CN113621017A - Comprehensive utilization method of camellia seed meal - Google Patents
Comprehensive utilization method of camellia seed meal Download PDFInfo
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- CN113621017A CN113621017A CN202110980062.3A CN202110980062A CN113621017A CN 113621017 A CN113621017 A CN 113621017A CN 202110980062 A CN202110980062 A CN 202110980062A CN 113621017 A CN113621017 A CN 113621017A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/005—Synthetic soaps
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/02—Compositions of detergents based essentially on soap on alkali or ammonium soaps
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/26—Organic compounds, e.g. vitamins containing oxygen
- C11D9/262—Organic compounds, e.g. vitamins containing oxygen containing carbohydrates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/40—Proteins
Abstract
The invention belongs to the technical field of processing and utilization, and discloses the technical field of a comprehensive utilization method of camellia seed meal. The method comprises the steps of treating degreased camellia oleifera seed meal by adopting a mixed solvent of a polar solvent and a nonpolar solvent, performing alcohol extraction to obtain tea saponin, then recovering residual liquid after alcohol extraction, using the recovered solvent as an extracting solution for continuous use, adding alkali liquor with a certain concentration into the recovered solid impurities, and stirring for reaction to obtain a washing product with washing and decontamination capabilities. The invention can change the product which can only be discharged as impurities originally into an excellent washing product, which further improves the added value of the tea seed cake product on the basis of the original patent technology.
Description
Technical Field
The invention relates to the technical field of processing and utilization of camellia seeds, in particular to a comprehensive utilization method of camellia seed meal.
Background
The camellia oleifera is a special edible oil tree species in China, and meanwhile, China is also the country with the largest area for cultivating the camellia oleifera in the world. By 2017, the planting area of the Chinese camellia has been enlarged to 6550 ten thousand mu, about 38 ten thousand tons of tea seed oil are produced annually, and about 20 ten thousand tons of corresponding byproduct camellia seed meal are produced annually. Tea seed cake typically contains: 12-18% of tea saponin, < 2% of residual oil, 12-16% of protein, 30-50% of starch and sugar, 10-12% of fiber, < 12% of water, and < 2% of impurities, etc., wherein the tea saponin contained in the oil tea meal is a natural nonionic surfactant, is a very important industrial raw material, and is widely used in the aspects of building materials, daily chemical industry, medicines, pesticides, etc.; the tea seed cake after extracting tea saponin can be used as excellent feed. Therefore, the comprehensive utilization level of the tea meal is closely related to the extraction process level of the tea saponin.
The extraction process of tea saponin is continuously improved from the traditional water extraction process to the extraction process of aqueous alcohol. For example, patent documents CN1754883A, CN101497642A, CN101747403A and CN101440117A all adopt an aqueous extraction method or an aqueous alcohol extraction method. In recent years, the anhydrous extraction process is receiving more and more attention, but the anhydrous ethanol extraction method still has the defect of low extraction rate from literature reports.
The inventor previously disclosed patent document CN108997471A, which discloses a green preparation method of high-purity tea saponin, wherein the extraction rate and purity of the product are both improved by using absolute ethyl alcohol, and the production process is green. However, the above process still has the following problems: in the process, whether the extractant needs to be recovered can be determined according to requirements, and once the extractant (mainly small molecular alcohols such as absolute ethyl alcohol) is recovered, a large amount of other impurities including substances such as tea oil, protein and small molecular saccharides are generated. Therefore, the comprehensive utilization method of the camellia seed meal is provided, the extraction agent is recycled, and the impurities in the recycling process are changed into valuable things which are important.
Disclosure of Invention
The invention provides a comprehensive utilization method for solving the technical problem that an extractant after high-purity tea saponin purification in the prior art cannot be recycled.
In order to solve the technical problems, the invention adopts the following technical scheme:
a comprehensive utilization method of oil-tea camellia seed meal comprises the steps of processing degreased oil-tea camellia seed meal by adopting a mixed solvent of a polar solvent and a non-polar solvent, performing alcohol extraction to obtain tea saponin, recovering residual liquid after alcohol extraction, using the recovered solvent as an extracting solution for continuous use, adding alkali liquor with a certain concentration into solid impurities obtained through recovery, and performing stirring reaction to obtain a washing product with washing and decontamination capabilities.
The alkali liquor is sodium hydroxide or sodium carbonate solution; the concentration of the alkali liquor is 10-250 g/L.
The feed liquid of the fixed impurities and the alkali liquor is 1-5g:1-10 mL. The stirring reaction time is 1-5h, the stirring reaction temperature can be kept in a boiling state, and preferably, the stirring reaction temperature is over 78 ℃.
