CN112795434A - Processing technology of triglyceride type prickly ash seed oil - Google Patents
Processing technology of triglyceride type prickly ash seed oil Download PDFInfo
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- CN112795434A CN112795434A CN202110018751.6A CN202110018751A CN112795434A CN 112795434 A CN112795434 A CN 112795434A CN 202110018751 A CN202110018751 A CN 202110018751A CN 112795434 A CN112795434 A CN 112795434A
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- seed oil
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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
- C11C3/06—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with glycerol
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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Abstract
The invention provides a processing technology of triglyceride type pricklyash seed oil, which comprises the following steps: adding glycerin and a composite alkaline catalyst into the raw pricklyash seed oil, wherein the composite alkaline catalyst is a compound of zinc oxide and at least one of sodium hydroxide and potassium hydroxide; and secondly, performing esterification reaction on the crude pricklyash seed oil and the glycerol under the action of a composite alkaline catalyst to obtain triglyceride pricklyash seed oil. According to the invention, the edible-grade pricklyash seed oil obtained by subcritical extraction is subjected to transesterification by adopting the composite alkaline catalyst to generate triglyceride pricklyash seed oil, so that the raw material cost is low, the equipment investment is less, the method is suitable for large-scale production, and the deep processing cost of the high-acid-value pricklyash seed oil is greatly reduced; the finally obtained product is rich in essential nutrient components such as EPA, DHA and the like which can not be synthesized by human bodies, overcomes the defects of unbalanced proportion of long-chain fatty acid and poor absorption of human bodies in the existing pricklyash peel seed oil, and has very high edible nutritive value and medicinal value.
Description
Technical Field
The invention belongs to the technical field of oil processing, and particularly relates to a processing technology of triglyceride type pricklyash seed oil.
Background
The pepper seed oil is rich in EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid), and has wide development and application prospects when being used as a raw material of a medicine or a raw material of a health-care food. The triglyceride type pricklyash seed oil has good nutrition and health care value as a new variety of triglyceride type edible oil, and is listed in a new resource food catalog of the Ministry of health. In the prior art, the zanthoxylum seed oil obtained by a squeezing process or the zanthoxylum seed oil obtained by an extraction process has higher acid value (generally between 40 and 60), cannot reach the edible standard, has high cost of the subsequent processing process and very low oil yield of the finished oil. The Chinese patent application No. 201310525232.4 discloses a catalyst for esterification and deacidification reaction of zanthoxylum seed oil with high acid value, the catalyst is used for converting the zanthoxylum seed oil with high acid value into raw materials for preparing biodiesel through esterification reaction, and the obtained product has excessive residues which can not reach the edible level; the chinese patent application No. 200610105197.0 discloses a method for producing biodiesel using zanthoxylum seed oil, wherein the chemical residue in the intermediate product esterified zanthoxylum seed oil is also very much and does not meet the edible standard. How to process the zanthoxylum seed oil with high acid value into the zanthoxylum seed oil with edible grade and reduce the processing cost is a technical problem to be solved at present.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a processing technology of triglyceride type pricklyash seed oil.
The technical scheme of the invention is realized as follows:
a processing technology of triglyceride type pricklyash seed oil comprises the following operation steps:
adding glycerin and a composite alkaline catalyst into crude pepper seed oil, wherein the composite alkaline catalyst is a compound of zinc oxide and at least one of sodium hydroxide and potassium hydroxide;
and secondly, performing esterification reaction on the crude pricklyash seed oil and the glycerol under the action of a composite alkaline catalyst to finally obtain triglyceride pricklyash seed oil.
In the traditional transesterification reaction, concentrated sulfuric acid is generally used as a catalyst, although the catalytic effect is good, the chemical residues are more, and the finally obtained product can not reach the edible standard. Stannous chloride, aluminum trichloride and zinc oxide are used as catalysts, and zinc oxide is particularly used as a catalyst, so that although the catalytic effect is good, the defect that the metal residues are difficult to remove exists. The existing catalysts cause the subsequent residue removal operation to be complicated and incomplete, and the possibility of meeting the edible standard is low. According to the method, at least one of sodium hydroxide and potassium hydroxide is used for replacing part of zinc oxide, so that the using amount of zinc oxide is remarkably reduced, a good catalytic effect can be kept, the metal residue is remarkably reduced, the operation of removing residues in a product is simplified, the effect of removing residues is improved, and the transesterification of the pricklyash seed oil into edible triglyceride pricklyash seed oil is possible.
