210 tons.Therefore, with micro-algae raw material substitution oil production ethylene glycol to CO 2the reduction of discharging effect be huge.
(3) can realize the production of other high value added products, such as micro-algae albumen, micro-phycochrome etc. simultaneously.
(4) micro-algae culture process is simple, and productive rate is high, and, to cultivating water and land used without high requirement, can utilize nitrogen and phosphorus in waste water, realizes the utilization of resources of nutritive substance in the time of carbon emission reduction.Therefore, be with a wide range of applications.
The accompanying drawing explanation
Below in conjunction with accompanying drawing and embodiment, the present invention is further detailed explanation:
Fig. 1 is process flow sheet of the present invention.
Embodiment
The chemical reagent below related to if not otherwise specified, is all commercially produced product.
The carrier of catalyzer comprises: one or more in gac, diatomite, aluminum oxide, sial.
Embodiment 1
From the agar plate of BG-11 substratum, picking one chlorella (Chlorella sp.) amplification culture in 400ml air lift type test tube (photoreactor), maintain the temperature at 20～35 ℃, logical 5%CO 2, and control micro-algae and cultivate the substratum used, the formula of this substratum is as follows:
NaNO 30.4g/L, K 2hPO 40.04g/L, MgSO 47H 2o0.07g/L, CaCl 27H 2o0.03g/L, citric acid 0.005g/L, ironic citrate 0.006g/L, Na 2eDTA0.001g/L, micro-A5 solution 1ml and water.
Wherein, consisting of of micro-A5 solution: H 3bO 42.86g/L, MnCl 24H 2o1.81g/L, ZnSO 40.222g/L, Na 2moO 40.39g/L, CuSO 45H 2o0.079g/L, Co (NO 3) 26H 2o49.4g/L.
Cultivate after 5 days, chlorella concentration reaches the 5g/L(dry weight), total sugar content reaches the 50%(mass percent).Then, chlorella is carried out to natural sedimentation in standing 2 hours, form algae liquid, wherein, the algae slurry concentration 20～80g/L after precipitation.
Above-mentioned algae liquid is put into to the 500ml hydrothermal reaction kettle and carry out the reaction of hydro-thermal catalysis coupling hydro, wherein, reaction conditions is as follows:
250 ℃ of temperature of reaction, reaction times 0.5h, hydrogen pressure 4.0MPa, with the mass ratio of 30%(and reactant) Ni/W 2c is catalyzer.
Reaction is carried out conventional separating-purifying, and is utilized HPLC to be analyzed product after finishing, and the overall yield of the dibasic alcohol obtained is 60.0%.
Embodiment 2
From the agar plate of BG-11 substratum, picking one strain grid algae (Scenedesmus sp.) amplification culture in 1000ml air lift type test tube, maintain the temperature at 25～35 ℃, logical 10%CO 2, and control micro-algae and cultivate the substratum used, the formula of this substratum is as follows:
NaNO 30.8g/L, K 2hPO 40.02g/L, MgSO 47H 2o0.05g/L, CaCl 27H 2o0.03g/L, citric acid 0.005g/L, ironic citrate 0.006g/L, Na 2eDTA0.001g/L, micro-A5 solution 1ml and water.
Wherein, consisting of of micro-A5 solution: H 3bO 42.86g/L, MnCl 24H 2o1.81g/L, ZnSO 40.222g/L, Na 2moO 40.39g/L, CuSO 45H 2o0.079g/L, Co (NO 3) 26H 2o49.4g/L.
Cultivate after 5 days, the grid concentration of algae reaches the 6g/L(dry weight), total sugar content reaches the 60%(mass percent).Then, after the grid algae is concentrated into to solid holdup 5～10% by the air supporting mode, by 1～5%(mass percent) dilute sulphuric acid heating hydrolysis (100 ℃ of hydrolysis temperatures, hydrolysis time 3 hours), the liquid glucose obtained after hydrolysis is put into the 500ml hydrothermal reaction kettle, carry out the reaction of hydro-thermal catalysis coupling hydro, wherein, reaction conditions is as follows:
245 ℃ of temperature, reaction times 1.0h, hydrogen pressure 5.0MPa, take the mass ratio of 30%(and reactant) Ni/ZnO be catalyzer.
Reaction is carried out conventional separating-purifying, and is utilized HPLC to be analyzed product after finishing, and the overall yield that obtains dibasic alcohol is 63.1%.
Embodiment 3
From the agar plate of BG-11 substratum, picking one chlorella (Chlorella sp.) amplification culture in the dull and stereotyped reactor of 20L air lift type, maintain the temperature at 25～30 ℃, logical 15%CO 2, CO 2constantly recycle, and control micro-algae and cultivate the substratum used, the formula of this substratum is as follows:
NaNO 30.85g/L, K 2hPO 40.02g/L, MgSO 47H 2o0.04g/L, CaCl 27H 2o0.03g/L, citric acid 0.005g/L, ironic citrate 0.006g/L, Na 2eDTA0.001g/L, micro-A5 solution 1ml and water.
Wherein, consisting of of micro-A5 solution: H 3bO 42.86g/L, MnCl 24H 2o1.81g/L, ZnSO 40.222g/L, Na 2moO 40.39g/L, CuSO 45H 2o0.079g/L, Co (NO 3) 26H 2o49.4g/L.
Cultivate after 5 days, chlorella concentration reaches the 5.5g/L(dry weight), total sugar content reaches the 58%(mass percent).Chlorella is centrifugal under 4000rpm, and centrifugal rear algae slurry concentration 50～80g/L, be adjusted to 10 with 1M NaOH by pH, stirring and leaching, then, more centrifugal 30min under the condition of 10000 * g, supernatant liquor adjusts pH to 4.5 to carry out isoelectric point precipitates albumen with 1M HCl.
Then, the algae-residue after the most of chlorella albumen of extraction is put into to the 2L hydrothermal reaction kettle and carry out the reaction of hydro-thermal catalysis coupling hydro, wherein, reaction conditions is as follows:
240 ℃ of temperature, reaction times 1.5h, hydrogen pressure 4.5MPa, take the mass ratio of 30%(and reactant) Ru/C be catalyzer.
Reaction is carried out conventional separating-purifying, and is utilized HPLC to be analyzed product after finishing, and the overall yield that obtains dibasic alcohol is 65.0%.