The comprehensive utilization method of the camellia seed meal specifically comprises the following steps:
(1) pretreatment of raw materials: crushing the camellia seed meal, and sieving the crushed camellia seed meal with a sieve of 20 meshes to 80 meshes to obtain camellia seed meal powder;
(2) adding an organic solvent into the camellia seed meal obtained in the step (1) according to the material-liquid ratio of (1g:6mL) - (1g:15mL), and mixing, wherein the organic solvent is a mixed solvent of a polar solvent and a non-polar solvent; the polar solvent is absolute ethyl alcohol, and the nonpolar solvent is camellia seed oil;
(3) carrying out heat preservation treatment on the feed liquid mixture in the step (2), wherein the heat preservation temperature is 80-100 ℃, the heat preservation time is 3-6h, and carrying out alcohol extraction;
(4) then carrying out solid-liquid separation, cooling the obtained filtrate, separating out precipitate, and drying to obtain tea saponin;
(5) recovering the residual liquid after the tea saponin is obtained in the step (4), wherein the recovered ethanol can be used as an extracting solution to be returned to the step (2) for continuous use;
(6) and (5) adding alkali liquor into the fixed impurities after the solvent is recovered in the step (5), and stirring and reacting for a certain time to obtain a washing product.
Preferably, in the step (1), the polar solvent is one or a mixture of absolute ethyl alcohol and water; the non-polar solvent is one or a mixture of vegetable oil and glycerol; the vegetable oil is camellia seed oil. The oil content of the camellia seed meal in the step (1) is 0-15%. More preferably, in the step (1), the camellia seed meal is crushed and sieved by a 60-mesh sieve.
Preferably, the oil-tea camellia seed meal powder obtained in the step (2) is added with an organic solvent according to the weight ratio of 1g to 10mL of the feed liquid.
Preferably, the heat preservation temperature in the step (3) is 80 ℃, and the heat preservation time is 4 h.
Preferably, in the step (4), the solid-liquid separation adopts filtration or centrifugation, the solid-liquid separation can be carried out once or for multiple times, and the temperature of the solid-liquid separation process is kept to be the same as the heat preservation temperature in the step (3); the cooling temperature is 0-30 ℃; the precipitate is washed with cold ethanol before drying and then dried. More preferably, the drying is vacuum drying.
After the tea saponin is obtained through the steps (1) to (4), once the extractant in the step (5) is recovered, fixed impurities are left, and the inventor learns through analysis that the solid impurities comprise parts of the tea saponin, the tea oil, the protein, the micromolecule saccharides and other substances, so that the washing product with good washing and decontamination capability can be finally obtained by adding the alkali solution with a certain concentration into the fixed impurities containing the substances. The reason is that the residual part of the tea saponin is a surfactant and has good washing and decontaminating capacity; after the residual tea oil reacts with alkali, corresponding fatty acid sodium salt can be generated and also becomes a good surfactant; the rest protein and the small molecular saccharides are substances with good water solubility and alcohol solubility, and can be used for improving the viscosity, the color and the like of the product although the substances do not play a role in decontamination, and the washing products with excellent performance can be obtained just through the comprehensive effects of the protein, the small molecular saccharides and the substances. According to the technical scheme, the product which can only be discharged as impurities originally is changed into an excellent washing product through a simple one-step reaction, and the added value of the tea seed cake product is further improved on the basis of the original patent technology.
Drawings
Fig. 1 is a process flow chart of the comprehensive utilization method of camellia seed meal provided by the invention.
Detailed Description
The invention discloses a comprehensive utilization method of camellia seed meal, which can be realized by appropriately improving process parameters by referring to the content in the text by the technical personnel in the field. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The following detailed description of the invention refers to specific embodiments thereof for better understanding by those skilled in the art.
Example 1
(1) Pretreatment of raw materials: taking degreased camellia seed meal, wherein the residual oil content is 2% of the mass of the camellia seed meal, drying, crushing, and sieving with a 60-mesh sieve, and taking the sieved camellia seed meal for later use.
(2) And (2) taking 10g of the camellia seed meal obtained in the step (1), adding 95mL of absolute ethyl alcohol and 5mL of camellia seed oil, and uniformly stirring.
(3) Adjusting the temperature of the feed liquid in the step (2) to 50 ℃, preserving heat for pretreatment for 3 hours, and performing alcohol extraction.
