CN102268303B - Method for preparing biological diesel oil by using sludge from municipal wastewater treatment plant - Google Patents
Method for preparing biological diesel oil by using sludge from municipal wastewater treatment plant Download PDFInfo
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- CN102268303B CN102268303B CN201110188716.5A CN201110188716A CN102268303B CN 102268303 B CN102268303 B CN 102268303B CN 201110188716 A CN201110188716 A CN 201110188716A CN 102268303 B CN102268303 B CN 102268303B
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- sludge
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- biological diesel
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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
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Abstract
The invention relates to development of clean energy, in particular to a method for preparing biological diesel oil by using sludge from a municipal wastewater treatment plant. The method comprises the following steps of: with primary sludge or remaining sludge produced by the wastewater treatment plant as a raw material, precipitating and concentrating, then adding 20-40ml of pure yeast with OD600 of 0.5-0.6, and performing enhanced hydrolysis at the temperature of 35 DEG C for 2-4 days; adding methanol and a concentrated sulfuric acid solution, stirring and performing esterification reaction at the temperature of 70-80 DEG C for 24 hours; and finally, naturally cooling the chemically esterified mixed solution to room temperature in air, adding normal hexane, mixing for 3-5 minutes, centrifuging at the rotation speed of 3,000-3,500rpm for 3-5 minutes and extracting. On the premise of saving energy, esterifiable components in the remaining sludge are retained as much as possible, so that the concentration of high molecular organic acid is increased, and further, the conversion rate of the biological diesel oil is increased to the greatest extent and the cost for preparing the biological diesel oil from the sludge is reduced.
Description
Technical field
The invention belongs to development of clean energy field, relate to the preparation of biofuel, be specifically related to utilize the method for municipal sewage sludge preparing biological diesel oil.
Background technology
A large amount of construction of municipal sewage plant, make that excess sludge is a large amount of to be produced and become large important source of pollution that affects atmosphere and water surrounding, but in excess sludge, contain have an appointment 20% can esterification composition.On the other hand, biofuel, as clean renewable energy source, is the petroleum diesel surrogate of high-quality.Biofuel be take the oil plant waterplant such as oil-yielding shrubs fruit, the engineering microalgaes such as the oil crops such as soybean and Semen Brassicae campestris, oil palm and Chinese pistache and animal grease, waste cooking oil etc. and is made as raw material, and 75% of its preparation cost comes from starting material.
Utilize sludge from wastewater treatment plant preparing biological diesel oil not yet to have at home report, external patent has 2 at present: (1) number of patent application: US20040956069, holder of the patent right: Zappi Mark E; French William Todd; Hernandez Rafael; Dufreche Stephen Thomas, patent name: Production of biodiesel and other valuable chemicals from wastewater treatment plant sludges; (2) number of patent application: US20090429858, holder of the patent right: Miguel ASCON; Dolores ASCON, patent name: Methods and systems for production of biofuels and bioenergy products from sewage sludge..Above patent, all adopts dewatered sludge to carry out former bit esterified, but in mud drying process, forms the outermost layer of the phosphatide of cell walls in biological plastid, make its condition that is converted into organic ester very harsh, and the organic acid wrapping in cell walls can only partial esterification.On the other hand, in mud drying process, need to be through processes such as centrifugal, oven dry, pulverizing for obtaining the dewatered sludge of 5% water ratio, will consume a large amount of energy, and in mud drying course, part VFA and alcohols also will inevitably vapor away, and reduce the transformation efficiency of excess sludge to biofuel.In a word, former bit esterified dry excess sludge, cannot avoid that enzymatic synthesis condition is high, energy charge is large, the problem of biofuel low conversion rate.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of method of utilizing municipal sewage sludge preparing biological diesel oil, under energy-conservation prerequisite, retain as far as possible in excess sludge can esterification composition to improve the concentration of macromolecule organic acid, thereby improve most possibly the transformation efficiency of biofuel and reduce mud preparing biological diesel oil cost.
To achieve these goals, the technical solution used in the present invention is:
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, and first precipitation is concentrated makes its concentration in 20～25g/L scope, then adds OD in every liter of mud after concentrated
600be pure yeast 20～40ml of 0.5～0.6, enhanced hydrolysis is 2～4 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1～1.2L methyl alcohol, then to drip 0.07～0.1L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 70～80 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 3～5min, centrifugal 3～5min under 3000～3500rpm rotating speed.
For improving productive rate, described extraction process can be carried out three times repeatedly.
