CN104611072A - Method for preparing biodiesel from gutter oil - Google Patents
Method for preparing biodiesel from gutter oil Download PDFInfo
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- CN104611072A CN104611072A CN201510020690.1A CN201510020690A CN104611072A CN 104611072 A CN104611072 A CN 104611072A CN 201510020690 A CN201510020690 A CN 201510020690A CN 104611072 A CN104611072 A CN 104611072A
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- biodiesel
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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 the crossing field of comprehensive utilization of resources and chemical engineering, in particular to a method for preparing biodiesel from gutter oil. The method comprises steps as follows: the raw material gutter oil is subjected to centrifugal impurity removal treatment, phosphoric acid is added to obtain a mixture, the mixture is dephosphorized, degummed and dehydrated with a natural gravity settlement mode, concentrated sulfuric acid with the concentration of 98% is added after the mixture is dehydrated, gas phase methanol is introduced from the bottom to enable fatty acid in the raw material to be completely transformed into fatty acid methyl ester, separation is performed with a settlement mode, a supernatant methyl ester phase is collected and added with a sodium hydroxide and methanol solution to have an interesterification reaction, the interesterification reaction of fatty glyceride and methanol is promoted, and the biodiesel is obtained. According to the method for preparing the biodiesel from the gutter oil, the work section of dehydration after esterification is avoided, meanwhile, the condition that production cannot be performed normally due to the fact that moisture removal is not up to the standard and saponification is serious in a hydrolysis follow-up interesterification reaction process can be avoided, and the biodiesel prepared with the method can meet the national standard of biodiesel.
Description
Technical field
The present invention relates to the field that comprehensive utilization of resources intersects with chemical industry, particularly a kind of method utilizing Preparation of biodiesel from waste oils.
Background technology
The edible oil Year's consumption of existing Beijing is about 600,000 tons.Have 15% to change into waste grease to estimate in the food oils consumed according to the measuring and calculating of the national grain and oil stdn council, producing meal kitchen waste grease existing Beijing year is 90,000 tons (247t/d).The waste grease consuming food oils generation except small part urban and rural residents enters except Sewage treatment systems, and all the other are the waste grease that food and beverage sevice unit consumption food oils produce.
It returns the phenomenon of dining table to utilize Preparation of biodiesel from waste oils effectively to contain, can turn waste into wealth simultaneously, change sewer oil into the energy---biofuel, utilize as fuel recovery, biofuel has more advantages compared with petrifaction diesel, such as completely, CO2 emissions is low in burning.Now adopt soda acid two-step approach to prepare after the maximum difficult point of biodiesel processes is esterification technique, if moisture controls bad, the transesterification reaction generation saponification under follow-up alkaline condition may be caused, cause separation difficulty, even may affect production.Another one technological difficulties are, carry out esterification in acid condition, the reaction times is longer, and industrial production required equipment is huge, cause cost of equipment too high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method utilizing Preparation of biodiesel from waste oils.
For achieving the above object, the present invention adopts technical scheme to be:
A kind of method utilizing Preparation of biodiesel from waste oils:
By centrifugal for raw material sewer oil removing impurities process, add phosphoric acid afterwards to utilize gravity natural subsidence mode dephosphorization, come unstuck and dewater, the vitriol oil that concentration is 98% is added after dehydration, and pass into gas-phase methanol from bottom, make after in raw material, lipid acid is converted into fatty acid methyl ester completely, the mode of sedimentation is utilized to be separated, collect upper liquid methyl esters phase, and add the solution generation transesterification reaction of sodium hydroxide and methyl alcohol wherein, promote glycerin fatty acid ester and methyl alcohol generation transesterification reaction, namely obtain biofuel.
To pass into distillation tower and purify by reactant after transesterification reaction, the cut collecting 220 ~ 250 DEG C can obtain biodiesel oil product.
The concentration adding 0.5%-3% (v/v) after described dehydration is the vitriol oil of 98%, and pass into gas-phase methanol from bottom, at 120 ~ 170 DEG C, pressure-controlling makes lipid acid in raw material be converted into fatty acid methyl ester completely under 0.3 ~ 0.8MPa condition, when in raw material, acid value is no more than 3, reaction terminates; Wherein methanol flow rate is 2 ~ 40L/min, and methyl alcohol add-on is that in raw material, fatty acid content and quantity of methyl alcohol mol ratio are 1.1:1 ~ 3:1.
