CN114699503B - Spray drying method for Chinese medicinal extract and preparation method of granule - Google Patents

Spray drying method for Chinese medicinal extract and preparation method of granule Download PDF

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CN114699503B
CN114699503B CN202210322163.6A CN202210322163A CN114699503B CN 114699503 B CN114699503 B CN 114699503B CN 202210322163 A CN202210322163 A CN 202210322163A CN 114699503 B CN114699503 B CN 114699503B
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image
monitoring area
spray drying
pixel ratio
screening
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CN114699503A (en
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马善恒
马号
张友飞
唐永红
王磊
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Hunan Dongjian Pharmaceutical Co ltd
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Hunan Dongjian Pharmaceutical Co ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/284—Atractylodes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/06—Fungi, e.g. yeasts
    • A61K36/07—Basidiomycota, e.g. Cryptococcus
    • A61K36/076—Poria
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/17—Gnetophyta, e.g. Ephedraceae (Mormon-tea family)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236—Ligusticum (licorice-root)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/34—Campanulaceae (Bellflower family)
    • A61K36/346—Platycodon
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484—Glycyrrhiza (licorice)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
    • A—HUMAN NECESSITIES
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/57—Magnoliaceae (Magnolia family)
    • A61K36/575—Magnolia
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/65—Paeoniaceae (Peony family), e.g. Chinese peony
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/75—Rutaceae (Rue family)
    • A61K36/752—Citrus, e.g. lime, orange or lemon
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/888—Araceae (Arum family), e.g. caladium, calla lily or skunk cabbage
    • A61K36/8888—Pinellia
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/906—Zingiberaceae (Ginger family)
    • A61K36/9068—Zingiber, e.g. garden ginger
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605—Excipients; Inactive ingredients
    • A61K9/1629—Organic macromolecular compounds
    • A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
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    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682—Processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0082—Regulation; Control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract

A spray drying method for extracting clear paste from traditional Chinese medicine and a production process of Wuji granules relate to the technical field of production and processing of Chinese patent medicines. The invention judges whether the corresponding monitoring area in the drying tower is adhered by analyzing the difference value of the average brightness value of the images of the monitoring areas, and estimates the particle size and the content of the powder distributed in the corresponding monitoring area in the real-time image by screening the differential image obtained by subtracting the real-time image from the initial image and analyzing the pixel ratio of the screened image to the differential image, thereby prejudging whether the wall adhesion phenomenon is likely to occur in the subsequent spray drying process.

Description

Spray drying method for Chinese medicinal extract and preparation method of granule
Technical Field
The invention relates to the technical field of Chinese patent medicine production and processing, in particular to a spray drying method for extracting a clear paste from traditional Chinese medicine and a production process of five-drug granules.
Background
Spray drying technology was used in the food field in the early days and has gradually been applied in the production and processing of Chinese herbs in recent years. Because the components of the traditional Chinese medicine extracting solution are complex, the wall adhesion phenomenon is more likely to occur in the spray drying process. Wall sticking refers to that in the spraying process of the traditional Chinese medicine extraction concentrated solution, products are accumulated and adhered to the surface of the inner wall of the drying tower, the medicinal powder stays on the hot tower wall for a long time, the heating time is prolonged, the product quality is influenced, the normal production is not facilitated, and the wall sticking phenomenon is influenced by multiple factors such as the material liquid characteristics, the process parameters and the like. Different from traditional Chinese medicine products with relatively single raw materials, the Wuji granules relate to a plurality of raw materials, and the quality fluctuation of any one raw material can cause the change of the characteristics of spray-dried feed liquid, so that the production process parameters of the previous batch can not be suitable for the current batch, and therefore, a specially-assigned person needs to be arranged to pay attention to the situation in the drying tower all the time, and how to quickly find a targeted measure to eliminate or reduce the phenomenon of powder wall adhesion becomes a difficulty in the production process, and the popularization and application of the spray-drying process in the production of the Wuji granules are also hindered.
In view of the above reasons, there are still many traditional Chinese medicine factories that use the traditional process similar to that in chinese patent document CN1116531A to produce wuji granules, namely, firstly extracting volatile oil from rhizoma atractylodis, fructus aurantii, pericarpium citri reticulatae, cassia twig, rhizoma zingiberis, radix angelicae, angelica sinensis and ligusticum wallichii, decocting the dregs after extracting the volatile oil with platycodon grandiflorum, ephedra, pinellia ternate, liquorice and radix paeoniae alba in water to obtain filtrate, combining the obtained filtrate and the steeping liquor obtained by warm soaking of poria cocos, concentrating the mixture into clear paste, then preparing magnolia officinalis extract through cortex magnoliae officinalis through dipping, mixing the extract with the clear paste, adding dextrin, granulating, spraying the volatile oil, and mixing uniformly. However, the process has the defects of difficult uniform mixing, long drying time and low consistency of product quality due to the fact that the amount of the extracted clear paste (including magnolia officinalis extract) is large.