Compared with prior art, the invention has the beneficial effects as follows:
The sludge from wastewater treatment plant of take carries out esterification preparing biological diesel oil as starting material enhanced hydrolysis and to its supernatant liquor, without the centrifugal mummification of mud and grease leaching process, at mud preparing biological diesel oil transformation efficiency, improved the 20-30% that reduces mud preparing biological diesel oil cost under 25% condition.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment mono-
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 20g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.5 pure yeast 40ml, enhanced hydrolysis is 4 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1L methyl alcohol, then to drip 0.1L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 80 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 5min, under 3000rpm rotating speed, centrifugal 5min, obtains biofuel.
Embodiment bis-
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 25g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.5 pure yeast 20ml, enhanced hydrolysis is 2 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1.2L methyl alcohol, then to drip 0.07L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 70 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 3min, under 3000rpm rotating speed, centrifugal 5min, obtains biofuel.
Embodiment tri-
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 21.5g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.56 pure yeast 35ml, enhanced hydrolysis is 3 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1.2L methyl alcohol, then to drip 0.084L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 80 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 5min, under 3500rpm rotating speed, centrifugal 3min, obtains biofuel.
Embodiment tetra-
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 24g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.6 pure yeast 25ml, enhanced hydrolysis is 4 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1L methyl alcohol, then to drip 0.1L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 75 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 5min, under 3300rpm rotating speed, centrifugal 4min, obtains biofuel.
Embodiment five
The method of utilizing municipal sewage sludge preparing biological diesel oil, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 23g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.5 pure yeast 40ml, enhanced hydrolysis is 4 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1.04L methyl alcohol, then to drip 0.07L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 80 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 3min, under 3000rpm rotating speed, centrifugal 3min, obtains biofuel.
Under the condition of embodiment five, biodiesel production rate is 9.24% (in dewatered sludge), and the present invention's reagent such as pure yeast, the vitriol oil, methyl alcohol and normal hexane used are cheap, and wide material sources, effectively reduce preparation cost.
In addition, for further improving the productive rate of biofuel, the extraction in preparation process can be carried out three times repeatedly, the supernatant liquor of at every turn getting extraction results last time further extracts, and adds the amount of reagent normal hexane slightly to reduce.
Claims (1)
1. the method for utilizing municipal sewage sludge preparing biological diesel oil, is characterized in that, comprises the following steps:
The first step, biological reinforced hydrolysis: primary sludge or the excess sludge that sewage work produces of take is raw material, first concentrated to make its concentration be 23g/L to precipitation, then in every liter of mud after concentrated, adds OD
600be 0.5 pure yeast 40ml, enhanced hydrolysis is 4 days at 35 ℃;
Second step, chemical esterification: get the biological reinforced hydrolyzing sludge mixed solution after 1L hydrolysis, add 1.04L methyl alcohol, then to drip 0.07L massfraction be 98% concentrated sulfuric acid solution, stirring reaction is 24 hours at 70～80 ℃ of temperature;
The 3rd step, extraction: the mixed solution after chemical esterification is naturally cooled in air to room temperature, adds 1L normal hexane, mix 3～5min, under 3000～3500rpm rotating speed, centrifugal 3～5min, obtains biofuel, and described extraction process carries out three times repeatedly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110188716.5A CN102268303B (en) | 2011-07-06 | 2011-07-06 | Method for preparing biological diesel oil by using sludge from municipal wastewater treatment plant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110188716.5A CN102268303B (en) | 2011-07-06 | 2011-07-06 | Method for preparing biological diesel oil by using sludge from municipal wastewater treatment plant |
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| Publication Number | Publication Date |
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| CN102268303A CN102268303A (en) | 2011-12-07 |
| CN102268303B true CN102268303B (en) | 2014-03-12 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| KR101436428B1 (en) * | 2013-05-15 | 2014-09-01 | 고려대학교 산학협력단 | Method for biodiesel from sludge and equipment comprising the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962820A (en) * | 2006-11-29 | 2007-05-16 | 任春山 | Process for making bio-diesel oil by using municipal sludge |
| CN101018867A (en) * | 2003-10-02 | 2007-08-15 | 密西西比州立大学 | Production of biodiesel and other valuable chemicals from wastewater treatment plant sludges |
| WO2009132249A3 (en) * | 2008-04-25 | 2009-12-30 | Evolution Energy Production, Inc. | Methods and systems for producing biofuels and bioenergy products from sewage sludge, including recalcitrant sludge |
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2011
- 2011-07-06 CN CN201110188716.5A patent/CN102268303B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101018867A (en) * | 2003-10-02 | 2007-08-15 | 密西西比州立大学 | Production of biodiesel and other valuable chemicals from wastewater treatment plant sludges |
| CN1962820A (en) * | 2006-11-29 | 2007-05-16 | 任春山 | Process for making bio-diesel oil by using municipal sludge |
| WO2009132249A3 (en) * | 2008-04-25 | 2009-12-30 | Evolution Energy Production, Inc. | Methods and systems for producing biofuels and bioenergy products from sewage sludge, including recalcitrant sludge |
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