CN104004552A - Method for preparing biodiesel from municipal sludge based on in-situ ester exchange - Google Patents
Method for preparing biodiesel from municipal sludge based on in-situ ester exchange Download PDFInfo
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- CN104004552A CN104004552A CN201410235722.5A CN201410235722A CN104004552A CN 104004552 A CN104004552 A CN 104004552A CN 201410235722 A CN201410235722 A CN 201410235722A CN 104004552 A CN104004552 A CN 104004552A
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- sludge
- original position
- transesterify
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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
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention provides a method for preparing biodiesel from sludge in an urban sewage treatment plant based on in-situ ester exchange. The method comprises the following steps: (1) performing heat drying on the sludge as a raw material in the sewage treatment plant to obtain dry sludge; (2) performing in-situ ester exchange reaction on the dry sludge under the catalytic action of sulfuric acid by taking methanol as an ester exchange agent and a solvent to obtain a mixed solution after in-situ ester exchange; (3) extracting the mixed solution by taking n-hexane as an extracting agent, collecting supernatant and abandoning subnatant; (4) washing the supernatant by a potassium bicarbonate solution and collecting an upper-layer n-hexane phase; (5) filtering, evaporating and collecting a product. According to the method, the sludge drying process is subjected to energy-saving optimization, the sludge pre-treatment is carried out by adopting the heat drying process, the reactions of sludge dissolution, ester extraction and ester exchange are carried out in one step, the ester extraction process is omitted, the cost for preparing the biodiesel from the sludge is reduced, and the reaction efficiency is improved.
Description
Technical field
The invention belongs to development of clean energy and changing waste into resources field, be specifically related to a kind of method of the municipal sludge preparing biological diesel oil based on original position transesterify.
Background technology
World energy sources crisis now and ecocrisis impel the exploitation of new clean energy to become the task of top priority.Utilizing city sludge to manufacture biofuel is exactly one of settling mode.Expert estimates that the energy containing in town sewage is ten times of Treating Municipal Sewage energy used, and more than 50% energy containing in town sewage has been transferred in mud through sewage treatment process, in mud, contain 10%-20% can transesterify composition, by mud preparing biological diesel oil, be practicable.On the other hand; biofuel is as clean renewable energy source; it is with soybean; Semen Brassicae campestris, Sunflower Receptacle, palm; coconut wet goods be raw materials cost account for whole biofuel goods total cost 70% to 80%; the cost of manufacture of this great number has hindered the supply of biofuel, compares and has also lost competitive edge, and caused such as crisis in food etc. in interior international problem with traditional fossil energy.Under the background of Chinese arable land scarcity of resources, we need to find the raw material source of more biofuel.The mud of urban wastewater treatment firm is an extraordinary raw material just, it both abundant, continually and cost low, can greatly reduce the production cost of biofuel and can guarantee raw material supply, meanwhile, also solved the problem of sludge treatment difficulty.If thereby to utilize the heavy mud of primary sludge/secondary to carry out preparing biological diesel oil will be very promising application.
Summary of the invention
The object of this invention is to provide a kind of method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify.The mud of Qi Yi municipal sewage plant is starting material, carries out original position transesterify preparing biological diesel oil, to obtain maximum biodiesel production rate.
The method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify provided by the present invention, comprises the steps:
(1) sludge pretreatment: the mud that sewage work obtains of take is raw material, processes through heat drying, obtains dewatered sludge;
(2) original position transesterify: take methyl alcohol as transesterify agent and solvent, make described dewatered sludge carry out original position transesterification reaction under sulfuric acid catalysis effect, obtain the mixed solution after original position transesterify;
(3) extraction: the normal hexane of take extracts as the mixed solution of extraction agent after to described original position transesterify, collects supernatant liquor, and subnatant is discarded;
(4) clean: with scavenging solution, described supernatant liquor is cleaned, collect upper strata normal hexane phase;
(5) filtration, evaporation and product-collecting: make described normal hexane mutually by the filtration unit containing water-removal agent, collect filtrate; To described filtrate evaporation process, to remove remaining organic solvent, collect the resistates after evaporation, obtain biofuel goods.
