CN101899334A - Biomass pyrolysis oil refining method - Google Patents
Biomass pyrolysis oil refining method Download PDFInfo
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Abstract
The invention belongs to the technical field of biomass energy conversion, and relates to a biomass pyrolysis oil refining method. The method comprises the following steps: mixing biological oil stock solution and isooctyl alcohol in the volume ratio of 5:1, adding 2-10 zeolite grains, keeping the low vacuum of 0.02 Mpa, and distilling under reduced pressure in a 80 DEG C water bath until no water can be distilled off, thereby obtaining low-water biological oil; during magnetic stirring, adding equal volume of acetyl chloride to react until no bubbles burst out, thereby obtaining anhydrous biological oil; calculating the generation amount of acetic acid according to the amount of the anhydrous biological oil, adding ethanol to acetic acid in the mol ratio of 2.8:1, mixing catalyst and the anhydrous biological oil in the mass ratio of 1:35, adding 2-10 zeolite grains, stirring, heating for back flow at 80 DEG C, and esterifying to obtain the esterified biological oil; adding anhydrous magnesium sulfate to esterified biological oil in the mass ratio of 1:5 to dehydrate and regulate the acidity; and filtering under reduced pressure to remove solid, thereby obtaining the refined biological oil. The invention has the advantages of simple process route, favorable dehydration effect and high product yield.
Description
Technical field:
The invention belongs to biomass energy transformation technology field, relate to a kind of biomass pyrolysis oil refining method, but bio-oil is refined into the oil fuel that mass-producing is used through the catalysis acid adjustment post-modification that dewaters.
Background technology:
Biomass energy is the fourth-largest energy that is only second to coal, oil, Sweet natural gas, occupies critical role in whole energy resource system.Biomass energy is not only safe, the most stable energy, and by a series of switch technologies, can produce the energy of different varieties, can produce high-quality solid fuel as biomass solid and charing, gasifying biomass can process gas fuel, and biomass liquefying can obtain liquid fuel or the like.That biomass pyrolysis liquefaction can be converted into low-quality, low-calorie biomass energy is high-quality, high heating value, be easy to transport the liquid fuel of storage, can be used as the alternative fuel of petroleum products after the modification upgrading.See that with regard to the present state of the art principal element that influences the biomass pyrolysis liquefaction product has: pyrolysis is temperature, temperature rise rate, gas residence time, influence, pressure and the catalyzer of biological material characteristic, the condensing rate of gas phase bio oil etc. eventually.The bio oil that biomass through pyrolysis is produced belongs to the non-equilibrium product of chemical thermodynamics, therefore has unstable, even liquid ingredient also serial polymerization or condensation reaction can take place in normal temperature is deposited.Bio oil is the mixture of the organic composition of the high complexity of oxygen level, its classes of compounds have hundreds of more than, almost comprised oxygen-bearing organic matter such as all kinds such as ether, ester, aldehyde, ketone, phenol, organic acid, alcohol.In all bio oil, the content of phenol, anthracene, naphthalene and number acid is relative more.Therefore, the physicochemical property difference of bio oil and mineral fuel oil is very big, character such as its high-moisture, rich oxygen content, high viscosity, low heat value and high acid value have hindered it greatly as being extensive use of of hydrocarbon fuel, and especially rich oxygen content causes bio-oil to touch air being easy to adhesive-hardening.Existing in the prior art several different methods is made with extra care to improve its quality bio-oil, satisfy the act as a fuel requirement of oil of bio-oil, the core of bio-oil purification techniques is the oxygen of removing wherein, improves the H/C ratio, make it that enough thermal values be arranged, and have suitable viscosity and pH.
