CN1858162A - Method for preparing biological diesel oil from saurauia tristyla var oldhamii oil - Google Patents
Method for preparing biological diesel oil from saurauia tristyla var oldhamii oil Download PDFInfo
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- CN1858162A CN1858162A CNA2006100427375A CN200610042737A CN1858162A CN 1858162 A CN1858162 A CN 1858162A CN A2006100427375 A CNA2006100427375 A CN A2006100427375A CN 200610042737 A CN200610042737 A CN 200610042737A CN 1858162 A CN1858162 A CN 1858162A
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- 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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The process of preparing biological diesel oil with alder Alnus oil includes the following steps: collecting alder Alnus fruit, pre-treatment and squeezing to obtain coarse alder Alnus oil; refining alder Alnus oil through depositing, filtering, degumming, deacidifying, washing and dewatering; the esterification between refined alder Alnus oil and fatty alcohol in the weight ratio of 100 to 10-20 at 40-70 deg.c under stirring and in the presence of alkaline catalyst for 30-60 min; and distilling, filtering, separating, washing and drying to obtain biological diesel oil and glycerin. The present invention has simple technological process, low cost and low power consumption, and the biological diesel oil product has excellent quality.
Description
Technical field
The present invention relates to a kind of preparation method of biofuel, particularly prepare method of bio-diesel oil by the water white gourd oil.
Background technology
Biofuel is meant fatty acid methyl ester or the ethyl ester that grease (comprising vegeto-animal fat) obtains through a series of processing and chemical reaction.Mentioned raw oil material is nothing but a rapeseed oil in all both at home and abroad at present relevant reports, soybean oil, peanut oil, oleum gossypii seminis, water oil and so under plam oil and restaurant swill oil or the animal, these raw materials all are not suitable for the national conditions of China, the reasons are as follows: (1) China 1,300,000,000 people's big country, on limited arable area, at first will solve is people's grain ration and edible oil problem, it is reported, China at present per capita the level of consumption of edible oil be the last 1/3 of whole world consumption per head, so this situation Chinesely can not large-arealy be taken out limited arable land and removes to plant the land used that is used to do biodiesel raw material with regard to having determined.(2) other raw materials are because the complicacy of output and scale or component all can not form industrialized production on a large scale.(3) comparing no any superiority with petrifaction diesel economically with the biofuel of above all raw material production that are mentioned to can say.China will develop biofuel and must walk out a new road that meets China's actual conditions.
The water wax gourd is being commonly called as of root or bark of Nepal Mallotus (Idesia polycarpa Maxim) and mutation Idesia polycarpa (Idesiapolycarpa Var.vestita Giels), have another name called the chair paulownia, the mountain Chinese parasol tree, the bucket frost is red, belonging to a kind of large-scale arbor of Flacourtiaceae, be a kind of wild woody oil tree species of China's special product, was wild originally, adaptability is strong, like moistening rich soil, but also drought-resistant barren, the low temperature below the ability-15 ℃, on acid and neutral or subalkaline soil, can both well grow, the result, also have at saline and alkaline terraneous report, especially fit and plant, the root system hypertrophy in the deserted mountain barren hill, retaining is strong, also is suitable for doing greening street ornamental tree species.
The preparation method of existing biofuel is that animal-plant oil is carried out esterification through after the refining under the condition of high temperature (more than 200 ℃), high pressure (more than the 0.8MPa) and catalyzer, and the big energy consumption of this technology investment is high and security that produce is also poor.
Summary of the invention
Technical problem to be solved by this invention is exactly at raw material and the existing shortcoming of production technique in the at present domestic and international production biofuel, and brand-new raw material of a kind of usefulness and simple and safe low power technology are provided, and prepares method of bio-diesel oil by the water white gourd oil.
The present invention solves the technical scheme that its technical problem adopts: a kind ofly prepare method of bio-diesel oil by the water white gourd oil, comprise refining of water white gourd oil and esterification technique, water white gourd oil refinery practice comprises the steps: water wax gourd fruit harvesting, dry, collection, after carrying out pre-treatment again and removing impurity, squeezing water outlet wax gourd crude oil, to precipitate, crude oil after the filtration is through coming unstuck, depickling, washing, obtain refining oil after the dehydration, esterification technique comprise the steps: with water wax gourd refining oil and Fatty Alcohol(C12-C14 and C12-C18) by 100: 10～20 mass ratioes under 40～70 ℃ of temperature and basic catalyst condition, stir carried out esterification in 20～60 minutes after, again through the distillation, filter, separate, washing, drying can make biofuel and glycerine.
