CN103800415A - Method for recovering byproducts generated in processing process of medicinal chrysanthemum flowers - Google Patents
Method for recovering byproducts generated in processing process of medicinal chrysanthemum flowers Download PDFInfo
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- CN103800415A CN103800415A CN201410038301.3A CN201410038301A CN103800415A CN 103800415 A CN103800415 A CN 103800415A CN 201410038301 A CN201410038301 A CN 201410038301A CN 103800415 A CN103800415 A CN 103800415A
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Abstract
The invention discloses a method for recovering byproducts generated in processing process of medicinal chrysanthemum flower. The method comprises the following steps: deactivating enzymes of fresh medicinal chrysanthemum flowers at 100-110DEG C for 45-55 s, and drying medicinal chrysanthemum flowers at 70-75DEG C for 6.5-7.5 h, wherein water-oil mixed vapor generated in 2-6 h of drying is collected and fed into a condenser, a cooling tower and an oil-water separator in sequence, and after separation in the oil-water separator, the obtained upper oil layer is volatile oil, and the lower water layer is aromatic water. The method disclosed by the invention can reutilize the waste generated during processing process of chrysanthemum flowers, and extract volatile oil and other byproducts from the waste, does not need additional chrysanthemum flower raw material and heat energy, and can change waste into valuables and reduce waste and improve efficiency. The obtained volatile oil has good quality, and has good economic benefits and social benefits.
Description
Technical field
The present invention relates to the processing technique of Chrysanthemum morifolium, relate in particular to the recovery method of the by-products such as the volatile oil, Aromatic water and the chrysanthemum juice that produce in the Chrysanthemum morifolium course of processing.
Background technology
Flos Chrysanthemi is the dry capitulum of feverfew Flos Chrysanthemi (Chrysanthemum morifolium Ramat.), is the conventional Chinese medicine of China's tradition, is again one of important outlet medical material.Flos Chrysanthemi extract can strengthen capillary resistance, reduce metabolism of lipid and cholesterol content in blood, have the effect that improves myocardial nutrition, antiinflammatory, energy Scavenger of ROS free radical simultaneously, has certain effect to suppressing tumor, slow down aging and strengthening body immunity.Volatile oil also claims quintessence oil, is one of main activity extract of Flos Chrysanthemi, be present in a class in plant have volatility, can be with the general name of vapor distillation oily liquids out.Modern study shows that Flos Chrysanthemi volatile oil pharmaceutically all has effect of wind and heat dispersing, eliminating inflammation and expelling toxin, basically identical with the medicinal effects of Flos Chrysanthemi, and on market, the demand to chrysanthemum essential oil is increasing.
Existing Flos Chrysanthemi volatile oil is separation and Extraction from the plants such as Flos Chrysanthemi Indici mostly, conventionally adopts steam distillation, and extraction temperature is higher, separating technology is complicated, consumes ample resources, and production cost is high.Concrete operations are by pulverizing medicinal materials, and long-time immersion makes medical material deliquescing, after histiocyte expands, recover its native state, and the leaching that is easy to effective ingredient is extracted.But long soaking time, may cause composition to change, cause that medical material fermentation is rotten.And steam distillation is not suitable for the extraction of thermally labile component, easily there is chemical change in long-time and water high temperature azeotropic; To some heat-sensitive materials be easily oxidized, the reaction such as polymerization causes degeneration; As water-soluble in berry extract vapour pressure can significantly decline, and the Chinese crude drug dissolving each other for some and water can not effectively extract; If the impurity in reactant mixture has volatility, just can not guarantee the purity of extracted volatile oil, and the yield of volatile oil is also very low, required time is longer, is difficult to keep the original fresh fragrance of volatile oil, also can exert an influence to the curative effect of some preparations.Find that after deliberation most of Chinese crude drugs all exist a best moisture content (7～13%), in this numerical range, in medical material, the content of effective ingredient remains unchanged substantially, and its molecular structure is in metastable state; But when moisture content lower (especially in the condition of high temperature), the effective ingredient in medical material can promptly be damaged, cause drug effect to reduce.Volatile oil is mixture, and without fixing boiling point, the boiling point of heterogeneity is between 70～300 ℃, and traditional volatile oil extracts temperature higher (higher than 100 ℃), therefore must cause the loss of more low boiling volatile oil.
