WO2022095174A1 - 一种新型蝙蝠蛾拟青霉提取工艺 - Google Patents

一种新型蝙蝠蛾拟青霉提取工艺 Download PDF

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WO2022095174A1
WO2022095174A1 PCT/CN2020/132612 CN2020132612W WO2022095174A1 WO 2022095174 A1 WO2022095174 A1 WO 2022095174A1 CN 2020132612 W CN2020132612 W CN 2020132612W WO 2022095174 A1 WO2022095174 A1 WO 2022095174A1
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paecilomyces
drying
novel
batmoth
extraction process
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PCT/CN2020/132612
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English (en)
French (fr)
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徐庆阳
王英燕
袁峰
王鹏
范祎立
耿燕
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江苏神华药业有限公司
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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
    • A61K36/06—Fungi, e.g. yeasts
    • A61K36/062—Ascomycota
    • A61K36/066—Clavicipitaceae
    • A61K36/068—Cordyceps
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/001—Drying-air generating units, e.g. movable, independent of drying enclosure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/003—Supply-air or gas filters
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/004—Nozzle assemblies; Air knives; Air distributors; Blow boxes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
    • F26B25/005—Treatment of dryer exhaust gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
    • F26B25/04—Agitating, stirring, or scraping devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/10—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it
    • F26B3/12—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it in the form of a spray, i.e. sprayed or dispersed emulsions or suspensions
    • 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • 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
    • 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

Definitions

  • the invention relates to a novel extraction process of Paecilomyces spp., in particular to a novel material drying method.
  • Paecilomyces batmoth is an asexual generation strain obtained by tissue isolation from the natural Cordyceps sinensis sublocus.
  • the main active components of its mycelium are Cordyceps polysaccharides, amino acids, nucleosides, etc.
  • Modern medical research has found that it has various pharmacological effects such as analgesia, antibacterial, anti-inflammatory, enhancing immunity, lowering blood lipids, anti-oxidation, and anti-cancer.
  • the extraction process of Paecilomyces batmoth mostly adopts the traditional method: it first filters the fermentation broth through a plate and frame, and then goes through a series of drying processes, including ribbon drying, hot air drying, and boiling drying, to obtain low-moisture materials, and finally The product is obtained after crushing, screening and packaging.
  • the method has many steps and takes a long time.
  • the plate and frame filtration takes 4-7 hours, the ribbon drying is 18-24 hours, the hot air drying is 10-16 hours, and the boiling drying is 3 hours.
  • the total time is 35-50 hours.
  • the traditional process steps are complex and time-consuming, resulting in low extraction yield and serious product loss.
  • the object of the present invention is to provide a novel extraction process of Paecilomyces batmoth in view of the deficiencies of traditional techniques.
  • the process can save a lot of time, shorten the process flow, and significantly improve the extraction yield.
  • a novel extraction process of Paecilomyces batmoth the fermented liquid of Paecilomyces batmoth is filtered through a ceramic membrane to obtain a filtrate and a concentrated liquid, and the concentrated liquid is then dried by a spray feed air flow.
  • Spray feed air drying is to use a spray feed air drying system.
  • the concentrated liquid filtered by the ceramic membrane is passed through the pressure nozzle of the air dryer to form droplets and dispersed in the pipeline, and mixed with the opposite high-speed hot air to make the concentrated liquid.
  • the mist droplets are suspended in the hot air, and are dried during the air conveying process, and the dried product is recovered by a cyclone separator at the outlet of the drying pipe.
  • the discharge port of the material storage tank is connected to the feed port of the airflow dryer through a pipeline, and the airflow dryer is mainly composed of an airflow drying tube, a blower, a heater and a cyclone separator located at the airflow outlet of the airflow drying tube.
  • a pressure nozzle at the feed port of the airflow dryer, the air line outlet of the blower is connected to a heater, the outlet of the heater is connected with the outlet of the pressure nozzle through an airflow drying pipe, and a stirring device is provided at the connection.