Described water wax gourd degumming raw oil operation steps is as follows: crude oil is heated with stirring to 50～65 ℃, adds the water of the same oil temperature of quality of crude oil 2～3%, stirs 30～40 minutes, precipitates 6～8 hours, detects phosphorus content less than 20 * 10
-6Mg/Kg.
Described water wax gourd crude oil depickling operation steps is as follows: the water white gourd oil temperature after will coming unstuck is adjusted to 20～30 ℃, adds alkali lye, concentration of lye 18Be
-～22Be
-, stirring 30～40 minutes, stirring velocity slows down gradually, and oil is warming up to 55～65 ℃ simultaneously, staticly settles 6～8 hours, and oily soap separates, and the test free fatty acid content is less than 0.5%.
Described water wax gourd crude oil washs, the dehydration operation step is as follows: oily temperature is heated to 80～95 ℃, 10～20% synthermal water washings of adding oil quality 2～3 times, oily water separation is heated to 100～110 ℃ with oil, dehydration, crude oil dehydration back Water in oil amount is lower than 0.06%.
Described water wax gourd crude oil is the full fruit oil of water wax gourd fruit.
Described Fatty Alcohol(C12-C14 and C12-C18) is a methyl alcohol.
Described basic catalyst is sodium hydroxide or potassium hydroxide.
The invention has the beneficial effects as follows: the invention provides a kind of new raw material and safety in production technology simple and low-cost, less energy-consumption of production biofuel, make China's large-scale industrial production low price biofuel become possibility.Water wax gourd tree is developed as the reasons are as follows of biodiesel raw material seeds: (1) does not account for the arable land, deserted mountain barren hill afforestation, as long as in front of the door behind the house assorted ground, river bank have some place of soil just can grow.(2) splendid by the biodiesel quality of water white gourd oil production, product is through Research Institute of Petro-Chemical Engineering's Analysis and Identification, and leading indicator is much better than the standard of GB GB252-2000 solar oil, and product is not before adding any additives, and cold filter clogging temperature is between GB-10
#～-20
#Between the diesel oil, this has just remedied northern China winter-10
#～-20
#The situation of diesel oil wretched insufficiency.(3) profitable through agent, because the full fruit of water wax gourd oil length up to 35～38%, more than the average produce oil 15Kg of individual plant, utilizes the cost of hillside fields, deserted mountain plantation will be significantly less than the expense that takies the arable land.The comprehensive production cost of estimating biofuel per ton is about 4000 yuan.And petrifaction diesel has reached 5000 yuan per ton at present.(4) accounting on the non-agricultural arable land of the area overwhelming majority plantation water wax gourd tree in China provide an inexhaustible raw material site will for the biofuel industry of China.(5) widely popularize plantation water wax gourd tree in the vast mountain area of China, particularly poverty-stricken area, Midwest, all will play very positive effect and comprehensive benefit difficult to the appraisal solving China's rural economy, rural development and rural demography, environmental protection soil erosion problem and national Oil Safety problem.
Description of drawings
Fig. 1 is a refinery practice schema of the present invention.
Fig. 2 is an esterification technique schema of the present invention.
Embodiment
Embodiment 1
One, water wax gourd crude oil production technique
1, raw water wax gourd fruit
Adopt down the fruit that becomes redness (a little has yellow fruit) on the water wax gourd tree the annual last ten-days period in October, dries the collection warehouse-in.
2, pre-treatment
Air dried water wax gourd fruit is store in the storehouse utilizes means such as selection by winnowing, magnetic separation to remove various impurity in the fruit.
