CN102071103A - Novel dry-method degumming method for abandoned oil - Google Patents
Novel dry-method degumming method for abandoned oil Download PDFInfo
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- CN102071103A CN102071103A CN 201110026477 CN201110026477A CN102071103A CN 102071103 A CN102071103 A CN 102071103A CN 201110026477 CN201110026477 CN 201110026477 CN 201110026477 A CN201110026477 A CN 201110026477A CN 102071103 A CN102071103 A CN 102071103A
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Abstract
The invention mainly aims to solve the problems caused by degumming in the process of processing abandoned oil serving as raw materials. By dry-method degumming, the series of problems can be solved effectively. The method comprises the following steps of: adding a certain amount of acid (strong phosphoric acid: citric acid is 2:1) into a material system, and reacting at the temperature of 100 and 115 DEG C for 55 to 85 minutes, so that phospholipid in the abandoned oil serving as the raw materials is flocculated to form large granular flocculate; stirring a mixture, which serves as an adsorbent, of quantitative silica gel and carclazyte continuously for 50 and 80 minutes under the vacuum degree of between 0.080 and 0.098 MPa, wherein the addition of the adsorbent is between 0.5 and 2.0 percent; and cooling the integral material system to a certain extent, filtering the hot material system, and filtering out colloid and part of pigments by adsorption. The process has a simple operational condition, does not generate oilfoot, is less in pollution, can improve the yield of products by over 2 percent, achieves the discoloring effect while degumming, and improves the quality of oils obviously.
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
There is lack of raw materials at present remains the primary factor that limits biofuel price and large-scale production.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 not cause many adverse factors: influence grease stability, moisture absorption hydrolysis easily if do not remove; 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.
The main purpose of coming unstuck is that the phosphatide in the grease is removed, method much as the aquation method come unstuck, thermal polymerization method comes unstuck, acid system comes unstuck, chemical-agent technique comes unstuck etc.For example, Chinese granted patent CN1079985 provides a kind of absorption degumming technique of edible oil, and its adopts adsorption medium that peptized impurities is adsorbed, and the adsorption medium that will adsorb peptized impurities by press filtration removes then, reaches the purpose of coming unstuck.Advantages such as this degumming technology has device simple, and working pressure hangs down to be controlled conveniently, and filtering material is easily changed cleaning, and the neutral oil loss is few, and production cost is also relatively low, and oil foot can directly be used as feed or recovery fully utilizes, and reduce environmental pollution.
China granted patent CN1112156 discloses the enzymatic degumming method of a vegetable oil, be this vegetables oil pH value is transferred to 6 from 3, and with contain phospholipase A1, the aqueous solution of a kind of enzyme among A2 or the B; This enzyme works to vegetables oil in the reactor that comes unstuck that stir on the limit under temperature is 20 ℃～90 ℃; Before or after the vegetables oil after separation is come unstuck, with a kind of separation promoter or solubilizing agent, at 20 ℃～90 ℃ liquid that add down from the reactor that comes unstuck; Recovery contains the solution that does not in fact have sludge of exhausted enzyme, and is recycled to the position of the reactor front of coming unstuck to small part.Wherein the content of round-robin exhausted enzyme accounts for 10% of dispersive enzyme total amount in the vegetables oil at least.
China granted patent CN101058770 provides a kind of glyceride stock hydration degum method of biofuel, utilize the wetting ability of peptized impurities such as phosphatide, water or ionogen dilute solution with some amount, add in the crude oil and mix, make the water-swelling of colloid energy, cohesion forms bigger " hydrate " of relative oil density, the centrifugal force separating machine separates then, hydration degum and centrifugation combination can improve degumming rate like this, and have improved processing speed.
In addition, Chinese granted patent CN101381298 discloses a kind of method of utilizing Idesia polycarpa oil to prepare conjugated linolic acid, belongs to medicine, food and field of fodder.This technology comprises that the acid system of crude oil comes unstuck, and it is characterized in that utilizing sour method for degumming to obtain degummed oil, and dephosphorization fat is thorough.
Degumming technology of the present invention compares filter membrane and all reductions greatly of operational condition requirement owing to carry out press filtration again after adopting adsorption medium elder generation adsorption-flocculation particulate colloid 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, save water resources; Have very big price variance with enzymatic degumming, the enzymatic degumming price is higher, and this law cost of material that comes unstuck is cheap, can not produce the great number cost; The technology operational conditions is simple, and is of reduced contamination, and product yield can improve more than 2%, and also played the effect of decolouring when coming unstuck, and oil quality has had obvious improvement.