Add the mixture of methyl alcohol and sodium hydroxide in described methanol phase, carry out generation transesterification reaction at room temperature, at a normal, wherein in methyl alcohol and raw material, sweet three fat mol ratios are 2:1 ~ 5:1, and sodium hydroxide concentration is the 0.5%-3% (v/v) of raw material.
The method utilizing Preparation of biodiesel from waste oils provided by the invention, utilize by oil for raw material through dephosphorization, come unstuck, the pretreatment technology such as dehydration, again through gas-phase methanol technique, ester exchange process, finally purify through distillation tower, the biofuel of national standard relevant regulatory requirements can be met.
Accompanying drawing explanation
The Application way process flow sheet utilizing Preparation of biodiesel from waste oils that Fig. 1 provides for the embodiment of the present invention.
Embodiment
First raw material sewer oil is carried out removing impurities process through whizzer by the present invention, pumps into dephosphorization afterwards, retort of coming unstuck, and adds phosphoric acid, stirring and evenly mixing, static after phosphatide, colloid sedimentation, is separated by upper strata grease with lower floor thing.The object of dehydration is reached in the process of sedimentation simultaneously.After dehydration, raw material is squeezed into reactor, in reactor, add the vitriol oil that concentration is 98%, add-on is 0.5%-3% (v/v), bottom reactor, pass into gas-phase methanol, methanol usage is depending on raw material acid value, and fatty acid content and quantity of methyl alcohol mol ratio are 1.1:1 ~ 3:1, guarantee that lipid acid is converted into fatty acid methyl ester completely, temperature of reaction at 120 DEG C ~ 170 DEG C, pressure-controlling at 0.3 ~ 0.8MPa, when acid value lower than 3 time, reaction terminates, 70 ~ 120 minutes reaction times.To reaction product be separated after, be added to methyl alcohol and basic catalyst (sodium hydroxide) to methyl esters, in and the vitriol oil.Excessive sodium hydrate, as catalyzer, promotes glycerin fatty acid ester and methyl alcohol generation transesterification reaction, generates fatty acid methyl ester and glycerine, 80 ~ 100 minutes reaction times.
Embodiment 1
As shown in Figure 1, the present invention relates to a kind of Application way utilizing Preparation of biodiesel from waste oils, comprise the following steps:
First the sewer oil being 100 by 1 ton of acid value carries out removing impurities process through whizzer, pumps into dephosphorization afterwards, retort of coming unstuck, and adds phosphoric acid, stirring and evenly mixing, static after phosphatide, colloid, wet-laid, is separated by upper strata grease with lower floor thing.
After dehydration, raw material is squeezed into reactor, the vitriol oil 2 ~ 4kg that concentration is 98% is added in reactor, and gas-phase methanol is passed into bottom reactor, methanol usage is 4 ~ 6L/min, and temperature of reaction is 130 ~ 160 DEG C, pressure-controlling is at 0.4 ~ 0.8MPa, acid value lower than 3 time, reaction terminate, 80 ~ 120 minutes reaction times.Then be separated the mode of product utilization sedimentation, in upper liquid, add the solution generation transesterification reaction of sodium hydroxide and methyl alcohol afterwards, addition amount of sodium hydroxide is 4 ~ 6kg, and methyl alcohol adds 500 ~ 800kg, in and the vitriol oil.Excessive sodium hydrate, as catalyzer, promotes glycerin fatty acid ester and methyl alcohol generation transesterification reaction, and generate fatty acid methyl ester and glycerine, temperature of reaction is normal temperature, and reaction pressure is normal pressure.70 ~ 90 minutes reaction times.
Pass into distillation tower after reaction terminates to purify, the cut proposing 220 ~ 250 DEG C can obtain biodiesel oil product.
Embodiment 2
As shown in Figure 1, the present invention relates to a kind of Application way utilizing Preparation of biodiesel from waste oils, comprise the following steps:
First the sewer oil being 80 by 3 tons of acid values carries out removing impurities process through whizzer, pumps into dephosphorization afterwards, retort of coming unstuck, and adds phosphoric acid, stirring and evenly mixing, static after phosphatide, colloid, wet-laid, is separated by upper strata grease with lower floor thing.