Disclosure of Invention
One of the purposes of the invention is to provide a spray drying method of the Chinese medicine extract, which can reduce the phenomenon that the medicine powder is adhered to the wall in the spray drying production process and improve the product quality.
The spray drying method for extracting the clear paste from the traditional Chinese medicine comprises the steps of arranging a backlight module for illuminating a spray drying chamber on one side of a spray drying tower, and arranging a camera module for acquiring images in the spray drying chamber on the side opposite to the backlight module;
acquiring an initial image in a spray drying chamber before spray drying starts each time, periodically acquiring a real-time image in the spray drying chamber in the spray drying process, and taking a top area close to the top wall of the tower body as a # 1 monitoring area, one side or two side areas close to the side wall of the tower body as a # 2 monitoring area and a bottom area close to the conical bottom wall of the tower body as a # 3 monitoring area in the initial image and the real-time image;
calculating the difference value of the average brightness of each monitoring area in the initial image and the real-time image; carrying out differential processing on the initial image and the real-time image, screening the images in the differential image through a set size specification, and calculating the pixel ratio of the screened image to the differential image;
and regulating and controlling spray drying process parameters according to the average brightness difference value and the pixel ratio calculation result of each monitoring area.
In an embodiment of the invention, the spray drying method includes the following steps:
1. acquiring and analyzing a monitoring image;
respectively calculating the average brightness values of a 1# monitoring area, a 2# monitoring area and a 3# monitoring area in the initial image and the real-time image, and calculating the average brightness difference value of the corresponding monitoring areas in the initial image and the real-time image;
extracting pixels of a No. 1 monitoring area, a No. 2 monitoring area and a No. 3 monitoring area in the initial image and the real-time image, subtracting the pixels in the initial image and the real-time image from the pixels in the corresponding monitoring area to obtain a differential image, screening the differential image through one large dimension and one small dimension, respectively removing figures smaller than the two dimensions and reserving figures larger than the two dimensions, and respectively calculating the pixel ratio of the two screened images to the differential image after obtaining the screened image;
2. adjusting spray drying process parameters;
if the average brightness difference value of a certain monitoring area is larger than a set upper limit value, controlling a powder removing device to remove powder accumulated in the monitoring area;
if the pixel ratio of the screening image and the difference image corresponding to a certain monitoring area exceeds a set range, one or more of the air inlet flow, the air exhaust flow, the feeding speed, the atomizing pressure and the air inlet temperature of the spray drying chamber are adjusted until the pixel ratio of the screening image and the difference image corresponding to the monitoring area is within the set range.
In the first step, when the differential image is screened and the pixel ratio of the screened image to the differential image is calculated: removing the graphs with the size smaller than the small-size specification and the graphs with the size above the small-size specification in the differential image to obtain a first screening image; removing the graphs with the size smaller than the large-size specification and the graphs with the size above the large-size specification in the differential image to obtain a second screening image; respectively calculating the pixel ratio of the first screening image to the difference image and the pixel ratio of the second screening image to the difference image;
in the second step, if the pixel ratio of the first screening image to the differential image and/or the pixel ratio of the second screening image to the differential image corresponding to a certain monitoring area exceeds a set range, one or more of the air inlet flow, the air exhaust flow, the feeding speed, the atomizing pressure and the air inlet temperature of the spray drying chamber are adjusted until the pixel ratio of the first screening image to the differential image and the pixel ratio of the second screening image to the differential image corresponding to the monitoring area are within the set range.
In an embodiment of the present invention, if the pixel ratio of the first screened image and the differential image corresponding to the 1# monitoring area is less than or equal to the first threshold, the exhaust flow of the spray drying chamber is increased and the atomization pressure is decreased at a given rate until the pixel ratio of the first screened image and the differential image corresponding to the monitoring area is greater than the first threshold.
In an embodiment of the present invention, if the pixel ratio of the second classified image and the differential image corresponding to the 1# monitoring area is greater than or equal to the second threshold, the exhaust flow and the atomization pressure of the spray drying chamber are increased at a given rate until the pixel ratio of the second classified image and the differential image corresponding to the monitoring area is less than the second threshold.
In an embodiment of the present invention, if the pixel ratio of the first screening image and the differential image corresponding to the # 2 monitoring area is smaller than or equal to the first threshold, the exhaust air flow rate and the intake air temperature of the spray drying chamber are increased at a given rate, and the atomization pressure is reduced until the pixel ratio of the first screening image and the differential image corresponding to the monitoring area is greater than the first threshold.
In an embodiment of the present invention, if the pixel ratio of the second screened image to the differential image corresponding to the # 2 monitoring area is greater than or equal to the second threshold, the exhaust flow rate and the atomization pressure of the spray drying chamber are increased and the feeding speed is decreased at a given rate until the pixel ratio of the second screened image to the differential image corresponding to the monitoring area is less than the second threshold.