In the prior art, press the reaction process of biomass flash pyrolysis, the process for purification that improves the bio-oil quality is reduced three classes: the first kind is the dehydration and the dealkalize metal treatment of carrying out raw material before quick scission reaction; Second class is to make bio oil steam without the direct upgrading of condensation in the scission reaction process fast, it is carried out catalytic pyrolysis or hydrogenation; The 3rd class is to adopt the bio oil of collecting is carried out wherein one or more means bonded method for modifying such as shortening, catalytic pyrolysis, catalytic esterification, emulsification, interpolation solvent or interpolation antioxidant after scission reaction is finished fast; And wherein the most stubborn problem be that biological water content in oil and tart are removed, lack maturation in the prior art and processing method efficiently; Since the thermo-sensitivity of bio oil, industrial can not the dehydration by the method for air distillation; And because moisture and oily mutual solubility are good, and density is close, also can't reach the purpose of dehydration fully with centrifugal separation method.At present, the quality of bio oil, stability, storage and application also can't be compared with traditional mineral fuel oil, and prior biological oil modified technique is immature, the cost height, dewater and not exclusively (seldom can remove to below 5%), calorific value does not reach standard, deacidification technology imperfection, remaining acid can be big to equipment corrosion in the bio oil, limited effective utilization of bio oil.Therefore, set up energy-conservation, efficient, the perfect bio oil modified technique of a cover and have practical significance.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists, seek to design and a kind of bio oil is made with extra care, improve its physical chemistry quality, make the shared processing methodes such as gasoline of its usefulness that can act as a fuel, this method feature of environmental protection is good, simple to operate, preparation technology is safe and reliable, can effectively remove moisture and acidic substance in the bio oil.
To achieve these goals, solve dewatering of existing in the existing bio oil modification technology technology and acid adjustment not thoroughly, shortcomings such as complex process, operation or auxiliary agent cost height, the biomass thermal cracking oil catalytic esterification that the present invention relates to and the acid adjustment purified method of dewatering comprise that decompression steams that water, Acetyl Chloride 98Min. dewater, catalytic esterification and four processing steps of acid adjustment that dewater:
Water is steamed in decompression: for delaying oil deterioration under the high temperature, by bio oil stoste: 2-10 grain zeolite is mixed and added to the volume ratio of isooctyl alcohol=5: 1, utilize vacuum pump to bleed and keep the rough vacuum of 0.02Mpa, under 80 ℃ of water-baths underpressure distillation 30-60 minute, fractionate out up to anhydrous, after being steamed, 80% above moisture and a small amount of low boiling component must lack aquatic organism oil, and few and oxygen level is high because of the low boiling component amount that steams, and needn't separate again and reclaim;
Acetyl Chloride 98Min. dewaters: reaction can be removed moisture under Acetyl Chloride 98Min. and the water normal temperature, and produces a large amount of acetate and be used for catalytic esterification, lays a good foundation for polyester more generates (raising calorific value); Water few aquatic organism oil afterwards slowly adds equal volume under the magnetic agitation condition Acetyl Chloride 98Min. (Acetyl Chloride 98Min. and water volume ratio reaction in 1: 1 is steamed in decompression, the maintenance Acetyl Chloride 98Min. is excessive a little in order thoroughly to dewater), water absorbs HCl volatilize away and recycles, when no bubble is emerged realization dewater fully anhydrous bio oil;
Catalytic esterification: the add-on of the anhydrous bio oil after dewatering by Acetyl Chloride 98Min. is calculated the growing amount of acetate, and press acetate: the mol ratio of ethanol=1: 2.8 adds ethanol, the immobilized tosic acid of gac is made catalyzer, press catalyzer: the mass ratio of anhydrous bio oil=1: 35 mixes, add 2-10 grain zeolite again, use magnetic stirrer, 80 ℃ of following reflux 2 hours, esterification yield reaches more than 80%, makes the esterification bio oil;
Acid adjustment dewaters: by anhydrous magnesium sulfate: the mass ratio of esterification bio oil=1: 5 adds anhydrous magnesium sulfate and dewaters, suction filtration is removed the compound of the magnesium sulfate heptahydrate of generation, adds the triethylamine of 1/5th volumes and fully stirring in the bio oil liquid behind suction filtration; Acetate, residual hydrogenchloride and triethylamine reaction generate quaternary ammonium salt, bio oil liquid is dissolved with a little quaternary ammonium salt can form pH near neutral buffered soln, and quaternary ammonium salt can be used as a kind of tensio-active agent, evenly miscible with bio oil and diesel oil, after pH transferred to 6.27～7.00, acid generates a large amount of quaternary ammonium salt crystallizations and separates out with triethylamine, or sub-fraction is dissolved in the liquid, and decompress filter is removed solid and promptly got and make with extra care the finished product bio oil.