  • a liquid pump is provided between the material storage tank and the air flow dryer, which is used to drive the feed pipe connected to the outlet of the material storage tank to deliver the material to the pressure spray head.
  • an air filter is arranged between the blower and the heater, and a heating coil and a stirring shaft are installed inside the material storage tank.
  • the stirring device is connected to the motor, and the motor is installed outside the air drying pipe.
  • Several flanges are arranged on the air drying pipe for positioning connection.
  • a product outlet is connected to the bottom outlet of the cyclone.
  • a tail gas treatment device is connected to the exhaust gas outlet at the top of the cyclone separator.
  • the drying process of the material through this system is as follows: the material (concentrated liquid) in the material storage tank is heated by the heating coil, stirred by the stirring shaft, and transported by the liquid pump to the air drying pipe of the air dryer, and the material will pass through the pressure nozzle before entering the mist to form a mist. drop.
  • the air is blown into the pipeline by the blower, and then passes through the air filter and the heater to form sterile hot air.
  • the hot air and the material droplets form convection, and then pass through the stirring device to be fully pulverized and mixed, dried in the airflow drying tube, and finally passed through the cyclone.
  • the separator separates and the dried product is collected at the product outlet. At the same time, the waste gas separated by the cyclone is discharged after being treated by the tail gas treatment device.
  • the pore size of the ceramic membrane used in the ceramic membrane filtration is 0.05 ⁇ m
  • the operating pressure is set to 1.5-3.0 bar
  • the operating temperature is set to 40-75° C.
  • the filtration time of the ceramic membrane is 1-2 h.
  • the pore size of the ceramic membrane used in the ceramic membrane filtration is 0.05 ⁇ m
  • the operating pressure is 1.5-3.0 bar
  • the operating temperature is 45-55° C.
  • the filtration time is 1.2-1.8 h.
  • the ceramic membrane filtration of the invention concentrates the solid content of mycelium in the fermentation broth of Paecilomyces bat moth from the original 2%-5% to 20%-40%, and the most preferred total solid content of the concentrated fermentation broth is 30% .
  • the loss rate of ceramic membrane filtration material is less than 2.5%.
  • the particles of the dried material passing through the spray feed air drying system are generally smaller than 50 ⁇ m.
  • the diameter of the droplets of the concentrated solution dispersed in the hot air is less than 100 ⁇ m.
  • the speed of the concentrate passing through the air dryer is 100-200ml/min, and the concentrate is preheated to 60-65°C before passing through the sprayer, that is, it is preheated to 60-65°C in the material storage tank.
  • the temperature of the high-speed hot air flowing through the airflow drying tube is 160-180°C, preferably 160°C, and the speed of the high-speed hot air flowing through the airflow drying tube is 20-40m/s.
  • the drying time of the spray feed air stream is 2-3 min.
  • the loss rate of drying materials through spray feed air flow is less than 2%, and the moisture content of outlet materials is less than 0.2%.
  • the present invention has the following beneficial effects:
  • the 2-5% mycelial solid content in the fermentation stock solution is concentrated to 20%-40% of the total solid content of the fermentation stock solution. % (preferably 30%), the volume of the concentrated feed liquid saves a lot of time for subsequent spray-type feed drying and the spray is uniform.
  • the traditional extraction process takes 35-50h from the fermentation broth to the finished product, and the extraction steps are many and take a long time, resulting in a low extraction yield;
  • the novel Paecilomyces batmoth of the present invention has few extraction process steps, only ceramic membrane filtration (time 1 ⁇ 2h), spray feed air drying (time 0.5 ⁇ 1h) two steps, especially the one-step drying process, saves a lot of time, shortens the process flow, and greatly increases the extraction yield.
  • the concentrated liquid is preheated to 60 ⁇ 65°C before passing through the airflow drying tube, so that the material liquid can be quickly heated to the water vapor evaporation temperature after entering the airflow drying tube, saving the time of material moisture vaporization; at the same time, the speed of the material passing through the pressure nozzle can be
  • the temperature of the high-speed hot air flowing through the drying tube is 160-180 °C, which can shorten the heating time of the material without destroying the mycelium of Paecilomyces batmoth.
