CN106085583A - A kind of improve the method for fat content in primary sludge - Google Patents
A kind of improve the method for fat content in primary sludge Download PDFInfo
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- CN106085583A CN106085583A CN201610532812.XA CN201610532812A CN106085583A CN 106085583 A CN106085583 A CN 106085583A CN 201610532812 A CN201610532812 A CN 201610532812A CN 106085583 A CN106085583 A CN 106085583A
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- mud
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/02—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with glycerol
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Sludge (AREA)
Abstract
The present invention relates to a kind of improve the method for fat content in primary sludge, comprise the steps: the step that sewage is stirred；Make mud carry out the step precipitated, owing to the mud settling rate in a heated condition of different fat contents is different, be partially separated out by high for fat content according to this；The dirty mud as a raw material that selective precipitation speed is fast, obtains the mud being dried through heated drying；The step that mud is ground；The step of extraction, uses the method for surname extraction to extract；The step being evaporated extractant, the material after being extracted by oils and fats heats, and extractant evaporates complete post-drying, becomes the fat extract of solid-state；Fat extract carries out the step of esterification, and the fat extract in solid-state adds people's sulphuric acid, methanol solution generation esterification reaction of organic acid, then adopts extraction product, obtains biodiesel；The present invention is simple to operate, safety, and extraction effect is good, solves the technical problem that in primary sludge of the prior art, fat content is too low.
Description
[technical field]
The invention belongs to chemical field, relate to a kind of biodiesel, oils and fats in specifically a kind of raising primary sludge
The method of content.
[background technology]
At present, although China's energy industry sustainable development, it is made that positive contribution for economic development, but energy crisis
The most day by day highlight with problem of environmental pollution.Energy crisis and environmental crisis promote reproducible clean energy resource be developed into work as
It is engaged in anxious.The raw material producing biodiesel at present is mainly soybean oil, Oleum Brassicae campestris, Oleum helianthi, Petiolus Trachycarpi oil etc., these raw materials
Cost account for the 70%-80% of biodiesel goods totle drilling cost, and the cost of manufacture of this great number seriously hinders Biodiesel
Development.Simultaneously because the substantial amounts of soil of the growth needs of these plants, rob the growing space that account for cereal crops, easily cause
Crisis in food.
And the mud of municipal sewage plant is due to inherently garbage, pollutant, so obtaining its cost very
Low.Its abundance, and the cost requirement of production of biodiesel can be met continually, raw material supply can be ensured again,
After also can solve the process problem of mud.Therefore, preparing biodiesel with municipal sludge is an application the most promising.Mesh
Before, prepare, with municipal sludge, the fat content that the subject matter of biodiesel is in mud too low, cause the life of biodiesel
Producing high cost, improving the fat content in mud will be the basic method solving this problem.Primary sludge is for having just enter into dirt
The sewage of water treatment plant's preliminary sedimentation tank.Primary sludge is the sewage having just enter into sewage treatment plant's preliminary sedimentation tank, and the oils and fats inside it comes
Coming from the oils and fats not having to decompose in sewage, therefore, it is low that the basic skills of the most heavy mud fat content of raising removes fat content exactly
Part mud, choose the part mud that fat content is high.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency and provide a kind of and improve the side of fat content in primary sludge
Method, simple to operate, safety, and extraction effect are good, solve the technology that in primary sludge of the prior art, fat content is too low
Problem.
Design for achieving the above object and a kind of improve the method for fat content in primary sludge, comprise the steps,
1) step being stirred sewage: with sewage as raw material, then enters with blender under conditions of heating 80 DEG C
Row stirring, then stands 2 hours；
2) mud is made to carry out the step precipitated: the sewage after standing is put in pyriform liquid separatnig container, is then divided by mud
Become upper, middle and lower three part；
3) step that mud is dried: with the dirty mud as a raw material separated, obtain the mud being dried through heated drying；
4) step that mud is ground: it is 70-80 μm that mud is ground to particle diameter, then in the baking oven of 50-70 DEG C
Toast, toast 4-8 hour, finally cool down room temperature；
5) step extracted: with normal hexane as extractant, uses the method for surname extraction to extract；
6) step that extractant is evaporated: the material after being extracted by oils and fats heats, until extractant is evaporated
Entirely, then put and dry in an oven, become the fat extract of solid-state；
7) fat extract to solid-state carries out the step of esterification: add sulphuric acid, first in the fat extract of solid-state
, at 50-80 DEG C, there is esterification reaction of organic acid, then use normal hexane solvent extraction fatty acid methyl ester, obtain biological bavin in alcoholic solution
Oil.