Compared with the prior art the present invention has following advantage: the one, and decompression is steamed water and is dewatered in conjunction with Acetyl Chloride 98Min., has thoroughly removed the moisture in the bio oil, and lays a good foundation for improving esterification yield and product oil calorific value because of the acetate that generates; The 2nd, the gac form biomass pyrolysis solid product coke that catalytic esterification adopted further activates and gets, the specific surface area height, and the mesothyrid microtexture is suitable for doing the carrier of catalyzed reaction, and makes biomass resource be fully utilized; The 3rd, water and bio oil separate easily that esterification produces, water removal effect is better fully once more to adopt anhydrous magnesium sulfate; The 4th, organic basess such as employing triethylamine carry out esterification and the bio oil after dewatering are carried out acid adjustment handling, not only make the pH value of modified oil be increased to 6～7, the corrodibility of modified oil obviously reduces, the quaternary ammonium salt that reaction generates has the characteristics of tensio-active agent, is beneficial to the miscible of modification artifact oil and petrochemical industry oil; The 5th, upgrading modification artifact oil viscosity, acid value, calorific value and water ratio all reach the fuel oil index of direct utilization, should with the miscible use of petrochemical industry oil product, become the petrochemical industry oil alternative fuel of clean energy type.
Description of drawings:
Fig. 1 is a process for refining flowage structure principle schematic of the present invention.
Fig. 2 is the infrared absorpting light spectra of bio-oil before the invention process.
Fig. 3 is for making the infrared absorpting light spectra of refining biological oil after the invention process.
Embodiment:
Also further specify in conjunction with the accompanying drawings below by embodiment.
The used biomass thermal cracking oil of present embodiment is with sawdust, maize straw, cotton straw raw material, carries out pyrolytic gasification in independently developed bed furnace and mechanical fluidisation sedimentation furnace pyrolysis system, rapid condensation is collected resulting liquid bio oil production; Pyrolysis temperature is 500 ± 10 ℃ in the stove; Go into the stove sawdust and be preheating and drying to water ratio 10wt% when following, liquid bio oil quality yield is 54wt%, and moisture content is about 30% of a liquid oils; The drying water ratio is not when the 15wt% left and right sides to go into the stove sawdust, and liquid bio oil quality yield is 56wt%, and moisture content is about 50% of a liquid oils; And the oil yield of stalk powder raw material only is about 44wt%, is lower than the sawdust raw material; The basic physical properties of bio oil is analyzed as shown in table 1:
The Physical Property Analysis of table 1 bio oil
Present embodiment is the bio oil of raw material by the refining burning of following process with the above-mentioned bio oil that makes:
Water is steamed in decompression: for delaying oil deterioration under the high temperature, by bio oil stoste: 2-10 grain zeolite is mixed and added to the volume ratio of isooctyl alcohol=5: 1, utilize vacuum pump to bleed and keep the rough vacuum of 0.02Mpa, under 80 ℃ of water-baths underpressure distillation 30-60 minute, fractionate out up to anhydrous, after being steamed, 80% above moisture and a small amount of low boiling component must lack aquatic organism oil, and few and oxygen level is high because of the low boiling component amount that steams, and needn't separate again and reclaim;
Acetyl Chloride 98Min. dewaters: reaction can be removed moisture under Acetyl Chloride 98Min. and the water normal temperature, and produces a large amount of acetate and be used for catalytic esterification, lays a good foundation for polyester more generates (raising calorific value); Water few aquatic organism oil afterwards slowly adds equal volume under the magnetic agitation condition Acetyl Chloride 98Min. (Acetyl Chloride 98Min. and water volume ratio reaction in 1: 1 is steamed in decompression, the maintenance Acetyl Chloride 98Min. is excessive a little in order thoroughly to dewater), water absorbs HCl volatilize away and recycles, when no bubble is emerged realization dewater fully anhydrous bio oil;
Catalytic esterification: the add-on of the anhydrous bio oil after dewatering by Acetyl Chloride 98Min. is calculated the growing amount of acetate, and press acetate: the mol ratio of ethanol=1: 2.8 adds ethanol, the immobilized tosic acid of gac is made catalyzer, press catalyzer: the mass ratio of anhydrous bio oil=1: 35 mixes, add 2-10 grain zeolite again, use magnetic stirrer, 80 ℃ of following reflux 2 hours, esterification yield reaches more than 80%, makes the esterification bio oil;
Acid adjustment dewaters: by anhydrous magnesium sulfate: the mass ratio of esterification bio oil=1: 5 adds anhydrous magnesium sulfate and dewaters, suction filtration is removed the compound of the magnesium sulfate heptahydrate of generation, adds the triethylamine of 1/5th volumes and fully stirring in the bio oil liquid behind suction filtration; Acetate, residual hydrogenchloride and triethylamine reaction generate quaternary ammonium salt, bio oil liquid is dissolved with a little quaternary ammonium salt can form pH near neutral buffered soln, and quaternary ammonium salt can be used as a kind of tensio-active agent, evenly miscible with bio oil and diesel oil, after pH transferred to 6.27～7.00, acid generates a large amount of quaternary ammonium salt crystallizations and separates out with triethylamine, or sub-fraction is dissolved in the liquid, and decompress filter is removed solid and promptly got and make with extra care the finished product bio oil.