There is data to show: in Flos Chrysanthemi flowers in 2002 (Borneolum Syntheticum 13.27%, Camphora 10.99%), in dry flower (Borneolum Syntheticum 0.340%, Camphora 0.0867%); In flower, volatile oil content is 0.57%, is 0.40% after microwave processing, after tradition steams, is 0.19%.Meanwhile, also there were significant differences for the volatile oil content of different parts, and in blade, volatile oil content is the highest, respectively than approximately high 3 times in stem, approximately high 7 times in beguine.And the processing of traditional Flos Chrysanthemi is just dried into fresh carrying out green removal on chrysanthemum merely dry Flos Chrysanthemi, but do not consider to recycle volatile oil in this process, the exploitation of volatile oil in blade are ignored especially, thereby cause a large amount of volatile oil to scatter and disappear, to such an extent as to always " The fragrance-of-flowers is wafted li away " of annual Flos Chrysanthemi in the November place of production caused the significant wastage of resource.
Summary of the invention
Goal of the invention: the object of this invention is to provide and a kind ofly reclaim by-product in the Chrysanthemum morifolium course of processing, realize resource and effectively recycle, and can advance the method for Chrysanthemum morifolium industrial chain extension.
Technical scheme: the recovery method of by-product in the Chrysanthemum morifolium course of processing of the present invention, comprises the steps:
(1) to the processing that completes of fresh Chrysanthemum morifolium, the temperature that completes is 100～110 ℃, and fixation time is 45～55s;
(2) Chrysanthemum morifolium after completing is dried, bake out temperature is 70～75 ℃, and drying time is 6.5～7.5h,
Wherein, the water oil mixed vapour that collection drying time produces in 2～6h also enters condenser, cooling tower and oil water separator successively, and separating through oil water separator the upper strata oil reservoir obtaining is volatile oil, and lower aqueous layer is Aromatic water.
In step (2), collect the water oil mixed vapour that described drying time produces in 3～6h and carry out subsequent treatment, separate and obtain Aromatic water; The yield of Aromatic water is no more than 1.5～2 times of Chrysanthemum morifolium fresh weight (being fresh Flos Chrysanthemi weight), if 1.5～2 times of Chrysanthemum morifolium dry weight, the Aromatic water quality obtaining is better.
Collect the water oil mixed vapour that described drying time produces in 3～5h and carry out subsequent treatment, separating and obtain volatile oil.
Meanwhile, collection starts to enter the raw water oil mixed vapour of condenser front baking dry labor from oven dry and carries out the processing that completes step (1), and the oily mixed vapour of water of then collecting the generation that completes enters cycle condenser, and cooling recovery obtains chrysanthemum juice.Collect and dry water oil mixed vapour that last 0.5～1h produces and use as step (1) steam of processing that completes.If corresponding above-mentioned " collect the water oil mixed vapour that described drying time produces in 3～5h and carry out subsequent treatment; separating and obtain volatile oil ", collects and dries water oil mixed vapour that last 1.5～2h produces and use as step (1) steam of processing that completes.
After step (1) finishes, before step (2) generation, collect the water oil mixed vapour producing in the above-mentioned process that completes and enter cycle condenser, cooling recovery obtains chrysanthemum juice; The yield of simultaneously controlling chrysanthemum juice is no more than the fresh weight of Chrysanthemum morifolium, if be no more than the dry weight of Chrysanthemum morifolium, the chrysanthemum juice quality obtaining is better.
Reaction mechanism: Chrysanthemum morifolium volatile oil is mixture, without determining boiling point, and the boiling point of heterogeneity is between 70～300 ℃.Fresh Flos Chrysanthemi is completing in drying course, the moisture on Flos Chrysanthemi top layer is together with the rising vaporization of volatility medicinal ingredient, in the time that the steam partial pressure on Flos Chrysanthemi surface is greater than water in air partial vapour pressure, the moisture on Flos Chrysanthemi surface is to air evaporation, cause the moisture rate variance of Flos Chrysanthemi inside and outside, thereby make Flos Chrysanthemi internal moisture to its diffusion into the surface, finally make the volatile ingredient of Flos Chrysanthemi inside and moisture with the mixed style of liquid gaseous state along with the evaporation of top layer moisture to external migration.Along with the transmission of heat, the inner moisture content of Flos Chrysanthemi is occurring to change, and in the time that the steam on Flos Chrysanthemi top layer equates with the humidity pressure in atmosphere, Flos Chrysanthemi inner vapor just can not be spread in atmosphere, thereby formation relative equilibrium, now Flos Chrysanthemi water content has also reached pharmacopeia required standard.Volatile ingredient scatters and disappears with water vapour, and therefore the fuel-displaced rule of volatile oil and the evaporation rules of moisture present certain similarity.As shown in Figure 2, in the starting stage, fresh Flos Chrysanthemi water content is larger, although have fuel-displacedly, general performance is that quality is not high and content is lower, now reclaims volatile oil economical and practical not.The water oil mixed vapour of this part is made simply antibacterial, concentration after circulating condensing, can be used as primary product chrysanthemum juice.Along with scattering and disappearing of top layer moisture, the reducing of the wet poor and vapour pressure of inside and outside water, the volatile oil of inside sends with aqueous dispersion, the