CN111001366A - Method for reducing concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil - Google Patents
Method for reducing concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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Abstract
本发明公开了一种降低污泥水热液化生物油中多环芳烃浓度的方法，包括步骤如下：(1)将新鲜污泥放置于微波化学反应炉中，预加热；(2)至高温高压反应釜中，密封，通入N2，在常压下加热进行水热液化处理；(3)冷却至室温，排空气体后，取出混合物，固液分离，得到液体产物；(4)用二氯甲烷萃取获得油相组分，蒸发，分离得到生物油。本发明利用微波能具有高穿透性、加热均匀、加热效率高等优点，在相同输出功率下，微波可以在极短的时间内加热，再转移至高温高压反应釜内，能低；微波具有高穿透性，可将污泥内部的难以低温裂解的有机物转化为易于低温裂解的小分子物质，降低水热液化生物油中的多环芳烃浓度，提升生物油品质。The invention discloses a method for reducing the concentration of polycyclic aromatic hydrocarbons in sludge hydrothermal liquefaction bio-oil, comprising the following steps: (1) placing fresh sludge in a microwave chemical reaction furnace, and preheating; In the reaction kettle, sealed, fed with N 2 , heated under normal pressure to carry out hydrothermal liquefaction treatment; (3) cooled to room temperature, and after exhausting the gas, the mixture was taken out, and the solid-liquid separation was performed to obtain a liquid product; (4) with two Extraction with methyl chloride to obtain oil phase components, evaporation, and separation to obtain bio-oil. The invention utilizes the microwave energy to have the advantages of high penetration, uniform heating and high heating efficiency. Under the same output power, the microwave can be heated in a very short time, and then transferred to the high temperature and high pressure reaction kettle, and the energy is low; the microwave has high energy The penetrability can convert the organic substances in the sludge that are difficult to crack at low temperature into small molecules that are easy to crack at low temperature, reduce the concentration of polycyclic aromatic hydrocarbons in the hydrothermal liquefied bio-oil, and improve the quality of the bio-oil.
Description
Technical Field
The invention relates to the field of preparation of biological oil, and particularly relates to a method for reducing concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction biological oil.
Background
Sludge is an inevitable by-product produced during sewage treatment. By the end of 2017, the total amount of sludge produced in China in the whole country is over 4000 million tons and shows a trend of increasing year by year, and the sludge yield in China in the whole country is expected to reach 6000 million tons by 2020. Sludge, called "biosolids" by the world's aquatic environment organization, is very complex in composition, typically including organic matter (lipids, sugars, proteins, cellulose, etc.), heavy metals (Pb, Cr, Cd, Ni, Cu, etc.), pathogens, and inorganic minerals (CaO, SiO)2Etc.) and the like; but the sludge contains a large amount of organic matters (50-80 percent) and has extremely high resource utilization value.
At present, the thermochemical treatment of sludge is widely accepted as an efficient stabilization, reduction, harmless and recycling treatment mode, the thermochemical treatment can effectively solve the problems brought by the traditional sludge treatment mode, and organic matters in the sludge are recycled to form available energy.
The subcritical water technology is gradually concerned by the field of bio-oil preparation by sludge hydrothermal liquefaction due to the characteristics of greenness, no pollution, relatively easy control of operation, relatively low cost and the like. The subcritical water is water which is between 100 ℃ and 374 ℃ and still keeps liquid under the condition of external pressure. Under subcritical conditions, the concentration of hydrogen ions and hydroxyl ions is increased, so that water can be used as a solvent, can also be in the form of an acid/base catalyst or can be used as a reactant to participate in chemical reaction, and the chemical reaction rate is increased due to the action of high temperature and high pressure.
Polycyclic aromatic hydrocarbons are common components in sludge hydrothermal liquefaction biological oil, are usually colorless solids (a small amount of crystals are light yellow and deep yellow) at normal temperature, are mostly insoluble in water, have strong carcinogenic, teratogenic and mutagenic effects (for organisms), and also have a bioaccumulation effect. Therefore, the high content of polycyclic aromatic hydrocarbon in the sludge hydrothermal liquefaction bio-oil limits the application of the sludge hydrothermal liquefaction bio-oil in the later period.
The microwave heating technology has the advantages of uniform heating, high thermal efficiency and capability of selectively heating organic matters. Compared with the traditional method, the method has the advantages that the content of nitrogen-containing compounds in the oil generated by microwave sludge pyrolysis is much less, and the quality of the biological oil can be further improved.
Therefore, it is highly desirable to develop a technique to reduce the concentration of polycyclic aromatic hydrocarbons in the sludge-liquefied bio-oil so as to obtain high-quality bio-oil and realize the real energy utilization of sludge.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil, which has the advantages of high chemical reaction rate and good bio-oil quality.
The technical scheme of the invention is summarized as follows:
a method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) placing fresh sludge in a microwave chemical reaction furnace, and preheating;
(2) transferring the preheated sludge into a high-temperature high-pressure reaction kettle, sealing the reaction kettle and introducing N2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating under normal pressure;
(3) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(4) and (4) extracting the liquid product obtained in the step (3) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and separating to obtain the biological oil.
The microwave power for preheating in the step (1) is 150-600W, and the preheating time is 5-30 min.
The microwave power for preheating in the step (1) is 360W, and the preheating time is 20 min.
In the step (2), the hydrothermal liquefaction treatment temperature is 280 plus 360 ℃ under normal pressure, and the heat preservation residence time is 30-60 min.
The temperature of rotary evaporation in the step (4) is 42-50 ℃.
