CN105219418A - A kind of method adopting municipal sludge to prepare biofuel - Google Patents
A kind of method adopting municipal sludge to prepare biofuel Download PDFInfo
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- CN105219418A CN105219418A CN201510678394.0A CN201510678394A CN105219418A CN 105219418 A CN105219418 A CN 105219418A CN 201510678394 A CN201510678394 A CN 201510678394A CN 105219418 A CN105219418 A CN 105219418A
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- municipal sludge
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Abstract
The invention provides a kind of method adopting municipal sludge to prepare biofuel, comprise one by the step of municipal sludge drying; A step of grinding mud, is ground to particle diameter between 70-80 μm, then toasts by mud; A step extracted mud take mixed solvent as extraction agent, and adopt the method for surname extraction to extract, a step of evaporating extraction agent, then puts and dry in an oven, obtains solid-state fat extract; One is carried out the step of esterification to grease, adds the vitriol oil, methyl alcohol in solid-state fat extract, at 50 ~ 80 DEG C, esterification reaction of organic acid occurs; Then adopt organic solvent to extract, obtain biofuel.The set of the present invention advantage of surname extraction and mixing solutions, by the disposable extraction of the grease of heterogeneity in mud, whole experimentation is simple, safety.
Description
Technical field
The invention belongs to chemical field, relate to a kind of biofuel, specifically a kind of method adopting municipal sludge to prepare biofuel.
Background technology
At present, although China's energy industry sustainable development, for positive contribution has been made in Economic development, energy dilemma and problem of environmental pollution still highlight day by day.Energy dilemma and ecocrisis impel the exploitation of reproducible clean energy to become the task of top priority.Utilizing the mud of the sewage treatment plants in cities and towns to prepare biofuel is one of settling mode wherein.Annual China all can produce a large amount of municipal sludges, and the process of these mud not only cost is high but also easily cause secondary pollution.On the other hand containing 10%-20% in mud can the composition of transesterify, it is feasible for preparing biofuel by mud.
Raw material mainly soybean oil, rapeseed oil, sunflower oil, the palm wet goods of current production biofuel, the cost of these raw materials account for the 70%-80% of biofuel goods total cost, and the cost of manufacture of this great number seriously hinders the development of Biodiesel.Simultaneously due to the soil that the growth needs of these plants is a large amount of, rob the growing space that account for food crop, easily cause crisis in food.And the mud of municipal sewage plant is due to inherently waste, pollutent, so the cost obtaining it is very low.Its abundance, and the cost requirement that can meet production of biodiesel continually, can ensure raw material supply again, finally also can solve the process problem of mud.Therefore, preparing biofuel with municipal sludge is a very promising application.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of method adopting municipal sludge to prepare biofuel, the method that described this employing municipal sludge prepares biofuel solves municipal sludge of the prior art and is not well utilized, the technical problem of contaminate environment.
The invention provides a kind of method adopting municipal sludge to prepare biofuel, comprise the steps:
1) one by the step of municipal sludge drying, the mud obtained with sewage work is raw material, obtain dry mud through heated drying;
2) step of grinding mud, is ground to particle diameter between 70-80 μm by mud, then toasts 4 ~ 8 hours in 50 ~ 70 DEG C of baking ovens, then cools room temperature;
3) step extracted mud take mixed solvent as extraction agent, and adopt the method for surname extraction to extract, described mixed solvent is made up of polar solvent and non-polar solvent, and described polar solvent boiling point is lower than non-polar solvent.
4) step of evaporating extraction agent, heats the reactant of step 3), until extraction agent evaporation completely, then puts and dries in an oven, obtain solid-state fat extract;
5) one is carried out the step of esterification to grease, adds people's sulfuric acid, methanol solution, solid-state fat extract: sulfuric acid: the mass volume ratio of methanol solution is 5g:2 ~ 4ml:198ml, at 50 ~ 80 DEG C, esterification reaction of organic acid occurs in the grease extracted; Then adopt normal hexane solvent extraction fatty acid methyl ester, obtain biofuel, detect through GC-MS and show that the content of longer chain fatty acid methyl esters reaches more than 96%.