  • Fig. 1 is the schematic diagram of spray feed air flow drying system
  • Ceramic membrane filtration The Paecilomyces bat moth fermentation broth (solid content is about 4%) is filtered through a ceramic membrane, the membrane pore size is 0.05 ⁇ m, the operating pressure of the microfiltration process is set to 1.5 bar, and the operating temperature is set to At 45°C, the filtration time is 1.8h, the material loss rate is 2%, and the total solid content of the obtained concentrate is 30%.
  • Spray feed air drying Preheat the concentrated solution obtained by ceramic membrane filtration to 60 °C, and pass through the pressure nozzle of the air dryer to form droplets with a diameter of less than 100 ⁇ m.
  • the droplets are dispersed in the pipeline, and the material passes through the air flow.
  • the speed of the dryer is 100ml/min; the hot material is mixed with the opposite high-speed hot air, the temperature of the high-speed hot air in the airflow drying tube is 160°C, and the speed is 20m/s; the mist droplets are dried and dried in the process of conveying through the hot airflow.
  • the time is 3 minutes, and finally, the dry product is recovered by a cyclone separator at the outlet of the drying pipe, and the particles of the dry material are below 50 ⁇ m.
  • Ceramic membrane filtration The Paecilomyces bat moth fermentation broth was filtered through a ceramic membrane, the membrane pore size was 0.05 ⁇ m, the operating pressure of the microfiltration process was set to 2 bar, the operating temperature was set to 50 °C, the filtration time was 1.6 h, and the material loss was The total solid content in the concentrate is 36%.
  • Spray feed air drying Preheat the concentrated solution obtained by ceramic membrane filtration to 60 °C, and pass through the pressure nozzle of the air dryer to form droplets with a diameter of less than 100 ⁇ m.
  • the droplets are dispersed in the pipeline, and the material passes through the air flow.
  • the speed of the dryer is 150ml/min; the hot material is mixed with the opposite high-speed hot air, the temperature of the high-speed hot air in the airflow drying tube is 170°C, and the speed is 30m/s; the mist droplets are dried and dried in the process of conveying through the hot airflow.
  • the time is 2.6min, and finally, the dry product is recovered by a cyclone separator at the outlet of the drying tube, and the particles of the dry material are below 50 ⁇ m.
  • Ceramic membrane filtration The Paecilomyces batmoth fermentation broth was filtered through a ceramic membrane, the membrane pore size was 0.05 ⁇ m, the operating pressure of the microfiltration process was set to 3 bar, the operating temperature was set to 55 °C, the filtration time was 1.3 h, and the material loss was The rate is 2.5%, and the concentrate is diluted to 40% of the total solid content of the fermentation stock.
  • Spray feed air drying Preheat the concentrated solution obtained by ceramic membrane filtration to 60 °C, and pass through the pressure nozzle of the air dryer to form droplets with a diameter of less than 100 ⁇ m.
  • the droplets are dispersed in the pipeline, and the material passes through the air flow.
  • the speed of the dryer is 200ml/min; the hot material is mixed with the opposite high-speed hot air, the temperature of the high-speed hot air in the airflow drying tube is 180°C, and the speed is 35m/s; the mist droplets are dried during the hot airflow conveying process.
  • the time is 2.63min, and finally, the dry product is recovered with a cyclone separator at the outlet of the drying tube, and the particle size of the dry material is below 50 ⁇ m.
  • the spray-type feed air drying system used in Example 1-3 includes a material storage tank 13 and an air flow dryer.
  • the discharge port of the material storage tank 13 is connected to the feed port of the air flow dryer through a pipeline, and the air flow dryer is mainly composed of air flow.
  • the drying pipe 6, the blower 1, the heater 3 and the cyclone separator 7 arranged at the air flow outlet of the airflow drying pipe 6 are composed of a pressure type nozzle 11 at the feed port of the airflow dryer 16, and the air line outlet of the blower 1 is provided.