As preferably, step 1) in, described sewage is the sewage having just enter into sewage treatment plant's preliminary sedimentation tank.
As preferably, step 1) in, sewage stirring is to be 800-900r/min at rotating speed, and mixing time is 4-10min's
Under the conditions of complete.
As preferably, step 2) in, the sludge settling speed according to fat contents different in sewage is different, and is contained by oils and fats
Measure high mud to separate.
As preferably, step 2) in, according to the Precipitation of mud, being divided into four time periods precipitates, precipitation
Time period is respectively 0-10min, 10-60min, 1-3h, 3-24h.
As preferably, step 3) in, drying sludge is to be dried at oil bath pan, and treatment conditions are, is dried 10 little at 105 DEG C
Time, the water content of gained dewatered sludge is less than 1%.
As preferably, step 6) in, first, it is dried at 105 DEG C in oil bath pan, after extractant all evaporates, is put
Enter in baking oven, be dried 12 hours at 80 DEG C, be cooled to room temperature the most in dry environments, finally weigh.
As preferably, step 7) in, the mass percent concentration of described sulfuric acid solution is 98%, and described methanol solution is nothing
Water methanol.
As preferably, step 7) in, calculate with the fat extract of 1g solid-state, if the fat extract of 5g solid-state is put
Enter in reaction vessel, then add 198ml absolute methanol and be allowed to dissolve, add 2-4ml concentrated sulphuric acid, heat back at 50-80 DEG C
Stream 20-50min, then adds normal hexane extraction esterification product, takes out supernatant, and lower floor washs with normal hexane again, separates, finally
The supernatant obtained is evaporated again.
The present invention compared with the existing technology, has the advantage that
(1) as the raw material of preparation biodiesel, the municipal sludge annual output oils and fats greatly and containing suitable content, meet
Biodiesel raw material is with low cost, the requirement of sustainable supply, also reduces Treatment of Sludge cost and risk simultaneously, provides for mud
The utilization in source have found new approaches；
(2) according to sludge settling speed and the difference of sedimentation time of different fat contents, and they are separated, by oils and fats
The mud that content is high is separated, and to obtain the mud of optimal fat content, thus improves the fat content of this partial sludge,
Reduce this partial sludge and produce the cost of biodiesel；
(3) method that oils and fats extracts is surname extraction, and its advantage is simple to operate, safety, and extraction effect is good, solves
The technical problem that in primary sludge of the prior art, fat content is too low.
[detailed description of the invention]
The present invention is made further explained below below in conjunction with specific embodiment:
Embodiment 1
A kind of improve the method for fat content in primary sludge, comprise the steps:
(1) stirring of sewage: with enter sewage treatment plant sewage as raw material, then heating 80 degree under conditions of with little
Type liquid stirrers stirs 5min with the rotating speed of 850r/min；
(2) precipitation of mud: the sewage after stirring is put in pear shape separatory funnel and precipitates 2 hours, then mud is divided
Become upper, middle and lower three part；
(3) mud is dry: with the dirty mud as a raw material of bottom, obtain the mud being dried through heated drying；
(4) grinding of mud: use mortar grinder mud, is ground to 70-80 μm, toasts 6 less in 60 DEG C of baking ovens
Time, finally cool down room temperature, extract for oils and fats；
(5) extraction: with normal hexane as extractant, uses the method for surname extraction to extract；
(6) evaporation of extractant: oils and fats extracts after terminating, and round-bottomed flask is placed on 105 DEG C of oil baths and adds and hanker, until extracting
Agent is evaporated completely completely.Flask is taken out and puts 12 hours in an oven, weigh after second day room temperature；
(7) oils and fats esterification: extract oils and fats in add people's sulphuric acid, methanol solution, the fat extract amount of solid-state be 5g,
, at 50～80 DEG C, there is esterification reaction of organic acid in concentrated sulphuric acid 2ml, methanol solution 198ml；Then normal hexane solvent extraction fat is used
Acid methyl ester, obtains biodiesel (showing that the content of long-chain fatty acid methyl ester reaches 96% through GC-MS detection).