Embodiment 1:
Be that sawdust raw material bio oil about 30wt% is done Infrared spectroscopy earlier, at 1000cm to water ratio
-1Near stronger absorption peak is arranged is the symmetrical stretching vibration of the C-O-C in the ethers; At 1300cm
-1Near strong absorption peak is arranged is the stretching vibration of C-O key; At 1400cm
-1Near have a more weak absorption peak to be in the alkane-CH
3Charateristic avsorption band; 1600cm
-1Near absorption peak is arranged is the absorption peak of C=C in the aromatic ring, be the skeletal vibration of phenyl ring; At 1700cm
-1Near a very strong absorption peak is arranged is the stretching vibration of C=O, be infrared in the absorption peak of easy identification; At 3000cm
-1Near have several more weak absorption peaks be in the phenyl ring C-H and-CH
3,-CH
2The stretching vibration absorption peak of middle C-H; At 3400cm
-1Near very strong absorption peak is arranged is to form hydrogen bond and associating-OH stretching vibration; Above-mentioned analysis can draw, and contains macromolecular alkane (n＞4) in the biological oil product of raw material, contains ether material, carboxylic acid and alcohols material; Contain the aromatic ring material, may contain ketone, Ester and alkene.
The decompression of present embodiment steam water be get 80mL at a slow speed oil pour matrass into, the isooctyl alcohol (can delay oil deterioration under the high temperature) and the 2-5 grain zeolite that add 1/5 volume, utilize bleeding of vacuum pump to keep the rough vacuum of 0.02Mpa, underpressure distillation under 80 ℃ of water-baths, do not flow out up to there being cut substantially, this technology can be finished in one hour, and most water (about 80%) and low boiling component can be steamed, the low boiling component that cause steams seldom, and oxygen level is very high, so needn't separate and reclaim; It is to measure certain volume (about 20mL) decompression to steam water bio oil afterwards that Acetyl Chloride 98Min. dewaters, Acetyl Chloride 98Min. (Acetyl Chloride 98Min. and the water reaction in 1: 1 that the limit slowly splashes into equal volume is stirred with magneton in the limit, this moment is excessive a little for the maintenance Acetyl Chloride 98Min. that thoroughly dewaters), water absorbs the HCl that volatilizees away and recycles, and finishes when no bubble is emerged; Catalytic esterification is the ethanol that adds 56.7mL in above-mentioned oil (about 35mL) after dewatering with Acetyl Chloride 98Min., add the immobilized tosic acid of 1.2g gac and make catalyzer, add several zeolites again, 80 ℃ of following reflux 2 hours, esterification yield can reach more than 80% with magnetic stirring apparatus; The dehydration acid adjustment is to get the intact oil of 25mL esterification, and adding 5g anhydrous magnesium sulfate stirs the enough time and dewaters, thereafter suction filtration.In the liquid behind suction filtration, add the triethylamine of about 1/5th volumes, fully stir, pH is transferred to 6.27～7.00.Acid generates a large amount of quaternary ammonium salts with triethylamine, and mostly crystallization is separated out, and sub-fraction is dissolved in the liquid, decompress filter remove solid get final product the finished product refining biological oil.