In aforesaid method step (1), described mud can be the mud that any treatment step of sewage work obtains.
Described heat drying is processed and is carried out in baking oven, and the condition that described heat drying is processed is: at 103～105 ℃, toast 10h-12h.The water content of gained dewatered sludge is less than 1%.
Described sludge pretreatment step also comprises the step that the dewatered sludge obtaining is shaken on vibration mill to processing, and the time that described vibrations are processed is 2～3min.
In aforesaid method step (2), described sulfuric acid be take the form of the sulphuric acid soln that mass concentration is 98% and is added; In described original position transesterification reaction, also add normal hexane to dissolve to increase lipid.
The sulphuric acid soln that described dewatered sludge and methyl alcohol, mass concentration are 98%, the proportioning of normal hexane are followed successively by 10g:100-150mL:1.5-10mL:50-100mL.
The temperature of reaction of described original position transesterification reaction is 45-75 ℃, and the reaction times is 4-8h.
Described original position transesterification reaction can under agitation be carried out, and the stir speed (S.S.) of described stirring is 300-600rpm.
In aforesaid method step (3), described extraction step is also included in the front step that mixed solution after the original position transesterify obtaining is cooled to room temperature of extraction.
In above-mentioned extraction process, also can in the mixed solution after described original position transesterify, add sodium chloride saturated solution, to reduce the solubleness of product in solution, the product that obtains as much as possible, and can suppress the generation of emulsification.
After described extraction finishes, also comprise centrifugal step; Described centrifugal condition is 3000-5000rpm, and the centrifugal time is 5-10min.
In addition, in order further to improve the productive rate of biofuel, also the subnatant after step (3) extraction can be extracted to (as repeatedly extracted 3 times) repeatedly according to the operation of step (3).In each extraction, the add-on of normal hexane can slightly reduce.
In aforesaid method step (4), described scavenging solution be selected from following at least one: potassium bicarbonate solution, distilled water and sodium hydrogen carbonate solution, potassium bicarbonate solution.The mass concentration of described potassium bicarbonate solution is 2-4%.
Described cleaning is carried out in separating funnel.Described cleaning can be carried out 3-5 time.
In aforesaid method step (5), described water-removal agent be selected from following at least one: anhydrous sodium sulphate, anhydrous magnesium sulfate and Calcium Chloride Powder Anhydrous.Described evaporation process is carried out in vacuum rotary evaporator, and the temperature of described evaporation process is 40-50 ℃, and pressure is 0.01-0.02MPa, and the time is 20-25min.
Compared with prior art, the invention has the beneficial effects as follows: the sludge from wastewater treatment plant of take passes through original position transesterify preparing biological diesel oil as starting material, what sludge pretreatment adopted is heat drying, sludge drying process has been carried out to energy saving optimizing, adopt original position ester-interchange method, mud dissolve, lipid extraction and this three phases reaction of transesterification reaction be combined in a step and carry out, and omitted lipid extraction process, reduce mud preparing biological diesel oil cost, improved reaction efficiency.
Embodiment
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.
The experimental technique using in following embodiment if no special instructions, is ordinary method; In following embodiment, reagent used, material etc., if no special instructions, all can obtain from commercial channels.
Following embodiment raw sludge used is from Gaobeidian City sewage work, and wherein the content of total fat is 10%.
Embodiment 1
1. sludge pretreatment
The mud 100g obtaining with sewage work at 105 ℃ of baking ovens baking 12h, shakes 2min on vibration mill, obtains water content lower than 1% dewatered sludge 17g.
2. original position transesterify
Get gained dewatered sludge 10g, add 101ml methyl alcohol and 50ml normal hexane, the sulphuric acid soln that 4.5ml mass concentration is 98%, 75 ℃ of temperature, reacts under 300rpm stir speed (S.S.) 8 hours, obtains the mixed solution after original position transesterify.
