CN102154058A - Process for carrying out pretreatment on waste oil - Google Patents

Process for carrying out pretreatment on waste oil Download PDF

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Publication number
CN102154058A
CN102154058A CN 201110058106 CN201110058106A CN102154058A CN 102154058 A CN102154058 A CN 102154058A CN 201110058106 CN201110058106 CN 201110058106 CN 201110058106 A CN201110058106 A CN 201110058106A CN 102154058 A CN102154058 A CN 102154058A
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China
Prior art keywords
waste grease
waste oil
gross weight
decomposition agent
discharge
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CN 201110058106
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Chinese (zh)
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CN102154058B (en
Inventor
陈恒顺
严小建
张宇
金健
沈建平
申圣良
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CHONGQING HAOTAI ENERGY CO., LTD.
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JIANGSU HENGSHUNDA BIO-ENERGY Co Ltd
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Publication of CN102154058A publication Critical patent/CN102154058A/en
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Expired - Fee Related legal-status Critical Current
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Abstract

The invention discloses a process for carrying out pretreatment on waste oil, which comprises steps of waste oil dissolution, addition of a disintegrant for performing a reaction, sedimentation and impurity removal, electrolysis treatment and the like. The process has the advantages that in the process for carrying out pretreatment on the waste oil, the disintegrant with the specific components and content is added, so that most of fat-soluble colloidal impurities in the waste oil are transformed into water-soluble colloidal impurities; and under the action of electrolyte, colloidal particles adsorb water and are expanded, aggregated and settled to be discharged, so that various colloidal substances and unsaponifiable matter in the waste oil are effectively removed, the quality of the refined oil is well improved, good raw material quality guarantee is provided for the subsequent esterification and ester exchange process of biodiesel, and the degree of coking and carbon deposition in the esterification process is greatly reduced.