  • the heater 3 is connected, and the outlet of the heater 3 is communicated with the outlet of the pressure type spray head 11 through the airflow drying pipe 6, and a stirring device 4 is provided at the communication place.
  • a liquid pump 12 is provided between the material storage tank 13 and the airflow dryer, which is used to drive the feed pipe connected to the outlet of the material storage tank 13 to deliver the material to the pressure type spray head 11 .
  • An air filter 2 is arranged between the blower 1 and the heater 3 , and a heating coil 14 and a stirring shaft 15 are installed inside the material storage tank 13 .
  • the stirring device 4 is connected to the motor 8 , and the motor 8 is installed outside the air drying tube 6 .
  • Several flanges 5 are arranged on the air drying pipe 6 for positioning connection.
  • a product outlet 9 is connected to the bottom outlet of the cyclone 7 .
  • a tail gas treatment device 10 is connected to the exhaust gas outlet at the top of the cyclone separator 7 .
  • the drying process of the material through this system is as follows: the material (concentrated liquid) in the material storage tank 13 is heated by the heating coil, stirred by the stirring shaft 15, and transported by the liquid pump to the air drying pipe 6 of the air dryer, and the material passes through the pressure type before entering.
  • the spray head 11 forms mist droplets.
  • the air is blown into the pipeline by the blower 1, and then passes through the air filter 2 and the heater 3 to form sterile hot air.
  • the hot air and the material droplets form convection, and then pass through the stirring device 4 to be fully pulverized and mixed.
  • After drying it is finally separated by the cyclone separator 7 , and the dried product is collected at the product outlet 9 .
  • the exhaust gas separated by the cyclone separator 7 is treated by the exhaust gas treatment device 10 and then discharged.
  • the above system adopts the material gas storage tank with built-in heating tube coil and stirring shaft.
  • the material Before entering the pipeline for drying, the material can be fully preheated, so that the material liquid can be quickly heated to the water vapor evaporation temperature after entering the air drying tube, saving the material moisture and gas.
  • the drying time promotes the subsequent rapid and efficient drying of the material, and the stirring is conducive to uniform preheating and rapid heating.
  • the airflow drying tube greatly breaks through the drying effect of the traditional box-type drying room, which is more conducive to the flow and drying of hot air, and can excellently dry viscous materials without problems such as sticking to the wall.
  • the outlet of the heater is communicated with the outlet of the pressure type nozzle through an airflow drying pipe, and a stirring device is provided at the communication place, which can solve the problem of difficult drying and agglomeration of viscous materials, save costs and improve drying efficiency.
  • Paecilomyces batmoth the fermentation broth of Paecilomyces batmoth (solid content is about 4%) is subjected to plate and frame filtration, plate and frame filtration conditions: 800 mesh filter screen, time 4-7h; screw belt drying: time 18-24h; hot air drying, temperature 60°C, time 10-16h; boiling drying: heating room temperature 107°C, inlet air temperature 58°C, time 3h, and finally obtained after crushing and sieving.
  • the loss rate of the obtained product is 25%, the water content is below 0.2%, and the total yield is 75%.
  • the new bat moth Paecilomyces spp. extraction process is selected, the total product yield reaches more than 95%, and the product loss rate is low.
  • the Paecilomyces hepiali fermentation broth used in the above Examples 1-3 and Comparative Examples was prepared by the following method: the Paecilomyces hepiali strain preservation number is CGMCC 20758. After the strain seed tank is cultivated, fermenter cultivation is carried out, and the inoculation amount is 5-10%. Seed medium (g/L): glucose 20g/L, yeast powder 3g/L, potassium dihydrogen phosphate 2g/L, magnesium sulfate heptahydrate 2g/L, natural pH. Seed culture conditions: temperature 26 °C, speed 150rpm, ventilation 1:0.5-1, cycle 40-50h.
  • Fermentation medium glucose 30g/L, yeast powder 2g/L, potassium dihydrogen phosphate 2g/L, magnesium sulfate heptahydrate 2g/L, natural pH. Fermentation culture conditions: temperature 26°C, rotation speed 150rpm, ventilation rate 1:0.5-1, cycle 40-50h; after the fermentation is completed, a fermentation broth is obtained.