Preferably, the composite basic catalyst is prepared by mixing the following components in a weight ratio of (10-15): (10-15): (5-10) a mixture of sodium hydroxide, potassium hydroxide and zinc oxide. The composite alkaline catalyst composed according to the proportion has the catalytic effect which is equal to about 90 percent of that of zinc oxide used as the catalyst, and greatly reduces the residue of metallic zinc in the product while maintaining the good catalytic performance.
More preferably, in the first step, the weight ratio of the crude pepper seed oil, the glycerol and the composite alkaline catalyst is (100- & ltSUB & gt 150-): (10-15): (0.2-1.5).
Further preferably, in the second step, the temperature during the esterification reaction is 180-.
Further preferably, during the esterification reaction, the system is continuously vacuumized to remove water generated by the esterification reaction, and the water generated by the esterification reaction is continuously removed during the vacuumization after being evaporated at a high temperature, so that the continuous esterification reaction is kept.
Preferably, the third step, after the esterification reaction is finished, adding water for washing, stirring, standing for layering, and removing a water layer to obtain a crude product; then, heating the reaction kettle to 80-100 ℃, vacuumizing until the vacuum degree is 0.7-0.9MPa, sequentially adding activated clay and activated carbon into the crude product in the reaction kettle, decoloring the crude product, keeping the temperature and the vacuum degree in the decoloring process, cooling to 40-50 ℃ after decoloring, filtering and collecting filtrate, wherein the obtained filtrate is the triglyceride type pepper seed oil.
More preferably, the amount of activated clay added is 2.4% to 2.5% by weight of the crude product and the amount of activated carbon added is 0.5% to 0.6% by weight of the crude product.
Most preferably, the raw pricklyash seed oil is edible pricklyash seed oil extracted by a subcritical extraction process, and the glycerol is edible glycerol.
The production of edible triglyceride type pricklyash seed oil by using pricklyash seed oil as a raw material has not been reported. According to the invention, the edible-grade pricklyash seed oil obtained by subcritical extraction is subjected to transesterification by adopting the composite alkaline catalyst to generate triglyceride pricklyash seed oil, so that the raw material cost is low, the equipment investment is less, the method is suitable for large-scale production, and the deep processing cost of the high-acid-value pricklyash seed oil is greatly reduced; the triglyceride type pricklyash seed oil obtained by the processing technology of the invention is rich in EPA and DHA which are both omega-3 polyunsaturated fatty acids and are important nutrient components which can not be synthesized by human bodies and are indispensable, overcomes the defects of unbalanced proportion of long-chain fatty acids and poor absorption of human bodies in the existing pricklyash seed oil, and has very high nutritional value and medicinal value.
Detailed Description
The technical solutions in the present specification will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The raw pricklyash seed oil used in the following examples is subcritical extraction food grade pricklyash seed oil from Shanxi Debio agricultural science and technology Limited, and the acid value is 35. The glycerol used was a commercially available food grade glycerol.
Example 1
A processing technology of triglyceride type pricklyash seed oil comprises the following operation steps:
adding glycerin and a composite alkaline catalyst into the crude pricklyash seed oil, wherein the weight of the crude pricklyash seed oil, the weight of the glycerin and the weight of the composite alkaline catalyst are respectively 150kg, 13kg and 0.2kg, and the weight ratio of the sodium hydroxide to the zinc oxide is 1: 1;
secondly, performing esterification reaction on the raw pricklyash seed oil and glycerol under the action of a composite alkaline catalyst, wherein the temperature during the esterification reaction is 200 ℃, the vacuum degree is 0.8MPa, and the esterification reaction time is 1 h; during the esterification reaction, continuously vacuumizing the system to remove water generated by the esterification reaction, and finally obtaining triglyceride type pricklyash seed oil;
thirdly, after the esterification reaction is finished, firstly adding water for washing, stirring, standing for layering, and removing a water layer to obtain a crude product; then, heating the reaction kettle to 100 ℃, vacuumizing to the vacuum degree of 0.8MPa, sequentially adding activated clay and activated carbon into the crude product in the reaction kettle, decoloring the crude product, keeping the temperature and the vacuum degree in the decoloring process, cooling to 40 ℃ after decoloring, filtering and collecting filtrate, wherein the obtained filtrate is triglyceride type pepper seed oil; wherein the addition amount of activated clay is 2.5% of the weight of the crude product, and the addition amount of activated carbon is 0.55% of the weight of the crude product.