(4) Filtering the feed liquid obtained in the step (3) with a Buchner funnel while the feed liquid is hot to obtain a filtrate, wherein the temperature during filtering is the same as that in the step (3), washing the obtained filter residue with 80 ℃ absolute ethyl alcohol twice, wherein each time is 20mL, and collecting washing liquid; and (3) drying the washed filter residue in a drying oven at 105 ℃ to obtain the soaped tea seed cake, directly using the soaped tea seed cake as feed or for other purposes after drying, and determining whether to recover the organic solvent according to the requirement.
(5) Mixing the filtrate with washing liquid, filtering with a separating funnel, cooling the filtrate obtained after the filtration in a refrigerator at 4 ℃, and performing solid-liquid separation by a filtering method after cooling, or standing and layering for 24 hours after cooling until the solution is precipitated out and deposited, thus obtaining supernatant and lower solid-phase precipitates. And (3) directly carrying out vacuum drying on the lower-layer precipitate, namely the crude product of the tea saponin, wherein the vacuum drying condition is 60 ℃, and the drying time is 30 minutes, but other conditions can also be adopted, such as temperature rise and the like, which only change the drying speed and have no influence on the result, so as to obtain the off-white tea saponin product.
(6) Recovering the residual liquid after the tea saponin is obtained in the step (5) under reduced pressure, and returning the recovered ethanol to the step (2) for continuous use; the obtained solid impurities are recovered, the amount of the solid impurities is about 2.08g, 2.08mL of sodium hydroxide solution with the concentration of 250g/L is added, the stirring is carried out for 4 hours, the stirring temperature is 80 ℃, and finally about 3.02 g of mixed liquid final washing products are obtained.
Example 2
(1) Pretreatment of raw materials: taking degreased camellia seed meal, wherein the residual oil content is 2% of the mass of the camellia seed meal, drying, crushing, sieving with a 80-mesh sieve, and taking camellia seed meal powder which is sieved for later use.
(2) And (2) taking 10g of the camellia seed meal obtained in the step (1), adding 95mL of absolute ethyl alcohol and 5mL of camellia seed oil, and uniformly stirring.
(3) Adjusting the temperature of the feed liquid in the step (2) to 80 ℃, preserving heat for pretreatment for 6 hours, and performing alcohol extraction.
(4) Filtering the feed liquid obtained in the step (3) with a Buchner funnel while the feed liquid is hot to obtain a filtrate, wherein the temperature during filtering is the same as that in the step (3), washing the obtained filter residue with 80 ℃ absolute ethyl alcohol twice, wherein each time is 20mL, and collecting washing liquid; and (3) drying the washed filter residue in a drying oven at 105 ℃ to obtain the soaped tea seed cake, directly using the soaped tea seed cake as feed or for other purposes after drying, and determining whether to recover the organic solvent according to the requirement.
(5) Mixing the filtrate with washing liquid, filtering with a separating funnel, washing the filtrate with cold ethanol (cold ethanol refers to ethanol with the same cooling temperature, here refers to absolute ethanol at 4 ℃, the same below) obtained after the filtration, cooling, and performing solid-liquid separation by a filtration method, or cooling until the solution is separated out and precipitated, standing and layering for 24 hours, and obtaining supernatant and lower solid-phase precipitate. And (3) directly carrying out vacuum drying on the lower-layer precipitate, namely the crude product of the tea saponin, wherein the vacuum drying condition is 60 ℃, and the drying time is 30 minutes, but other conditions can also be adopted, such as temperature rise and the like, which only change the drying speed and have no influence on the result, so as to obtain the off-white tea saponin product.
(6) Recovering the residual liquid after the tea saponin is obtained in the step (5) under reduced pressure, and returning the recovered ethanol to the step (2) for continuous use; the solid impurities thus obtained were recovered in an amount of about 3.1g, and 9mL of a sodium carbonate solution having a concentration of 10g/L was added thereto, followed by stirring at 90 ℃ for 1 hour to finally obtain about 11.1 g of a final washing product of the mixed solution.
Example 3 example 1 was repeated, except that 20.8mL of 120g/L NaOH solution was added in step (6) of this example, and the mixture was stirred for 4 hours at 79 ℃ to obtain about 22.1 g of the final washing product.
Comparative example 1
Example 1 was repeated, and this comparative example 1 differs from example 1 in that no lye was added in step (6) to obtain fixed impurities. The fixed impurities are viscous solids, about 2 g, and water is added to form white turbid liquid, which has unpleasant odor and is not suitable for use as a washing product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A comprehensive utilization method of oil-tea camellia seed meal is characterized in that after the degreased oil-tea camellia seed meal is treated by a mixed solvent of polar and non-polar solvents, alcohol extraction is carried out to obtain tea saponin, then residual liquid after alcohol extraction is recovered, the recovered solvent is used as an extracting solution for continuous use, solid impurities obtained through recovery are added into alkali liquor with a certain concentration, and stirring reaction is carried out to obtain a washing product with washing and dirt-removing capacity.