In an embodiment of the present invention, if the pixel ratio of the first screened image and the difference image corresponding to the 3# monitoring area is less than or equal to the first threshold, the air inlet flow and the air inlet temperature of the spray drying chamber are increased at a given rate, and the atomization pressure is reduced until the pixel ratio of the first screened image and the difference image corresponding to the monitoring area is greater than the first threshold.
In an embodiment of the present invention, if the pixel ratio of the second screening image and the differential image corresponding to the # 3 monitoring area is greater than or equal to the second threshold, the air inlet flow and the air inlet temperature of the spray drying chamber are increased at a given rate, and the feeding speed is decreased until the pixel ratio of the second screening image and the differential image corresponding to the monitoring area is less than the second threshold.
Based on the spray drying method, the invention also relates to a production process of the Wuji powder granules, which specifically comprises the following steps:
1. extracting volatile oil and making clear paste dry powder;
1.1 adding water into rhizoma atractylodis, fructus aurantii, dried orange peel, cassia twig, dried ginger, radix angelicae, angelica sinensis and ligusticum wallichii to extract volatile oil, separating oil from water to obtain volatile oil for later use, and collecting the aqueous solution and the dregs in another container respectively;
1.2 decocting the residues obtained in the step 1.1, platycodon grandiflorum, ephedra, pinellia ternate, liquorice and radix paeoniae alba in water, and filtering decoction; boiling Poria in water, soaking for several times, and filtering the soaking solution;
1.3 concentrating the filtrate obtained in the step 1.2 and the aqueous solution obtained in the step 1.1 into clear paste, and preparing the clear paste into dry powder by adopting the spray drying method;
2. preparing magnolia officinalis extract, adding a proper amount of dextrin into the extract, uniformly mixing, drying, crushing, uniformly mixing the obtained powder with the dry powder obtained in the step 1.3, adding a proper amount of dextrin, uniformly mixing, adding a proper amount of ethanol, preparing into granules, diluting the volatile oil obtained in the step 1.1 with a proper amount of absolute ethanol, spraying the obtained granules, stewing, and uniformly mixing to obtain the Wuji powder granules.
The spray drying chamber is divided into three monitoring areas, namely a top monitoring area, a side monitoring area and a bottom monitoring area, whether the corresponding monitoring area is sticky or possibly sticky is judged by comparing and calculating a real-time image acquired in the operation process with an initial image acquired before the operation is started, and then corresponding treatment and preventive measures are taken. Specifically, the invention judges whether the corresponding monitoring area is sticky or not by analyzing the difference value of the average brightness values of the images of the monitoring areas, and estimates the particle size and the content of the powder distributed in the corresponding monitoring area in the real-time image by screening the differential image (subtracting the real-time image from the initial image) and analyzing the pixel ratio of the screened image to the differential image, thereby prejudging whether the sticky wall phenomenon is likely to occur or not. In addition, the backlight module used for illuminating the spray drying chamber is arranged on one side of the spray drying tower, the camera module used for acquiring the image in the spray drying chamber is arranged on the side opposite to the backlight module, and the camera module and the backlight module are oppositely arranged, so that in the image shot by adopting backlight, a main body (powder particles) and a background (drying chamber) have high contrast, and the extraction and analysis of a target object in the image are facilitated, the calculated amount is reduced, the operation speed is improved, and the timeliness of a judgment result can be better ensured. Different from the traditional manual watching mode, the spray drying method adopted by the invention can judge/predict the wall sticking condition in the tower in real time and take corresponding measures, thereby reducing the wall sticking phenomenon of the medicinal powder in the spray drying production process and improving the product quality.
Drawings
FIG. 1 is a flow chart of a production process of five-particle granules in the example.
FIG. 2 is a schematic diagram of the spray drying process parameter control of Chinese medicinal fluid extract.
Detailed Description
To facilitate understanding of those skilled in the art, the present invention will be further described with reference to the following detailed description and accompanying drawings.
The formula of the raw materials for preparing the wuji granules in this example is as follows: 200g of rhizoma atractylodis (stir-fried with bran), 150g of platycodon grandiflorum, 125g of fructus aurantii (stir-fried with bran), 125g of dried orange peel, 125g of cassia twig, 100g of ephedra, 100g of magnolia officinalis (processed with ginger), 75g of dried ginger, 75g of pinellia ternate (processed), 75g of poria cocos, 75g of liquorice, 75g of radix angelicae, 75g of angelica sinensis, 75g of radix paeoniae alba and 50g of ligusticum wallichii.