3. extraction
Mixed solution after the transesterify of gained original position is cooled to room temperature, adds 100ml hexane solution, 10ml saturated nacl aqueous solution, fully mixes 4min, and centrifugal 5min under 3000rpm condition extracts supernatant liquor, and subnatant is discarded.
4. clean
By gained supernatant liquor, by separating funnel, with the potassium bicarbonate solution of 20ml mass concentration 2%, clean 3 times, collect the normal hexane phase on upper strata.
5. filtration, evaporation and product-collecting
By gained normal hexane phase, by being covered with the filtration unit of anhydrous sodium sulphate, collect filtrate.The filtrate of collecting is through at 40 ℃ of temperature, and vacuum tightness be-vacuum rotary evaporator of 0.08-0.09MPa, to remove remaining normal hexane and methanol solution, collect the resistates 1.02g after evaporating, obtain biofuel goods.
Under this condition, biodiesel production rate is 10.2% (in dewatered sludge).
Embodiment 2
1. sludge pretreatment
The mud 100g obtaining with sewage work at 105 ℃ of baking ovens baking 12h, shakes 2min on vibration mill, obtains water content lower than 1% dewatered sludge 17g.
2. original position transesterify
Get gained dewatered sludge 10g, add 125ml methyl alcohol and 50ml normal hexane, the sulphuric acid soln that 7ml mass concentration is 98%, 75 ℃ of temperature, reacts under 300rpm stir speed (S.S.) 8 hours, obtains the mixed solution after original position transesterify.
3. extraction
Mixed solution after the transesterify of gained original position is cooled to room temperature, add 100ml hexane solution, 10ml saturated sodium-chloride, fully mix 3～5min, centrifugal 5min under 3000rpm condition, extracts supernatant liquor, subnatant is repeated to extract 3 times according to aforesaid operations, hexane solution used is 100mL altogether, is followed successively by 40mL, 30mL, 30mL, merges supernatant liquor.
4. clean
By gained supernatant liquor, by separating funnel, with the potassium bicarbonate solution of 20ml mass concentration 2%, clean 4 times, collect the normal hexane phase on upper strata.
5. filtration, evaporation and product-collecting
By gained normal hexane phase, by being covered with the filtration unit of anhydrous sodium sulphate, collect filtrate.The filtrate of collecting is through at 40 ℃ of temperature, and vacuum tightness be-vacuum rotary evaporator of 0.08-0.09MPa, to remove remaining normal hexane and methanol solution, collect the resistates 1.29g after evaporating, obtain biofuel goods.
Under this condition, biodiesel production rate is 12.9% (in dewatered sludge).
Embodiment 3
1. sludge pretreatment
The mud 100g obtaining with sewage work at 105 ℃ of baking ovens baking 12h, shakes 2min on vibration mill, obtains water content lower than 1% dewatered sludge 17g.
2. original position transesterify
Get gained dewatered sludge 10g, add methyl alcohol and the 50ml normal hexane of 151.5ml, the sulphuric acid soln that 10ml mass concentration is 98%, 45 ℃ of temperature, reacts under 300rpm stir speed (S.S.) 8 hours, obtains the mixed solution after original position transesterify.
3. extraction
Mixed solution after the transesterify of gained original position is cooled to room temperature, the hexane solution that adds 100ml, 10ml saturated sodium-chloride, fully mix 5min, centrifugal 5min under 3000rpm condition, extracts supernatant liquor, subnatant is repeated to extract 3 times according to aforesaid operations, hexane solution used is 100mL altogether, is followed successively by 40mL, 30mL, 30mL, merges supernatant liquor.
4. clean
By gained supernatant liquor, by separating funnel, with the potassium bicarbonate solution of 20ml concentration 2%, clean 3 times, collect the normal hexane phase on upper strata.
