CN115180790B - Method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction - Google Patents
Method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction Download PDFInfo
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- CN115180790B CN115180790B CN202210886643.5A CN202210886643A CN115180790B CN 115180790 B CN115180790 B CN 115180790B CN 202210886643 A CN202210886643 A CN 202210886643A CN 115180790 B CN115180790 B CN 115180790B
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- 239000010802 sludge Substances 0.000 title claims abstract description 97
- 230000003750 conditioning effect Effects 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 35
- 230000018044 dehydration Effects 0.000 claims abstract description 48
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 238000002156 mixing Methods 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 239000002699 waste material Substances 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000007873 sieving Methods 0.000 claims abstract description 17
- 238000005496 tempering Methods 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000005086 pumping Methods 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 241000233866 Fungi Species 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- 239000003093 cationic surfactant Substances 0.000 claims description 9
- 239000010902 straw Substances 0.000 claims description 9
- 238000000855 fermentation Methods 0.000 claims description 8
- 230000004151 fermentation Effects 0.000 claims description 8
- 230000003113 alkalizing effect Effects 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000012258 culturing Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 5
- 239000002504 physiological saline solution Substances 0.000 claims description 5
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 5
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 230000001954 sterilising effect Effects 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 239000012075 bio-oil Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 241000223259 Trichoderma Species 0.000 claims 1
- 238000007781 pre-processing Methods 0.000 abstract description 8
- 208000005156 Dehydration Diseases 0.000 description 38
- 239000002994 raw material Substances 0.000 description 23
- 150000001720 carbohydrates Chemical class 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 241000596490 Trichoderma citrinoviride Species 0.000 description 4
- 238000010563 solid-state fermentation Methods 0.000 description 4
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007792 gaseous phase Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/122—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/126—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using drum filters
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/147—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using organic substances
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/148—Combined use of inorganic and organic substances, being added in the same treatment step
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention provides a method for preparing biological oil based on sludge tempering and continuous hydrothermal liquefaction, which comprises the following steps: s1, pretreatment of a hardening and tempering agent: crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm; s2, mixing sludge and agricultural and forestry waste: mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 1-10g/L calculated according to the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 300-600r/min, and the stirring time is 10-20min; s3, mechanical dehydration: dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.1-0.4MPa, the dehydration time is 10-30min, and finally controlling the solid content of the obtained sludge mixture to be about 15%; s4, continuous hydrothermal liquefaction: and conveying the sludge mixture subjected to tempering and dehydration into a continuous hydrothermal liquefaction reaction device in a pumping mode.
Description
Technical Field
The invention relates to the technical field of preparation of hydrothermal liquefied biological oil, in particular to a method for preparing biological oil based on sludge tempering and continuous hydrothermal liquefaction.
Background
In recent years, sludge and some agricultural wastes have been studied by expert students in various countries for their characteristics of large yield, high organic matter content, low utilization rate, and the like. Municipal sludge has the dual properties of multi-medium complexity and pollution and resource, and improper treatment causes secondary pollution to the environment and wastes a large amount of resources. At present, the sludge recycling technology comprises anaerobic digestion, drying incineration, composting, a thermochemical treatment method and the like.
The continuous hydrothermal liquefying technology for biomass belongs to a thermochemical treatment mode, and is a technology for realizing continuous feeding and continuous discharging at the reaction temperature and pressure of between 150 and 400 ℃ and between 5 and 30MPa and rapidly converting biomass into biological oil in a short time, and has development potential and competitiveness. The technology can convert organic components such as fat, protein, carbohydrate and the like contained in biomass into biological oil. Wherein the fat conversion is highest, about 90-95%; secondly, protein, the conversion rate is 25-35%; the minimum carbohydrate conversion is 10-20%. The organic components of the sludge are mainly proteins, but the water content is as high as 99%, and the sludge can be subjected to continuous hydrothermal liquefaction after dehydration treatment. The agricultural and forestry waste components generally take lignocellulose (carbohydrate) as a main component, the raw material structure is not suitable for pumping, the continuous hydrothermal liquefaction can be carried out only by adding solvent and tempering, and the current research result shows that the sludge and the agricultural and forestry waste are directly mixed to obtain the hydrothermal liquefaction biological oil with low oil yield and insignificant synergistic effect, and the yield of the hydrothermal liquefaction biological oil can be improved by preprocessing the raw materials.