Fig. 1 shows the process of preparing penta-particles in this example. The method comprises the following specific steps:
1. extracting rhizoma Atractylodis, fructus Aurantii, pericarpium Citri Tangerinae, ramulus Cinnamomi, zingiberis rhizoma, radix Angelicae Dahuricae, radix Angelicae sinensis, and rhizoma Ligustici Chuanxiong with 3 times of water to obtain volatile oil, separating oil and water, collecting the volatile oil and water solution and residue in another container.
2. Decocting the above residue, radix Platycodi, herba Ephedrae, rhizoma Pinelliae, glycyrrhrizae radix, and radix Paeoniae alba with water twice, 6 times of water for the first time, 1.5 hr for the second time, 4 times of water for 1.5 hr for the second time, and filtering the decoction.
3. Adding water into Poria, boiling, soaking twice at 80 deg.C for 3 hr with 8 times of water, soaking for 2 hr with 8 times of water, and filtering.
4. Mixing the filtrate obtained in the steps 2 and 3 with the aqueous solution obtained in the step 1, concentrating the mixture to obtain clear paste with the relative density of 1.10 (60 ℃), and performing spray drying to obtain dry powder.
5. Coarsely crushing the magnolia officinalis, soaking the crushed magnolia officinalis in 60% ethanol as a solvent for 24 hours, slowly percolating the magnolia officinalis, collecting about 1100ml of percolate, recovering ethanol under reduced pressure, concentrating the percolate until the relative density is 1.10 (60 ℃), adding a proper amount of dextrin into the percolate, mixing the percolate with the dry powder obtained in the step (4), drying the mixture, crushing the mixture, adding a proper amount of dextrin into the dry powder obtained in the step (4), uniformly mixing the mixture with the dextrin, adding a proper amount of 65% ethanol into the mixture, preparing the mixture into granules, spraying the volatile oil obtained in the step (1) (diluting the volatile oil with a proper amount of absolute ethanol), and uniformly mixing the granules after the mixture is stuffy, so as to obtain the Wujie granules.
Different from the traditional process, the traditional Chinese medicine extract is concentrated to a certain degree and then directly sprayed into dry powder, the magnolia officinalis is dried according to the fluid extract and then crushed, and then the dry powder and the magnolia officinalis are mixed and granulated. In addition, compare in traditional concentrated mode, this embodiment can also greatly increased production efficiency through adopting the spray drying technology, reduces the energy consumption, improves the product yield.
It should be noted that, because the five-volume granules relate to a plurality of kinds of raw materials, and the quality fluctuation of any raw material may cause the characteristics of the spray-dried material liquid to change, so that the production process parameters of the previous batch may not be suitable for the current batch, thereby causing the phenomenon of sticking of powder to the wall in the spray-drying process of the clear paste by using the traditional process, and the factory needs to arrange a special person to watch and frequently stop the machine for processing. In order to solve the above problems, the present example is an improvement of the spray drying method for extracting the fluid extract from the traditional Chinese medicine. The core thought of the improved spray drying process is to judge whether the corresponding monitoring area is adhered to the wall or not by analyzing the difference value of the average brightness value of the images of the monitoring areas in the drying tower before the operation starts and analyzing the pixel ratio of the screened image to the differential image to estimate the particle size and content of the powder distributed in the corresponding monitoring area in the real-time image, thereby judging whether the wall adhesion phenomenon is possible or not.
When the method is implemented, firstly, a backlight module used for illuminating the spray drying chamber is arranged on one side of the spray drying tower, and a camera module used for acquiring images in the spray drying chamber is arranged on the other side (the side opposite to the backlight module) of the spray drying tower. The initial image in the spray drying chamber is obtained before the spray drying starts at every time through the camera module, and the real-time image in the spray drying chamber is periodically obtained in the spray drying process. Because the camera module and the backlight module are arranged oppositely, in an image shot by adopting backlight, the main body (powder particles) and the background (drying chamber) have high contrast, and the extraction and analysis of a target object in the image are more facilitated, so that the calculated amount is reduced, the operation speed is increased, and the timeliness of a judgment result can be better ensured. Meanwhile, in the obtained initial image and the real-time image, the top area close to the top wall of the tower body is a # 1 monitoring area, the area on one side or two sides close to the side wall of the tower body is a # 2 monitoring area, and the bottom area close to the conical bottom wall of the tower body is a # 3 monitoring area. The method comprises the steps of calculating average brightness difference values corresponding to monitoring areas in an initial image and a real-time image, carrying out difference processing on the initial image and the real-time image, screening graphs in the difference image through a set size specification, calculating a pixel ratio of the obtained screened image to the obtained difference image, and finally regulating and controlling spray drying process parameters according to the average brightness difference values and the pixel ratio calculation results of the monitoring areas.
