CN102351640A - Preparation method of very-long-chain fatty saturated normal monohydric primary alcohol - Google Patents
Preparation method of very-long-chain fatty saturated normal monohydric primary alcohol Download PDFInfo
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- CN102351640A CN102351640A CN2011102392850A CN201110239285A CN102351640A CN 102351640 A CN102351640 A CN 102351640A CN 2011102392850 A CN2011102392850 A CN 2011102392850A CN 201110239285 A CN201110239285 A CN 201110239285A CN 102351640 A CN102351640 A CN 102351640A
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Abstract
The invention relates to a preparation method of a very-long-chain fatty saturated normal monohydric primary alcohol, and particularly relates to a preparation method of n-triacontanol and n-octacosanol. The preparation method of a very-long-chain fatty saturated normal monohydric primary alcohol comprises the following steps: placing raw materials into a reaction kettle, adding anhydrous calcium chloride when heating to a temperature above the melting point, and taking out a rough wax product after the reaction; then, filtering to obtain a mixture of fatty acid calcium and a long-chain fatty alcohol; subsequently, crushing, and dropwisely adding acetone for extraction in vacuum to obtain an extracted fatty alcohol; and finally, carrying out high-temperature rectification on the fatty alcohol obtained after the extraction while depressurizing. The invention has the advantages of higher product yield and higher purity.
Description
Technical field
The present invention relates to the preparation method of the saturated positive structure monobasic primary alconol of a kind of speciality chain fatty class, relate in particular to the preparation method of myricyl alcohol, n-Octacosanol.
Background technology
The homology long chain aliphatic alcohol that contains C22～C38 in the rice bran wax is a kind of positive structure monobasic primary alconol of growing carbochain, and its major part is combined into wax ester with longer chain fatty acid, becomes the Fatty Alcohol(C12-C14 and C12-C18) of free state on a small quantity, and long chain aliphatic alcohol content is more than half in the pure rice bran wax.This long chain aliphatic alcohol contains octacosanol, triacontanol etc.Octacosanol is the antifatigue material of generally acknowledging, triacontanol is effective plant-growth regulator, farm crop is had the effect that promotes growth.Rice bran wax is to produce the desirable feedstock that long chain aliphatic alcohol reached and then extracted octacosanol, triacontanol etc.But rice bran wax is difficult saponified, and physico-chemical constant character such as the fusing point of long chain aliphatic alcohol C22～C38 and longer chain fatty acid C16～C36, boiling point are close, through general method, is difficult to obtain high yield, highly purified long chain aliphatic alcohol.
Application number is that 02112420.5 Chinese invention patent discloses and a kind ofly produces the method for long chain aliphatic alcohol by rice bran wax, and the technical scheme that this invention is taked is: raw material is chosen smart chaff wax or chaff wax, uses the dry type saponification; Get moist quicklime or calcium hydroxide, the ratio of itself and water is 1:0.5～10, and the consumption of quicklime or calcium hydroxide is 10～30% of a rice bran wax weight; The saponification reaction temperature is 95～180 ℃, and the reaction times is 2～10 hours, gets the mixture of fatty acid calcium and long chain aliphatic alcohol after reaction finishes to cool off; Carry out SX after it is ground into powder; With powder and solvent thorough mixing, give removing by filter insoluble fatty acid calcium again, from mother liquor, reclaim solvent again; And getting long chain aliphatic alcohol, solvent can be chosen ethanol or acetone or methyl alcohol.
The present invention is applicable to from rice bran wax and produces long chain aliphatic alcohol, and and then extracts useful matteies such as octacosanol, triacontanol.
Summary of the invention
The objective of the invention is to provide in addition the preparation method of a kind of yield saturated positive structure monobasic primary alconol of speciality chain fatty class that more high purity is higher.
Above-mentioned technical purpose of the present invention is achieved through following technical scheme:
The preparation method of the saturated positive structure monobasic primary alconol of speciality chain fatty class may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, add Calcium Chloride Powder Anhydrous when being warming up to the raw material fusing, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.4～0.6 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 80～90 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1～2MPa, 340～360 ℃ condition, carry out rectification under vacuum.
Preferred as technique scheme, it also comprises the crushing screening step, said crushing screening technology is that the product that 3. obtains through step is pulverized the back after sieve.
The a complete set of technology of the present invention does not add water, and this is than having higher technical difficulty in the aqueous phase saponification in the background technology, and the technique effect that it brought also is significantly, and is higher like the efficient of saponification reaction.It is to adopt anhydrous saponification that the present invention is different from the topmost characteristic of background technology, and its gordian technique is the control of selecting for use of Calcium Chloride Powder Anhydrous and its consumption.
In sum, the present invention has following beneficial effect:
The present invention adopts anhydrous saponification technology that raw material is carried out the height saponification; Then under vacuum state, extract again; Last again under 1～2MPa, 340～360 ℃ condition, carrying out rectification under vacuum, make the present invention have the higher technique effect of high purity of product yield.
Embodiment
This specific embodiment only is to explanation of the present invention; It is not a limitation of the present invention; Those skilled in the art can make the modification that does not have creative contribution to present embodiment as required after reading this specification sheets, but as long as in claim scope of the present invention, all receive the protection of patent law.
