CN102304420A - Dry degumming method of raw abandoned oil used for producing biodiesel - Google Patents
Dry degumming method of raw abandoned oil used for producing biodiesel Download PDFInfo
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- CN102304420A CN102304420A CN201110226843A CN201110226843A CN102304420A CN 102304420 A CN102304420 A CN 102304420A CN 201110226843 A CN201110226843 A CN 201110226843A CN 201110226843 A CN201110226843 A CN 201110226843A CN 102304420 A CN102304420 A CN 102304420A
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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Abstract
The invention discloses a dry degumming method of raw abandoned oil used for producing biodiesel. The method comprises steps that: (1) the abandoned oil is dehydrated; (2) a composite acid with a weight of 0.2 to 1.0% of that of the abandoned oil is added to the abandoned oil, wherein the composite acid is composed of strong phosphoric acid and citric acid according to a ratio of 2:1; the mixture is subject to a reaction for 50 to 90min under a reaction temperature of 100 to 120 DEG C, such that phospholipids form macro flocculating constituents; (3) a degumming absorbent with a mass of 0.5 to 2.0% of that of the raw materials is added to the raw materials; a vacuum degree is controlled at 0.080 to 0.098Mpa, a temperature is controlled at 110 to 130 DEG C, and the mixture is stirred for 30 to 60 min with a rate of 50 to 70r/min; (4) the mixture is processed through press filtration, and an obtained filtrate is a production raw material of biodiesel. The method provided by the invention has advantages of simple technology, high yield, and low production cost. Also, the method is energy saving and environment friendly.
Description
Technical field
The invention belongs to biodiesel raw material pre-treatment manufacture field, be specifically related to a kind of abendoned oil dry degumming method.
Background technology
At present there is lack of raw materials remains the primary factor of restriction biofuel price and large-scale production for biofuel.Not only can stop waste oil backflow dining table with sewer oil, hogwash fat, acidifying wet goods waste grease production biofuel, can also turn waste into wealth, from truly having solved the use problem of waste grease.But contain a large amount of colloids in the abendoned oil, can cause many adverse factors: influence grease stability, moisture absorption hydrolysis easily product; Influence the stock oil refining effect, cause emulsification, increase behind the consumption, deodorization of discoloring agent color reversion etc.; Influence the application of oil product, when heating distillation spume, bumping etc.Existing Degumming method as: CN1112156 discloses the enzymatic degumming method of a vegetable oil, and cost value is higher but biological enzyme comes unstuck; CN101381298 discloses a kind of strong acid that utilizes and has removed gelationus method in the grease; Be under strong acid and nitrogen protection condition, to carry out; Colloid can be dissociated into hydrated phospholipid; Change aqueous phase over to; Thereby it is removed from crude oil, but phosphoric acid is acid more intense, in reality, adopts single phosphoric acid greasy degumming effect and incorrect; And to cause the loaded down with trivial details and cost rising of program with nitrogen as protection.
Summary of the invention
Main purpose of the present invention is to overcome the defective of existing Degumming method, provides that a kind of technology is simple, product yield is high, production cost is low, save energy, environmental friendliness, is suitable for the method for biodiesel raw material degumming of oil.
The present invention includes following steps:
(1) dehydration: abendoned oil is imported in the reaction kettle, be heated to 100～120 ℃, control vacuum tightness 0.075～0.098Mpa under the stirring of 100～120r/min, with moisture evaporation 30～60min in the stock oil, does not have water vapor bubbles to produce until the oil reservoir surface;
(2) flocculation: the dehydrated raw material grease is cooled to 95～99 ℃, under stirring fast, adds weight of oil percentage ratio 0.2～1.0 % by strong phosphoric acid
:Hydrocerol A=2
:1 compound acid reduces stirring velocity to 50～60 r/min, rises to 100～120 ℃ of temperature of reaction again, and reaction 50～90 min, phosphatide generate macrobead shape flocs unit;
(3) absorption: the sorbent material that comes unstuck that in reaction kettle, adds raw materials quality percentage ratio 0.5～2.0%; Control vacuum tightness is 0.080～0.098 Mpa, and temperature is 110～130 ℃, under 50～70 r/min, stirs 30～60 min;
(4) press filtration: stock oil imports pressure filter, and controlling oily temperature is 70～90 ℃, and control pressure is 0.15～0.45 MPa, and the filtrating after the press filtration is the production of biodiesel raw material.
The said raw oil material sorbent material that comes unstuck is the mixture of silica gel and carclazyte, and the two weight ratio is 0.5～1
:2～6.
The said raw oil material sorbent material that comes unstuck activates 50～100 min before use under 150～200 ℃ of conditions.