2. The comprehensive utilization method according to claim 1, wherein the alkali solution is sodium hydroxide or sodium carbonate solution; the concentration of the alkali liquor is 10-250 g/L.
3. The comprehensive utilization method of claim 1, wherein the feed liquid of the fixed impurities and the lye is 1-5g:1-10 mL.
4. The comprehensive utilization method according to claim 1, wherein the stirring reaction time is 1-5h, and the stirring reaction temperature is such that the reaction solution is kept in a boiling state.
5. The comprehensive utilization method according to claim 1, wherein the stirring reaction time is 1-5h, and the stirring reaction temperature is above 78 ℃.
6. A comprehensive utilization method as claimed in claim 1, specifically comprising the steps of:
(1) pretreatment of raw materials: crushing the camellia seed meal, and sieving the crushed camellia seed meal with a sieve of 20 meshes to 80 meshes to obtain camellia seed meal powder;
(2) adding an organic solvent into the camellia seed meal obtained in the step (1) according to the material-liquid ratio of (1g:6mL) - (1g:15mL), and mixing, wherein the organic solvent is a mixed solvent of a polar solvent and a non-polar solvent; the polar solvent is absolute ethyl alcohol, and the nonpolar solvent is camellia seed oil;
(3) carrying out heat preservation treatment on the feed liquid mixture in the step (2), wherein the heat preservation temperature is 80-100 ℃, the heat preservation time is 3-6h, and carrying out alcohol extraction;
(4) then carrying out solid-liquid separation, cooling the obtained filtrate, separating out precipitate, and drying to obtain tea saponin;
(5) recovering the residual liquid after the tea saponin is obtained in the step (4), wherein the recovered ethanol can be used as an extracting solution to be returned to the step (2) for continuous use;
(6) and (5) adding alkali liquor into the fixed impurities after the solvent is recovered in the step (5), and stirring and reacting for a certain time to obtain a washing product.
7. The comprehensive utilization method according to claim 6, wherein in the step (1), the polar solvent is one or a mixture of absolute ethyl alcohol and water; the non-polar solvent is one or a mixture of vegetable oil and glycerol; the vegetable oil is camellia seed oil.
8. The comprehensive utilization method according to claim 6, wherein in the step (4), the solid-liquid separation is performed by filtration or centrifugation, the solid-liquid separation can be performed once or more times, and the temperature of the solid-liquid separation process is kept to be the same as the heat preservation temperature in the step (3); the cooling temperature is 0-30 ℃; the precipitate is washed with cold ethanol before drying and then dried.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105176719A (en) * | 2015-10-10 | 2015-12-23 | 泉州市福达科技咨询有限公司 | Natural handmade soap containing camellia seeds and preparation method of soap |
| CN105441215A (en) * | 2015-12-16 | 2016-03-30 | 泉州市福达科技咨询有限公司 | Environmentally friendly camellia seed detergent and preparation method thereof |
| CN105695163A (en) * | 2016-01-15 | 2016-06-22 | 普洱健源油脂有限公司 | Preparation method of tea seed washing powder and washing agent |
| CN105969537A (en) * | 2016-05-23 | 2016-09-28 | 长沙理工大学 | Washing sheet prepared from waste residue of aqueous-phase tea-seed oil extraction technology and method thereof |
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| CN108997471A (en) * | 2018-09-17 | 2018-12-14 | 中国科学院青岛生物能源与过程研究所 | A kind of environment-friendly preparation method thereof of high-purity tea saponin |
| CN111440673A (en) * | 2020-05-09 | 2020-07-24 | 佛山市南海区旭展洗涤用品厂 | Tea saponin detergent and preparation method thereof |
| CN112679556A (en) * | 2020-12-29 | 2021-04-20 | 青岛职业技术学院 | Production process of high-purity tea saponin |
-
2021
- 2021-08-25 CN CN202110980062.3A patent/CN113621017A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105176719A (en) * | 2015-10-10 | 2015-12-23 | 泉州市福达科技咨询有限公司 | Natural handmade soap containing camellia seeds and preparation method of soap |
| CN105441215A (en) * | 2015-12-16 | 2016-03-30 | 泉州市福达科技咨询有限公司 | Environmentally friendly camellia seed detergent and preparation method thereof |
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| CN105969537A (en) * | 2016-05-23 | 2016-09-28 | 长沙理工大学 | Washing sheet prepared from waste residue of aqueous-phase tea-seed oil extraction technology and method thereof |
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