The invention has the following beneficial effects:
the invention utilizes the advantages of high penetrability, uniform heating, high heating efficiency and the like of microwave energy, and the microwave can heat the sludge to 80-100 ℃ in a very short time under the same output power and then quickly transfer the sludge into the high-temperature high-pressure reaction kettle, thereby reducing the energy consumption in the experiment; the microwave has high penetrability, can convert organic matters which are difficult to crack at low temperature in the sludge into micromolecular substances which are easy to crack at low temperature, reduces the concentration of polycyclic aromatic hydrocarbon in the hydrothermal liquefied bio-oil, and improves the quality of the bio-oil.
Drawings
FIG. 1 shows the types and concentrations of polycyclic aromatic hydrocarbons in bio-oil according to example 1 and comparative example 1 of the present invention.
FIG. 2 shows the types and concentrations of polycyclic aromatic hydrocarbons in bio-oil according to example 2 and comparative example 2 of the present invention.
FIG. 3 shows the types and concentrations of polycyclic aromatic hydrocarbons in bio-oil according to example 3 and comparative example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples. However, the present invention is not limited to these examples.
Example 1
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is placed in a microwave chemical reaction furnace, and preheated for 20min under the microwave power of 360W;
(2) transferring the preheated sludge into a high-temperature high-pressure reaction kettle, sealing the reaction kettle and introducing N2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating to 300 ℃ and keeping the temperature for 45min under normal pressure;
(3) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(4) and (4) extracting the liquid product obtained in the step (3) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at the temperature of 45 ℃ to obtain the biological oil.
Example 2
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is placed in a microwave chemical reaction furnace, and preheated for 30min under 150W of microwave power;
(2) transferring the preheated sludge into a high-temperature high-pressure reaction kettle, sealing the reaction kettle and introducing N2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating to 360 ℃ and preserving the temperature for 30min under normal pressure;
(3) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(4) and (4) extracting the liquid product obtained in the step (3) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at 50 ℃ to obtain the biological oil.
Example 3
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is placed in a microwave chemical reaction furnace, and preheated for 5min under 600W of microwave power;
(2) transferring the preheated sludge into a high-temperature high-pressure reaction kettle, sealing the reaction kettle and introducing N2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating to 280 ℃ and preserving the heat for 60min under normal pressure;
(3) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(4) and (4) extracting the liquid product obtained in the step (3) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at 42 ℃ to obtain the biological oil.
Comparative example 1
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is put into a high-temperature high-pressure reaction kettle, the kettle body is sealed, and N is introduced2The air in the kettle is exhausted, and hydrothermal liquefaction treatment is carried out at the hydrothermal temperature of 300 ℃ and the heat preservation time of 45min under normal pressure;
(2) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(3) and (3) extracting the liquid product obtained in the step (2) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at the temperature of 45 ℃ to obtain the biological oil.
Comparative example 2
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is put into a high-temperature high-pressure reaction kettle, the reaction kettle is sealed, and N is introduced2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating to 360 ℃ and preserving the temperature for 30min under normal pressure;
(2) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(3) and (3) extracting the liquid product obtained in the step (2) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at 50 ℃ to obtain the biological oil.
Comparative example 3
A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil comprises the following steps:
(1) 200g of fresh sludge is placed in a high-temperature high-pressure reaction kettle, the reaction kettle is sealed, and N is introduced2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating to 280 ℃ and preserving the heat for 60min under normal pressure;
(2) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(3) and (3) extracting the liquid product obtained in the step (2) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into a rotary evaporator, and performing rotary evaporation at 42 ℃ to obtain the biological oil.
The bio-oils of examples 1 to 3 and comparative examples 1 to 3 were subjected to GC-MS detection, and the percentage content of each species was determined by functional group classification and area normalization according to peak area to identify the species and concentration of polycyclic aromatic hydrocarbons in the bio-oil. As can be seen from the graphs 1-3, the concentration of polycyclic aromatic hydrocarbon in the bio-oil can be obviously reduced by adding microwave pretreatment in the preparation process of the sludge hydrothermal liquefaction bio-oil.
By implementing the method, the concentration of the polycyclic aromatic hydrocarbon in the sludge hydrothermal liquefaction bio-oil can be obviously reduced by utilizing the characteristic of microwave, so that the feasibility of later-stage utilization of the bio-oil is improved.
The method of the present invention has been described in detail with reference to the above embodiments, but the present invention is not limited to the above embodiments, and the experimental conditions and method can be flexibly modified without departing from the scope of the present invention.
Claims (5)
1. A method for reducing the concentration of polycyclic aromatic hydrocarbon in sludge hydrothermal liquefaction bio-oil is characterized by comprising the following steps:
(1) placing fresh sludge in a microwave chemical reaction furnace, and preheating;
(2) transferring the preheated sludge into a high-temperature high-pressure reaction kettle, sealing the reaction kettle and introducing N2The air in the reaction kettle is exhausted, and the hydrothermal liquefaction treatment is carried out by heating under normal pressure;
(3) stopping heating the reaction kettle, naturally cooling to room temperature, emptying the gas in the reaction kettle, opening the reaction kettle, taking out the mixture, and performing solid-liquid separation to obtain a liquid product;
(4) and (4) extracting the liquid product obtained in the step (3) by using dichloromethane to obtain an oil phase component, transferring the oil phase component into an evaporator, and separating to obtain the biological oil.
2. The method as claimed in claim 1, wherein the microwave power for preheating in step (1) is 150-600W, and the preheating time is 5-30 min.
3. The method according to claim 2, wherein the microwave power for preheating in step (1) is 360W, and the preheating time is 20 min.
4. The method according to claim 1, wherein the hydrothermal liquefaction treatment temperature in step (2) is 280-360 ℃ at normal pressure, and the retention time is 30-60 min.
5. The method according to claim 1, wherein the temperature of the evaporation in the step (4) is 42-50 ℃.
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