Claims (7)

1. one kind by the method for algae hydrothermal conversion Valuable Chemicals, it is characterized in that, comprises step:
(1) micro-algae is put into to photoreactor, and the composition of regulation culture base, nutrient solution formed through cultivating;
(2) nutrient solution of step (1) is carried out to pre-treatment, obtain the treatment solution;
(3) treatment solution of step (2) is put into to hydrothermal reaction kettle, carry out the reaction of hydro-thermal catalysis coupling hydro, obtain the liquid product containing chemical.
2. the method for claim 1, it is characterized in that: in described step (1), micro-algae comprises: one or more in chlorella, grid algae, spirulina, salt algae, chlamydomonas, Chlorococcum, micro-plan ball algae, four slit bamboo or chopped wood algaes;
Photoreactor comprises: air lift type, tubular type or flat photoreactor;
The formula of substratum is:
NaNO 30.2～1.0g/L, K 2hPO 40.02～0.06g/L, MgSO 47H 2o0.03～0.10g/L, CaCl 27H 2o0.02～0.06g/L, citric acid 0.003～0.006g/L, ironic citrate 0.003～0.007g/L, Na 2eDTA0.001～0.004g/L, micro-A5 solution 1ml and water;
Wherein, consisting of of micro-A5 solution: H 3bO 42.86g/L, MnCl 24H 2o1.81g/L, ZnSO 40.222g/L, Na 2moO 40.39g/L, CuSO 45H 2o0.079g/L, Co (NO 3) 26H 2o49.4g/L;
Culture condition is: CO 2concentration 1～15vol%, 20～35 ℃ of culture temperature, the concentration of nutrient solution reaches the micro-algae/L of 2～10g.
3. the method for claim 1, it is characterized in that: in described step (2), pre-treatment comprises: protein is separated or extracted to concentrated, sugar;
Wherein, concentrated method is: by separation method, nutrient solution is concentrated into to the algae liquid of solid content 1～10wt%, treats subsequent disposal; Separation method comprises: one or more in natural subsidence, flocculation sediment, filtration, centrifugal, air supporting;
The method that sugar is separated is: by nutrient solution directly or through above-mentioned concentrated after, add the dilute sulphuric acid of 5～20wt% to carry out heating hydrolysis, 90～160 ℃ of hydrolysis temperatures, hydrolysis time 0.5～5 hour, obtain sugary hydrolyzed solution, treats subsequent disposal;
Method for extracting proteins is: through the alkali extraction and acid precipitation method, wherein, the molten employing of alkali NaOH is adjusted to 10～11 by pH, and the heavy method of acid adopts HCl that pH is adjusted to 4～5, and the protein in stripping algae liquid obtains removing the algae liquid of protein, treats subsequent disposal.
4. the method for claim 1 is characterized in that: in described step (3), the condition of hydro-thermal catalysis coupling hydro reaction is:
200～300 ℃ of temperature, hydrogen pressure 2.0～10.0MPa is reacted under catalyzer exists.
5. method as claimed in claim 4, it is characterized in that: the proportion that the consumption of described catalyzer accounts for reactant is 5.0～50%, reacts 0.5～8h;
The active ingredient of described catalyzer comprises: group VIII metal element or subgroup metallic element; The carrier of catalyzer comprises: one or more in gac, diatomite, aluminum oxide, sial;
Wherein, the group VIII metal element comprises: one or more in Ni, Ru, Rh, Pt;
The subgroup metallic element comprises: one or more in Cu, Zn, Cr, Mo, W.
6. the method for claim 1, it is characterized in that: in described step (3), chemical comprises: ethylene glycol, propylene glycol, butyleneglycol, methyl alcohol, ethanol or propyl alcohol.
7. the method for claim 1, it is characterized in that: described method also comprises: the liquid product to step (3) carries out separating-purifying.
CN2013104054472A 2013-09-09 2013-09-09 Method for preparing chemicals from algae through hydrothermal conversion Pending CN103451243A (en)

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Cited By (6)

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CN103864573A (en) * 2014-03-13 2014-06-18 中国科学院上海高等研究院 Method for preparing chemical products by direct hydrothermal hydrogenation of microalgae
CN103966101A (en) * 2014-05-26 2014-08-06 临沂大学 Culture medium and culture method for cultivating Tetraselmis subcordiformis by utilizing winery wastewater
CN104130964A (en) * 2014-07-31 2014-11-05 青岛农业大学 Seawater spirulina culture solution
CN105646644A (en) * 2016-02-22 2016-06-08 北京珍生康业生物科技有限公司 Preparation method of euglena protein
CN111232949A (en) * 2020-02-02 2020-06-05 江苏省农业科学院 Preparation method of chlorella hydrothermal carbon material and application of chlorella hydrothermal carbon material in rice production
CN112439417A (en) * 2020-11-19 2021-03-05 中国矿业大学 Iron-aluminum-carbon composite catalytic material, preparation method and organic wastewater degradation method

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN103864573A (en) * 2014-03-13 2014-06-18 中国科学院上海高等研究院 Method for preparing chemical products by direct hydrothermal hydrogenation of microalgae
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CN104130964A (en) * 2014-07-31 2014-11-05 青岛农业大学 Seawater spirulina culture solution
CN105646644A (en) * 2016-02-22 2016-06-08 北京珍生康业生物科技有限公司 Preparation method of euglena protein
CN111232949A (en) * 2020-02-02 2020-06-05 江苏省农业科学院 Preparation method of chlorella hydrothermal carbon material and application of chlorella hydrothermal carbon material in rice production
CN111232949B (en) * 2020-02-02 2022-11-25 江苏省农业科学院 Preparation method of chlorella hydrothermal carbon material and application of chlorella hydrothermal carbon material in rice production
CN112439417A (en) * 2020-11-19 2021-03-05 中国矿业大学 Iron-aluminum-carbon composite catalytic material, preparation method and organic wastewater degradation method
CN112439417B (en) * 2020-11-19 2022-09-06 中国矿业大学 Iron-aluminum-carbon composite catalytic material, preparation method and organic wastewater degradation method

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Application publication date: 20131218