CN106906052A - A kind of new method for preparing vegetable fatty acetoacetic ester - Google Patents
A kind of new method for preparing vegetable fatty acetoacetic ester Download PDFInfo
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- CN106906052A CN106906052A CN201710169201.8A CN201710169201A CN106906052A CN 106906052 A CN106906052 A CN 106906052A CN 201710169201 A CN201710169201 A CN 201710169201A CN 106906052 A CN106906052 A CN 106906052A
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- oil
- koh
- acetoacetic ester
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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
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to a kind of new method for preparing vegetable fatty acetoacetic ester, comprise the following steps：（1）Take vegetable oil and be preheated to 65~75 DEG C；（2）Take KOH to be put into absolute ethyl alcohol, and KOH is completely dissolved in absolute ethyl alcohol using ultrasonication, obtain KOH ethanol solutions；（3）Preheated vegetable oil is mixed with KOH ethanol solutions, equipment of Hydrodynamic Cavitation 10~30min of circular response under the conditions of 65~75 DEG C is then connected；（4）After reaction terminates, the pH value of product is adjusted to neutral, 25~35min is rotated under the conditions of 65~75 DEG C, obtain vegetable fatty acetoacetic ester.The present invention prepares fatty-acid ethyl ester with vegetable oil as main raw material(s) using Hydrodynamic Cavitation Technology, prepares that effect is good, and with easy to use, low cost, small investment can effectively improve reaction rate, reduce the reaction time, the advantages of lower energy consumption.
Description
Technical field
The present invention relates to a kind of new method for preparing vegetable fatty acetoacetic ester.
Background technology
Fatty-acid ethyl ester is to react generation, that is, ethyl ester biodiesel using ethanol and grease.Biodiesel is used as stone
Oily diesel oil substitute, is a class from the obtained energy of each quasi-grease reaction, and is typical " green energy resource " at present, to the energy
The contemporary society for starting shortage brings hope.And, being contrasted with traditional petroleum diesel, biodiesel is biodegradable, right
The pollution of environment is few, and the discharge capacity especially for pollutants such as carbon dioxide, sulfide, dust is than relatively low, so greatly
Power research and development biodiesel is significant.
At present, the conventional method of fatty-acid ethyl ester is paddling process, and reaction speed is easily influenceed by mixing speed, works as product
Measure big reaction vessel it is big when, it is uneven so as to the situation for causing reaction rate to decline easily to occur local mixing during stirring,
Have impact on industrialization, scale process.
The content of the invention
The technical problem to be solved in the present invention is：A kind of new method for preparing vegetable fatty acetoacetic ester, the method are provided
With vegetable oil as main raw material(s), Hydrodynamic Cavitation Technology is used in the preparation process of vegetable fatty acetoacetic ester, effectively contracted
Short preparation time, improves reaction efficiency.
Solving the technical scheme of above-mentioned technical problem is：A kind of new method for preparing vegetable fatty acetoacetic ester, including with
Lower step：
（1）Take vegetable oil and be preheated to 65~75 DEG C；
（2）It is the 1~1.5% of plant weight of oil by KOH weight, absolute ethyl alcohol is 9.5~10.5: 1 with the mol ratio of vegetable oil
Meter, takes KOH and is put into absolute ethyl alcohol, and KOH is completely dissolved in absolute ethyl alcohol using ultrasonication, obtains KOH ethanol molten
Liquid；
（3）Preheated vegetable oil is mixed with KOH ethanol solutions, equipment of Hydrodynamic Cavitation is then connected under the conditions of 65~75 DEG C
10~30min of circular response；
（4）After reaction terminates, the pH value of product is adjusted to neutral, 25~35min is rotated under the conditions of 65~75 DEG C, obtain plant
Oil fatty acid ethyl ester.
Step（2）The time of middle ultrasonication is 4min~6min, and the power of ultrasonic wave is 150~250W.
Step（4）In for adjusting the material of pH value be hydrochloric acid.
Described vegetable oil is tea-seed oil, rapeseed oil, cottonseed oil, soybean oil or palm oil.
Hydrodynamic cavitation technology has excellent reinforcing reaction effect, while there is capacity usage ratio higher, for equipment
Damage it is small, the features such as continuous prodution can be reached, be widely used at present in strengthening some physics, chemical process.This hair
Bright is a kind of to prepare the new technical method of vegetable fatty acetoacetic ester, it is adaptable to edible vegetable oil such as tea-seed oil, rapeseed oil, cottonseed
The vegetable fat such as oil, soybean oil or palm oil, fatty-acid ethyl ester is prepared by using Hydrodynamic Cavitation Technology, and preparation effect is good, tool
Have easy to use, low cost, small investment can effectively improve reaction rate, reduce the reaction time, the advantages of lower energy consumption.
Specific embodiment
Embodiment 1：A kind of new method for preparing vegetable fatty acetoacetic ester, comprises the following steps：
（1）The cottonseed oil for taking 50g is preheated to 70 DEG C in thermostat water bath.
（2）Weigh a certain amount of KOH（The 1.25% of cottonseed weight of oil）It is put into a certain amount of absolute ethyl alcohol for weighing up（Anhydrous second
Alcohol is 10 with cottonseed molar equivalent:1）In, and KOH is completely dissolved in ethanol using ultrasonication 4min~6min, ultrasound
The power of ripple is 200W.
（3）By preheated cottonseed oil with the KOH and absolute ethyl alcohol dissolved with ultrasonic wave while pouring into three mouthfuls of 250ml
Flask, then connects at equipment of Hydrodynamic Cavitation circulates 70 DEG C and reacts 15min.
（4）After reaction terminates, the watery hydrochloric acid that 0.5mol/L is added dropwise is used for adjusting the pH value of product to neutral, in 70 DEG C of revolvings
30min obtains vegetable fatty acetoacetic ester.