There is a need in the art for a solution that can improve the yield of continuous co-hydrothermal liquefaction bio-oil.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction.
The aim of the invention can be achieved by the following technical scheme:
a method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction, which comprises the following steps:
s1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
s2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 1-10g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 300-600r/min, and the stirring time is 10-20min;
s3, mechanical dehydration:
dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.1-0.4MPa, the dehydration time is 10-30min, and finally controlling the solid content of the obtained sludge mixture to be about 15%;
s4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
The step S1 specifically comprises the following steps:
crushing agricultural and forestry waste, adding 5-10mL/g of 2mol/L NaOH solution based on the dry weight of the agricultural and forestry waste, alkalizing for 1 hour at normal temperature, adding 0.1-0.5mol/L cationic surfactant solution with equal volume concentration, etherifying for 3 hours at 70 ℃, drying at 105 ℃, grinding and sieving to obtain the conditioner with the thickness of 0.18-0.30 mm.
The step S1 specifically comprises the following steps:
the agricultural and forestry waste such as straw is taken as a raw material, 0.01g/g of monopotassium phosphate, 0.01g/g of calcium carbonate and 0.025-0.05g/g of sodium nitrate are added based on the dry weight of the raw material, distilled water is added, and the raw material is uniformly mixed, and then the mixture is placed in an autoclave for sterilization at 121 ℃ for 2 hours. Mixing 0.01g/g Trichoderma citrinoviride with physiological saline based on dry weight of raw materials, mixing with sterilized straw, adjusting water content to 70-90%, setting temperature in incubator to 21-27deg.C, and air relative humidity to 75%, and culturing for 3-9 days. And (3) placing the fungus chaff after the solid fermentation in a baking oven at 105 ℃, and grinding and sieving to obtain the conditioning agent with the thickness of 0.18-0.30 mm.
In the step S3, the mechanical mode is one of vacuum filtration dehydration, gas pressurization dehydration, plate-frame press filtration or drum dehydration.
Compared with the prior art, the invention has the beneficial effects that:
in the prior art, coal/agriculture and forestry waste is used as a filter aid to assist in sludge dewatering, the water content is reduced as much as possible (30-40%), and the overall heat value of the mixture of sludge and coal/agriculture and forestry waste is improved, because the higher the water content is, the more unfavorable the incineration is. Compared with the prior art, the method has the advantages that the content of lignocellulose organic matters is high, the heat value and the energy of the mixture are improved, but the purpose is to prepare raw materials suitable for corresponding technologies better, the water content (85%) of the sludge mixture in the method is easy to achieve, the requirement is low, and the process difficulty is simplified.
In the prior art, the sludge is mixed with coal/agriculture and forestry waste/plastic/excrement to be subjected to hydrothermal liquefaction, and the physical characteristics of raw materials, such as water content, viscosity, softness and pumpability are not required to be considered in an intermittent experiment mode; or the sludge and other biomasses are mixed and continuously subjected to hydrothermal liquefaction, the raw materials are hardly treated before and after mixing, and the oil yield is correspondingly low. In the application, the function of auxiliary dehydration of lignocellulose is utilized, and the lignocellulose has high organic content, and the pretreatment changes the components of the lignocellulose, so that the hydrothermal liquefaction is facilitated; and thirdly, the physical properties after mixing tempering, including the water content and pumpability, can meet the feeding requirement of continuous hydrothermal liquefaction.
Pretreatment of the conditioning agent: unlike mixing sludge directly with agricultural and forestry waste, the method adopts modified agricultural and forestry waste as modifier and aims at raising the yield of hydrothermal liquefied biological oil. The specific surface area of the pretreated conditioning agent is increased, the compressibility of the sludge mixture can be reduced in the dehydration process, the sludge mixture serves as a framework structure construct, and the sludge mixture has good effect in the low-pressure dehydration process; the cationic surfactant is used for pretreatment, and the pretreated cationic surfactant is mixed with sludge to neutralize the negative charges on the surfaces of sludge particles, weaken negative repulsion, destroy the stability of flocs and improve the dehydration speed; compared with other oxidants, the COD, TOC, TN and other contents of the filtrate are lower, the ash content is higher, so that organic components are reserved in the sludge, the utilization efficiency of the sludge mixture is improved, the filtrate is more convenient and safer to recycle, and the environmental hazard is smaller.