After dehydration, raw material is squeezed into reactor, the vitriol oil 6.5 ~ 9.5kg that concentration is 98% is added in reactor, and gas-phase methanol is passed into bottom reactor, methanol usage is 12 ~ 15L/min, and temperature of reaction is 120 ~ 140 DEG C, pressure-controlling is at 0.3 ~ 0.5MPa, acid value lower than 3 time, reaction terminate, 90 ~ 120 minutes reaction times.Then be separated the mode of product utilization sedimentation, in upper liquid, add the solution generation transesterification reaction of sodium hydroxide and methyl alcohol afterwards, addition amount of sodium hydroxide is 8.5 ~ 11kg, and methyl alcohol adds 1300 ~ 1500kg, in and the vitriol oil.Excessive sodium hydrate, as catalyzer, promotes glycerin fatty acid ester and methyl alcohol generation transesterification reaction, and generate fatty acid methyl ester and glycerine, temperature of reaction is normal temperature, and reaction pressure is normal pressure.70 ~ 90 minutes reaction times.
Pass into distillation tower after reaction terminates to purify, the cut proposing 220 ~ 250 DEG C can obtain biodiesel oil product.
Embodiment 3
As shown in Figure 1, the present invention relates to a kind of Application way utilizing Preparation of biodiesel from waste oils, comprise the following steps:
First the sewer oil being 120 by 4 tons of acid values carries out removing impurities process through whizzer, pumps into dephosphorization afterwards, retort of coming unstuck, and adds phosphoric acid, stirring and evenly mixing, static after phosphatide, colloid, wet-laid, is separated by upper strata grease with lower floor thing.
After dehydration, raw material is squeezed into reactor, the vitriol oil 13 ~ 20kg that concentration is 98% is added in reactor, and gas-phase methanol is passed into bottom reactor, methanol usage is 20 ~ 30L/min, and temperature of reaction is 130 ~ 160 DEG C, pressure-controlling is at 0.4 ~ 0.7MPa, acid value lower than 3 time, reaction terminate, 80 ~ 110 minutes reaction times.Then be separated the mode of product utilization sedimentation, in upper liquid, add the solution generation transesterification reaction of sodium hydroxide and methyl alcohol afterwards, addition amount of sodium hydroxide is 13 ~ 22kg, and methyl alcohol adds 2600 ~ 3000kg, in and the vitriol oil.Excessive sodium hydrate, as catalyzer, promotes glycerin fatty acid ester and methyl alcohol generation transesterification reaction, and generate fatty acid methyl ester and glycerine, temperature of reaction is normal temperature, and reaction pressure is normal pressure.80 ~ 100 minutes reaction times.
Pass into distillation tower after reaction terminates to purify, the cut proposing 220 ~ 250 DEG C can obtain biodiesel oil product, output plant asphalt at the bottom of tower.
The various embodiments described above detected in the cut that 220 ~ 250 DEG C propose, detect and need GB/T20828-2007 according to biodiesel oil product, namely " diesel-fuel mediation biofuel (BD100) " standard is as the criterion, and concrete indices is see table 1.
Table 1
The method of Preparation of biodiesel from waste oils that utilizes provided by the invention has the following advantages:
1. the present invention has carried out continuous print pre-treatment to raw material sewer oil, whizzer is utilized to achieve deviating from trench well cuts, utilize medicament to achieve phosphatide, the deviating from of colloid, utilize natural gravity sedimentation to achieve deviating from of moisture, can subsequent technique be met through continuous pretreated grease.
2. intermediate reaction link of the present invention have employed vapour phase esterification technique, passes into reaction vessel by gas-phase methanol, by controlling methanol flow rate, effectively can control speed of response, and can go out moisture wherein.
3. the present invention is determined through experimentation the consumption of Exchange Ester Process basic catalyst, and the factor relevant to consumption.
