CN101255344A - Method for co-production of bio-diesel and vitamin E, phytosterol by using plant oil - Google Patents
Method for co-production of bio-diesel and vitamin E, phytosterol by using plant oil Download PDFInfo
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- CN101255344A CN101255344A CNA2007100516000A CN200710051600A CN101255344A CN 101255344 A CN101255344 A CN 101255344A CN A2007100516000 A CNA2007100516000 A CN A2007100516000A CN 200710051600 A CN200710051600 A CN 200710051600A CN 101255344 A CN101255344 A CN 101255344A
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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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- 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
- 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
Abstract
The invention proposes a biological diesel and vitamin E, sterol combined production by vegetable fat, which pertains to oil chemistry field. The invention process includes steps of degumming, methyl esterification, water washing, cold precipitation, dehydration, molecular distillation. The invention uses vegetable fat as raw material, directly esterify triglyceride and free fatty acids together without refining step, and adopt molecular distillation to obtain biological diesel and natural vitamin E, sterol simultaneously, which is a novel production process that simplify procedures, reduces production cost and increases economic benefit.
Description
Technical field
The present invention relates to the method for a kind of usefulness Vegetable oil lipoprotein co-producing biodiesel and vitamin-E, sterol, belong to field of grease chemical technology.
Background technology
Biofuel more and more is subject to people's attention with its unique feature of environmental protection and reproducibility.Mainly produce thing diesel oil next life for raw material both at home and abroad at present with the animal-plant oil.All reported with the animal-plant oil to be the raw material production method of bio-diesel oil as CN1238468C, CN1181161C, CN1197937C, CN1626621A etc., but aforesaid method is not all considered the comprehensive utilization of vitamin-E in the Vegetable oil lipoprotein, sterol.
It is raw material that the production of natural VE, sterol both at home and abroad at present mainly slips out thing with the deodorization of vegetable oil and fat refining by product.All reported with the deodorization distillate to be the method for raw material production vitamin-E and sterol as CN1418877A, CN1108299C, CN1037769C etc.But it is loaded down with trivial details that deodorization slips out the reparation technology of thing, and promptly Vegetable oil lipoprotein needs a plurality of operations such as strict process is come unstuck, depickling, decolouring, deodorization just can obtain, and has complex process, and flow process is immutable, problems such as energy consumption height.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that can utilize Vegetable oil lipoprotein co-producing biodiesel and vitamin-E, sterol, and this production method has characteristics such as technology is simple, production cost is low, good in economic efficiency.
The present invention for the technical scheme that problem adopted of the above-mentioned proposition of solution is:
(1) come unstuck: after Vegetable oil lipoprotein is heated to 80～95 ℃, add 80～95 ℃ of hot water, consumption is 10～30% (weight) of Vegetable oil lipoprotein consumption, after stirring is mixed, separates oil foot and grease.
(2) esterification: according to the content of triglyceride level in the Vegetable oil lipoprotein and free fatty acids, calculate the theoretical methanol consumption, actual add-on is 3-7 a times of theoretical amount: add the vitriol oil and make catalyzer, consumption is the 3-20% (weight) of methanol usage, and (65-85 ℃) reaction is 2～6 hours under stirring and reflux temperature.
(3) washing: above-mentioned material is added entry, and consumption is 1～5 times (weight) of methanol usage, and standing demix removes mixed phase such as sub-cloud glycerine, methyl alcohol, water, sulfuric acid, and the hot wash 1～3 time of using 80～98 ℃ again is to neutral.
(4) cold analysis: the material after will washing carries out cold analysis, under agitation is quickly cooled to-5～5 ℃, is incubated 5～20 hours, and most sterols are separated out.The sterol washing with acetone of separating out, oven dry again gets white sterol product.
(5) dehydration: with the material after the cold analysis vacuum tightness be under 400～2000Pa and temperature be to carry out processed under 95～115 ℃.