Further, the mud that described mud obtains for any treatment step of sewage work.
Further, described mixed solvent is the mixture of normal hexane and acetone or normal hexane and chloroform or normal hexane and methyl alcohol composition, described normal hexane and the volume ratio of acetone are 2:1, and the volume ratio of normal hexane and chloroform is 2:1, and the volume ratio of normal hexane and methyl alcohol is 2:1.
Further, the mass percent concentration of described concentrated sulfuric acid solution is 98%, and described methanol solution is anhydrous methanol.
Further, in the mixed solvent of extraction, described low-boiling polar solvent accounts for 1/2 of extractor volume, and mixed solvent entirety accounts for 1/3 of extraction vessel volume.
Further, carry out in the step of esterification at one to grease, the solid-state fat extract of 5g calculates, fat extract solid-state for 5g is put into a reaction vessel, add people 198ml anhydrous methanol and make it to dissolve, then add people 2 ~ 4ml vitriol oil, reflux 20 ~ 50min at 50 ~ 80 DEG C, reflux 20 ~ 50min at 50 ~ 80 DEG C, then, adds normal hexane extraction esterification product, take out supernatant liquor, lower floor uses n-hexane again, is separated, the supernatant liquor finally obtained evaporate to dryness again.
Concrete, described drying sludge is in oil bath pan drying, and treatment condition are: drying 7 ~ 15 hours at 100 ~ 120 DEG C, the water content of gained dewatered sludge is less than 1%.
Concrete, the baking step of described solid-state fat extract is: first, dry at 100 ~ 120 DEG C in oil bath pan, after solvent all evaporates, to put it in baking oven at 60`90 DEG C dry 5 ~ 20 hours, afterwards cool to room temperature in dry environments, finally weigh.
Concrete, step 5) in, the concentration of the described vitriol oil is 98%.
The present invention adopts municipal sludge as the raw material of preparation biofuel, the large and grease containing suitable content of municipal sludge annual output, meets that biodiesel raw material is with low cost, the requirement of sustainable supply; Also reduce sludge treatment cost and risk, the utilization for sludge resource have found new approaches simultaneously.The mixed solvent selected according to the feature of fat content in mud when grease of the present invention extracts, is conducive to the extraction to grease in mud.The method that grease extracts is surname extraction, and its advantage is exactly simple to operate, safety, and extraction effect is good.Only need to change amount and the composition that extraction agent just can change grease extraction.
The present invention compares with prior art, and its technical progress is significant.The present invention with the mud of municipal sewage plant for raw material, being extraction agent with mixed solvent, take surname extraction as extracting method, and it is convenient that its advantage is that grease extracts, the output extracted is high, and the composition simultaneously changing extraction agent can well change extraction yield and extract component.
Embodiment
embodiment 1
(1) drying of mud
Mud sewage work obtained carries out drying under oil bath heating condition.
(2) grinding of mud
Use mortar grinder mud, be ground to 70-80 μm, and then toast 6 hours in 60 DEG C of baking ovens, finally cool room temperature, extract for grease.
(3) extract
With the mixing solutions of normal hexane and acetone for extraction agent, adopt the method for surname extraction to extract, acetone soln accounts for 1/2 of extraction tube volume, and in mixed solvent, the volume ratio of normal hexane and acetone is 2:1.
(4) evaporation of extraction agent
Round-bottomed flask is placed on 105 DEG C of oil baths and adds and hanker, until extraction agent evaporates completely completely after extracting and terminating by grease.Flask is taken out and puts 12 hours in an oven, weigh after second day room temperature.
(5) grease esterification
Calculate with the fat extract that 5g is solid-state, fat extract solid-state for 5g is put into a reaction vessel, add people 198ml anhydrous methanol to make it to dissolve, add people 2 ~ 4ml vitriol oil again, reflux 20 ~ 50min at 50 ~ 80 DEG C, at 50 ~ 80 DEG C, then reflux 20 ~ 50min adopts normal hexane solvent extraction fatty acid methyl ester, obtains biofuel (detect through GC-MS and show that the content of longer chain fatty acid methyl esters reaches 96%).
embodiment 2
(1) drying of mud
Mud sewage work obtained carries out drying under oil bath heating condition.