3, oil is got in squeezing
The water wax gourd fruit of removing impurity is put into hydraulic oil press for 100 jin squeeze continuously, obtain 24.4 jin of water wax gourd crude oils.For improving oil yield,, the oil cake that squeezes leached again get oil according to the condition of equipment and technology.The fatty acid component of the water wax gourd crude oil of obtaining in order to last method is: WT%
Palmitinic acid C
16: 0 13.9
Palm monoenoic acid C
16: 1 6.4
Stearic acid C
18: 0 1.2
Oleic acid C
18: 1 7.6
Linolic acid C
18: 2 67.8
Linolenic acid C
18: 3 1.3
Mountain Yu acid C
22: 0 0.3
Erucic acid C
22: 1 0.9
Because the place of production and the harvest season difference of water wax gourd, its component also has a little difference.The full oil of really squeezing out or leaching of water wax gourd tree is commonly called as crude oil, includes a large amount of impurity in the crude oil, comprises phosphatide, protein, phlegmatic temperament etc., and these grease peptized impurities must be rejected through refining.The water white gourd oil belongs to high acid value oil in addition, because the existence of free fatty acids wherein can influence the effect of refining and esterification, useless or deleterious composition must be removed, and carries out esterification then and produces biofuel.
Two, the refinery practice of water white gourd oil
1, technical process
Fig. 1 is seen in technical process
2, master operation key points for operation
(A) come unstuck
Get 1500 gram water wax gourd crude oils (about 1800 milliliters), amount of water is 30 grams, water wax gourd crude oil behind the sedimentation and filtration is put into 2000 ml beakers be heated to 50 ℃, begin to add water and stir, add in 7 minutes, continue stirring and stop after 20 minutes stirring, leave standstill insulation after 4 hours, oil obviously separates with soap stock (being commonly called as freight), takes out the oil sample check, and phosphorus content is 18 * 10
-6Mg/Kg.
(B) depickling
Get degummed oil 1282 grams, this oily acid number is 10, needs 18Be as calculated
-Sodium hydroxide lye 93 grams.Oily temperature is adjusted to 20 ℃, stir and add alkali, alkali lye added in 5 minutes, mixing speed is 70 rev/mins during beginning, is kept to 30 rev/mins after 17 minutes, simultaneously oily temperature is heated to 60 ℃, stop in the time of 30 minutes stirring, leave standstill insulation after 6 hours, oily soap obviously separates.You free fatty acid content is 0.2% after tested.
Oil after the soap stock separation is heated to 85 ℃, adds the light salt soft water of the 175 synthermal heat of gram, first pass is 1% light salt brine preferably, and spray is sprinkled upon on the pasta and stirred gently for 5 seconds, precipitates draining in 30 minutes.Second time, the 3rd time each wash with hot soft water 200 grams, after the draining oil is heated to 110 ℃, dewatered 30 minutes, and at this moment You water content reaches 0.04%, gets oily 1150 grams.
Three, esterification technique
With 1150 grams of the water wax gourd refining oil behind the drying and dehydrating, add methyl alcohol 151 grams, catalyzer sodium hydroxide 11.5 grams, catalyzer is added methanol mixed to be poured the water wax gourd refining oil that places 2000 milliliters of Erlenmeyer flasks to be preheating to 50 ℃ into and stirs heat temperature raising simultaneously, temperature remains on 55 ℃, reacts 30 minutes, stops to stir, heat to 80 ℃, steam residual methyl alcohol.Left standstill 30 minutes, light phase coarse biodiesel is separated with the heavy phase raw glycerine.Sodium hydroxide residue filtering in the heavy phase is promptly got raw glycerine.In light phase coarse biodiesel, add 8% dilute sulphuric acid, 120 grams, stir gently, then precipitation, discharge precipitation water, and then wash two times with about 50 ℃ warm water, drain water after, oil is heated to 110 ℃ of dehydrations 20 minutes, promptly gets limpid transparent biofuel 1140 grams, yield is 99.13%.
Embodiment 2
One, water wax gourd crude oil production technique is identical with embodiment 1.
Two, the refinery practice of water white gourd oil
(1) comes unstuck
Pressure oil expression 1500 grams (about 1800 milliliters), amount of water is 45 grams, and oily temperature is heated with stirring to 65 ℃, in 9 minutes after water injection, continue to stir, rotating speed is 60 rev/mins, stops after 30 minutes stirring, and leaves standstill insulation after 3 hours, oil obviously separates with soap stock, takes out the oil sample check, and phosphorus content is 15 * 10
-6Mg/Kg.
(2) depickling
Get degummed oil 1400 grams, this oily acid number is 10, needs 22Be as calculated
-Sodium hydroxide lye 80 grams.Oily temperature is adjusted to 30 ℃, stir and add alkali, alkali lye added in 10 minutes, mixing speed is 60 rev/mins during beginning, when continuing to be stirred to obvious oily soap and separating, rotating speed is reduced to 30 rev/mins, simultaneously with oily Wen Jiawen to 60 ℃, stop in the time of 30 minutes stirring, leave standstill insulation after 8 hours, oily soap obviously separates.Drawing oil sample and analyzing the fatty acid content that dissociates in the oil is 0.4%, for qualified.