4. the workshop section dewatered after present invention, avoiding esterification, can avoid because moisture removal is not up to standard simultaneously, causes in the follow-up ester-exchange reaction of hydrolysis and occurs serious saponification, cause production normally to run.Gas-phase methanol is introduced by the present invention, while raising speed of reaction, achieve dewatering in raw material, can dehydration procedure be reduced, for the stable of transesterification reaction provides the foundation, solve the problems such as the saponification adopting soda acid two-step approach thoroughly may not cause owing to dewatering.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to example to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (4)
1. utilize a method for Preparation of biodiesel from waste oils, it is characterized in that:
By centrifugal for raw material sewer oil removing impurities process, add phosphoric acid afterwards to utilize gravity natural subsidence mode dephosphorization, come unstuck and dewater, the vitriol oil that concentration is 98% is added after dehydration, and pass into gas-phase methanol from bottom, make after in raw material, lipid acid is converted into fatty acid methyl ester completely, the mode of sedimentation is utilized to be separated, collect upper liquid methyl esters phase, and add the solution generation transesterification reaction of sodium hydroxide and methyl alcohol wherein, promote glycerin fatty acid ester and methyl alcohol generation transesterification reaction, namely obtain biofuel.
2. the method utilizing Preparation of biodiesel from waste oils according to claim 1, is characterized in that:
To pass into distillation tower and purify by reactant after transesterification reaction, the cut collecting 220 ~ 250 DEG C can obtain biodiesel oil product.
3. the method utilizing Preparation of biodiesel from waste oils according to claim 1, is characterized in that:
The concentration adding 0.5%-3% (v/v) after described dehydration is the vitriol oil of 98%, and pass into gas-phase methanol from bottom, at 120 ~ 170 DEG C, pressure-controlling makes lipid acid in raw material be converted into fatty acid methyl ester completely under 0.3 ~ 0.8MPa condition, when in raw material, acid value is no more than 3, reaction terminates; Wherein methanol flow rate is 2 ~ 40L/min, and methyl alcohol add-on is that in raw material, fatty acid content and quantity of methyl alcohol mol ratio are 1.1:1 ~ 3:1.
4. the method utilizing Preparation of biodiesel from waste oils according to claim 1, it is characterized in that: the mixture adding methyl alcohol and sodium hydroxide in described methanol phase, carry out generation transesterification reaction at room temperature, at a normal, wherein in methyl alcohol and raw material, sweet three fat mol ratios are 2:1 ~ 5:1, and sodium hydroxide concentration is the 0.5%-3% (v/v) of raw material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510020690.1A CN104611072A (en) | 2015-01-15 | 2015-01-15 | Method for preparing biodiesel from gutter oil |
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| CN201510020690.1A CN104611072A (en) | 2015-01-15 | 2015-01-15 | Method for preparing biodiesel from gutter oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221942A (en) * | 2016-08-19 | 2016-12-14 | 佛山市凯特科科技有限公司 | Waste oil is processed into the method for alcohol ether burning diesel oil |
| CN110511823A (en) * | 2019-07-17 | 2019-11-29 | 臧树良 | A method of second generation biodiesel is prepared with food processing waste oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012388A (en) * | 2007-01-19 | 2007-08-08 | 张伟明 | Method of manufacturing biological diesel oil from hogwash oil |
| CN101705155A (en) * | 2009-11-07 | 2010-05-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for industrially preparing biological diesel by waste grease |
| CN103421548A (en) * | 2012-05-14 | 2013-12-04 | 陕西德融新能源股份有限公司 | Preparation technology of biodiesel produced from non refined grease |
| CN103468413A (en) * | 2013-09-25 | 2013-12-25 | 陕西合盛生物柴油技术开发有限公司 | Production method of biodiesel |
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2015
- 2015-01-15 CN CN201510020690.1A patent/CN104611072A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012388A (en) * | 2007-01-19 | 2007-08-08 | 张伟明 | Method of manufacturing biological diesel oil from hogwash oil |
| CN101705155A (en) * | 2009-11-07 | 2010-05-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for industrially preparing biological diesel by waste grease |
| CN103421548A (en) * | 2012-05-14 | 2013-12-04 | 陕西德融新能源股份有限公司 | Preparation technology of biodiesel produced from non refined grease |
| CN103468413A (en) * | 2013-09-25 | 2013-12-25 | 陕西合盛生物柴油技术开发有限公司 | Production method of biodiesel |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221942A (en) * | 2016-08-19 | 2016-12-14 | 佛山市凯特科科技有限公司 | Waste oil is processed into the method for alcohol ether burning diesel oil |
| CN110511823A (en) * | 2019-07-17 | 2019-11-29 | 臧树良 | A method of second generation biodiesel is prepared with food processing waste oil |
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Application publication date: 20150513 |
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