Fig. 2 shows the principle of regulating and controlling the technological parameters of spray drying, and the process of regulating and controlling the technological parameters comprises the following steps:
1. acquiring and analyzing a monitoring image;
1.1 calculating the average brightness values of the No. 1 monitoring area, the No. 2 monitoring area and the No. 3 monitoring area in the initial image and the real-time image respectively and calculating the average brightness difference value of the corresponding monitoring area in the initial image and the real-time image. Taking the # 1 monitoring region as an example, when calculating the average brightness value in the initial image, for each pixel in the initial image, the brightness value Lum (x, y) of the pixel is calculated first, then the natural logarithm of the brightness value is obtained, then the logarithms of the brightness values of all the pixels are averaged, and then the natural index value of the average value is obtained, so as to obtain the average brightness value of the # 1 monitoring region in the initial image. Similarly, the average brightness value of the 1# monitoring region in the real-time image can be calculated by the same method. And finally, subtracting the two images to obtain the average brightness difference value of the 1# monitoring area in the initial image and the real-time image.
1.2, extracting the pixels of the No. 1 monitoring area, the No. 2 monitoring area and the No. 3 monitoring area in the initial image and the real-time image (the image of the monitoring area can be subjected to binarization processing according to requirements), and subtracting the pixels in the initial image and the real-time image from the corresponding monitoring area to obtain a difference image. And screening the difference image according to two different sizes, namely a large size and a small size, respectively removing the graphs smaller than the two sizes, and reserving the graphs larger than the two sizes to obtain a screened image, and then respectively calculating the pixel ratio of the two screened images to the difference image. When screening the differential image and calculating the pixel ratio of the screened image to the differential image, the differential image can be binarized, then the image can be screened for graphic elements by using a closed operation, and the graphics with the size smaller than the small-size specification and the graphics with the size above the small-size specification in the differential image are removed to obtain a first screened image. And similarly, removing the graphs with the size smaller than the large-size specification and the graphs with the size above the large-size specification in the differential image to obtain a second screening image. And finally, respectively calculating the pixel ratio of the first screening image to the difference image and the pixel ratio of the second screening image to the difference image.
It should be noted that, the above-mentioned one big one little two kinds of different size specifications can be confirmed through carrying out earlier stage test to the spray drying system, and during earlier stage test, through setting up different size specifications and testing its response sensitivity of prejudging to the wall sticking phenomenon, can obtain the wall sticking under the different size specification condition through a large amount of earlier stage tests and prejudge the test record, sieve out suitable size specification from the test record that obtains again.
2. Adjusting spray drying process parameters;
and 2.1 if the average brightness difference value of a certain monitoring area is larger than a set upper limit value, controlling a powder removing device to remove powder accumulated in the monitoring area. The principle of judging whether the wall sticking phenomenon occurs or not through the average brightness difference value is as follows: after the wall sticking phenomenon occurs, a large amount of powder is adhered to the inner wall of the drying tower, the powder adhered to the wall of the drying tower has light impermeability, the light reflectivity of the powder material is also obviously lower than that of a smooth tower wall, and the average brightness value of a real-time image is obviously lower than that of an initial image. Considering that the powder dispersed in the air in the spray drying process can shield the light emitted by the backlight module, and the shielding formed by the powder dispersed in the air is limited, in this embodiment, an upper limit value of the average brightness difference is set, and the condition that the powder shielding in the air and the powder sticking wall/pseudo sticking wall with a very small amount (the powder falls off when adhering to a section of the tower wall, which is called pseudo sticking wall, and the powder amount of the pseudo sticking wall is generally less) are filtered through the upper limit value, only when a large amount of powder sticking wall occurs, it is determined that the sticking wall phenomenon has occurred in the monitoring area, and then the powder removing device is controlled to remove the powder accumulated in the monitoring area.
2.2 if the pixel ratio of the screening image and the difference image corresponding to a certain monitoring area exceeds a set range, adjusting one or more of the air inlet flow, the air outlet flow, the feeding speed, the atomizing pressure and the air inlet temperature of the spray drying chamber until the pixel ratio of the screening image and the difference image corresponding to the monitoring area is within the set range.