(6) molecular distillation: the material after will dewatering under different temperature and the vacuum condition carries out the level Four molecular distillation, and conditions at different levels are as follows: 1. one-level :-0.05～-0.099M Pa, 100～115 ℃; 2. secondary: 5～150Pa, 130～180 ℃; 3. three grades: 0.5～5Pa, 150～170 ℃; 4. level Four: 0.5～5Pa, 170～190 ℃.Obtaining fatty acid methyl ester at secondary is biofuel, and three grades of overhead products return secondary and distill once more, and level Four obtains natural VE.
Beneficial effect of the present invention is:
(1) production technique is simple, the present invention is directly with vegetable fat methyl esterization, can be simultaneously triglyceride level in the Vegetable oil lipoprotein and free fatty acids esterification together, and to adopt molecular distillation technology to obtain the good fatty acid methyl ester of quality be biofuel, saved operations such as neutralization after the esterification of existing production of biodiesel technology, washing; Adopt cold analysis to obtain sterol, in molecular distillation, obtain natural VE after the esterification, avoided existing technology must through coming unstuck, a plurality of refining procedures such as depickling, decolouring, deodorization obtain deodorization distillate, the loaded down with trivial details operation of sterol, vitamin-E is produced in regeneration;
(2) utilize Vegetable oil lipoprotein to be raw material, but not only production biofuel also can obtain high value added products such as natural VE, sterol, has improved economic benefit.
The advantage of the technology of the present invention is significantly, is raw material with the Vegetable oil lipoprotein, without refining procedure, directly esterification, and adopt molecular distillation to obtain biofuel and natural VE, sterol simultaneously, simplified technical process, improved economic benefit, thereby made the present technique economy better.
Embodiment
The present invention is described further below in conjunction with specific embodiment.
Embodiment 1:
(1) come unstuck, soybean oil is heated to 85 ℃ after, add 90 ℃ of hot water, consumption is 10% (weight) of Vegetable oil lipoprotein consumption, stir mixed after, separate oil foot and grease.
(2) esterification, by weight with grease: methyl alcohol: the vitriol oil is 40: 6: 1, is 70 ℃ of following reactions 4 hours in stirring and reflux temperature.
(3) washing adds entry with above-mentioned material, and consumption is 3 times (weight) of methanol usage, and standing demix removes mixed phase such as sub-cloud glycerine, methyl alcohol, water, sulfuric acid, and the hot wash 2 times of using 95 ℃ again is to neutral.
(4) cold analysis is carried out cold analysis with the material after the washing, under agitation is quickly cooled to 1 ℃, is incubated 20 hours, and most sterols are separated out.The sterol washing with acetone of separating out, oven dry again gets white sterol product.
(5) dehydration, with the material after the cold analysis vacuum tightness be under the 500Pa and temperature be to carry out processed under 105 ℃.
(6) molecular distillation, the material after will dewatering under different temperature and the vacuum condition carries out the level Four molecular distillation, and conditions at different levels are as follows: 1. one-level: 8-0.08M Pa, 105 ℃; 2. secondary: 100Pa, 150 ℃; 3. three grades: 4Pa, 165 ℃; 4. level Four: 2Pa, 180 ℃.Obtaining fatty acid methyl ester at secondary is biofuel, and three grades of overhead products return secondary and distill once more, and level Four obtains natural VE.
Embodiment 2:
(1) come unstuck, rapeseed oil is heated to 80 ℃ after, add 95 ℃ of hot water, consumption is 15% (weight) of Vegetable oil lipoprotein consumption, stir mixed after, separate oil foot and grease.
(2) esterification, by weight with grease: methyl alcohol: the vitriol oil is 200: 30: 6, is 70 ℃ of following reactions 4.5 hours in stirring and reflux temperature.
(3) washing adds entry with above-mentioned material, and consumption is 2.5 times (weight) of methanol usage, and standing demix removes mixed phase such as sub-cloud glycerine, methyl alcohol, water, sulfuric acid, and the hot wash 1 time of using 90 ℃ again is to neutral.