Continuous hydrothermal liquefaction: the sludge mixture formed by mixing and dehydrating the agricultural and forestry waste serving as the conditioner is softer, so that the pumpability is improved, the sludge mixture is not easy to settle in a continuous hydrothermal liquefaction pipeline, and the homogeneity of mixed slurry is improved; the pretreatment of the cationic surfactant has certain softening performance, the pumpability is improved, and the pretreatment of the cationic surfactant in the hydrothermal liquefaction process have certain promotion effect on the conversion of organic components into biological oil; the change of the organic components of the conditioning agent after pretreatment is more beneficial to the hydrothermal liquefaction to produce the biological oil.
Detailed Description
The invention is further illustrated below with reference to examples. The specific examples are provided only for further elaboration of the invention and do not limit the scope of the claims of the present application.
Example 1
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction comprises the following steps of
S1, pretreatment of a hardening and tempering agent:
crushing, pre-treating and grinding the collected agricultural and forestry waste, and sieving to obtain 0.18-0.30
A mm hardening and tempering agent;
the step S1 specifically includes:
crushing agricultural and forestry waste, adding 5mL/g of 2mol/L NaOH solution based on the dry weight of the agricultural and forestry waste, alkalizing for 1 hour at normal temperature, adding 0.1mol/L cationic surfactant solution with equal volume concentration, etherifying for 3 hours at 70 ℃, drying at 105 ℃, grinding and sieving to obtain the conditioner with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 10g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 300r/min, and the stirring time is 10min.
S3, mechanical dehydration:
dehydrating the uniformly mixed sludge mixture mechanically at a dehydration pressure of 0.2
The dehydration time is 5min under MPa, and the solid content of the obtained sludge mixture is controlled to be about 15%.
In the step S3, the mechanical mode is plate-and-frame press filtration or drum dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
The pretreated conditioning agent has positive charges, can neutralize negative electricity of sludge and improve dehydration speed; the mixture is alkaline after being mixed with sludge, which is beneficial to the transformation of carbohydrate in the hydrothermal liquefaction process; the conditioner is mixed with the sludge after the treatment of the anionic surfactant to change the wettability of the surface of the sludge, so that organic components in sludge cells are dispersed, and the conversion in the hydrothermal liquefaction process is facilitated; the pre-treated conditioning agent can adsorb organic components and prevent the organic components from losing in the dehydration process, and compared with the conditioning agent not used, the ash content in the filtrate is increased by 34.7%. Wherein, continuous hydrothermal liquefaction device includes: the device comprises a feeding pipeline, a preheater, a reaction kettle, a filter and a collecting kettle which are connected in sequence. And S4, conveying the dehydrated sludge mixture obtained in the step S4 to a feeding pipeline, preheating the sludge mixture through a preheater, then entering a reaction kettle for hydrothermal liquefaction reaction, collecting a gaseous phase product after the reaction through a gaseous phase collecting device connected with the reaction kettle, collecting a solid phase of a non-gaseous phase product after the reaction through a filter, collecting an unfiltered oil phase and an unfiltered water phase in the collecting kettle, layering the oil phase and the water phase due to density difference, and collecting the oil phase through a centrifugal mode after the reaction is finished.
Example two
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction comprises the following steps of
S1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
the step S1 specifically includes:
crushing agricultural and forestry waste, adding 10mL/g of 2mol/L NaOH solution based on the dry weight of the agricultural and forestry waste, alkalizing for 1 hour at normal temperature, adding 0.5mol/L cationic surfactant solution with equal volume concentration, etherifying for 3 hours at 70 ℃, drying at 105 ℃, grinding and sieving to obtain the conditioner with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 1g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 600r/min, and the stirring time is 20min.
S3, mechanical dehydration:
and (3) dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.4MPa, the dehydration time is 30min, and finally, controlling the solid content of the obtained sludge mixture to be about 15%.