The step is mainly to regulate and control the drying process parameters of the shed by pre-judging the possibility of the wall sticking phenomenon in the monitoring area (the wall sticking phenomenon is considered to be possible to occur if the pixel ratio exceeds a set range) so as to prevent the wall sticking phenomenon from really occurring in the monitoring area. The principle of prejudging the occurrence of the wall sticking phenomenon by screening the pixel ratio of the image to the differential image is as follows: assume that the small size specification is 4 × 4 and the large size specification is 8 × 8. During screening processing, a matrix with structural elements of 4 multiplied by 4 is selected, and the result of closing operation on the differential image after binarization processing enables all graphic elements with the size smaller than 4 multiplied by 4 to be eliminated, so as to obtain a first screened image; and selecting a matrix with structural elements of 8 multiplied by 8, and eliminating all graphic elements with the size smaller than 8 multiplied by 8 as a result of closing the differential image to obtain a second screening image. Thus, in the first screening image, the powder images with the size smaller than 4 × 4 are all screened out, and only the powder images with the size larger than 4 × 4 are left; in the second sifted image, the powder images with the size smaller than 8 × 8 are all sifted out, and only the powder images with the size larger than 8 × 8 are left. By analyzing the pixel ratio of the first screening image, the second screening image and the difference image, the particle size and the content of the powder distributed in the corresponding monitoring area in the real-time image can be estimated. The occurrence of the wall sticking phenomenon is closely related to the region in which the powder is distributed, the particle size range of the distributed powder in the region, and the content thereof. For example, the smaller the particle size of the powder, the better the drying effect, and the less likely semi-wet wall-sticking phenomenon, but the smaller the particle size, the larger the specific surface area, the more likely dry wall-sticking (also referred to as "dry wall-sticking") occurs, and this can be avoided well by controlling the particle size distribution of the powder within a reasonable range. For another example, if a large amount of powder is distributed in the top 1# monitoring area (the powder appearing in the 1# monitoring area is generally small in particle size), it is indicated that the powder is back on the top in the tower, and a wall sticking phenomenon is likely to occur at the top wall. By analyzing the powder distribution condition in each monitoring area, the possibility of wall adhesion in the monitoring area can be estimated.
For example, in the process of spray drying operation, if the pixel ratio of the first screened image to the differential image or the pixel ratio of the second screened image to the differential image corresponding to a certain monitoring area exceeds a set range, one or more of the air inlet flow, the air outlet flow, the feeding speed, the atomizing pressure and the air inlet temperature of the spray drying chamber are adjusted until the pixel ratio of the first screened image to the differential image and the pixel ratio of the second screened image to the differential image corresponding to the monitoring area are both within the set range.
Specifically, if the pixel ratio of the first screening image to the differential image corresponding to the 1# monitoring area is smaller than or equal to a first threshold (that is, the powder with small particle size returns to the top and the content of the powder exceeds the limit), the exhaust flow of the spray drying chamber is increased at a given rate, the atomization pressure is reduced (the negative pressure in the tower is increased after the exhaust flow is increased, so that the phenomenon of returning to the top is reduced, the particle size of the atomized liquid drops can be increased by reducing the atomization pressure, so that the particle size of the dried powder is increased, and the phenomenon of returning to the top is also reduced when the particle size of the powder is increased) until the pixel ratio of the first screening image to the differential image corresponding to the monitoring area is larger than the first threshold. If the pixel ratio of the second screening image corresponding to the 1# monitoring area to the differential image is larger than or equal to a second threshold value (namely the powder with large particle size returns to the top and the content of the powder exceeds the limit), the exhaust flow and the atomization pressure of the spray drying chamber are increased at a given speed (the negative pressure in the tower is increased after the exhaust flow is increased, so that the phenomenon of returning to the top is reduced, the particle size of atomized liquid drops can be reduced by increasing the atomization pressure, so that the particle size of the dried powder is reduced, the drying effect of the powder is ensured, and semi-wet wall adhesion is avoided) until the pixel ratio of the second screening image corresponding to the monitoring area to the differential image is smaller than the second threshold value. If the pixel ratio of the first screening image and the differential image corresponding to the 2# monitoring area is smaller than or equal to a first threshold value (namely, the powder with small particle size overflows to the periphery of the drying chamber and the content of the powder exceeds the limit), the exhaust flow rate and the intake air temperature of the spray drying chamber are increased at a given rate, and the atomization pressure is reduced (the negative pressure in the tower is increased after the exhaust flow rate is increased, so that the powder is more concentrated in the central area of the drying chamber, the problem that the atomized liquid drops overflow to the periphery of the drying chamber is solved, the particle size of the atomized liquid drops can be increased by reducing the atomization pressure, the particle size of the dried powder is increased, the problem that the atomized liquid drops/dried fine powder overflows to the periphery of the drying chamber is better avoided, and the pixel ratio of the first screening image and the differential image corresponding to the monitoring area is larger than the first threshold value. If the pixel ratio of the second screening image corresponding to the No. 2 monitoring area to the differential image is larger than or equal to a second threshold value (namely, the powder with large particle size overflows to the periphery of the drying chamber and the content of the powder exceeds the limit), the exhaust flow and the atomization pressure of the spray drying chamber are increased at a given rate, the feeding speed is reduced (the negative pressure in the tower is increased after the exhaust flow is increased, so that the powder is more concentrated in the central area of the drying chamber, the problem that the atomized liquid drops overflow to the periphery of the drying chamber is solved, the particle size of the atomized liquid drops can be reduced by increasing the atomization pressure, the drying effect is packaged, the semi-wet wall sticking situation is prevented, the quantity of the liquid drops atomized into the drying chamber in unit time can be reduced by reducing the feeding speed, the problem that the atomized liquid drops/dried powder overflow to the periphery of the drying chamber