Embodiment 2
A kind of improve the method for fat content in primary sludge, comprise the steps:
(1) stirring of sewage: with enter sewage treatment plant sewage as raw material, then under conditions of 80 degree, use small-scale liquid
Body blender stirs 5min with the rotating speed of 850r/min；
(2) precipitation of mud: the sewage after stirring is put in pear shape separatory funnel, then mud is divided into upper, middle and lower three
Part；
(3) mud is dry: with the dirty mud as a raw material of bottom, obtain the mud being dried through heated drying；
(4) grinding of mud: use mortar grinder mud, is ground to 70-80 μm, toasts 6 less in 60 DEG C of baking ovens
Time, finally cool down room temperature, extract for oils and fats；
(5) extraction: with normal hexane as extractant, uses the method for surname extraction to extract；
(6) evaporation of extractant: oils and fats extracts after terminating, and round-bottomed flask is placed on 105 DEG C of oil baths and adds and hanker, until extracting
Agent is evaporated completely completely.Flask is taken out and puts 12 hours in an oven, weigh after second day room temperature；
(7) oils and fats esterification: extract oils and fats in add people's sulphuric acid, methanol solution, the fat extract amount of solid-state be 5g,
, at 50～80 DEG C, there is esterification reaction of organic acid in concentrated sulphuric acid 2ml, methanol solution 198ml；Then normal hexane solvent extraction fat is used
Acid methyl ester, obtains biodiesel (showing that the content of long-chain fatty acid methyl ester reaches 96% through GC-MS detection).
Embodiment 3
A kind of improve the method for fat content in primary sludge, comprise the steps:
(1) sewage is stirred: with enter sewage treatment plant sewage as raw material, then heating 80 degree under blender
It is stirred 10min, then stands 2 hours；
(2) make mud precipitate: the sewage after standing is put in pyriform liquid separatnig container, advise according to the precipitation of mud
Rule, being divided into several time period precipitates, as being divided into 0-10min, 10-60min, 1-3h, 3-24h the sedimentation time；
(3) mud is dried: with the dirty mud as a raw material separated, obtain the mud being dried through heated drying；
(4) mud is ground: mud is ground to particle diameter between 70-80 μm, then carries out in the baking oven of 70 DEG C
Baking, toasts 4 hours, finally cools down room temperature；
(5) extraction: with normal hexane as extractant, uses the method for surname extraction to extract；
(6) extractant is evaporated: the material after being extracted by oils and fats heats, until extractant evaporation is completely, so
After put and dry in an oven, become the fat extract of solid-state；
(7) fat extract to solid-state carries out esterification: the fat extract in solid-state adds people's sulphuric acid, methanol solution,
The mass percent concentration of sulfuric acid solution is 98%, and methanol solution is absolute methanol, if the fat extract amount of solid-state is 5g, then
, at 50-80 DEG C, there is esterification reaction of organic acid in concentrated sulphuric acid 2ml, methanol solution 198ml；Then normal hexane solvent extraction fat is used
Acid methyl ester, obtains biodiesel.
Embodiment 4
A kind of improve the method for fat content in primary sludge, comprise the steps:
(1) sewage is stirred: with enter sewage treatment plant sewage as raw material, then heating 80 degree under blender
It is stirred 4min, then stands 2 hours；
(2) mud is made to precipitate: the sewage after standing is put in pyriform liquid separatnig container, according to oils and fatss different in sewage
The difference of the sludge settling speed of content, and mud high for fat content is separated；
(3) mud is dried: with the dirty mud as a raw material separated, obtain the mud being dried through heated drying；
(4) mud is ground: mud is ground to particle diameter between 70-80 μm, then carries out in the baking oven of 50 DEG C
Baking, toasts 8 hours, finally cools down room temperature；
(5) extraction: with normal hexane as extractant, uses the method for surname extraction to extract；
(6) extractant is evaporated: the material after being extracted by oils and fats heats, until extractant evaporation is completely, so
After put and dry in an oven, become the fat extract of solid-state；
(7) fat extract to solid-state carries out esterification: the fat extract in solid-state adds people's sulphuric acid, methanol solution,
The mass percent concentration of sulfuric acid solution is 98%, and methanol solution is absolute methanol, the fat extract of 5g solid-state is put into
In one reaction vessel, add people's 198ml absolute methanol and be allowed to dissolve, then add people 2～4ml concentrated sulphuric acid, heat at 50～80 DEG C
Backflow 20～50min, then, adds normal hexane extraction esterification product, takes out supernatant, and lower floor washs with normal hexane again, separates,
The supernatant finally obtained is evaporated again.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention and principle
Lower made change, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, be included in the protection model of the present invention
Within enclosing.