quick increase that general performance is volatile oil content; Along with wet poor the reducing of inside and outside water, Flos Chrysanthemi is moisture loss in dry run, cell dehydration, and cellularity shrinks, and low boiling volatile oil content reduces, and volatile oil content increase tends towards stability.Along with reducing of the wet difference of inside and outside water and further reducing of vapour pressure, internal component and structure tend towards stability, and the content increase of volatile oil progressively reduces and tends towards stability.As shown in Figure 3, Aromatic water is gained after oil mixing with water steam refrigerated separation, its changes of contents trend and volatile oil exist larger relatedness and concordance, only therefore can present the trend different from volatile oil because moisture is more in Aromatic water, and the changes of contents of Aromatic water is to reach maximum at 5h, progressively reduce subsequently.(accompanying drawing only represents trend, does not represent real content; The oil pump capacity of volatile oil when Fig. 2 vertical coordinate represents that Flos Chrysanthemi fresh weight is 100g; Fig. 3 vertical coordinate is the absorbance of the Aromatic water of mensuration, infers its content with this)
Beneficial effect: compared with prior art, its remarkable advantage is in the present invention:
1, the present invention is the recycling of the garbage (oil mixing with water steam) to the generation of the Flos Chrysanthemi course of processing, therefrom extracts volatilization wet goods by-product, without Flos Chrysanthemi raw material and heat energy are additionally provided, can turn waste into wealth, fall useless potentiation.
2, to be that the relatively traditional volatile oil of the temperature (70～75 ℃) that uses of Flos Chrysanthemi drying production line extracts temperature (>=100 ℃) low for the extraction temperature of Flos Chrysanthemi volatile oil of the present invention, and the molten boiling point of Organic substance is lower, degree of unsaturation is higher, and therefore the volatile oil degree of unsaturation of gained of the present invention is high, quality is more excellent.
3, the average fresh Flos Chrysanthemi of every 5～6kg can be processed 1kg dry Flos Chrysanthemi, and every processing 1t dry Flos Chrysanthemi can reclaim 1.2kg volatile oil.Chrysanthemum essential oil price is about 1200 Yuan/㎏ on the market at present, if adopt recovery process of the present invention, can realize on the original basis every mu and at least increase income 300 yuan, the additional output value that only Chrysanthemum morifolium volatile oil reclaims is about 1,440 ten thousand yuan/year, chrysanthemum juice and Aromatic water all can produce corresponding added value in addition, can produce thus good economic benefit and social benefit.
4, the proposition of volatile oil recovery theory of the present invention is that resource response is saved eco-friendly call, is again the concrete behave that advances Chrysanthemum morifolium industrial chain extension, simultaneously also for other comprehensive development and utilizations containing volatile oil component medical material are offered reference.
5, recovery process of the present invention easy row convenient and simple for operation.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is the fuel-displaced rule figure of volatile oil of the present invention;
Fig. 3 is the changes of contents figure of Aromatic water of the present invention.
The specific embodiment
Below by embodiment, technical scheme of the present invention is elaborated.
Embodiment 1: fresh Chrysanthemum morifolium enters after automatization's fixing dryer, first passes through 100 ℃ of green removing in high temperature of 50s; Then automatically proceeding to dehydrator dries, bake out temperature is 75 ℃, drying time is 7h, wherein, in drying time 2～6h, collect the water oil mixed vapour producing and enter successively the cooling and oil water separator of condenser, cooling tower and carry out oil-water separation, after profit fully separates, the oil reservoir of opening oil water separator collection upper strata obtains volatile oil, and the water layer of collecting lower floor obtains Aromatic water, and the yield of Aromatic water is no more than 1.5～2 times of Chrysanthemum morifolium fresh weight.
Embodiment 2: fresh Chrysanthemum morifolium enters after automatization's fixing dryer, first pass through 110 ℃ of green removing in high temperature of 45s, now having the high boiling volatile oil of part scatters and disappears out with water vapour, because this part of water oil mixed vapour water content is larger, overall volatile oil content is lower, considering to be not suitable as volatile oil for economic aspect reclaims, therefore passed through circulation condensation device, cooling recovery, and carry out simple processed and can be developed into the primary product such as chrysanthemum juice, for guaranteed quality, the yield of chrysanthemum juice is no more than the fresh weight of Flos Chrysanthemi.Then, Flos Chrysanthemi is proceeded to dehydrator automatically and dry, controlling bake out temperature is 70 ℃, and drying time is 6.5h.Known according to the experience in the course of processing, initial vapour pressure of drying Flos Chrysanthemi surface in 3h can obviously be greater than airborne vapour pressure, surface water branch experiences a diffusion process fast, because moisture is higher, therefore be also not suitable for the oil recovery that volatilizees, can directly lead back steam beating dehydrator and produce steam for the use that completes.Certainly, also can collect this steaming that completes process generation and become chrysanthemum juice, and the yield of chrysanthemum juice should not exceed the fresh weight of Flos Chrysanthemi.