is solved), and the pixel ratio of the second screening image corresponding to the monitoring area to the differential image is smaller than the second threshold value. If the pixel ratio of the first screening image corresponding to the 3# monitoring area to the differential image is smaller than or equal to a first threshold value (namely, the powder with small particle size overflows to the conical bottom of the drying chamber and the content of the powder exceeds the limit), the air inlet flow and the air inlet temperature of the spray drying chamber are increased at a given rate, the atomization pressure is reduced (the drying speed can be increased by increasing the air inlet flow and the air inlet temperature, the particle size of atomized liquid drops can be increased by reducing the atomization pressure, the particle size of the powder formed by drying can be increased by the two means acting together while the drying effect is ensured, and the common situation that the powder sticks to the wall at the conical bottom is avoided until the pixel ratio of the first screening image corresponding to the monitoring area to the differential image is larger than the first threshold value. If the pixel ratio of the second screening image corresponding to the No. 3 monitoring area to the differential image is larger than or equal to a second threshold value (namely, the powder with large particle size overflows to the conical bottom of the drying chamber and the content of the powder exceeds the limit), the air inlet flow and the air inlet temperature of the spray drying chamber are increased at a given rate, the feeding speed is reduced (the drying speed can be increased by increasing the air inlet flow and the air inlet temperature, and the feeding speed can be reduced by reducing the number of liquid drops atomized into the drying chamber in unit time, so that the situation that the atomized liquid drops collide with each other and are combined into overlarge liquid drops is relieved. It should be noted that the "given rate" in the above-mentioned different cases may be set differently. In addition, in a general case, a situation that the pixel ratios of the 1# monitoring region and the 3# monitoring region both exceed a set range (on the premise that the size of the drying tower is reasonably designed, the top-returning sticky wall and the cone bottom sticky wall do not generally appear at the same time) does not occur, but a situation that the pixel ratios of the 1# monitoring region and the 2# monitoring region both exceed the set range or the pixel ratios of the 2# monitoring region and the 3# monitoring region both exceed the set range sometimes occurs, and at this time, the above means for regulating and controlling the single situation can be combined to obtain a process parameter regulating and controlling scheme under a composite situation. According to the analysis, the method is different from the traditional manual watching mode, the spray drying method adopted in the embodiment judges/predetermines the wall sticking condition in the tower and adopts corresponding measures by analyzing the real-time images of all monitoring areas, the automation degree of the spray drying process is higher, the powder wall sticking phenomenon in the spray drying production process can be effectively reduced, and the product quality is ensured.
The above embodiments are preferred implementations of the present invention, and the present invention can be implemented in other ways without departing from the spirit of the present invention.
Some of the figures and descriptions of the present invention have been simplified to provide a convenient understanding of the modifications of the invention relative to the prior art, and to omit elements for clarity, as those skilled in the art will recognize may also constitute the subject matter of the present invention.

Claims (8)

1. The spray drying method of the Chinese medicine extract is characterized in that:
arranging a backlight module for illuminating the spray drying chamber on one side of the spray drying tower, and arranging a camera module for acquiring images in the spray drying chamber on the side opposite to the backlight module;
acquiring an initial image in a spray drying chamber before spray drying starts each time, periodically acquiring a real-time image in the spray drying chamber in the spray drying process, and taking a top area close to the top wall of the tower body as a # 1 monitoring area, one side or two side areas close to the side wall of the tower body as a # 2 monitoring area and a bottom area close to the conical bottom wall of the tower body as a # 3 monitoring area in the initial image and the real-time image;
calculating the average brightness difference value corresponding to each monitoring area in the initial image and the real-time image, and judging whether the corresponding monitoring area is sticky or not by analyzing the difference value of the average brightness values of the images of each monitoring area: respectively calculating the average brightness values of a 1# monitoring area, a 2# monitoring area and a 3# monitoring area in the initial image and the real-time image, and calculating the average brightness difference value of the corresponding monitoring areas in the initial image and the real-time image;
if the average brightness difference value of a certain monitoring area is larger than a set upper limit value, controlling a powder removing device to remove powder accumulated in the monitoring area;
carrying out differential processing on the initial image and the real-time image, screening the image in the differential image through a set size specification, calculating the pixel ratio of the screened image to the differential image, estimating the particle size and the content of powder distributed in a corresponding monitoring area in the real-time image by analyzing the pixel ratio of the screened image to the differential image, and further judging whether the wall sticking phenomenon possibly occurs or not in advance: extracting pixels of a No. 1 monitoring area, a No. 2 monitoring area and a No. 3 monitoring area in the initial image and the real-time image, subtracting the pixels in the initial image and the real-time image from the pixels in the corresponding monitoring area to obtain a differential image, screening the differential image through two different size specifications of one large size and one small size, removing graphs with the size smaller than the small size specification and graphs with the size above the small size specification in the differential image to obtain a first screened image; removing the graphs with the size smaller than the large-size specification and the graphs with the size above the large-size specification in the differential image to obtain a second screening image; respectively calculating the pixel ratio of the first screening image to the difference image and the pixel ratio of the second screening image to the difference image;
if the pixel ratio of the first screening image to the differential image or the pixel ratio of the second screening image to the differential image corresponding to a certain monitoring area exceeds a set range, one or more of the air inlet flow, the air exhaust flow, the feeding speed, the atomizing pressure and the air inlet temperature of the spray drying chamber are adjusted until the pixel ratio of the first screening image to the differential image and the pixel ratio of the second screening image to the differential image corresponding to the monitoring area are within the set range.