Oil after the soap stock separation is heated to 85 ℃, adds 85 ℃ of light salt soft water 180 grams, stir gently, left standstill effluent then 30 minutes.Reusable heat soft water washing two times, divides dried up after, oil is heated to 110 ℃, dry 20 minutes, water content is that 0.05% refining oil 1200 restrains.
Three, esterification technique
Water wax gourd refining oil 1200 grams are inserted in 2000 milliliters of Erlenmeyer flasks, add methyl alcohol 181 grams, catalyzer sodium hydroxide 9.68 grams, mix and stir heat temperature raising simultaneously in the water wax gourd refining oil of pouring 40 ℃ into, temperature remains on 60 ℃, and stirring reaction 40 minutes stops to stir, heat to 80 ℃, steamed residual methyl alcohol in 20 minutes.Cooling was left standstill 60 minutes, and light phase coarse biodiesel is separated with the heavy phase raw glycerine.The bottom heavy phase is filtered to such an extent that sodium hydroxide residue 16 restrains, and gets raw glycerine 174 grams.In light phase coarse biodiesel, add 8% dilute sulphuric acid, 120 grams, stir gently, precipitate then, discharge precipitation water, and then wash two times with about 40 ℃ warm water, drain water after, biofuel is heated to 110 ℃, drying and dehydrating 20 minutes promptly gets water wax gourd methyl esters biofuel 1192 grams, and yield is 99.34%.
Embodiment 3
One, water wax gourd crude oil production technique is identical with embodiment 1.
Two, the refinery practice of water white gourd oil is identical with embodiment 2.
Three, esterification technique
Get the dried water wax gourd of refining refining oil 415 grams, add methyl alcohol 50 grams, catalyzer potassium hydroxide 2.08 grams, methyl alcohol and potassium hydroxide mixing are poured in 1000 milliliters of Erlenmeyer flasks adorning 415 gram water wax gourd refining oils, be warmed to 40 ℃, stirring reaction 60 minutes stops to stir, heat to 80 ℃, steam residual methyl alcohol.Cooling was left standstill 60 minutes, and light phase coarse biodiesel is separated with the heavy phase raw glycerine.With the potassium hydroxide residue filtering in the heavy phase of bottom, get raw glycerine 70 grams.In light phase coarse biodiesel, add 8% dilute sulphuric acid, 40 grams, washing, and then with about 50 ℃ warm water washing two times, drain water after, biofuel is heated to 120 ℃, after 20 minutes, promptly get water wax gourd methyl esters biofuel 411 and restrain, yield is 99.04%.
Above biofuel product by gas chromatographic analysis esterification rate greater than 97%, through national Research Institute of Petro-Chemical Engineering Analysis and Identification: density is 0.8885 in the time of 20 ℃, viscosity is 5.084 in the time of 40 ℃, flash-point＞170 ℃, sulphur content 1.3mg/L (being 1.46ppm), cetane value 45.6, cold filter clogging temperature are-7 ℃.These indexs obviously are better than the standard of GB GB252-2000 solar oil, particularly cold filter clogging temperature and are-7 ℃ not adding under the situation of any additives, in GB252-2000-10
#With-20
#Between the solar oil, such product is to solving the northern area of China winter-10
#With-20
#The serious situation in short supply of diesel oil will play active effect.
Claims (7)
1, a kind ofly prepare method of bio-diesel oil by the water white gourd oil, comprise refining of water white gourd oil and esterification technique, it is characterized in that: water white gourd oil refinery practice comprises the steps: water wax gourd fruit harvesting, dry, collection, after carrying out pre-treatment again and removing impurity, squeezing water outlet wax gourd crude oil, to precipitate, crude oil after the filtration is through coming unstuck, depickling, washing, obtain refining oil after the dehydration, esterification technique comprise the steps: with water wax gourd refining oil and Fatty Alcohol(C12-C14 and C12-C18) by 100: 10～20 mass ratioes under 40～70 ℃ of temperature and basic catalyst condition, stir carried out esterification in 30～60 minutes after, again through the distillation, filter, separate, washing, drying can make biofuel and glycerine.