Claims (9)
1. one kind is improved the method for fat content in primary sludge, it is characterised in that comprise the steps,
1) step being stirred sewage: with sewage as raw material, then stirs with blender under conditions of heating 80 DEG C
Mix, then stand 2 hours；
2) mud is made to carry out the step precipitated: the sewage after standing is put in pyriform liquid separatnig container, is then divided into by mud
Three parts under in；
3) step that mud is dried: with the dirty mud as a raw material separated, obtain the mud being dried through heated drying；
4) step that mud is ground: it is 70-80 μm that mud is ground to particle diameter, then carries out in the baking oven of 50-70 DEG C
Baking, toasts 4-8 hour, finally cools down room temperature；
5) step extracted: with normal hexane as extractant, uses the method for surname extraction to extract；
6) step being evaporated extractant: the material after being extracted by oils and fats heats, until extractant evaporation is completely, so
After put and dry in an oven, become the fat extract of solid-state；
7) fat extract to solid-state carries out the step of esterification: add sulphuric acid, methanol in the fat extract of solid-state molten
, at 50-80 DEG C, there is esterification reaction of organic acid, then use normal hexane solvent extraction fatty acid methyl ester, obtain biodiesel in liquid.
2. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 1) in, described
Sewage is the sewage having just enter into sewage treatment plant's preliminary sedimentation tank.
3. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 1) in, sewage
Stirring is to be 800-900r/min at rotating speed, and mixing time is to complete under conditions of 4-10min.
4. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 2) in, according to
In sewage, the sludge settling speed of different fat contents is different, and is separated by mud high for fat content.
5. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 2) in, according to
The Precipitation of mud, being divided into four time periods precipitates, and sedimentation time section is respectively 0-10min, 10-60min, 1-
3h、3-24h。
6. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 3) in, mud
Being dried is to be dried at oil bath pan, and treatment conditions are, is dried 10 hours at 105 DEG C, and the water content of gained dewatered sludge is less than 1%.
7. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 6) in, first,
In oil bath pan at 105 DEG C be dried, after extractant all evaporates, put it in baking oven, at 80 DEG C be dried 12 hours, afterwards
It is cooled to room temperature in dry environments, finally weighs.
8. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 7) in, described
The mass percent concentration of sulfuric acid solution is 98%, and described methanol solution is absolute methanol.
9. the method for fat content in raising primary sludge as claimed in claim 1, it is characterised in that: step 7) in, with 1g
The fat extract of solid-state calculates, if putting in reaction vessel by the fat extract of 5g solid-state, then adds 198ml without water beetle
Alcohol is allowed to dissolve, and adds 2-4ml concentrated sulphuric acid, is heated to reflux 20-50min at 50-80 DEG C, then adds normal hexane extraction methyl ester
Changing product, take out supernatant, lower floor washs with normal hexane again, separates, and the supernatant finally obtained is evaporated again.
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| CN201610532812.XA CN106085583A (en) | 2016-07-08 | 2016-07-08 | A kind of improve the method for fat content in primary sludge |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219418A (en) * | 2015-10-20 | 2016-01-06 | 上海应用技术学院 | A kind of method adopting municipal sludge to prepare biofuel |
| CN105219419A (en) * | 2015-10-20 | 2016-01-06 | 上海应用技术学院 | A kind of method adopting mud to prepare biofuel |
-
2016
- 2016-07-08 CN CN201610532812.XA patent/CN106085583A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219418A (en) * | 2015-10-20 | 2016-01-06 | 上海应用技术学院 | A kind of method adopting municipal sludge to prepare biofuel |
| CN105219419A (en) * | 2015-10-20 | 2016-01-06 | 上海应用技术学院 | A kind of method adopting mud to prepare biofuel |
Non-Patent Citations (2)
| Title |
|---|
| 望亭发电厂编著: "《火力发电机组运行人员现场规范操作指导书》", 30 April 2015, 中国电力出版社 * |
| 王怡，等: "城市污水处理厂污泥醇化制取生物柴油的研究现状", 《中国给水排水》 * |
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Application publication date: 20161109 |