5. filtration, evaporation and product-collecting
By gained normal hexane phase, by being covered with the filtration unit of anhydrous sodium sulphate, collect filtrate.The filtrate of collecting is through at 40 ℃ of temperature, and vacuum tightness be-vacuum rotary evaporator of 0.08-0.09MPa, to remove remaining normal hexane and methanol solution, collect the resistates 1.29g after evaporating, obtain biofuel goods.
Under this condition, biodiesel production rate is 12.9% (in dewatered sludge).
Embodiment 4
1. sludge pretreatment
The mud 100g obtaining with sewage work at 105 ℃ of baking oven baking 12h, shakes 2min on vibration mill, obtains water content lower than 1% dewatered sludge 17g.
2. original position transesterify
Get gained dewatered sludge 10g, add methyl alcohol and the 50ml normal hexane of 151.5ml, the sulphuric acid soln that 6ml mass concentration is 98%, at 55 ℃, reacts under 300rpm stir speed (S.S.) 8 hours, obtains the mixed solution after original position transesterify.
3. extraction
Mixed solution after the transesterify of gained original position is cooled to room temperature, the hexane solution that adds 100ml, 10ml saturated sodium-chloride, fully mix 5min, centrifugal 5min under 3000rpm condition, extracts supernatant liquor, subnatant is repeated to extract 3 times according to aforesaid operations, hexane solution used is 100mL altogether, is followed successively by 40mL, 30mL, 30mL, merges supernatant liquor.
4. clean
By gained supernatant liquor, by separating funnel, with the potassium bicarbonate solution of 20ml concentration 2%, clean 5 times, collect the normal hexane phase on upper strata.
5. filtration, evaporation and product-collecting
By gained normal hexane phase, by being covered with the filtration unit of anhydrous sodium sulphate, collect filtrate.The filtrate of collecting is through at 40 ℃ of temperature, and vacuum tightness be-vacuum rotary evaporator of 0.08-0.09MPa, to remove remaining normal hexane and methanol solution, collect the resistates 1.23g after evaporating, obtain biofuel goods.
Under this condition, biodiesel production rate is 12.3% (in dewatered sludge).
Claims (9)
1. the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify, comprises the steps:
(1) sludge pretreatment: the mud that sewage work obtains of take is raw material, processes through heat drying, obtains dewatered sludge;
(2) original position transesterify: take methyl alcohol as transesterify agent and solvent, make described dewatered sludge carry out original position transesterification reaction under sulfuric acid catalysis effect, obtain the mixed solution after original position transesterify;
(3) extraction: the normal hexane of take extracts as the mixed solution of extraction agent after to described original position transesterify, collects supernatant liquor, and subnatant is discarded;
(4) clean: with scavenging solution, described supernatant liquor is cleaned, collect upper strata normal hexane phase;
(5) filtration, evaporation and product-collecting: make described normal hexane mutually by the filtration unit containing water-removal agent, collect filtrate; To described filtrate evaporation process, to remove remaining organic solvent, collect the resistates after evaporation, obtain biofuel goods.
2. the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify according to claim 1, is characterized in that: in step (1), described mud is the mud that any treatment step of sewage work obtains;
Described heat drying is processed and is carried out in baking oven, and the condition that described heat drying is processed is: at 103-105 ℃, toast 10-12h; The water content of gained dewatered sludge is less than 1%;
Described sludge pretreatment step also comprises the step that the dewatered sludge obtaining is shaken on vibration mill to processing, and the time that described vibrations are processed is 2-3min.
3. the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify according to claim 1 and 2, is characterized in that: in step (2), described sulfuric acid be take the form of the sulphuric acid soln that mass concentration is 98% and added; In described original position transesterification reaction, also add normal hexane;
The sulphuric acid soln that described dewatered sludge and methyl alcohol, mass concentration are 98%, the proportioning of normal hexane are followed successively by 10g:100-150mL:1.5-10mL:50-100mL.