It is as shown in table 2 that each stage of present embodiment obtains the rerum natura of liquid bio oil:
The physical properties of each stage oil of table 2
Embodiment 2:
Present embodiment is got the stalk bio oil of water ratio about 50%, and composition is complicated more, contains a large amount of organic carboxyl acid (as formic acid and acetate), makes the pH of bio oil lower (1～3); Its decompression steam water be get 80mL at a slow speed oil pour matrass into, isooctyl alcohol (can delay oil deterioration under the high temperature) and several zeolites of adding 1/5 volume, utilize bleeding of vacuum pump to keep the rough vacuum of 0.02Mpa, underpressure distillation under 80 ℃ of water-baths is not flowed out up to there being cut substantially, and this technology can be finished in one hour, and most water (about 80%) and low boiling component can be steamed, because of the low boiling component that steams seldom, and oxygen level is very high, so needn't separate and reclaim; It is to measure about 20mL decompression to steam water bio oil afterwards that its Acetyl Chloride 98Min. dewaters, Acetyl Chloride 98Min. (Acetyl Chloride 98Min. and the water reaction in 1: 1 that the limit slowly splashes into equal volume is stirred with magneton in the limit, this moment is excessive a little for the maintenance Acetyl Chloride 98Min. that thoroughly dewaters), water absorbs the HCl that volatilizees away and recycles, and finishes when no bubble is emerged; Its backwash is for adding excessive Acetyl Chloride 98Min., because of the existence of Acetyl Chloride 98Min. and be unfavorable for the carrying out of ensuing esterification.This experimental design adds ethanol according to step 2 back oil and ethanol volume ratio at 1: 0.5.The alcoholic acid adding has reached the purpose of removing excessive Acetyl Chloride 98Min.; Its catalytic esterification be above-mentioned dewater and backwash after the about 35mL of oil in the adding 56.7mL ethanol, add the immobilized tosic acid of 1.2g gac and make catalyzer, add several zeolites again, 80 ℃ of following reflux 2 hours, esterification yield was about 80% with magnetic stirrer; Its acid adjustment that dewaters is to get the intact oil of 25mL esterification, adds anhydrous silica gel and sewage sal epsom 6g altogether, stirs the enough time and dewaters, and adds the long-pending pyridine of about monoploid then in suction filtration and the liquid behind suction filtration, fully stirs, and pH is transferred to 5～6; Acid generates a large amount of salt crystallizations and separates out with pyridine, and sub-fraction is dissolved in the liquid, decompress filter remove solid get final product the finished product refining biological oil.
It is as shown in table 3 that each stage of present embodiment obtains the rerum natura of liquid bio oil:
The physical properties of each stage oil of table 3
Present embodiment has been removed unnecessary Acetyl Chloride 98Min. through backwash, has improved esterification yield, to improving playing a role clearly of bio oil calorific value.
The analysis of present embodiment products obtained therefrom in infrared absorpting light spectra as can be known, 703cm
-1Near stronger absorption is arranged, be-(CH
2)
n-, n＞4 rocking vibrations; 755cm
-1Near more weak absorption is arranged, be that the stretching vibration of C-Cl absorbs; 1050cm
-1Near medium absorption is arranged, be that C-O-C or C-O stretching vibration absorb; 1432cm
-1Near stronger absorption is arranged, be CH
3, CH
2The sex change absorption of vibrations also may be that the skeletal vibration of phenyl ring absorbs; 1587cm
-1Near medium absorption is arranged, be-the C=O stretching vibration absorbs; 1640cm
-1Near more weak absorption is arranged, be that the C=C stretching vibration absorbs; 2976cm
-1Near medium absorption is arranged, be that the stretching vibration of saturated C-H absorbs; 3392cm
-1Near very strong absorption is arranged, be that association-OH stretching vibration absorbs ,-NH
2The stretching vibration of ,-NH absorbs also in this scope; Contain in the bio oil after refining: alkane, chloro thing (compound that chlorine substituent is arranged), ester, ether, aromatic ring class, carboxylic acid, alcohol, amine.