(4) cold analysis is carried out cold analysis with the material after the washing, under agitation is quickly cooled to-1 ℃, is incubated 20 hours, and most sterols are separated out.The sterol washing with acetone of separating out, oven dry again gets white sterol product.
(5) dehydration, with the material after the cold analysis vacuum tightness be under the 1000Pa and temperature be to carry out processed under 110 ℃.
(6) molecular distillation, the material after will dewatering under different temperature and the vacuum condition carries out the level Four molecular distillation, and conditions at different levels are as follows: 1. one-level :-0.099M Pa, 110 ℃; 2. secondary: 120Pa, 160 ℃; 3. three grades: 3Pa, 160 ℃; 4. level Four: 1Pa, 175 ℃.Obtaining fatty acid methyl ester at secondary is biofuel, and three grades of overhead products return secondary and distill once more, and level Four obtains natural VE.
Embodiment 3:
(1) come unstuck, Oleum Gossypii semen is heated to 90 ℃ after, add 93 ℃ of hot water, consumption is 20% (weight) of Vegetable oil lipoprotein consumption, stir mixed after, separate oil foot and grease.
(2) esterification, by weight with grease: methyl alcohol: the vitriol oil is 180: 30: 5, is 67 ℃ of following reactions 5 hours in stirring and reflux temperature.
(3) washing adds entry with above-mentioned material, and consumption is 3 times (weight) of methanol usage, and standing demix removes mixed phase such as sub-cloud glycerine, methyl alcohol, water, sulfuric acid, and the hot wash 2 times of using 88 ℃ again is to neutral.
(4) cold analysis is carried out cold analysis with the material after the washing, under agitation is quickly cooled to 2 ℃, is incubated 18 hours, and most sterols are separated out.The sterol washing with acetone of separating out, oven dry again gets white sterol product.
(5) dehydration, with the material after the cold analysis vacuum tightness be under the 1500Pa and temperature be to carry out processed under 115 ℃.
(6) molecular distillation, the material after will dewatering under different temperature and the vacuum condition carries out the level Four molecular distillation, and conditions at different levels are as follows: 1. one-level :-0.09M Pa, 112 ℃; 2. secondary: 50Pa, 140 ℃; 3. three grades: 5Pa, 170 ℃; 4. level Four: 2Pa, 185 ℃.Obtaining fatty acid methyl ester at secondary is biofuel, and three grades of overhead products return secondary and distill once more, and level Four obtains natural VE.
Claims (1)
1. method of utilizing Vegetable oil lipoprotein co-producing biodiesel and vitamin-E, sterol is characterized in that technological process is made up of following each step:
(1) come unstuck: after Vegetable oil lipoprotein is heated to 80～95 ℃, add 80～95 ℃ of hot water, consumption is 10～30% (weight) of Vegetable oil lipoprotein consumption, after stirring is mixed, separates oil foot and grease.
(2) esterification: according to the content of triglyceride level in the Vegetable oil lipoprotein and free fatty acids, calculate the theoretical methanol consumption, actual add-on is 3-7 a times of theoretical amount; Add the vitriol oil and make catalyzer, consumption is the 3-20% (weight) of methanol usage, and (65-85 ℃) reaction is 2～6 hours under stirring and reflux temperature.
(3) washing: above-mentioned material is added entry, and consumption is 1～5 times (weight) of methanol usage, and standing demix removes mixed phase such as sub-cloud glycerine, methyl alcohol, water, sulfuric acid, and the hot wash 1～3 time of using 80～98 ℃ again is to neutral.
(4) cold analysis: the material after will washing carries out cold analysis, under agitation is quickly cooled to-5～5 ℃, is incubated 5～20 hours, and most sterols are separated out.The sterol washing with acetone of separating out, oven dry again gets white sterol product.
(5) dehydration: with the material after the cold analysis vacuum tightness be under 400～2000Pa and temperature be to carry out processed under 95～115 ℃.