Summary of the invention
At the defective of existing degumming technology, main purpose of the present invention is to provide 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, and its step comprises:
The I dehydration: raw oil material pre-treatment dehydration in reactor (4) in 100 ℃～120 ℃ of temperature, vacuum tightness (8) 0.075Mpa～0.098Mpa, under stirring velocity 100r/min～120r/min condition the raw material water content in oil is removed, do not had bubble to produce until the oil reservoir surface;
II acid-respons process: will be cooled to a little less than 100 ℃ through the raw material via interlayer (3) of dehydration and avoid high temperature oxidation, adding raw oil material weight 0.2%～1.0% sour reagent (strong phosphoric acid: 2: 1 compound acid of citric acid) by adding sour hole (11) under the whipped state fast, add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 50r/min～60r/min, rise to 100 ℃～120 ℃ of temperature of reaction by heating tube (5), the reaction times is 50min～90min;
The III adsorption process: the dry degumming sorbent material is the mixture of silica gel and carclazyte, the two part by weight is controlled at (0.5～1): (2～6), sorbent material will carry out 150 ℃～200 ℃ high-temperature activations before use, adds 0.5%～2.0% of raw material weight by adding sour hole (11).Adsorption process vacuum tightness is controlled at 0.080Mpa～0.098Mpa by (8), and temperature is controlled at 110 ℃～130 ℃ by (5), and continuous stirring condition is reaction 30min～60min down, and stirring velocity is controlled at 50r/min～70r/min;
The IV temperature-fall period: the grease that adsorption process finishes is kept its stirring velocity 50r/min～70r/min, by interlayer (3) cooling, controls 80 ℃～100 ℃ of whole material temperature;
The V pressure-filtering process: the raw oil material after the cooling imports pressure filter (9) by pipeline, and temperature is 70 ℃～90 ℃, and pressure range is 0.15MP～0.45MPa, adopts the filter cloth of high mechanical strength such as nylon, polyester material to carry out press filtration.Filtrate is biodiesel raw material.
Technique effect
1, do not make water and steam etc. in the degumming technology process, save water resources greatly.
2, operational condition is simple, does not need complicated processing unit;
3, of reduced contamination, there is not oil foot to produce, there are not generations such as sewage, waste gas;
4, product yield can improve more than 2% than hydration degum etc.; And carclazyte has also played the effect of decolouring when coming unstuck, and oil quality has had obvious improvement;
5, by control stirring velocity better utilised sorbent material, reach best adsorption effect;
6, technological design is cooled off material by interlayer, can prevent effectively that the high temperature raw oil material is exposed in the air and the oxygen catalytic oxidation, controls the acid number of biodiesel raw material oil better, helps next step esterification.
Description of drawings
Fig. 1 is the process flow sheet of abendoned oil dry degumming.
Referring to shown in Figure 1, in the process flow sheet of abendoned oil dry degumming, comprising: 1---storage tank; 2---toothed gear pump; 3---interlayer; 4---reactor; 5---heating tube; 6---fuel economizer; 7---water receiver; 8---vacuum pump; 9---pressure filter; 10---storage tank; 11---add sour hole
Embodiment
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1
The pre-crude product sewer oil of crossing fence of 500Kg is beaten to reactor by pipeline, is heated to 110 ℃～115 ℃, and control vacuum tightness is 0.090MPa, and stirring velocity 105r/min does not have boiling explosion phenomenon through the 40min material, and the oil reservoir surface does not have bubble yet and produces.Be cooled to 100 ℃, add grease weight 1.0kg acid reagent, add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 50r/min, and temperature of reaction is 100 ℃, and the reaction times is 70min.Finish, add sorbent material 5Kg, vacuum tightness 0.090Mpa, 120 ℃ of continuous stirring conditions of temperature are reaction 75min down, and stirring velocity is controlled at 60r/min.Slightly be cooled to 100 ℃,, enter next reactor by pressure filter.The back material quality that comes unstuck is as follows:
Comparative Examples 1 sewer oil hydration degum technology
0.5 the pre-crude product sewer oil of crossing fence of ton is beaten to retort by pipeline, warm waterization is come unstuck in the employing, is heated to 60 ℃, and amount of water is 15Kg, slowly stirs 30r/min～40r/min, aquation 40min.Behind the insulation sedimentation 8h, emit the upper strata absolute oil, the flocculation micelle is emitted from below.The back material quality that comes unstuck is as follows:
Embodiment 1 compares with Comparative Examples 1, the refining trench oil production yield that adopts dry degumming technology to obtain has improved 3.4%, foreign matter content and moisture content in the sewer oil of refining simultaneously all obviously reduce, refining trench oil colours pool by heat test dry degumming explained hereafter is constant, no precipitate illustrates that phosphorus content is low, and treatment effect is good, color and luster is more shallow than the hydrated adhesive color, illustrates certain effect has been played in decolouring.