Abstract

一种蝙蝠蛾拟青霉提取工艺，将蝙蝠蛾拟青霉发酵液通过陶瓷膜过滤得到浓缩液和滤过液，浓缩液再通过喷雾式进料气流干燥。采用陶瓷膜过滤方法得到蝙蝠蛾拟青霉菌丝体的同时，为后续喷雾式进料干燥节省大量的时间。同时采用喷雾式进料气流干燥工艺，一步式干燥得到成品，简单、高效，使得蝙蝠蛾拟青霉成品提取率高达95％以上，获得物料水分小于0.2％、物料损失率小于2％。

Description

一种新型蝙蝠蛾拟青霉提取工艺 技术领域
本发明涉及一种新型蝙蝠蛾拟青霉提取工艺，尤其是一种新型物料干燥方法。
背景技术
蝙蝠蛾拟青霉是从天然冬虫夏草子座中通过组织分离获得的无性世代菌株，其菌丝体的主要活性成分为虫草多糖、氨基酸、核苷等。现代医学研究发现，其具有镇痛、抗菌、消炎、增强免疫力、降血脂、抗氧化、抗癌等多种药理功效。
目前蝙蝠蛾拟青霉提取工艺多采用传统方法：其先将发酵液经过板框过滤，再经过一系列的干燥工艺，包括螺带干燥、热风烘干、沸腾干燥，得到低水分物料，最后在经过粉碎、筛分、包装得到产品。该方法步骤多、耗时长，其中板框过滤需要4～7h、螺带干燥18～24h、热风烘干10h～16h，沸腾干燥3h，总耗时35～50h。传统工艺步骤复杂，耗时长，导致提取收率低，产品损失严重。
上海天篙生物科技有限公司2017年申请专利CN 104151439 A中，其提取蝙蝠蛾拟青霉菌丝体多糖的方法为，将干燥的蝙蝠蛾拟青霉菌丝体超微粉碎、加水浸泡、乙醇沉淀，最后冷冻干燥。本研究通过设计新型喷雾式进料气流干燥工艺，将干燥、粉碎过程浓缩到一步反应中，减少干燥过程带来的产品损失。
发明内容
本发明的目的是针对传统工艺的不足，提供一种新型蝙蝠蛾拟青霉提取工艺。该工艺能够节省大量时间，缩短工艺流程，提取收率得到显著的提升。
本发明的目的是通过以下方式实现的：
一种新型蝙蝠蛾拟青霉提取工艺，将蝙蝠蛾拟青霉发酵液通过陶瓷膜过滤得到滤过液和浓缩液，浓缩液再通过喷雾式进料气流干燥。
喷雾式进料气流干燥具体是采用喷雾式进料气流干燥系统，将陶瓷膜过滤所得浓缩液通过气流干燥器的压力式喷头形成雾滴分散在管路中，与对面的高速热空气混合，使雾滴悬浮于热空气中，在气流输送过程中得到干燥，在干燥管出口处用旋风分离器回收干燥产品。
由于蝙蝠蛾拟青霉发酵液的浓缩液粘度大，在干燥过程中容易出现粘壁、干燥不充分且易结团等问题，优选采用如下结构的喷雾式进料气流干燥系统：包括物料储备罐和气流干燥器，物料储备罐的出料口通过管路连接气流干燥器的进料口，气流干燥器主要由气流干燥管、鼓风机、加热器和设于气流干燥管气流出口处的旋风分离器组成，在气流干燥器的进料口设有压力式喷头，鼓风机的空气管路出口连接加热器，加热器的出口与压力式喷头出口通过气流干燥管连通，且该连通处设有搅拌装置。
优选在物料储备罐与气流干燥器之间设有液泵，用于驱动物料储备罐出口连接的进料管输料至压力式喷头。
优选在鼓风机和加热器之间设有空气过滤器，物料储备罐罐体内部安装有加热盘管和搅拌轴。搅拌装置连接电机，且电机安装在气流干燥管管外。气流干燥管上设有若干法兰用于定位连接。旋风分离器的底部出口处连接有产品出口。旋风分离器的顶部废气出口处连接有尾气处理装置。
通过该系统物料干燥过程为：物料储备罐内物料(浓缩液)经过加热盘 管加热，搅拌轴搅拌，由液泵输送到气流干燥器的气流干燥管中，物料进入前经过压力式喷头形成雾滴。空气由鼓风机吹入管路，依次通过空气过滤器、加热器形成无菌热空气，热空气与物料雾滴形成对流，再经过搅拌装置充分粉碎、混匀，在气流干燥管中干燥，最后经过旋风分离器分离，干燥后的产品在产品出口收集。同时由旋风分离器分离产生的废气由尾气处理装置处理后排出。