Fatty-acid ethyl ester preparation is carried out using traditional paddling process under equal conditions（I.e. compared with Example 1, step（2）In
Eliminate ultrasonication operation, step（3）Course of reaction be to be carried out in common unit, be provided without equipment of Hydrodynamic Cavitation）,
Concrete outcome is as shown in the table.
As can be seen from the above table, when carrying out fatty-acid ethyl ester preparation using paddling process under equal conditions, hydroxyl value is in 30min
When reach peak, now hydroxyl value is 176.87mgKOH/g, but the present invention prepares fatty-acid ethyl ester using Hydrodynamic Cavitation Technology
When, reaction 15min hydroxyl values reach 183.09mgKOH/g.It can be seen that the present invention prepares fatty-acid ethyl ester using Hydrodynamic Cavitation Technology,
Not only prepare effect good, and preparation time can be significantly reduced, reaction rate is effectively improved, while improve yield
（The bigger yield for representing fatty-acid ethyl ester of hydroxyl value is higher in product）.
Raw material of the present invention is, with vegetable oil as primary raw material, in addition to using cottonseed oil, can also to use tea-seed oil, vegetable seed
Other edible oils such as oil, soybean oil or palm oil.
Equipment of Hydrodynamic Cavitation of the present invention is common equipment of Hydrodynamic Cavitation, such as Venturi tube, therefore herein not
The concrete structure of equipment of Hydrodynamic Cavitation is repeated again.
Claims (4)
1. a kind of new method for preparing vegetable fatty acetoacetic ester, it is characterised in that：Comprise the following steps：
（1）Take vegetable oil and be preheated to 65~75 DEG C；
（2）It is the 1~1.5% of plant weight of oil by KOH weight, absolute ethyl alcohol is 9.5~10.5: 1 with the mol ratio of vegetable oil
Meter, takes KOH and is put into absolute ethyl alcohol, and KOH is completely dissolved in absolute ethyl alcohol using ultrasonication, obtains KOH ethanol molten
Liquid；
（3）Preheated vegetable oil is mixed with KOH ethanol solutions, equipment of Hydrodynamic Cavitation is then connected under the conditions of 65~75 DEG C
10~30min of circular response；
（4）After reaction terminates, the pH value of product is adjusted to neutral, 25~35min is rotated under the conditions of 65~75 DEG C, obtain plant
Oil fatty acid ethyl ester.
2. a kind of new method for preparing vegetable fatty acetoacetic ester according to claim 1, it is characterised in that：Step（2）
The time of middle ultrasonication is 4min~6min, and the power of ultrasonic wave is 150~250W.
3. a kind of new method for preparing vegetable fatty acetoacetic ester according to claim 1 and 2, it is characterised in that：Step
（4）In for adjusting the material of pH value be hydrochloric acid.
4. a kind of new method for preparing vegetable fatty acetoacetic ester according to claim 1 and 2, it is characterised in that：It is described
Vegetable oil be tea-seed oil, rapeseed oil, cottonseed oil, soybean oil or palm oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710169201.8A CN106906052A (en) | 2017-03-21 | 2017-03-21 | A kind of new method for preparing vegetable fatty acetoacetic ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710169201.8A CN106906052A (en) | 2017-03-21 | 2017-03-21 | A kind of new method for preparing vegetable fatty acetoacetic ester |
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| Publication Number | Publication Date |
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| CN106906052A true CN106906052A (en) | 2017-06-30 |
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| CN201710169201.8A Pending CN106906052A (en) | 2017-03-21 | 2017-03-21 | A kind of new method for preparing vegetable fatty acetoacetic ester |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107858209A (en) * | 2017-12-12 | 2018-03-30 | 江西艾迪尔新能源有限公司 | A kind of method using vegetable oil as raw material continuous production fatty-acid ethyl ester |
| CN110846136A (en) * | 2019-11-21 | 2020-02-28 | 南京胜昔实业有限公司 | Preparation method for producing biodiesel by using cottonseed oil |
| CN112457189A (en) * | 2020-10-30 | 2021-03-09 | 广西大学 | Preparation method of palm oil fatty acid ethyl ester |
| CN114672371A (en) * | 2022-03-17 | 2022-06-28 | 广西科技大学 | Preparation method of epoxidized oil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357219A (en) * | 2014-10-25 | 2015-02-18 | 童必炎 | Method for preparing biodiesel by using paulownia seed oil |
-
2017
- 2017-03-21 CN CN201710169201.8A patent/CN106906052A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357219A (en) * | 2014-10-25 | 2015-02-18 | 童必炎 | Method for preparing biodiesel by using paulownia seed oil |
Non-Patent Citations (2)
| Title |
|---|
| 俞云良等: "水力空化强化高芥酸菜籽油联产生物柴油和芥酸甲酯", 《太阳能学报》 * |
| 郑国香等: "《能源微生物学》", 31 July 2013, 哈尔滨工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107858209A (en) * | 2017-12-12 | 2018-03-30 | 江西艾迪尔新能源有限公司 | A kind of method using vegetable oil as raw material continuous production fatty-acid ethyl ester |
| CN110846136A (en) * | 2019-11-21 | 2020-02-28 | 南京胜昔实业有限公司 | Preparation method for producing biodiesel by using cottonseed oil |
| CN112457189A (en) * | 2020-10-30 | 2021-03-09 | 广西大学 | Preparation method of palm oil fatty acid ethyl ester |
| CN114672371A (en) * | 2022-03-17 | 2022-06-28 | 广西科技大学 | Preparation method of epoxidized oil |
| CN114672371B (en) * | 2022-03-17 | 2023-09-19 | 广西科技大学 | Preparation method of epoxidized oil |
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Application publication date: 20170630 |