Embodiment one
The preparation method of n-Octacosanol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.4 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 80 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1MPa, 340 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Embodiment two
The preparation method of n-Octacosanol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.5 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 85 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1.5MPa, 350 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Embodiment three
The preparation method of n-Octacosanol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.6 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 90 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 2MPa, 360 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Embodiment four
The preparation method of myricyl alcohol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.4 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 80 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1MPa, 340 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Embodiment five
The preparation method of myricyl alcohol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.5 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 85 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1.5MPa, 350 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Embodiment six
The preparation method of myricyl alcohol may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, be warming up to fusing point and add Calcium Chloride Powder Anhydrous when above, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.6 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 90 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 2MPa, 360 ℃ condition, carry out rectification under vacuum; Extract the purpose product of various content according to the difference of boiling point;
4. will pass through the product that 3. step obtain and pulverize the back, reach the fineness that the client needs, pack after sieve.
Comparative Examples
1. get homemade chaff wax 200kg, its acetone solvend is 21%, 76 ℃ of fusing points, saponification value 89;
2. saponification reaction: above-mentioned raw materials is added the stainless steel cauldron that whipping appts is arranged, be heated to the rice bran wax fusing, under agitation slowly add 50% calcium hydroxide water slurry 60kg in the reaction kettle; Heating saponification 5 hours; Whole temperature is 150 ℃, reaction finish brown decorating film 213kg, yield 92.6%;
3. with decorating film after kibbler is pulverized, be fatty acid calcium and long chain aliphatic alcohol mix powder;
4. take by weighing said mixture powder 60kg, add the extractor that is equipped with cooling and reflux device, and add etoh solvent 900kg, heated 2 hours, filtered while hot, removing alcohol-insoluble substance is fatty acid calcium, stays the ethanolic soln that mother liquor promptly dissolves in long chain aliphatic alcohol;
5. with behind the mother liquor heating recovery ethanol, obtaining long chain aliphatic alcohol 23kg, is 40% to the wax yield.
Forming (C%) by its Fatty Alcohol(C12-C14 and C12-C18) of gas chromatographic analysis is: C
243.8, C
265.8, C
2810.7, C
3020.8, C
3219.2, C
3419.6, C
3611.1, C
382.3.
The present invention is owing to adopted anhydrous saponification method, and the yield of its crude product is higher, and embodiment one reaches 94.3%, and embodiment two reaches 94.9% embodiment three and reaches 94.6%, and embodiment four reaches 94.3%, and embodiment five reaches 94.9%, and embodiment six reaches 94.6%; And only can reach 92.6% in the Comparative Examples.In addition, the present invention is owing to adopted distillation technology, and needed product can reach higher purity.
Claims (2)
1. the preparation method of the saturated positive structure monobasic primary alconol of speciality chain fatty class may further comprise the steps:
1. raw material sugar-cane wax and/or rice bran wax are put into reaction kettle, add Calcium Chloride Powder Anhydrous when being warming up to the raw material fusing, the rough thing of wax is taken out in the reaction back; The rough thing of said wax is filtered, get the mixture of fatty acid calcium and long chain aliphatic alcohol; In this step, the addition of said Calcium Chloride Powder Anhydrous is 0.4～0.6 times of amount of substance of raw material;
2. said mixture is pulverized, under vacuum state, dripped acetone then and extract, the temperature of extraction is 80～90 ℃, the Fatty Alcohol(C12-C14 and C12-C18) that obtains extracting;
3. again the Fatty Alcohol(C12-C14 and C12-C18) that obtains after the said extraction is carried out the high temperature rectification under vacuum, under 1～2MPa, 340～360 ℃ condition, carry out rectification under vacuum.
2. the preparation method of the saturated positive structure monobasic primary alconol of a kind of speciality chain fatty class according to claim 1, it is characterized in that: it also comprises the crushing screening step, said crushing screening technology is that the product that 3. obtains through step is pulverized the back after sieve.
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| CN2011102392850A CN102351640A (en) | 2011-08-19 | 2011-08-19 | Preparation method of very-long-chain fatty saturated normal monohydric primary alcohol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838449A (en) * | 2012-09-27 | 2012-12-26 | 江西省科学院生物资源研究所 | Method for producing octacosanol with special content |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389445A (en) * | 2002-07-04 | 2003-01-08 | 许仁溥 | Method of preparing long-chain fatty alcohol from rice bran wax |
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- 2011-08-19 CN CN2011102392850A patent/CN102351640A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389445A (en) * | 2002-07-04 | 2003-01-08 | 许仁溥 | Method of preparing long-chain fatty alcohol from rice bran wax |
Non-Patent Citations (3)
| Title |
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| 崔杨棣等: "米糠蜡中制取三十醇", 《中国油脂》 * |
| 矫彩山等: "从米糠蜡中提取二十八和三十烷醇及产品分析", 《化学工程师》 * |
| 许仁溥: "米糠蜡制取高纯度二十八醇研究", 《粮食与油脂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838449A (en) * | 2012-09-27 | 2012-12-26 | 江西省科学院生物资源研究所 | Method for producing octacosanol with special content |
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Application publication date: 20120215 |