Advantage of the present invention: (1) this patent adopts the best proportioning of Hydrocerol A with phosphoric acid, and the acid Hydrocerol A simultaneously of reduction phosphoric acid itself has also played the characteristic of lipid-antioxidant activity, comes unstuck and under conventional environment, can accomplish, and need not any protection; (2) will flocculate with the sorbent material that comes unstuck and carry out press filtration again after the particulate colloid absorption, compare filter membrane and operational condition requires all to reduce greatly with other method; Do not make water and steam etc. in the degumming technology process, avoided the emulsion that produces in the hydration degum process, product yield can improve more than 2%, and the carclazyte of the sorbent material that when coming unstuck, comes unstuck also has the effect of decolouring, makes oil quality that obvious improvement arranged; (3) operational condition is simple, does not need complicated processing unit; Saved resource; (4) cost of material that comes unstuck is cheap, and the technology operational conditions is simple, can reduce product cost; (5) of reduced contamination, there is not oil foot to produce, there are not generations such as sewage, waste gas, waste residue is a kind of good boiler oil; (6) avoid pyroreaction, can prevent raw oil material and oxygen catalytic oxidation effectively, control the acid number of biodiesel raw material oil better, help next step esterification.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1:
Earlier with silica gel
:Carclazyte=1
:3 mix; Under 150～200 ℃ of conditions, activate 50～100 min.Be the sorbent material that comes unstuck.
Get the preparatory crude product sewer oil of crossing fence of 500 Kg and import in the reaction kettle through pipeline, be heated to 105 ℃, control vacuum tightness is 0.090 MPa, and stirring velocity 105 r/min do not have bubble through laminar surface behind the 50 min decompression dehydrations and produce; Reduce to 98 ℃, add the compound acid (strong phosphoric acid of grease weight 0.2 % again
:Hydrocerol A=2
:1), add acid and finish and reduce stirring velocity to 50 r/min, temperature is 100 ℃, reacts 70 min.Finish, add the grease weight 1.0 % sorbent material that comes unstuck, at vacuum tightness 0.090 Mpa, continuously stirring is reacted 30 min under 120 ℃ of conditions of temperature, and the control stirring velocity is 40 r/min.Raw material is cooled to 90 ℃, and the pressure filter pressure-controlling is at 0.30 MPa, and the grease after the press filtration is the production of biodiesel raw material.
The back glyceride stock quality of coming unstuck is as shown in table 1:
Embodiment 2
Earlier with silica gel
:Carclazyte=1
:4 mix; Under 150～200 ℃ of conditions, activate 50～100 min.Be the sorbent material that comes unstuck.
2.0 the preparatory crude product sewer oil of crossing fence of ton imports in the still through pipeline, is heated to 120 ℃, control vacuum tightness is 0.098MPa, and stirring velocity 100 r/min do not have boiling explosion phenomenon through the 30min material, and the oil reservoir surface does not have bubble yet and produces.Be cooled to 97 ℃, and the compound sour reagent of adding grease weight 0.8 % (strong phosphoric acid: Hydrocerol A 2:1), the reduction stirring velocity that finishes, stirring velocity is controlled at 60 r/min, and temperature of reaction is 110 ℃, and the reaction times is 90 min.Finish, add the grease weight 2.0 % activatory sorbent material that comes unstuck, control vacuum tightness 0.098 Mpa, 130 ℃ of continuous stirring conditions of temperature are reaction 60 min down, and stirring velocity is controlled at 60 r/min.Be cooled to 90 ℃, the pressure filter pressure-controlling through pressure filter, obtains the degummed oil fat raw material at 0.45MPa, and the back glyceride stock quality of coming unstuck is as shown in table 2:
Embodiment 3:
Earlier with silica gel
:Carclazyte=1
:5 mix; Under 150～200 ℃ of conditions, activate 50～100 min.Be the sorbent material that comes unstuck.