Claims (1)
1. biomass pyrolysis oil refining method, comprising that decompression steams that water, Acetyl Chloride 98Min. dewater, catalytic esterification and four processing steps of acid adjustment that dewater, it is characterized in that decompression steams water: by bio oil stoste: 2-10 grain zeolite is mixed and added to the volume ratio of isooctyl alcohol=5: 1, utilize vacuum pump to bleed and keep the rough vacuum of 0.02Mpa, under 80 ℃ of water-baths, fractionated out to anhydrous in underpressure distillation 30-60 minute, must lack aquatic organism oil after 80% above moisture and a small amount of low boiling component are steamed; Acetyl Chloride 98Min. dewaters: will reduce pressure and steam few aquatic organism oil after the water slowly adds equal volume under the magnetic agitation condition Acetyl Chloride 98Min., water absorbs the HCl that volatilize away and recycles, when no bubble is emerged realization dewater fully anhydrous bio oil; Catalytic esterification: the add-on of the anhydrous bio oil after dewatering by Acetyl Chloride 98Min. is calculated the growing amount of acetate, and press acetate: the mol ratio of ethanol=1: 2.8 adds ethanol, the immobilized tosic acid of gac is made catalyzer, press catalyzer: the mass ratio of anhydrous bio oil=1: 35 mixes, add 2-10 grain zeolite again, use magnetic stirrer, 80 ℃ of following reflux 2 hours, esterification yield reaches more than 80%, makes the esterification bio oil; Acid adjustment dewaters: again by anhydrous magnesium sulfate: the mass ratio of esterification bio oil=1: 5 adds anhydrous magnesium sulfate and dewaters, suction filtration is removed the compound of the magnesium sulfate heptahydrate of generation, adds the triethylamine of 1/5th volumes and fully stirring in the bio oil liquid behind suction filtration; Acetate, residual hydrogenchloride and triethylamine reaction generate quaternary ammonium salt, bio oil liquid is dissolved with quaternary ammonium salt and forms pH neutral buffered solution, quaternary ammonium salt is as tensio-active agent, make the evenly miscible of bio oil and diesel oil, after pH transferred to 6.27～7.00, acid generates the quaternary ammonium salt crystallization with triethylamine and separates out, or is dissolved in the liquid, and decompress filter is removed solid and promptly got and make with extra care the finished product bio oil.
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| CN102786986A (en) * | 2012-08-27 | 2012-11-21 | 青岛科技大学 | Refining technology of microalgae pyrolysis oil |
| WO2014180212A1 (en) | 2013-05-07 | 2014-11-13 | 武汉凯迪工程技术研究总院有限公司 | Method for modifying biomass pyrolysis oil |
| CN105219432B (en) * | 2015-09-11 | 2016-09-07 | 合肥工业大学 | A kind of method improving bio oil lubricity |
| CN110850015A (en) * | 2019-11-14 | 2020-02-28 | 中国人民大学 | Method for improving amount of detectable components in hydrothermal liquefied biological oil |
| CN114053759A (en) * | 2020-07-29 | 2022-02-18 | 北京紫光英力化工技术有限公司 | New process for adding salt and dehydrating water-containing organic matter |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786986A (en) * | 2012-08-27 | 2012-11-21 | 青岛科技大学 | Refining technology of microalgae pyrolysis oil |
| WO2014180212A1 (en) | 2013-05-07 | 2014-11-13 | 武汉凯迪工程技术研究总院有限公司 | Method for modifying biomass pyrolysis oil |
| CN105219432B (en) * | 2015-09-11 | 2016-09-07 | 合肥工业大学 | A kind of method improving bio oil lubricity |
| CN110850015A (en) * | 2019-11-14 | 2020-02-28 | 中国人民大学 | Method for improving amount of detectable components in hydrothermal liquefied biological oil |
| CN114053759A (en) * | 2020-07-29 | 2022-02-18 | 北京紫光英力化工技术有限公司 | New process for adding salt and dehydrating water-containing organic matter |
| CN114053759B (en) * | 2020-07-29 | 2023-05-05 | 北京紫光英力化工技术有限公司 | New process for salt-adding and dehydration of water-containing organic matter |
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