Embodiment 2
The pre-crude product sewer oil of crossing fence of 2000Kg is beaten to reactor by pipeline, is heated to 110 ℃～115 ℃, and control vacuum tightness is 0.090MPa, and stirring velocity 110r/min does not have boiling explosion phenomenon through the 40min material, and the oil reservoir surface does not have bubble yet and produces.Be cooled to 100 ℃, add grease weight 1.0kg acid reagent, add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 60r/min, and temperature of reaction is 100 ℃, and the reaction times is 55min.Finish, add sorbent material 5Kg, vacuum tightness 0.090Mpa, 120 ℃ of continuous stirring conditions of temperature are reaction 80min down, and stirring velocity is controlled at 60r/min.Slightly be cooled to 100 ℃,, enter next reactor by pressure filter.The back material quality that comes unstuck is as follows:
Embodiment 3
The pre-crude product sewer oil of crossing fence of 1000Kg is beaten to reactor by pipeline, is heated to 110 ℃～115 ℃, and control vacuum tightness is 0.090MPa, and stirring velocity 105r/min does not have boiling explosion phenomenon through the 40min material, and the oil reservoir surface does not have bubble yet and produces.Be cooled to 100 ℃, add grease weight 1.0kg acid reagent, add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 55r/min, and temperature of reaction is 100 ℃, and the reaction times is 85min.Finish, add sorbent material 5Kg, vacuum tightness 0.090Mpa, 120 ℃ of continuous stirring conditions of temperature are reaction 50min down, and stirring velocity is controlled at 60r/min.Slightly be cooled to 100 ℃,, enter next reactor by pressure filter.The back material quality that comes unstuck is as follows:
Claims (8)
1. novel abendoned oil dry degumming method, its step comprises:
The I dehydration: raw oil material pre-treatment dehydration in reactor (4) in 100 ℃～120 ℃ of temperature, vacuum tightness (8) 0.075Mpa～0.098Mpa, under stirring velocity 100r/min～120r/min condition the raw material water content in oil is removed, do not had bubble to produce until the oil reservoir surface;
II acid-respons process: will be cooled to a little less than 100 ℃ through the raw material via interlayer (3) of dehydration and avoid high temperature oxidation, adding raw oil material weight 0.2%～1.0% sour reagent (strong phosphoric acid: 2: 1 compound acid of citric acid) by adding sour hole (11) under the whipped state fast, add the acid reduction stirring velocity that finishes, stirring velocity is controlled at 50r/min～60r/min, rise to 100 ℃～120 ℃ of temperature of reaction by heating tube (5), the reaction times is 50min～90min;
The III adsorption process: the dry degumming sorbent material is the mixture of silica gel and carclazyte, the two part by weight is controlled at (0.5～1): (2～6), sorbent material will carry out 150 ℃～200 ℃ high-temperature activations before use, adds 0.5%～2.0% of raw material weight by adding sour hole (11).Adsorption process vacuum tightness is controlled at 0.080Mpa～0.098Mpa by (8), and temperature is controlled at 110 ℃～130 ℃ by (5), and continuous stirring condition is reaction 30min～60min down, and stirring velocity is controlled at 50r/min～70r/min;
The IV temperature-fall period: the grease that adsorption process finishes is kept its stirring velocity 50r/min～70r/min, by interlayer (3) cooling, controls 80 ℃～100 ℃ of whole material temperature;
The V pressure-filtering process: the raw oil material after the cooling imports pressure filter (9) by pipeline, and temperature is 70 ℃～90 ℃, and pressure range is 0.15MP～0.45MPa, adopts the filter cloth of high mechanical strength such as nylon, polyester material to carry out press filtration.Filtrate is biodiesel raw material.
2. described by right 1 requirement, abendoned oil is characterized in that comprising numerous kinds such as sewer oil, acidifying oil, hogwash fat, frying waste oil, vegetable oil refining tankage and meat product tankage.