2, water white gourd oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: described water wax gourd degumming raw oil operation steps is as follows: crude oil is heated with stirring to 50～65 ℃, the water that adds the same oil temperature of quality of crude oil 2～3%, stirred 20～40 minutes, precipitate 3～4 hours, detect phosphorus content less than 20 * 10
-6Mg/Kg.
3, water white gourd oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: described water wax gourd crude oil depickling operation steps is as follows: the water white gourd oil temperature after will coming unstuck is adjusted to 20～30 ℃, adds alkali lye, 18 ° of Be of concentration of lye
-～22 ° of Be
-, stirring 30～40 minutes, stirring velocity slows down gradually, and oil is warming up to 55～65 ℃ simultaneously, staticly settles 6～8 hours, and oily soap separates, and the test free fatty acid content is less than 0.5%.
4, water white gourd oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: described water wax gourd crude oil washs, the dehydration operation step is as follows: oily temperature is heated to 80～95 ℃, 10～20% synthermal water washings of adding oil quality 2～3 times, oily water separation, oil is heated to 100～110 ℃, dehydration, crude oil dehydration back Water in oil amount should be lower than 0.06%.
5, water white gourd oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: described water wax gourd crude oil is the full fruit oil of water wax gourd fruit.
6, water white gourd oil according to claim 1 prepares method of bio-diesel oil, it is characterized in that: described Fatty Alcohol(C12-C14 and C12-C18) is a methyl alcohol.
7, production water white gourd oil method of bio-diesel oil according to claim 1, it is characterized in that: described basic catalyst is sodium hydroxide or potassium hydroxide.
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| CNB2006100427375A CN100374529C (en) | 2006-04-26 | 2006-04-26 | Method for preparing biological diesel oil from saurauia tristyla var oldhamii oil |
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Cited By (6)
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| CN103131541A (en) * | 2013-03-11 | 2013-06-05 | 贵州大学 | Method for preparing biodiesel from Xanthium strumarium |
| CN103451009A (en) * | 2012-05-28 | 2013-12-18 | 中国石油天然气股份有限公司 | Preparation method of refined oil of inedible animal and plant crude oil |
| CN104031739A (en) * | 2014-06-17 | 2014-09-10 | 湖北民族学院 | Method for processing coptis chinensis seed oil and use thereof |
| CN104804877A (en) * | 2015-04-15 | 2015-07-29 | 上海应用技术学院 | Pure biodiesel and preparation method thereof |
| CN106635433A (en) * | 2016-12-20 | 2017-05-10 | 北京林业大学 | Lindera glauca biomass diesel manufacturing process |
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| CA2439577C (en) * | 2002-09-06 | 2011-05-31 | Fortum Oyj | Process for producing a hydrocarbon component of biological origin |
| CN1190471C (en) * | 2003-07-22 | 2005-02-23 | 清华大学 | Method for synthetizing biological diesel oil by oil and fat materials |
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| CN103451009A (en) * | 2012-05-28 | 2013-12-18 | 中国石油天然气股份有限公司 | Preparation method of refined oil of inedible animal and plant crude oil |
| CN103451009B (en) * | 2012-05-28 | 2015-05-20 | 中国石油天然气股份有限公司 | Preparation method of refined oil of inedible animal and plant crude oil |
| CN103131541A (en) * | 2013-03-11 | 2013-06-05 | 贵州大学 | Method for preparing biodiesel from Xanthium strumarium |
| CN104031739A (en) * | 2014-06-17 | 2014-09-10 | 湖北民族学院 | Method for processing coptis chinensis seed oil and use thereof |
| CN104031739B (en) * | 2014-06-17 | 2016-04-20 | 湖北民族学院 | A kind of working method of coptis seed oil and purposes |
| CN104804877A (en) * | 2015-04-15 | 2015-07-29 | 上海应用技术学院 | Pure biodiesel and preparation method thereof |
| CN106635433A (en) * | 2016-12-20 | 2017-05-10 | 北京林业大学 | Lindera glauca biomass diesel manufacturing process |
| CN107267285A (en) * | 2017-08-14 | 2017-10-20 | 宿松县春江粮油有限公司 | A kind of Rice oil alkali-refining deacidification method of utilization oxalic acid auxiliary degumming |
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