优选的，陶瓷膜过滤采用的陶瓷膜膜孔径为0.05μm，操作压力设为1.5～3.0bar，操作温度设为40～75℃，陶瓷膜过滤时间为1～2h。
进一步优选陶瓷膜过滤采用的陶瓷膜膜孔径为0.05μm，操作压力为1.5～3.0bar，操作温度为45～55℃，过滤时间为1.2～1.8h。
本发明陶瓷膜过滤将蝙蝠蛾拟青霉发酵液中菌丝体固含物含量有原来的2％-5％浓缩到20％-40％，最优选浓缩的发酵液总固含物为30％。陶瓷膜过滤物料损失率小于2.5％。
通过喷雾式进料气流干燥系统的干燥物料颗粒一般小于50μm。浓缩液分散于热空气的雾滴直径在100μm以下。
浓缩液经过气流干燥器的速度为100～200ml/min，在浓缩液通过喷雾器前先预热到60～65℃，即在物料储备罐中预热至60～65℃。
流过气流干燥管的高速热空气温度为160～180℃，优选温度160℃，高速热空气流过气流干燥管的速度为20～40m/s。
优选的，喷雾式进料气流干燥时间为2～3min。
通过喷雾式进料气流干燥物料损失率小于2％，出口物料含水率小于0.2％。
本发明与现有技术相比，具有以下有益效果：
1、采用陶瓷膜过滤方法，在过滤得到蝙蝠蛾拟青霉菌丝体的同时，将发 酵原液中2-5％的菌丝体固含物含量浓缩到发酵原液总固含物的20％-40％(优选30％)，浓缩后的料液体积为后续喷雾式进料干燥节省大量的时间且喷雾均匀。
2、传统工艺中采用多级干燥，每一步干燥都造成物料的损失，提取收率只有75％，造成物料的浪费；本研究采用喷雾式进料气流干燥工艺，一步式干燥得到成品，使得蝙蝠蛾拟青霉成品提取率高，提取收率大于95％，获得物料水分小于0.2％，物料损失率小于2％。
3、传统提取工艺从发酵液到成品需要35～50h，提取步骤多，花费时间长，造成提取收率低；本发明的新型蝙蝠蛾拟青霉提取工艺步骤少，只有陶瓷膜过滤(时间1～2h)、喷雾式进料气流干燥(时间0.5～1h)两步，特别是一步式干燥工艺，节省了大量时间，缩短了工艺流程，提取收率大大上升。
4、浓缩液通过气流干燥管前先预热到60～65℃，使得料液进入气流干燥管后能快速加热到水汽蒸发温度，节省物料水分气化时间；同时物料经过压力式喷头的速度能达到100～200ml/min，使得物料雾化彻底；流过干燥管的高速热空气温度为160～180℃，在不破坏蝙蝠蛾拟青霉菌丝体的同时，还能缩短物料加热时间。
附图说明
图1为喷雾式进料气流干燥系统的示意图；
图中：1、鼓风机；2、空气过滤器；3、加热器；4、搅拌装置；5、法兰；6、气流干燥管；7、旋风分离器；8、电机；9、产品出口；10、尾气处理装置；11、压力式喷头；12、液泵；13、物料储存罐；14、加热盘管；15、搅拌轴；16、气流干燥器。
具体实施方式
以下通过具体实施例对本发明进行解释说明：
实施例1
(1)陶瓷膜过滤：将蝙蝠蛾拟青霉发酵液(固含物约为4％)经过陶瓷膜过滤，膜孔径为0.05μm，微滤过程的操作压力设为1.5bar，操作温度设为45℃，过滤时间1.8h，物料损失率2％，得到的浓缩液总固含物为30％。
(2)喷雾式进料气流干燥：将陶瓷膜过滤所得浓缩液预热到60℃，经过气流干燥器的压力式喷头形成直径在100μm以下雾滴，雾滴分散在管路中，物料通过气流干燥器的速度为100ml/min；热物料与对面的高速热空气混合，气流干燥管中的高速热空气温度为160℃、速度为20m/s；雾滴通过热气流输送过程中得到干燥，干燥时间为3min，最后在干燥管出口处用旋风分离器回收干燥产品，干燥物料颗粒在50μm以下。
实施例2