(2) grinding of mud
Use mortar grinder mud, be ground to 70-80 μm, and then toast 6 hours in 60 DEG C of baking ovens, finally cool room temperature, extract for grease.
(3) extract
With the mixing solutions of normal hexane and chloroform for extraction agent, adopt the method for surname extraction to extract, chloroformic solution accounts for 1/2 of extraction tube volume, and in mixed solvent, the volume ratio of normal hexane and chloroform is 2:1.
(4) evaporation of extraction agent
Round-bottomed flask is placed on 105 DEG C of oil baths and adds and hanker, until extraction agent evaporates completely completely after extracting and terminating by grease.Flask is taken out and puts 12 hours in an oven, weigh after second day room temperature.
(5) grease esterification
Calculate with the fat extract that 5g is solid-state, fat extract solid-state for 5g is put into a reaction vessel, add people 198ml anhydrous methanol to make it to dissolve, add people 2 ~ 4ml vitriol oil again, reflux 20 ~ 50min at 50 ~ 80 DEG C, at 50 ~ 80 DEG C, then reflux 20 ~ 50min adopts normal hexane solvent extraction fatty acid methyl ester, obtains biofuel (detect through GC-MS and show that the content of longer chain fatty acid methyl esters reaches 96%).
embodiment 3
(1) drying of mud
Mud sewage work obtained carries out drying under oil bath heating condition.
(2) grinding of mud
Use mortar grinder mud, be ground to 70-80 μm, and then toast 6 hours in 60 DEG C of baking ovens, finally cool room temperature, extract for grease.
(3) extract
With the mixing solutions of normal hexane and methyl alcohol for extraction agent, adopt the method for surname extraction to extract, methanol solution accounts for 1/2 of extraction tube volume, and in mixing solutions, the volume ratio of normal hexane and methyl alcohol is 2:1.
(4) evaporation of extraction agent
Round-bottomed flask is placed on 105 DEG C of oil baths and adds and hanker, until extraction agent evaporates completely completely after extracting and terminating by grease.Flask is taken out and puts 12 hours in an oven, weigh after second day room temperature.
(5) grease esterification
Calculate with the fat extract that 5g is solid-state, fat extract solid-state for 5g is put into a reaction vessel, add people 198ml anhydrous methanol to make it to dissolve, add people 2 ~ 4ml vitriol oil again, reflux 20 ~ 50min at 50 ~ 80 DEG C, at 50 ~ 80 DEG C, then reflux 20 ~ 50min adopts normal hexane solvent extraction fatty acid methyl ester, obtains biofuel (detect through GC-MS and show that the content of longer chain fatty acid methyl esters reaches 96%).
Foregoing be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (6)
1. adopt municipal sludge to prepare a method for biofuel, it is characterized in that comprising the steps:
1) one by the step of municipal sludge drying, the mud obtained with sewage work is raw material, obtain dry mud through heated drying;
2) step of grinding mud, is ground to particle diameter between 70-80 μm by mud, then toasts 4 ~ 8 hours in 50 ~ 70 DEG C of baking ovens, then cools room temperature;
3) step extracted mud take mixed solvent as extraction agent, and adopt the method for surname extraction to extract, described mixed solvent is made up of polar solvent and non-polar solvent, and described polar solvent boiling point is lower than non-polar solvent;
4) step of evaporating extraction agent, heats the reactant of step 3), until extraction agent evaporation completely, then puts and dries in an oven, obtain solid-state fat extract;
5) one is carried out the step of esterification to solid-state fat extract, people's sulfuric acid, methanol solution is added in the grease extracted, solid-state fat extract: sulfuric acid: the mass volume ratio of methanol solution is 5g:2 ~ 4ml:198ml, at 50 ~ 80 DEG C, esterification reaction of organic acid occurs; Then adopt normal hexane solvent extraction fatty acid methyl ester, obtain biofuel, detect through GC-MS and show that the content of longer chain fatty acid methyl esters reaches more than 96%.
