CN107034025A - A kind of supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state - Google Patents
A kind of supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state Download PDFInfo
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- CN107034025A CN107034025A CN201710282551.5A CN201710282551A CN107034025A CN 107034025 A CN107034025 A CN 107034025A CN 201710282551 A CN201710282551 A CN 201710282551A CN 107034025 A CN107034025 A CN 107034025A
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- oil
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- nickel catalyst
- supercritical
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/12—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation
- C11C3/123—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by hydrogenation using catalysts based principally on nickel or derivates
Abstract
The present invention provides a kind of supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, when carbon dioxide reaches supercriticality, larger solvability can be shown, substantially reduce the resistance to mass tranfer of catalyst reaction process and then improve catalyst reaction speed, shorten reaction time and environment will not be polluted, simultaneously because the unique surface texture of nano nickel, hydrogen can be adsorbed to greatest extent and then catalytic efficiency is improved.By in supercritical carbon dioxide (SC CO2) under state, hydrogenation is carried out using nano nickel catalyst catalysis and one-level soybean oil and prepares hydrogenated oil and fat, reduction hydrogenated oil and fat content of trans fatty acids is realized.Present invention optimizes hydrogenation technology parameyers such as nano nickel catalyst consumption, reaction time, reaction pressure and reaction temperatures, reacted under the optimal condition, content of trans fatty acids can be reduced to 8.12% in hydrogenated oil and fat.
Description
Technical field
The invention belongs to edible oil and fat refining manufacture field, and in particular in supercritical CO2Under state, urged using nano nickel
The method that agent hydrogenation one-level soybean oil reaction prepares hydrogenated oil and fat.
Background technology
HYDROGENATION OF OILS AND FATS is the chemical process of oil modification, i.e., make catalyst using metals such as reproducibility nickel, hydrogen is added to
In triglycerides in the double bond of unrighted acid, the modified grease of gained is referred to as hydrogenated oil and fat.HYDROGENATION OF OILS AND FATS can reduce grease
Degree of unsaturation, raising fusing point, the content of increase hard fat；Grease is improved to oxygen and the stability of heat；Improve the color of grease
Pool, fragrance and local flavor etc..
Industrial production hydrogenated oil and fat is all to be carried out under normal conditions using nickel-base catalyst, and catalyst is hydrogenation
One of key condition, conventional industrial hydrogenation catalyst hydrogenated oil and fat can produce substantial amounts of trans-fatty acid.Research shows, trans
Aliphatic acid can increase LDL-C, reduce the HDL-C beneficial to human body, increase heart disease
With the occurrence probability of obesity；It also can result in tumour, the disease such as breast cancer and senile dementia, already as related neck in recent years
The focus of domain concern.
Nano nickel catalyst particle diameter is general in 1-l00nm, with specific surface area is big, surface atom and number of active center
Mesh is more, high catalytic efficiency and the features such as special selecting catalytic performance, and the adsorbable more hydrogen of nano nickel catalyst can avoid urging
Agent adsorption hydrogen deficient and cause the formation of trans-fatty acid,
Supercritical CO2Nano nickel catalyst oil with hydrogenated soybean is applied under state so that soybean oil is in supercritical CO2In fluid
Solubility it is big, and supercritical CO2The mass transfer rate of fluid is high, and then soybean oil is fully contacted with catalyst and hydrogen,
The probability for producing trans-fatty acid is reduced, and the speed of hydrogenation can be improved, the reaction time is greatly shortened.These features make
Its application in food industry has vast potential for future development.