The pre-filtered crude product sewer oil of 1000 Kg imports in the still through pipeline, is heated to 110～115 ℃, and control vacuum tightness is 0.095 MPa, and stirring velocity 105 r/min do not have boiling explosion phenomenon through 40min decompression dehydration material, and the oil reservoir surface does not have bubble yet and produces.Be cooled to 98 ℃, (strong phosphoric acid: Hydrocerol A 2:1), add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 55 r/min, and temperature of reaction is 100 ℃, and the reaction times is 85 min to add the compound sour reagent of grease weight 0.6 %.Finish, add the sorbent material that comes unstuck that oil weighs 1.5 %, vacuum tightness 0.095 Mpa, 120 ℃ of continuous stirring conditions of temperature are reaction 50 min down, and stirring velocity is controlled at 60 r/min.Slightly be cooled to 100 ℃, the pressure filter pressure-controlling is at 0.45 MPa.Through pressure filter, get into next reaction kettle, the back glyceride stock quality of coming unstuck is following:
Claims (3)
1. a biofuel is characterized in that with the dry degumming method of raw material abendoned oil, may further comprise the steps:
(1) dehydration: abendoned oil is imported in the reaction kettle, be heated to 100～120 ℃, control vacuum tightness 0.075～0.098Mpa under the stirring of 100～120r/min, with moisture evaporation 30～60min in the stock oil, does not have water vapor bubbles to produce until the oil reservoir surface;
(2) flocculation: the dehydrated raw material grease is cooled to 95～99 ℃; Stirring fast adding weight of oil percentage ratio 0.2～1.0 % down by strong phosphoric acid: the compound acid of Hydrocerol A=2: 1; Reduce stirring velocity to 50～60 r/min; Rise to 100～120 ℃ of temperature of reaction again; Reaction 50～90min, phosphatide generate macrobead shape flocs unit;
(3) absorption: the sorbent material that comes unstuck that in reaction kettle, adds raw materials quality percentage ratio 0.5～2.0%; Control vacuum tightness is 0.080～0.098 Mpa, and temperature is 110～130 ℃, under 50～70r/min, stirs 30～60min;
(4) press filtration: stock oil imports pressure filter, and controlling oily temperature is 70～90 ℃, and control pressure is 0.15～0.45MPa, and the filtrating after the press filtration is the production of biodiesel raw material.
2. biofuel according to claim 1 is characterized in that with the dry degumming method of raw material abendoned oil, and the said raw oil material sorbent material that comes unstuck is the mixture of silica gel and carclazyte, and the two weight ratio is 0.5～1:2～6.
3. biofuel according to claim 1 is characterized in that with the dry degumming method of raw material abendoned oil, and the said raw oil material sorbent material that comes unstuck activates 50～100min before use under 150～200 ℃ of conditions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110226843A CN102304420A (en) | 2011-08-09 | 2011-08-09 | Dry degumming method of raw abandoned oil used for producing biodiesel |
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| CN201110226843A CN102304420A (en) | 2011-08-09 | 2011-08-09 | Dry degumming method of raw abandoned oil used for producing biodiesel |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031218A (en) * | 2013-01-11 | 2013-04-10 | 广西大学 | Method for synthesizing biodiesel by base catalysis |
| CN103897718A (en) * | 2012-12-27 | 2014-07-02 | 中国石油天然气股份有限公司 | Method for producing diesel oil fraction and aviation fuel fraction from animal and vegetable oil |
| CN104419518A (en) * | 2013-08-23 | 2015-03-18 | 中国石油天然气股份有限公司 | Vegetable fat dissociation-chelating degumming method |
| CN111057616A (en) * | 2019-08-26 | 2020-04-24 | 易高生物化工科技(张家港)有限公司 | Treatment method for removing impurities from waste animal and vegetable oil |
| CN115161109A (en) * | 2022-07-18 | 2022-10-11 | 湖北碧美新能源科技有限公司 | Preparation method of industrial-grade mixed oil |
| CN116875379A (en) * | 2023-05-31 | 2023-10-13 | 山东三聚生物能源有限公司 | Method and system for demetallizing biological raw oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071103A (en) * | 2011-01-25 | 2011-05-25 | 湖南省生物柴油工程技术研究中心 | Novel dry-method degumming method for abandoned oil |
-
2011
- 2011-08-09 CN CN201110226843A patent/CN102304420A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071103A (en) * | 2011-01-25 | 2011-05-25 | 湖南省生物柴油工程技术研究中心 | Novel dry-method degumming method for abandoned oil |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103897718A (en) * | 2012-12-27 | 2014-07-02 | 中国石油天然气股份有限公司 | Method for producing diesel oil fraction and aviation fuel fraction from animal and vegetable oil |
| CN103897718B (en) * | 2012-12-27 | 2016-05-11 | 中国石油天然气股份有限公司 | Method for producing diesel oil fraction and aviation fuel fraction from animal and vegetable oil |
| CN103031218A (en) * | 2013-01-11 | 2013-04-10 | 广西大学 | Method for synthesizing biodiesel by base catalysis |
| CN103031218B (en) * | 2013-01-11 | 2014-05-14 | 广西大学 | Method for synthesizing biodiesel by base catalysis |
| CN104419518A (en) * | 2013-08-23 | 2015-03-18 | 中国石油天然气股份有限公司 | Vegetable fat dissociation-chelating degumming method |
| CN111057616A (en) * | 2019-08-26 | 2020-04-24 | 易高生物化工科技(张家港)有限公司 | Treatment method for removing impurities from waste animal and vegetable oil |
| CN115161109A (en) * | 2022-07-18 | 2022-10-11 | 湖北碧美新能源科技有限公司 | Preparation method of industrial-grade mixed oil |
| CN116875379A (en) * | 2023-05-31 | 2023-10-13 | 山东三聚生物能源有限公司 | Method and system for demetallizing biological raw oil |
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Application publication date: 20120104 |