2. a kind of method adopting municipal sludge to prepare biofuel according to claim 1, is characterized in that: the mud that described mud obtains for any treatment step of sewage work.
3. a kind of method adopting municipal sludge to prepare biofuel according to claim 1, it is characterized in that: described mixed solvent is the mixture of normal hexane and acetone or normal hexane and chloroform or normal hexane and methyl alcohol composition, described normal hexane and the volume ratio of acetone are 2:1, the volume ratio of normal hexane and chloroform is 2:1, and the volume ratio of normal hexane and methyl alcohol is 2:1.
4. a kind of method adopting municipal sludge to prepare biofuel according to claim 1, is characterized in that: the mass percent concentration of described concentrated sulfuric acid solution is 98%, and described methanol solution is anhydrous methanol.
5. according to a kind of method adopting municipal sludge to prepare biofuel according to claim 1, it is characterized in that: in the mixed solvent of extraction, described low-boiling polar solvent accounts for 1/2 of extractor volume, mixed solvent entirety accounts for 1/3 of extraction vessel volume.
6. a kind of method adopting municipal sludge to prepare biofuel according to claim 1, it is characterized in that: carry out in the step of esterification at one to grease, calculate with the fat extract that 5g is solid-state, fat extract solid-state for 5g is put into a reaction vessel, add people 198ml anhydrous methanol to make it to dissolve, add people 2 ~ 4ml vitriol oil again, reflux 20 ~ 50min at 50 ~ 80 DEG C, reflux 20 ~ 50min at 50 ~ 80 DEG C, then, add normal hexane extraction esterification product, take out supernatant liquor, lower floor uses n-hexane again, be separated, the supernatant liquor finally obtained evaporate to dryness again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510678394.0A CN105219418A (en) | 2015-10-20 | 2015-10-20 | A kind of method adopting municipal sludge to prepare biofuel |
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| CN201510678394.0A CN105219418A (en) | 2015-10-20 | 2015-10-20 | A kind of method adopting municipal sludge to prepare biofuel |
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| CN105219418A true CN105219418A (en) | 2016-01-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106085583A (en) * | 2016-07-08 | 2016-11-09 | 上海应用技术学院 | A kind of improve the method for fat content in primary sludge |
| CN112174475A (en) * | 2019-07-02 | 2021-01-05 | 中国人民大学 | Low-temperature drying synergistic lipid extraction treatment method for sludge |
| CN114192186A (en) * | 2020-09-02 | 2022-03-18 | 中国人民大学 | Carbon-based catalyst material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5489377A (en) * | 1994-08-12 | 1996-02-06 | Exxon Research And Engineering Company | Recovery of hard acids and soft bases from decomposed coal |
| CN103923685A (en) * | 2014-05-09 | 2014-07-16 | 北京师范大学 | Method for preparing biodiesel through activated sludge |
-
2015
- 2015-10-20 CN CN201510678394.0A patent/CN105219418A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5489377A (en) * | 1994-08-12 | 1996-02-06 | Exxon Research And Engineering Company | Recovery of hard acids and soft bases from decomposed coal |
| CN103923685A (en) * | 2014-05-09 | 2014-07-16 | 北京师范大学 | Method for preparing biodiesel through activated sludge |
Non-Patent Citations (1)
| Title |
|---|
| 李怡婧等: "城市污水处理厂污泥中能源物质利用的研究进展", 《净水技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106085583A (en) * | 2016-07-08 | 2016-11-09 | 上海应用技术学院 | A kind of improve the method for fat content in primary sludge |
| CN112174475A (en) * | 2019-07-02 | 2021-01-05 | 中国人民大学 | Low-temperature drying synergistic lipid extraction treatment method for sludge |
| CN114192186A (en) * | 2020-09-02 | 2022-03-18 | 中国人民大学 | Carbon-based catalyst material and preparation method and application thereof |
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Application publication date: 20160106 |