Example 2
A processing technology of triglyceride type pricklyash seed oil comprises the following operation steps:
adding glycerol and a composite alkaline catalyst into crude pepper seed oil, wherein the weight of the crude pepper seed oil, the weight of the glycerol and the weight of the composite alkaline catalyst are respectively 100kg, 15kg and 0.8kg, and the weight ratio of potassium hydroxide to zinc oxide is 1: 1;
secondly, performing esterification reaction on the raw pricklyash seed oil and glycerol under the action of a composite alkaline catalyst, wherein the temperature during the esterification reaction is 180 ℃, the vacuum degree is 0.9MPa, and the esterification reaction time is 2 hours; during the esterification reaction, continuously vacuumizing the system to remove water generated by the esterification reaction, and finally obtaining triglyceride type pricklyash seed oil;
thirdly, after the esterification reaction is finished, firstly adding water for washing, stirring, standing for layering, and removing a water layer to obtain a crude product; then, heating the reaction kettle to 80 ℃, vacuumizing to the vacuum degree of 0.9MPa, sequentially adding activated clay and activated carbon into the crude product in the reaction kettle, decoloring the crude product, keeping the temperature and the vacuum degree in the decoloring process, cooling to 45 ℃ after decoloring, filtering and collecting filtrate, wherein the obtained filtrate is triglyceride type pepper seed oil; wherein the addition amount of activated clay is 2.4% of the weight of the crude product, and the addition amount of activated carbon is 0.6% of the weight of the crude product.
Example 3
A processing technology of triglyceride type pricklyash seed oil comprises the following operation steps:
adding glycerin and a composite alkaline catalyst into the crude pepper seed oil, wherein the weight of the crude pepper seed oil, the weight of the glycerin and the weight of the composite alkaline catalyst are respectively 120kg, 10kg and 1.5kg, and the weight ratio of the composite alkaline catalyst to the weight of sodium hydroxide, potassium hydroxide and zinc oxide is 1: 1: 1;
secondly, performing esterification reaction on the raw pricklyash seed oil and glycerol under the action of a composite alkaline catalyst, wherein the temperature during the esterification reaction is 190 ℃, the vacuum degree is 0.7MPa, and the esterification reaction time is 3 hours; during the esterification reaction, continuously vacuumizing the system to remove water generated by the esterification reaction, and finally obtaining triglyceride type pricklyash seed oil;
thirdly, after the esterification reaction is finished, firstly adding water for washing, stirring, standing for layering, and removing a water layer to obtain a crude product; then, heating the reaction kettle to 90 ℃, vacuumizing to the vacuum degree of 0.7MPa, sequentially adding activated clay and activated carbon into the crude product in the reaction kettle, decoloring the crude product, keeping the temperature and the vacuum degree in the decoloring process, cooling to 50 ℃ after decoloring, filtering and collecting filtrate, wherein the obtained filtrate is triglyceride type pepper seed oil; wherein the addition amount of activated clay is 2.45% of the weight of the crude product, and the addition amount of activated carbon is 0.5% of the weight of the crude product.
Example 4
The composite alkaline catalyst is a mixture of 0.7kg of sodium hydroxide, 0.56kg of potassium hydroxide and 0.24kg of zinc oxide. The rest of the process was the same as in example 3.
Example 5
The composite alkaline catalyst is a mixture of 0.455kg of sodium hydroxide, 0.682kg of potassium hydroxide and 0.363kg of zinc oxide. The rest of the process was the same as in example 3.
Example 6
The composite alkaline catalyst was a mixture of 0.59kg of sodium hydroxide, 0.455kg of potassium hydroxide and 0.455kg of zinc oxide. The rest of the process was the same as in example 3.