(1)陶瓷膜过滤：将蝙蝠蛾拟青霉发酵液经过陶瓷膜过滤，膜孔径为0.05μm，微滤过程的操作压力设为2bar，操作温度设为50℃，过滤时间1.6h，物料损失率2.2％，浓缩液中总固含物含量为36％。
(2)喷雾式进料气流干燥：将陶瓷膜过滤所得浓缩液预热到60℃，经过气流干燥器的压力式喷头形成直径在100μm以下雾滴，雾滴分散在管路中，物料通过气流干燥器的速度为150ml/min；热物料与对面的高速热空气混合，气流干燥管中的高速热空气温度为170℃、速度为30m/s；雾滴通过热气流输送过程中得到干燥，干燥时间为2.6min，最后在干燥管出口处用旋风分离器回收干燥产品，干燥物料颗粒在50μm以下。
实施例3
(1)陶瓷膜过滤：将蝙蝠蛾拟青霉发酵液经过陶瓷膜过滤，膜孔径为 0.05μm，微滤过程的操作压力设为3bar，操作温度设为55℃，过滤时间1.3h，物料损失率2.5％，浓缩液稀释到发酵原液总固含物的40％。
(2)喷雾式进料气流干燥：将陶瓷膜过滤所得浓缩液预热到60℃，经过气流干燥器的压力式喷头形成直径在100μm以下雾滴，雾滴分散在管路中，物料通过气流干燥器的速度为200ml/min；热物料与对面的高速热空气混合，气流干燥管中的高速热空气温度为180℃、速度为35m/s；雾滴在热气流输送过程中得到干燥，干燥时间为2.63min，最后在干燥管出口处用旋风分离器回收干燥产品，干燥物料颗粒在50μm以下。
实施例4
实施例1-3使用的喷雾式进料气流干燥系统包括物料储备罐13和气流干燥器，物料储备罐13的出料口通过管路连接气流干燥器的进料口，气流干燥器主要由气流干燥管6、鼓风机1、加热器3和设于气流干燥管6气流出口处的旋风分离器7组成，在气流干燥器16的进料口设有压力式喷头11，鼓风机1的空气管路出口连接加热器3，加热器3的出口与压力式喷头11出口通过气流干燥管6连通，且该连通处设有搅拌装置4。在物料储备罐13与气流干燥器之间设有液泵12，用于驱动物料储备罐13出口连接的进料管输料至压力式喷头11。在鼓风机1和加热器3之间设有空气过滤器2，物料储备罐13罐体内部安装有加热盘管14和搅拌轴15。搅拌装置4连接电机8，且电机8安装在气流干燥管6管外。气流干燥管6上设有若干法兰5用于定位连接。旋风分离器7的底部出口处连接有产品出口9。旋风分离器7的顶部废气出口处连接有尾气处理装置10。
通过该系统物料干燥过程为：物料储备罐13内物料(浓缩液)经过加热盘管加热，搅拌轴15搅拌，由液泵输送到气流干燥器的气流干燥管6中，物料进入前经过压力式喷头11形成雾滴。空气由鼓风机1吹入管路，依次 通过空气过滤器2、加热器3形成无菌热空气，热空气与物料雾滴形成对流，再经过搅拌装置4充分粉碎、混匀，在气流干燥管6中干燥，最后经过旋风分离器7分离，干燥后的产品在产品出口9收集。同时由旋风分离器7分离产生的废气由尾气处理装置10处理后排出。
上述系统采用内置加热管盘和搅拌轴的物料储气罐，在进入管道干燥前，可以对物料进行充分预热，使得料液进入气流干燥管后能快速加热到水汽蒸发温度，节省物料水分气化时间促进了后续快速而高效的物料干燥，搅拌利于预热均匀，升温迅速。气流干燥管极大突破传统传统箱体式干燥室的干燥效果，更利于热空气流动和干燥，可以出色地干燥粘性物料，不会出现粘壁等问题。加热器的出口与压力式喷头出口通过气流干燥管连通，且该连通处设有搅拌装置，能够解决粘性物料难干燥且易结团的问题，节省成本，提高干燥效率。
对比例1
传统蝙蝠蛾拟青霉提取工艺：将蝙蝠蛾拟青霉发酵液(固含量约为4％)进行板框过滤，板框过滤条件：800目滤网，时间4-7h；螺带干燥：时间18-24h；热风烘干，温度60℃，时间10-16h；沸腾干燥:加热室温度107℃，进风温度58℃，时间3h，最后粉碎、筛分后得到。所得产品损失率25％，含水量0.2％以下，总收率75％。