Description

The waste grease pretreatment technology
Technical field
The present invention relates to a kind of waste grease pretreatment technology.
Background technology
Along with the day that world energy sources uses is becoming tight, the various new forms of energy that searching can substitute fossil energy become one of important research task of various countries, the world today.And biofuel has great advantage because of it at aspects such as dynamic performance, environmental-protecting performance and safety performances, receives much concern in recent years, has obtained development faster.
The producing and manufacturing technique that at present can heavy industrialization prepares biofuel mainly is a chemical method, and this method is under certain temperature, pressure, catalyzer condition, makes grease and methyl alcohol finish the process of esterification.A large amount of practical operation situation show, this method can produce a large amount of cokings in reaction process, carbon distribution, the colloid material, the steady running of production and the quality of subsequent product have seriously been influenced, and a major reason that causes the problems referred to above to produce is exactly to contain a considerable amount of phosphatide in the waste grease as raw material, protein, lymphatic temperament, peptized impurities and unsaponifiables such as aliphatic polymer and composite metal salt such as glycosyl triglyceride, in preprocessing process to waste grease, the removal degree of these not saponification components is to the follow-up esterification process of production of biodiesel, the continuous operation and the quality product for the treatment of process have very big influence.
Traditional oil refining process comprises filtration method, the aquation method, the alkali refining method, acid refining method and carclazyte absorption method etc., these methods mainly are to utilize the various physicochemical property of each impurity composition in the crude oil, adopt corresponding physical chemistry means to handle, these methods are the most of mechanical impuritys that can effectively remove wherein for the more stable conventional animal-plant oil of component, what water-soluble glue was assorted and fat-soluble glue is assorted, but for waste grease, because its source is unstable, oil is planted unfixing, the high temperature polymer that contains in the food and drink waste grease particularly, oxide compound, greatly increase unsaponifiables number of components and the content in the waste grease, only adopted above-mentioned traditional method to be difficult to remove effectively not saponification component.
Summary of the invention
Goal of the invention: at the problems referred to above, the purpose of this invention is to provide a kind of waste grease pretreatment technology, the oil quality after the refining is well improved, thereby reduce coking, carbon distribution, the colloid material that produces in the production of biodiesel process.
Technical scheme: a kind of waste grease pretreatment technology, this technology may further comprise the steps:
(1) waste grease is added reaction unit, be warming up to 80 ℃~98 ℃ under the whipped state gradually, be incorporated as the water of waste grease gross weight 20%~40% then;
(2) add decomposition agent, continue to be warming up to 120 ℃~140 ℃, keep temperature and pressure-stabilisation, when the reaction mass acid number rises to 140~160mgKOH/g, stop heating;
When (3) temperature drops to 95 ℃, close stirring, after reaction mass leaves standstill,, and continue to discharge bottom colloid class material till having oil phase to discharge the emptying of reaction unit lower aqueous;
(4) open stirring, be incorporated as the water of waste grease gross weight 5%~20%, intensification and holding temperature are at 60 ℃~90 ℃, add ionogen, leave standstill after the stirring,, and continue to discharge bottom colloid class material till having oil phase to discharge then with the emptying of reaction unit lower aqueous.
Decomposition agent described in the step (2) and consumption thereof are the vitriol oil 0.1%~2.5%, and it is the weight percent that radix calculates that phosphoric acid 0.1%~1.5%, sulfo group xylyl lipid acid 0.1%~1.5%, the consumption of the above decomposition agent are with the waste grease gross weight.
Ionogen described in the step (4) is that mass concentration is 20% Na 2SO 4And Al 2(SO 4) 3The aqueous solution, wherein solute Na 2SO 4With Al 2(SO 4) 3Mass ratio be 1:1, the consumption of described electrolyte solution is 10% of a waste grease gross weight.
The addition sequence of described decomposition agent is the vitriol oil, phosphoric acid, sulfo group xylyl lipid acid.
Beneficial effect: compared with prior art, advantage of the present invention is the decomposition agent that adds specific components and content in the pretreatment technology of waste grease, making in the waste grease most fat-soluble glue, assorted to change water-soluble glue into assorted, under electrolytical effect, make the micelle water-swelling, assemble, sedimentation and discharging, effectively remove all kinds of colloid class materials in the waste grease, unsaponifiables, improved the oil quality after the refining well, provide good material quality to guarantee for the follow-up esterification transesterify of biofuel process, greatly reduced coking in the esterification process, the degree of carbon distribution.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is used to the present invention is described and is not used in and limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Embodiment 1: a kind of waste grease pretreatment technology of the present invention, comprise the steps: waste grease is added in the withstand voltage reactor of reaction unit, and open steam under the whipped state gradually and be warming up to 80 ℃, be incorporated as the water of waste grease gross weight 40% then; Be sequentially added into following decomposition agent: 2.5% vitriol oil, 1.5% phosphoric acid, 1.5% sulfo group xylyl lipid acid, it is the weight percent that radix calculates that the consumption of the above decomposition agent is with the waste grease gross weight, continue to be warming up to 130 ℃, steam regulation pressure and feed rate, keep temperature and pressure-stabilisation, after this per hour with material acid number of reaction mass sampling and measuring, when the reaction mass acid number rose to 160mgKOH/g in about 4~6 hours, steam off stops heating; When temperature drops to 95 ℃, close stirring, after reaction mass leaves standstill about half an hour,, and continue to discharge bottom colloid class material till having oil phase to discharge the emptying of reaction unit lower aqueous; Unlatching is stirred, and is incorporated as the water of waste grease gross weight 5%, opens steam intensification and holding temperature at 70 ℃, and the adding mass concentration is 20% Na 2SO 4And Al 2(SO 4) 3The aqueous solution is as ionogen, and the consumption of described electrolyte solution is 10% of a waste grease gross weight, stirs to leave standstill 30 minutes after 10 minutes, then with the emptying of reaction unit lower aqueous, and continues to discharge bottom colloid class material till having oil phase to discharge.
Embodiment 2: a kind of waste grease pretreatment technology of the present invention, comprise the steps: waste grease is added in the withstand voltage reactor of reaction unit, and open steam under the whipped state gradually and be warming up to 85 ℃, be incorporated as the water of waste grease gross weight 30% then; Be sequentially added into following decomposition agent: 1.5% vitriol oil, 1.5% phosphoric acid, 1.5% sulfo group xylyl lipid acid, it is the weight percent that radix calculates that the consumption of the above decomposition agent is with the waste grease gross weight, continue to be warming up to 120 ℃~140 ℃, steam regulation pressure and feed rate, keep temperature and pressure-stabilisation, after this per hour with material acid number of reaction mass sampling and measuring, when the reaction mass acid number rose to 140mgKOH/g in about 4~6 hours, steam off stops heating; When temperature drops to 95 ℃, close stirring, after reaction mass leaves standstill about half an hour,, and continue to discharge bottom colloid class material till having oil phase to discharge the emptying of reaction unit lower aqueous; Unlatching is stirred, and is incorporated as the water of waste grease gross weight 8%, opens steam intensification and holding temperature at 90 ℃, and the adding mass concentration is 20% Na 2SO 4And Al 2(SO 4) 3The aqueous solution is as ionogen, and the consumption of described electrolyte solution is 10% of a waste grease gross weight, stirs to leave standstill 30 minutes after 10~20 minutes, then with the emptying of reaction unit lower aqueous, and continues to discharge bottom colloid class material till having oil phase to discharge.
Waste grease raw material index is not tolerant 2.1%, the unsaponifiables 2.7% of phosphatidase 11 .8%, acetone in the foregoing description, more than is the quality percentage composition.Use grease index after the technology of the present invention with use grease index behind the conventional acid refining degumming technology relatively classify following table as:
Grease index (quality percentage composition) Conventional acid refining degumming technology Technology of the present invention
Phosphatide (%) 1.2 0.15
Acetone not tolerant (%) 0.9 0.1
Unsaponifiables (%) 1.6 0.3
Esterification carbon distribution (%) 1.5 0.1
As seen the data listed by last table contrast, technology of the present invention can effectively be removed all kinds of colloid class materials, unsaponifiables in the waste grease, improved the oil quality after the refining well, provide good material quality to guarantee for the follow-up esterification transesterify of biofuel process, greatly reduced the degree of coking in the esterification process, carbon distribution.