In examples 1 to 6, the acid value of the final product after the completion of the esterification reaction was 2.8 at most, the acid value of the final product obtained after the third step of finishing treatment (washing with water, decoloring, etc.) was 1.7 at most, the content of triglyceride in the final product was increased by at least 11%, and the maximum amount of metallic zinc residues was only 52mg/kg, which reached the leading level in the industry.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A processing technology of triglyceride type pricklyash seed oil is characterized in that: the method comprises the following operation steps:
adding glycerin and a composite alkaline catalyst into crude pepper seed oil, wherein the composite alkaline catalyst is a compound of zinc oxide and at least one of sodium hydroxide and potassium hydroxide;
and secondly, performing esterification reaction on the crude pricklyash seed oil and the glycerol under the action of a composite alkaline catalyst to finally obtain triglyceride pricklyash seed oil.
2. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 1, which is characterized in that: the composite alkaline catalyst is prepared from the following components in percentage by weight (10-15): (10-15): (5-10) a mixture of sodium hydroxide, potassium hydroxide and zinc oxide.
3. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 2, which is characterized in that: in the first step, the weight ratio of the crude pepper seed oil, the glycerol and the composite alkaline catalyst is (100-) -150: (10-15): (0.2-1.5).
4. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 1, which is characterized in that: in the second step, the temperature during the esterification reaction is 180-.
5. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 4, which is characterized in that: during the esterification reaction, the system is continuously vacuumized to remove the water generated in the esterification reaction.
6. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 1, which is characterized in that: further comprising: and thirdly, after the esterification reaction is finished, washing with water to obtain a crude product, sequentially adding activated clay and activated carbon into the crude product in the reaction kettle at the temperature of 80-100 ℃ and the vacuum degree of 0.7-0.9MPa, decoloring the crude product, keeping the temperature and the vacuum degree in the decoloring process, cooling after decoloring, filtering and collecting filtrate, wherein the obtained filtrate is the triglyceride type pepper seed oil.
7. The processing technology of the triglyceride type zanthoxylum seed oil according to claim 6, which is characterized in that: the addition amount of the activated clay is 2.4-2.5% of the weight of the crude product, and the addition amount of the activated carbon is 0.5-0.6% of the weight of the crude product.
8. The processing technology of the triglyceride type zanthoxylum seed oil according to any one of claims 1 to 7, which is characterized in that: the crude pricklyash seed oil is edible pricklyash seed oil extracted by a subcritical extraction process, and the glycerol is edible glycerol.
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| CN202110018751.6A CN112795434A (en) | 2021-01-07 | 2021-01-07 | Processing technology of triglyceride type prickly ash seed oil |
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| CN202110018751.6A CN112795434A (en) | 2021-01-07 | 2021-01-07 | Processing technology of triglyceride type prickly ash seed oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015503A (en) * | 2021-11-08 | 2022-02-08 | 甘肃乾禾芸农业科技发展有限责任公司 | Decoloring method for spiral pressed prickly ash seed oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242969A (en) * | 2013-05-24 | 2013-08-14 | 四川欣美加生物医药有限公司 | Preparation method of triglyceride type fish oil and prepared triglyceride type fish oil |
| CN110437931A (en) * | 2019-08-17 | 2019-11-12 | 上海辰钿实业有限公司 | A kind of processing technology of low acid value Fructus Zanthoxyli oil |
| CN110684593A (en) * | 2019-11-11 | 2020-01-14 | 上海辰钿实业有限公司 | Preparation method of pepper seed flavor oil |
-
2021
- 2021-01-07 CN CN202110018751.6A patent/CN112795434A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242969A (en) * | 2013-05-24 | 2013-08-14 | 四川欣美加生物医药有限公司 | Preparation method of triglyceride type fish oil and prepared triglyceride type fish oil |
| CN110437931A (en) * | 2019-08-17 | 2019-11-12 | 上海辰钿实业有限公司 | A kind of processing technology of low acid value Fructus Zanthoxyli oil |
| CN110684593A (en) * | 2019-11-11 | 2020-01-14 | 上海辰钿实业有限公司 | Preparation method of pepper seed flavor oil |
Non-Patent Citations (1)
| Title |
|---|
| 马传国等: "分子蒸馏对高酸值花椒籽油脱酸的初步探讨", 《中国油脂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015503A (en) * | 2021-11-08 | 2022-02-08 | 甘肃乾禾芸农业科技发展有限责任公司 | Decoloring method for spiral pressed prickly ash seed oil |
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