Then, all to pass through condenser from drying steam all in 3rd～6h, cooling tower carries out cooling and enters oil water separator and separate, after profit fully separates, open oil water separator and collect the oil reservoir on upper strata and obtain volatile oil, the water layer of collecting lower floor obtains Aromatic water, and the yield of simultaneously guaranteeing Aromatic water is no more than 1.5～2 times of Chrysanthemum morifolium fresh weight, the Aromatic water quality now obtaining is better, collects comparatively economical.In half an hour, (finishing) subsequently Flos Chrysanthemi moisture to drying from drying 6h reduces very fast, in the situation that total volatile oil content is certain, can be considerably less with water vapor diffusion low boiling volatile oil content out, therefore volatile oil does not need to reclaim yet again, can directly lead back steam beating dehydrator yet and recycle.Also can collect this steaming that completes process generation and become chrysanthemum juice, and the yield of chrysanthemum juice is no more than the fresh weight of Flos Chrysanthemi.
Embodiment 3: basic step is identical with embodiment 2, difference is: the temperature that completes is controlled at 105 ℃, fixation time is 55s; Bake out temperature is 72 ℃, and drying time is 7.5h.The water oil mixed vapour that collection drying time produces in 3～5h also carries out subsequent treatment, separates and obtains volatile oil, and the volatile oil degree of unsaturation now obtaining is high, best in quality.
Claims (9)
1. a recovery method for by-product in the Chrysanthemum morifolium course of processing, is characterized in that comprising the steps:
(1) to the processing that completes of fresh Chrysanthemum morifolium, the temperature that completes is 100～110 ℃, and fixation time is 45～55s;
(2) Chrysanthemum morifolium after completing is dried, bake out temperature is 70～75 ℃, drying time is 6.5～7.5h, wherein, the water oil mixed vapour that collection drying time produces in 2～6h also enters condenser, cooling tower and oil water separator successively, separating through oil water separator the upper strata oil reservoir obtaining is volatile oil, and lower aqueous layer is Aromatic water.
2. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 1, is characterized in that: in step (2), collect the water oil mixed vapour that described drying time produces in 3～6h and carry out subsequent treatment, separating and obtain Aromatic water.
3. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 1, is characterized in that: in step (2), collect the water oil mixed vapour that described drying time produces in 3～5h and carry out subsequent treatment, separating and obtain volatile oil.
4. according to the recovery method of by-product in the Chrysanthemum morifolium course of processing described in claim 1,2 or 3, it is characterized in that: in step (2), collect from drying and start to dry the water oil mixed vapour producing and carry out the processing that completes in step (1) to entering condenser this one-phase, then the water oil mixed vapour that collecting completes produces enters cycle condenser, and cooling recovery obtains chrysanthemum juice.
5. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 1, is characterized in that: in step (2), collect and dry the water oil mixed vapour that produces in last 0.5～1h and use as step (1) steam of processing that completes.
6. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 1, it is characterized in that: after step (1) finishes, before step (2) generation, the collection water oil mixed vapour producing that completes enters cycle condenser, and cooling recovery obtains chrysanthemum juice.
7. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 4, is characterized in that: the yield of described chrysanthemum juice is no more than the fresh weight of Chrysanthemum morifolium.
8. the recovery method of by-product in the Chrysanthemum morifolium course of processing according to claim 6, is characterized in that: the yield of described chrysanthemum juice is no more than the fresh weight of Chrysanthemum morifolium.
9. according to the recovery method of by-product in the Chrysanthemum morifolium course of processing described in claim 1 or 2, it is characterized in that: in step (2), the yield of described Aromatic water is no more than 1.5～2 times of Chrysanthemum morifolium fresh weight.
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| CN114993025A (en) * | 2022-06-28 | 2022-09-02 | 浙江迪邦化工有限公司 | Continuous drying device and method for N, N-cyanoethyl benzyl aniline |
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| CN114993025A (en) * | 2022-06-28 | 2022-09-02 | 浙江迪邦化工有限公司 | Continuous drying device and method for N, N-cyanoethyl benzyl aniline |
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