In step S3, the mechanical means is gas pressurized dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
Example III
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction, which comprises the following steps:
s1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
the step S1 specifically includes:
crushing agricultural and forestry waste, adding 6mL/g of 2mol/L NaOH solution based on the dry weight of the agricultural and forestry waste, alkalizing for 1 hour at normal temperature, adding 0.2mol/L cationic surfactant solution with equal volume concentration, etherifying for 3 hours at 70 ℃, drying at 105 ℃, grinding and sieving to obtain the conditioner with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 5g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 500r/min, and the stirring time is 15min.
S3, mechanical dehydration:
and (3) dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.3MPa, the dehydration time is 20min, and finally, controlling the solid content of the obtained sludge mixture to be about 15%.
In step S3, the mechanical mode is vacuum filtration and dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
Example IV
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction, which comprises the following steps:
s1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
the step S1 specifically comprises the following steps:
agricultural and forestry waste such as straw is used as a raw material, 0.01g/g of monopotassium phosphate, 0.01g/g of calcium carbonate and 0.025g/g of sodium nitrate are added based on dry weight of the raw material, distilled water is added, and the raw material is uniformly mixed, and then the mixture is placed in an autoclave for sterilization at 121 ℃ for 2 hours. Mixing 0.01g/g Trichoderma citrinoviride with physiological saline based on dry weight of raw materials, mixing with sterilized straw, adjusting water content to 70%, setting temperature in an incubator at 21 ℃ during fermentation, and culturing for 3 days with air relative humidity of about 75%. And (3) placing the fungus chaff after the solid fermentation in a baking oven at 105 ℃, and grinding and sieving to obtain the conditioning agent with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 10g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 300r/min, and the stirring time is 20min.
S3, mechanical dehydration:
and (3) dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.4MPa, the dehydration time is 10min, and finally, controlling the solid content of the obtained sludge mixture to be about 15%.
In step S3, the mechanical mode is vacuum filtration and dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
The fungus chaff harvested after solid state fermentation pretreatment is changed in physical property and chemical property, and the physical property is as follows: the grain size of the fungus chaff after solid state fermentation is increased, the fiber is longer and the surface is rougher, which is favorable for fully mixing with sludge in the tempering process and for dehydration; chemical properties: the total organic matter content of the fungus chaff after solid state fermentation is increased (the protein and fat content is increased, the carbohydrate content is reduced), and the carbohydrate is converted into protein and fat which are more favorable for being converted into biological oil, so that the fungus chaff is more suitable for being used as a raw material for hydrothermal liquefaction. The content of the fungus chaff after solid state fermentation is increased from 85% to 89.1% relative to the total organic matter content of the raw materials, wherein the fat content is increased by 16 times, and the protein content is increased by 30%.
Example five
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction, which comprises the following steps:
s1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
the step S1 specifically comprises the following steps:
the agricultural and forestry waste such as straw is taken as a raw material, 0.01g/g of monopotassium phosphate, 0.01g/g of calcium carbonate and 0.05g/g of sodium nitrate are added based on dry weight of the raw material, distilled water is added, and the raw material is uniformly mixed, and then the mixture is placed in an autoclave for sterilization at 121 ℃ for 2 hours. Mixing 0.01g/g Trichoderma citrinoviride with physiological saline based on dry weight of raw materials, mixing with sterilized straw, adjusting water content to 90%, setting temperature in incubator at 27deg.C, and air relative humidity at 75%, and culturing for 9 days. And (3) placing the fungus chaff after the solid fermentation in a baking oven at 105 ℃, and grinding and sieving to obtain the conditioning agent with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is calculated to be 8g/L based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 400r/min, and the stirring time is 15min.
S3, mechanical dehydration:
and (3) dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.2MPa, the dehydration time is 15min, and finally, controlling the solid content of the obtained sludge mixture to be about 15%.