4. according to arbitrary described method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify in claim 1-3, it is characterized in that: in step (2), the temperature of reaction of described original position transesterification reaction is 45-75 ℃, and the reaction times is 4-8h;
Described original position transesterification reaction is under agitation carried out, and the stir speed (S.S.) of described stirring is 300-600rpm.
5. according to the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify described in any one in claim 1-4, it is characterized in that: in step (3), described extraction step is also included in the front step that mixed solution after the original position transesterify obtaining is cooled to room temperature of extraction;
In extraction process, also in the mixed solution after described original position transesterify, add sodium chloride saturated solution;
After described extraction finishes, also comprise centrifugal step; Described centrifugal condition is 3000-5000rpm, and the centrifugal time is 5-10min.
6. according to the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify described in any one in claim 1-5, it is characterized in that: in step (4), described scavenging solution be selected from following at least one: potassium bicarbonate solution, distilled water and sodium hydrogen carbonate solution; The mass concentration of described potassium bicarbonate solution and sodium hydrogen carbonate solution is 2-4%.
7. according to the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify described in any one in claim 1-6, it is characterized in that: in step (4), described cleaning is carried out in separating funnel; Described cleaning is carried out 3-5 time.
8. according to the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify described in any one in claim 1-7, it is characterized in that: in step (5), described water-removal agent be selected from following at least one: anhydrous sodium sulphate, anhydrous magnesium sulfate and Calcium Chloride Powder Anhydrous; Described evaporation process is carried out in vacuum rotary evaporator, and the temperature of described evaporation process is 40-50 ℃, and pressure is 0.01-0.02Mpa, and the time is 20-25min.
9. according to the method by sludge from wastewater treatment plant preparing biological diesel oil based on original position transesterify described in any one in claim 1-8, it is characterized in that: in step (5), described evaporation process is carried out in vacuum rotary evaporator, the temperature of described evaporation process is 40-50 ℃, pressure is 0.01-0.02Mpa, and the time is 20-25min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105506011A (en) * | 2016-01-13 | 2016-04-20 | 山东联星能源集团有限公司 | Method for preparing biodiesel through microbial oil |
| CN105670803A (en) * | 2016-02-26 | 2016-06-15 | 同济大学 | Method for preparing biodiesel by enhancing microorganisms in excess sludge to enrich and produce grease |
| CN108004030A (en) * | 2017-11-17 | 2018-05-08 | 天津大学 | The method that biodiesel is prepared using oily sludge two-step method |
| CN109306287A (en) * | 2017-07-28 | 2019-02-05 | 中国人民大学 | A method of biodiesel is prepared by raw material of sludge |
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| CN1962820A (en) * | 2006-11-29 | 2007-05-16 | 任春山 | Process for making bio-diesel oil by using municipal sludge |
| CN102925294A (en) * | 2012-11-26 | 2013-02-13 | 西安建筑科技大学 | Mehtod for preparing biodiesel by floating slag from in-situ esterification sewage treatment plant |
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| CN1962820A (en) * | 2006-11-29 | 2007-05-16 | 任春山 | Process for making bio-diesel oil by using municipal sludge |
| CN102925294A (en) * | 2012-11-26 | 2013-02-13 | 西安建筑科技大学 | Mehtod for preparing biodiesel by floating slag from in-situ esterification sewage treatment plant |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506011A (en) * | 2016-01-13 | 2016-04-20 | 山东联星能源集团有限公司 | Method for preparing biodiesel through microbial oil |
| CN105670803A (en) * | 2016-02-26 | 2016-06-15 | 同济大学 | Method for preparing biodiesel by enhancing microorganisms in excess sludge to enrich and produce grease |
| CN109306287A (en) * | 2017-07-28 | 2019-02-05 | 中国人民大学 | A method of biodiesel is prepared by raw material of sludge |
| CN108004030A (en) * | 2017-11-17 | 2018-05-08 | 天津大学 | The method that biodiesel is prepared using oily sludge two-step method |
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Application publication date: 20140827 |