3. described by right 1 requirement, sour reagent is characterized in that being strong phosphoric acid: the compound acid of citric acid (2: 1), its role is to impel phosphatide ring-opening polymerization flocculation, and be convenient to from oil phase, carry out dry method and separate.
4. described by right 1 requirement, sorbent material is characterized in that the mixture for silica gel and carclazyte, part by weight (0.5～1): (2～6), sorbent material will be carried out 150 ℃～200 ℃ high-temperature activations before use.
5. described by right 1 requirement, the stock oil preprocessing process is characterized in that 100 ℃～120 ℃ of temperature, under vacuum tightness 0.075Mpa～0.098Mpa condition the raw material water content in oil is removed, and does not have bubble to produce until the oil reservoir surface.
6. described by right 1 requirement, sour reagent react is characterized in that add-on is 0.2%～1.0% of total oil plant weight, and temperature of reaction is 100 ℃～120 ℃, and the reaction times is controlled at 55min～85min.
7. described by right 1 requirement, dry degumming absorption is characterized in that the sorbent material add-on weighs 0.5%～2.0% for oil, and at vacuum tightness 0.080Mpa～0.098Mpa, 110 ℃～130 ℃ continuous stirring conditions of temperature are reaction 50min～80min down.
8. described by right 1 requirement, glue separating of oil it is characterized in that is cooled to 80 ℃～100 ℃ with whole material, prevents that high temperature from exposing oxidation, by the pressure filter solid-liquid separation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110026477 CN102071103B (en) | 2011-01-25 | 2011-01-25 | Novel dry-method degumming method for abandoned oil |
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| CN 201110026477 CN102071103B (en) | 2011-01-25 | 2011-01-25 | Novel dry-method degumming method for abandoned oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304420A (en) * | 2011-08-09 | 2012-01-04 | 湖南省林业科学院 | Dry degumming method of raw abandoned oil used for producing biodiesel |
| 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 |
| CN102618390A (en) * | 2012-03-31 | 2012-08-01 | 国家粮食储备局武汉科学研究设计院 | Method for preparing biodiesel by using waste grease split-phase method |
| CN104073363A (en) * | 2014-06-30 | 2014-10-01 | 李安民 | Degumming and impurity removing process and equipment for waste oil |
| CN104419518A (en) * | 2013-08-23 | 2015-03-18 | 中国石油天然气股份有限公司 | Disassociation-chelating degumming method for plant grease |
| 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 |
| CN113444569A (en) * | 2021-06-29 | 2021-09-28 | 江西尊创新能源有限公司 | Method for refining waste animal and vegetable oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079985A (en) * | 1992-06-11 | 1993-12-29 | 王军 | Degumming process for edible oil |
| CN1523094A (en) * | 2003-09-12 | 2004-08-25 | 高元财 | Process for producing corn germ oil and table oil made by products produced thereby |
| CN101381298A (en) * | 2008-10-21 | 2009-03-11 | 四川省国政生物质能源科技发展股份有限公司 | Method for preparing conjugate linolic acid using idesia polycarpa maxim. var. vestita diels oil |
-
2011
- 2011-01-25 CN CN 201110026477 patent/CN102071103B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079985A (en) * | 1992-06-11 | 1993-12-29 | 王军 | Degumming process for edible oil |
| CN1523094A (en) * | 2003-09-12 | 2004-08-25 | 高元财 | Process for producing corn germ oil and table oil made by products produced thereby |
| CN101381298A (en) * | 2008-10-21 | 2009-03-11 | 四川省国政生物质能源科技发展股份有限公司 | Method for preparing conjugate linolic acid using idesia polycarpa maxim. var. vestita diels oil |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304420A (en) * | 2011-08-09 | 2012-01-04 | 湖南省林业科学院 | Dry degumming method of raw abandoned oil used for producing biodiesel |
| 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 |
| CN102618390A (en) * | 2012-03-31 | 2012-08-01 | 国家粮食储备局武汉科学研究设计院 | Method for preparing biodiesel by using waste grease split-phase method |
| CN104419518A (en) * | 2013-08-23 | 2015-03-18 | 中国石油天然气股份有限公司 | Disassociation-chelating degumming method for plant grease |
| CN104073363A (en) * | 2014-06-30 | 2014-10-01 | 李安民 | Degumming and impurity removing process and equipment for waste oil |
| 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 |
| CN113444569A (en) * | 2021-06-29 | 2021-09-28 | 江西尊创新能源有限公司 | Method for refining waste animal and vegetable oil |
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| CN102071103B (en) | 2013-02-06 |
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