In step S3, the mechanical means is gas pressurized dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
Example six
A method for preparing biological oil based on sludge conditioning and continuous hydrothermal liquefaction, which comprises the following steps:
s1, pretreatment of a hardening and tempering agent:
crushing, preprocessing and grinding the collected agricultural and forestry waste, and sieving to obtain a conditioning agent with the thickness of 0.18-0.30 mm;
the step S1 specifically comprises the following steps:
the agricultural and forestry waste such as straw is taken as a raw material, 0.01g/g of monopotassium phosphate, 0.01g/g of calcium carbonate and 0.033g/g of sodium nitrate are added based on dry weight of the raw material, distilled water is added, and the raw material is uniformly mixed, and then the mixture is placed in an autoclave for sterilization at 121 ℃ for 2 hours. Mixing 0.01g/g Trichoderma citrinoviride with physiological saline based on dry weight of raw materials, mixing with sterilized straw, adjusting water content to 80%, setting temperature in an incubator at 23 ℃ during fermentation, and culturing for 6 days with air relative humidity of about 75%. And (3) placing the fungus chaff after the solid fermentation in a baking oven at 105 ℃, and grinding and sieving to obtain the conditioning agent with the thickness of 0.18-0.30 mm.
S2, mixing sludge and agricultural and forestry waste:
mixing the sludge with high water content with the pretreated conditioning agent, wherein the adding amount of the conditioning agent is 1g/L calculated based on the volume of the sludge, and the mixing process is performed in a stirring manner, wherein the stirring speed is 600r/min, and the stirring time is 20min.
S3, mechanical dehydration:
and (3) dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.4MPa, the dehydration time is 30min, and finally, controlling the solid content of the obtained sludge mixture to be about 15%.
In step S3, the mechanical means is drum dehydration.
S4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
The improvement in the yield of continuous hydrothermal liquefaction bio-oil after pretreatment of the conditioning agent compared to the prior art is shown in table 1.
TABLE 1
The present invention is not limited to the above-described embodiments, and it is apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention.
Claims (2)
1. The method for preparing the biological oil based on sludge conditioning and continuous hydrothermal liquefaction is characterized by comprising the following steps of:
s1, pretreatment of a hardening and tempering agent:
crushing agricultural and forestry waste, adding 5-10mL/g of 2mol/L NaOH solution based on the dry weight of the agricultural and forestry waste, alkalizing for 1 hour at normal temperature, adding 0.1-0.5mol/L cationic surfactant solution with equal volume concentration, etherifying for 3 hours at 70 ℃, adding 0.01g/g monopotassium phosphate, 0.01g/g calcium carbonate and 0.025-0.05g sodium nitrate, adding distilled water, uniformly mixing, placing in an autoclave for sterilizing for 2 hours at 121 ℃, mixing 0.01g/g trichoderma citricola with sterilized straws after mixing physiological saline, adjusting the water content to 70-90%, setting the temperature in a culture box to 21-27 ℃ during fermentation, setting the air relative humidity to 75%, culturing for 3-9 days, placing fungus chaff after solid fermentation in an oven at 105 ℃, grinding and sieving to obtain a conditioner of 0.18-0.30 mm;
s2, mixing sludge and agricultural and forestry waste:
mixing sludge with high water content with the pretreated conditioning agent, wherein the addition amount of the conditioning agent is 1-10g/L calculated based on the volume of the sludge, the mixing process is carried out in a stirring manner, the stirring speed is 300-600r/min, and the stirring time is 10-20min;
s3, mechanical dehydration:
dehydrating the uniformly mixed sludge mixture in a mechanical mode, wherein the dehydration pressure is 0.1-0.4MPa, the dehydration time is 10-30min, and finally controlling the solid content of the obtained sludge mixture to be 15%;
s4, continuous hydrothermal liquefaction:
and conveying the dehydrated sludge mixture into a continuous hydrothermal liquefaction reaction device in a pumping mode.
2. The method for preparing bio-oil based on sludge tempering and continuous hydrothermal liquefaction according to claim 1, wherein in step S3, the mechanical means is one of vacuum filtration dehydration, gas pressurization dehydration, plate-and-frame press filtration or drum dehydration.
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| CN108659876A (en) * | 2018-05-18 | 2018-10-16 | 沈阳航空航天大学 | The method for preparing bio oil is combined in pretreatment of raw material with hydrothermal liquefaction |
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| 市政污泥与菌糠共水热液化制生物油的研究;林祥飞;《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》(第2021年第08期期);第12-13、15-16、20-35页 * |
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