The content of the invention
It is big it is an object of the invention to solve in Content in Hydrogenated Edible Oils to produce due to the limitation of catalyst and reaction condition
The problem of measuring trans-fatty acid, a large amount of intakes of trans-fatty acid can cause the generation of heart disease and obesity；It also can result in
The diseases such as tumour, breast cancer and senile dementia, the health of the serious infringement mankind.Existing HYDROGENATION OF OILS AND FATS method reaction temperature is high,
Time is long, and can produce substantial amounts of trans-fatty acid, and by supercritical carbon dioxide (SC-CO2) under state, using nanometer
Raney nickel prepares hydrogenated oil and fat with one-level soybean oil reaction, can substantially reduce reaction temperature, shortens the reaction time, makes hydrogen
Gas, nano nickel catalyst and soybean oil are fully contacted, and then reduce the generation of trans-fatty acid.Use supercritical CO2Should under state
Realized with the method for nano nickel catalyst oil with hydrogenated soybean by following steps：First, pre-treatment is reacted；2nd, hydrogenation；3rd,
Terminating reaction；4th, using the content of trans fatty acids of gas Chromatographic Determination hydrogenated oil and fat,
In supercritical CO2Using during nano nickel catalyst oil with hydrogenated soybean under state, due to the unique table of nano nickel
The adsorbable more hydrogen of face structure, and fluid carbon dioxide can substantially reduce the mass transfer resistance of course of reaction under supercriticality
Power, improves reaction rate, reduces reaction temperature, shortens reaction time, and then reduces the generation of trans-fatty acid.The present invention is stable
Property it is high, can be operated continuously for a long time, large-scale plant production can be carried out.
Embodiment：
Embodiment one：A kind of supercritical CO2Lead under state using the method for nano nickel catalyst oil with hydrogenated soybean
Cross following steps realization：First, pre-treatment is reacted：By a certain amount of nano nickel catalyst and a certain amount of one-level soybean oil and it is added to
In reactor, CO is poured after being put into rotor, sealing reactor2Ventilation two to three times, to ensure thoroughly to displace in dereaction kettle
Air, while reaction is placed in water into leak test；2nd, hydrogenation：CO is filled with the case of ensureing that reactor is sealed2, so
After be passed through H21MPa-5MPa makes gross pressure in reactor reach 12MPa, nano nickel catalyst consumption 0.05%-0.25%, will be anti-
Kettle is answered to be placed in thermostatical oil bath, in 70-110 DEG C of temperature, regulation rotating speed is 100r/min-500r/min, reacts 70min-
Product is obtained after 110min；3rd, terminating reaction：Reactor is taken out from oil bath pan, normal temperature is down to, CO in reactor is released2
And H2To normal pressure, the total material in reactor is taken out, separating catalyst and hydrogenated oil and fat, so as to obtain hydrogenated oil and fat production
Product；4th, the content of trans fatty acids of gas Chromatographic Determination hydrogenated oil and fat is utilized.
Embodiment two：Difference of the present embodiment from embodiment one is in step one to ensure anti-
H is filled with the case of answering kettle sealed21-5MPa causes the pressure in reactor to reach 12MPa, carries out hydrogenation.Other steps
It is identical with embodiment one.
Embodiment three：The difference of present embodiment and embodiment one is in step 2 to select nanometer
Under conditions of the addition of Raney nickel is 0.10%-0.20%, hydrogenation, other steps and embodiment are carried out
One is identical.
Embodiment four：Difference of the present embodiment from embodiment one is step 2 selection reaction temperature
Hydrogenation is carried out under the conditions of respectively 80-100 DEG C of degree, other steps are identical with embodiment one.
Embodiment five：Difference of the present embodiment from embodiment one is to select to stir in step 2
Speed is carries out hydrogenation under the conditions of 200r/min-400r/min, and other steps are identical with embodiment one.
Embodiment six：Difference of the present embodiment from embodiment one is to select to react in step 2
Time, other steps were identical with embodiment one to carry out hydrogenation under the conditions of 80min-100min.