(6) molecular distillation: the material after will dewatering under different temperature and the vacuum condition carries out the level Four molecular distillation, and conditions at different levels are as follows: 1. one-level :-0.05～-0.099MPa, 100～115 ℃; 2. secondary: 5～150Pa, 130～180 ℃; 3. three grades: 0.5～5Pa, 150～170 ℃; 4. level Four: 0.5～5Pa, 170～190 ℃.Obtaining fatty acid methyl ester at secondary is biofuel, and three grades of overhead products return secondary and distill once more, and level Four obtains natural VE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100516000A CN101255344A (en) | 2007-03-02 | 2007-03-02 | Method for co-production of bio-diesel and vitamin E, phytosterol by using plant oil |
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| CNA2007100516000A CN101255344A (en) | 2007-03-02 | 2007-03-02 | Method for co-production of bio-diesel and vitamin E, phytosterol by using plant oil |
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| CN101255344A true CN101255344A (en) | 2008-09-03 |
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| CNA2007100516000A Pending CN101255344A (en) | 2007-03-02 | 2007-03-02 | Method for co-production of bio-diesel and vitamin E, phytosterol by using plant oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942007A (en) * | 2010-08-23 | 2011-01-12 | 秦皇岛领先科技发展有限公司 | Method for extracting phytosterol from waste residues generated in biodiesel production and product thereof |
| CN103045664A (en) * | 2012-12-15 | 2013-04-17 | 华中科技大学 | Method for producing biodiesel, sterol and vitamin E from deodorized distillate |
| CN104861036A (en) * | 2014-02-24 | 2015-08-26 | 上海兰蒂斯生物医药科技有限公司 | Extract for prevention and treatment of prostatic diseases and preparation method thereof |
| CN105585553A (en) * | 2014-11-18 | 2016-05-18 | 陕西秦岭生物工程有限公司 | Natural tocopherol extract method |
| CN107722093A (en) * | 2017-09-28 | 2018-02-23 | 沧州市宝来金康生物科技股份有限公司 | A kind of new technology that sterol ester is extracted from plant oil deodorizing distillate |
| CN110028476A (en) * | 2019-04-29 | 2019-07-19 | 吉林绿博士生态科技发展有限公司 | A kind of method of continuously extracting natural VE, phytosterol, fatty acid methyl ester |
| CN111849628A (en) * | 2020-07-28 | 2020-10-30 | 宜春大海龟生命科学有限公司 | Method for treating rice bran acidification oil |
-
2007
- 2007-03-02 CN CNA2007100516000A patent/CN101255344A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942007A (en) * | 2010-08-23 | 2011-01-12 | 秦皇岛领先科技发展有限公司 | Method for extracting phytosterol from waste residues generated in biodiesel production and product thereof |
| CN103045664A (en) * | 2012-12-15 | 2013-04-17 | 华中科技大学 | Method for producing biodiesel, sterol and vitamin E from deodorized distillate |
| CN104861036A (en) * | 2014-02-24 | 2015-08-26 | 上海兰蒂斯生物医药科技有限公司 | Extract for prevention and treatment of prostatic diseases and preparation method thereof |
| CN105585553A (en) * | 2014-11-18 | 2016-05-18 | 陕西秦岭生物工程有限公司 | Natural tocopherol extract method |
| CN107722093A (en) * | 2017-09-28 | 2018-02-23 | 沧州市宝来金康生物科技股份有限公司 | A kind of new technology that sterol ester is extracted from plant oil deodorizing distillate |
| CN110028476A (en) * | 2019-04-29 | 2019-07-19 | 吉林绿博士生态科技发展有限公司 | A kind of method of continuously extracting natural VE, phytosterol, fatty acid methyl ester |
| CN111849628A (en) * | 2020-07-28 | 2020-10-30 | 宜春大海龟生命科学有限公司 | Method for treating rice bran acidification oil |
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Open date: 20080903 |