Claims (4)

1. waste grease pretreatment technology is characterized in that this technology may further comprise the steps:
(1) waste grease is added reaction unit, be warming up to 80 ℃~98 ℃ under the whipped state gradually, be incorporated as the water of waste grease gross weight 20%~40% then;
(2) add decomposition agent, continue to be warming up to 120 ℃~140 ℃, keep temperature and pressure-stabilisation, when the reaction mass acid number rises to 140~160mgKOH/g, stop heating;
When (3) temperature drops to 95 ℃, close stirring, after reaction mass leaves standstill,, and continue to discharge bottom colloid class material till having oil phase to discharge the emptying of reaction unit lower aqueous;
(4) open stirring, be incorporated as the water of waste grease gross weight 5%~20%, intensification and holding temperature are at 60 ℃~90 ℃, add ionogen, leave standstill after the stirring,, and continue to discharge bottom colloid class material till having oil phase to discharge then with the emptying of reaction unit lower aqueous.
2. waste grease pretreatment technology according to claim 1, it is characterized in that: decomposition agent described in the step (2) and consumption thereof are the vitriol oil 0.1%~2.5%, phosphoric acid 0.1%~1.5%, it is the weight percent that radix calculates that sulfo group xylyl lipid acid 0.1%~1.5%, the consumption of the above decomposition agent are with the waste grease gross weight.
3. waste grease pretreatment technology according to claim 1 is characterized in that: the ionogen described in the step (4) is that mass concentration is 20% Na 2SO 4And Al 2(SO 4) 3The aqueous solution, wherein solute Na 2SO 4With Al 2(SO 4) 3Mass ratio be 1:1, the consumption of described electrolyte solution is 10% of a waste grease gross weight.
4. waste grease pretreatment technology according to claim 2 is characterized in that: the addition sequence of described decomposition agent is the vitriol oil, phosphoric acid, sulfo group xylyl lipid acid.
CN201110058106A 2011-03-11 2011-03-11 Process for carrying out pretreatment on waste oil Expired - Fee Related CN102154058B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504945A (en) * 2011-11-04 2012-06-20 江苏恒顺达生物能源有限公司 Process for refining waste oil

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986737A (en) * 2005-12-19 2007-06-27 丁以钿 Process of producing biodiesel oil with catering waste oil
CN101113356A (en) * 2006-07-27 2008-01-30 上海中油企业集团有限公司 Method for producing biodiesel by trench oil
KR20100026079A (en) * 2008-08-29 2010-03-10 제이앤비오일(주) The method of manufacturing the high purity bio-diegel fuel with rancid oil
WO2011027353A1 (en) * 2009-09-07 2011-03-10 Council Of Scientific & Industrial Research Integrated process for the production of jatropha methyl ester and by products

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1986737A (en) * 2005-12-19 2007-06-27 丁以钿 Process of producing biodiesel oil with catering waste oil
CN101113356A (en) * 2006-07-27 2008-01-30 上海中油企业集团有限公司 Method for producing biodiesel by trench oil
KR20100026079A (en) * 2008-08-29 2010-03-10 제이앤비오일(주) The method of manufacturing the high purity bio-diegel fuel with rancid oil
WO2011027353A1 (en) * 2009-09-07 2011-03-10 Council Of Scientific & Industrial Research Integrated process for the production of jatropha methyl ester and by products

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 20090430 陈水根 "高酸价油脂制备生物柴油及甘油精制技术的研究" B019-65 , 第4期 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102504945A (en) * 2011-11-04 2012-06-20 江苏恒顺达生物能源有限公司 Process for refining waste oil

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