Claims (6)
1. one kind is in supercritical CO2Under state, the side of hydrogenated oil and fat is prepared using nano nickel catalyst and one-level soybean oil reaction
Method, it is characterised in that one kind is in supercritical CO2Pass through following step using the method for nano nickel catalyst oil with hydrogenated soybean under state
It is rapid to realize：First, by 0.05%-0.25% (oil weight) nano nickel catalyst and 50g one-levels soybean oil and it is added in reactor,
CO is poured after being put into rotor, sealing reactor2Ventilation two to three times, to ensure thoroughly to displace the air in dereaction kettle, together
When reaction is placed in water leak test；2nd, it is filled with CO in the case of ensureing that reactor is sealed2, then pass to H21MPa-5MPa makes
Gross pressure reaches 12MPa in reactor, and reactor is placed in thermostatical oil bath, and in 70-110 DEG C of temperature, regulation rotating speed is
Product is obtained after 100r/min-500r/min, reaction 70min-110min；3rd, reactor is taken out from oil bath pan, be down to often
Temperature, releases CO in reactor2And H2To normal pressure, the total material in reactor is taken out, catalyst and hydrogenated oil and fat is centrifuged
Fat, so as to obtain hydrogenated oil and fat product.
2. it is according to claim 1 in supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, its
It is characterised by step 1 0.10%-0.20% (oil weight) nano nickel catalyst being added in reactor.
3. it is according to claim 1 in supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, its
It is characterised by ensureing to be filled with H in the case of reactor is sealed in step 222MPa-4MPa, remaining is filled with CO2So that in reactor
Pressure reach 12MPa, carry out hydrogenation.
4. it is according to claim 1 in supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, its
It is characterised by step 2 reactor being placed in thermostatical oil bath, under the conditions of 80-100 DEG C of reaction temperature, progress hydrogenates anti-
Should.
5. it is according to claim 1 in supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, its
It is characterised by step 2 reactor being placed in thermostatical oil bath, in 80-100 DEG C of reaction temperature, speed of agitator is 200r/
Under the conditions of min-400r/min, hydrogenation is carried out.
6. it is according to claim 1 in supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state, its
It is characterised by selecting in step 2 entering hydrogenation under the conditions of reaction time 80-100min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710282551.5A CN107034025A (en) | 2017-04-26 | 2017-04-26 | A kind of supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710282551.5A CN107034025A (en) | 2017-04-26 | 2017-04-26 | A kind of supercritical CO2The method that nano nickel catalyst oil with hydrogenated soybean is applied under state |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422199A (en) * | 2008-09-04 | 2009-05-06 | 东北农业大学 | Wheat germ oil hydrogenation method using supercritical CO2 as dissolvent |
| US20110028773A1 (en) * | 2009-07-29 | 2011-02-03 | Bala Subramaniam | Deoxygenation of Bio-Oils and Other Compounds to Hydrocarbons in Supercritical Media |
| CN103431074A (en) * | 2013-07-23 | 2013-12-11 | 东北农业大学 | Method for hydrogenating sunflower seed oil by supercritical CO2 |
-
2017
- 2017-04-26 CN CN201710282551.5A patent/CN107034025A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422199A (en) * | 2008-09-04 | 2009-05-06 | 东北农业大学 | Wheat germ oil hydrogenation method using supercritical CO2 as dissolvent |
| US20110028773A1 (en) * | 2009-07-29 | 2011-02-03 | Bala Subramaniam | Deoxygenation of Bio-Oils and Other Compounds to Hydrocarbons in Supercritical Media |
| CN103431074A (en) * | 2013-07-23 | 2013-12-11 | 东北农业大学 | Method for hydrogenating sunflower seed oil by supercritical CO2 |
Non-Patent Citations (2)
| Title |
|---|
| JERRY W. KING ET AL: "Hydrogenation of Vegetable Oils Using Mixtures of Supercritical Carbon Dioxide and Hydrogen", 《JOURNAL OF THE AMERICAN OIL CHEMISTS’S SOCIETY》 * |
| 霍静等: "纳米镍加氢催化剂的研究现状与展望", 《粉末冶金工业》 * |
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Application publication date: 20170811 |