2. The spray drying method of claim 1, wherein: and if the pixel ratio of the first screening image and the differential image corresponding to the 1# monitoring area is smaller than or equal to a first threshold value, increasing the exhaust flow of the spray drying chamber at a given rate and reducing the atomization pressure until the pixel ratio of the first screening image and the differential image corresponding to the monitoring area is larger than the first threshold value.
3. The spray drying method of claim 1, wherein: and if the pixel ratio of the second screening image and the differential image corresponding to the No. 1 monitoring area is greater than or equal to a second threshold value, increasing the exhaust flow and the atomization pressure of the spray drying chamber at a given rate until the pixel ratio of the second screening image and the differential image corresponding to the monitoring area is less than the second threshold value.
4. The spray drying method of claim 1, wherein: and if the pixel ratio of the first screening image corresponding to the No. 2 monitoring area to the differential image is smaller than or equal to a first threshold value, increasing the exhaust flow and the inlet air temperature of the spray drying chamber at a given rate and reducing the atomization pressure until the pixel ratio of the first screening image corresponding to the monitoring area to the differential image is larger than the first threshold value.
5. The spray drying method of claim 1, wherein: and if the pixel ratio of the second screening image to the differential image corresponding to the No. 2 monitoring area is greater than or equal to a second threshold value, increasing the exhaust flow and the atomization pressure of the spray drying chamber at a given speed and reducing the feeding speed until the pixel ratio of the second screening image to the differential image corresponding to the monitoring area is less than the second threshold value.
6. The spray drying method of claim 1, wherein: and if the pixel ratio of the first screening image and the differential image corresponding to the No. 3 monitoring area is smaller than or equal to a first threshold value, increasing the air inlet flow and the air inlet temperature of the spray drying chamber at a given rate and reducing the atomization pressure until the pixel ratio of the first screening image and the differential image corresponding to the monitoring area is larger than the first threshold value.
7. The spray drying method of claim 1, wherein: and if the pixel ratio of the second screening image and the differential image corresponding to the No. 3 monitoring area is greater than or equal to a second threshold value, increasing the air inlet flow and the air inlet temperature of the spray drying chamber at a given speed and reducing the feeding speed until the pixel ratio of the second screening image and the differential image corresponding to the monitoring area is less than the second threshold value.
8. The preparation method of the five-accumulation granules comprises the following raw material formula: 200g of rhizoma atractylodis stir-fried with bran, 150g of platycodon grandiflorum, 125g of fructus aurantii stir-fried with bran, 125g of dried orange peel, 125g of cassia twig, 100g of ephedra, 100g of cortex magnoliae officinalis processed with ginger, 75g of dried ginger, 75g of processed pinellia ternate, 75g of poria cocos, 75g of liquorice, 75g of radix angelicae, 75g of angelica sinensis, 75g of radix paeoniae alba and 50g of ligusticum wallichii; the method is characterized by further comprising the following steps:
1. extracting volatile oil and making clear paste dry powder;
1.1, adding water into rhizoma atractylodis stir-fried with bran, fructus aurantii stir-fried with bran, dried orange peel, cassia twig, dried ginger, angelica dahurica, angelica and ligusticum wallichii to extract volatile oil, separating oil from water to obtain volatile oil for later use, and collecting the aqueous solution and dregs in another container respectively;
1.2 decocting the dregs obtained in the step 1.1, platycodon root, ephedra, prepared pinellia tuber, liquorice and white paeony root in water, and filtering decoction; boiling Poria in water, soaking for several times, and filtering the soaking solution;
1.3 concentrating the filtrate obtained in the step 1.2 and the aqueous solution obtained in the step 1.1 into clear paste, and preparing the clear paste into dry powder by adopting the spray drying method of any one of claims 1 to 7;
2. preparing ginger magnolia bark extract, adding a proper amount of dextrin into the extract, uniformly mixing, drying, crushing, uniformly mixing the obtained powder with the dry powder obtained in the step 1.3, adding a proper amount of dextrin, uniformly mixing, adding a proper amount of ethanol, granulating, diluting the volatile oil obtained in the step 1.1 with a proper amount of absolute ethanol, spraying the obtained granules, stewing, and uniformly mixing to obtain the Wujie granules.
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