表1实施例检测数据
Figure PCTCN2020132612-appb-000001
Figure PCTCN2020132612-appb-000002
由表1可以看出，选用新型蝙蝠蛾拟青霉提取工艺，产品总收率达到95％以上，产品损失率低。
上述实施例1-3及对比例采用的蝙蝠蛾拟青霉发酵液是通过以下方法制备得到的：蝙蝠蛾拟青霉(Paecilomyces hepiali)菌株保藏号为CGMCC 20758。菌株种子罐培养后进行发酵罐培养，接种量为5-10％。种子培养基(g/L)：葡萄糖20g/L，酵母粉3g/L，磷酸二氢钾2g/L，七水硫酸镁2g/L，pH自然。种子培养条件：温度26℃，转速150rpm，通气量1:0.5-1，周期40-50h。发酵罐培养基(g/L)：葡萄糖30g/L，酵母粉2g/L，磷酸二氢钾2g/L，七水硫酸镁2g/L，pH自然。发酵培养条件：温度26℃，转速150rpm，通气量1:0.5-1，周期40-50h；发酵完成后，得到发酵液。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

  1. 一种新型蝙蝠蛾拟青霉提取工艺，其特征在于将蝙蝠蛾拟青霉发酵液通过陶瓷膜过滤得到浓缩液和滤过液，浓缩液再通过喷雾式进料气流干燥。
  2. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的陶瓷膜过滤采用的陶瓷膜膜孔径为0.05μm，操作压力为1.5～3.0bar，操作温度为40～75℃，过滤时间为1～2h。
  3. 根据权利要求2所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的陶瓷膜过滤采用的陶瓷膜膜孔径为0.05μm，操作压力为1.5～3.0bar，操作温度为45～55℃，过滤时间为1.2～1.8h。
  4. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于将蝙蝠蛾拟青霉发酵液中菌丝体浓度浓缩到发酵液总固含物的20％-40％。
  5. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的通过喷雾式进料气流干燥系统的干燥物料颗粒小于50μm。
  6. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的浓缩液分散于热空气的雾滴直径在100μm以下。
  7. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的浓缩液经过气流干燥器的速度为100～200ml/min。
  8. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的浓缩液通过气流干燥器前先预热到60～65℃。
  9. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的流过干燥管的高速热空气温度为160～180℃，高速热空气流过气流干燥管的速度为20～40m/s。
  10. 根据权利要求1所述的新型蝙蝠蛾拟青霉提取工艺，其特征在于所述的喷雾式进料气流干燥时间为2～3min。
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