CN105777942A - Uniform-grain-size agarose gel microsphere production system and production process thereof - Google Patents
Uniform-grain-size agarose gel microsphere production system and production process thereof Download PDFInfo
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- CN105777942A CN105777942A CN201610163332.0A CN201610163332A CN105777942A CN 105777942 A CN105777942 A CN 105777942A CN 201610163332 A CN201610163332 A CN 201610163332A CN 105777942 A CN105777942 A CN 105777942A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
- C08B37/0039—Agar; Agarose, i.e. D-galactose, 3,6-anhydro-D-galactose, methylated, sulfated, e.g. from the red algae Gelidium and Gracilaria; Agaropectin; Derivatives thereof, e.g. Sepharose, i.e. crosslinked agarose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The invention relates to a uniform-grain-size agarose gel microsphere production system and a production process thereof. The system comprises a production area and a control area positioned beside the production area, a gel mill and a premix heating kettle are arranged in the production area, the gel mill is connected with a microwave heating kettle, the premix heating kettle is connected with an ultrasonic uniform defoaming kettle, both the microwave heating kettle and the ultrasonic uniform defoaming kettle are connected with an ultrasonic homogenizing kettle, a high-frequency ultrasonic homogenizing kettle is connected with an oil-water separator, a water-phase outlet of the oil-gas separator is connected with a microsphere cleaning device which is connected with a mixer, and the mixer is connected with a metering subpackaging machine. Large-scale production of agarose gel microspheres uniform in grain size, smooth in sphere form and free of impurities is realized, and the system plays a certain role in promoting development of biomedicine industry of China and has good social and economic benefit.
Description
Technical field
The present invention relates to the agarose gel microsphere production system of a kind of uniform particle diameter and production technology thereof, belong to processing biopharmaceutical materials field.
Background technology
In country " 12 " planning; put forth effort to promote economic restructuring and emerging strategic industries development; wherein one of state key developing direction is to put forth effort to promote biological medicine research and development ability; exploitation medicine new product; accelerate development biomedical engineering technology and product; advance biology to manufacture large-scale development, accelerate to build the modern biotechnology industrial system with international most advanced level, accelerate research and development and the industrialization of marine biotechnology and product.Agarose is a kind of natural marine organism polysaccharide separated from the large ocean algae such as Eucheuma gelatinosum, Thallus Porphyrae, Gracilaria tenuistipitata, with agarose be raw material production gel micro-ball because of have good biocompatibility, function base characteristic, high-hydrophilic, porous, the characteristic such as non-specific and become the controlled drug delivery system of a kind of high-quality.It is mainly used in the aspects such as the separation purification of the biomolecule such as albumen, antibody, enzyme, targeted drug, immune detection, cell separation, chemical analysis, has irreplaceable effect for exploitation biological medicine new product.As can be seen here, the development of China's Bio-pharmaceutical Industry and marine biomaterial industry is all had important function by agarose gel microsphere.
The agarose gel microsphere preparation method that the preparation method of agarose gel microsphere is mainly traditional is mainly emulsion process, there is more defect in this method, first the microsphere balling-up rate variance prepared, and size differs, breadth coefficient is wider, need to be easily separated by loaded down with trivial details follow-up sieving technology consuming time, cause product yield low and preparation poor repeatability, and some more advanced production technologies all exist and easily cause the defect such as pollution, technique length consuming time at present, it is impossible to meet China's Bio-pharmaceutical Industry development wilderness demand to agarose gel microsphere.Therefore, develop size uniformity agarose gel microsphere efficient, cleaning, scale quantity-produced technique significant.
Summary of the invention
In view of this, it is an object of the invention to provide the agarose gel microsphere production system of a kind of efficient, energy-conservation uniform particle diameter and production technology thereof, the microspherulite diameter prepared is homogeneous, and particle size distribution coefficient is little.
A kind of technical scheme that the present invention adopts is: the agarose gel microsphere production system of a kind of uniform particle diameter, including producing district and being positioned at the control zone producing district's side, rubber mill and premix heating kettle it is provided with in described production district, described rubber mill and a microwave heating still are connected, described premix heating kettle and the homogeneous froth breaking still of a ultrasound wave are connected, described microwave heating still is all connected with a ultrasound wave homogenizing still with the homogeneous froth breaking still of ultrasound wave, described high frequency ultrasound homogenizing still and an oil water separator are connected, the aqueous phase outlet of described oil water separator is connected with a microsphere washer, described microsphere washer and a vortex mixer are connected, described vortex mixer and a metering and separate loading machine are connected.
Further, being additionally provided with the cleanout fluid preparing tank being connected with described microsphere washer in described production district, described microsphere washer is also connected with a cleanout fluid purifying regeneration equipment, and described cleanout fluid purifying regeneration equipment is also connected with described cleanout fluid preparing tank；Described vortex mixer is also associated with an Agitation Tank.
Further, the oil phase outlet of described oil water separator separates purifier apparatus with oil product and is connected, and described oil purification equipment is also connected with described premix heating kettle.
Further, it is provided with the control station of production line panorama screen in described control zone, is provided with glass partition between described control zone and production district, in control zone, is provided with the visit passage being close to glass partition.
Further, the kettle inner top of the homogeneous froth breaking still of described microwave heating still, ultrasound wave and ultrasound wave homogenizing still three is provided with full-view camera, and the kettle peripheral part of three is provided with microwave heating equipment；The limit stirring paddle being positioned at week side and the dispersion wheel being centrally located it is provided with in the kettle of described microwave heating still；Being provided with centrally located emulsifying head in the kettle of described ultrasound wave homogeneous froth breaking still, autoclave body bottom is provided with high frequency ultrasound wave producer；Being provided with the limit stirring paddle being positioned at week side and the emulsifying head being centrally located in the kettle of described ultrasound wave homogenizing still, autoclave body bottom is provided with high frequency ultrasound wave producer.
The agarose gel microsphere high-efficient production technology that another solution is that a kind of uniform particle diameter that the present invention adopts, agarose gel microsphere production system including a kind of uniform particle diameter as above, and sequentially include the following steps: (1) agarose is joined in ultra-pure water by certain ratio, and it is delivered in microwave heating still and quickly fully dissolves forms glue A after being transported in rubber mill to process 10 ~ 20min；Light oil as solvent and the mink cell focus as surfactant are joined in premix heating kettle after Hybrid Heating with certain ratio simultaneously, be transported to and ultrasound wave homogeneous froth breaking still carries out process form the homogeneous B of phase without scald in warm oil；(2) the homogeneous B of phase without scald in warm oil is transported in ultrasound wave homogenizing still it is heated to predetermined temperature, open high frequency ultrasound wave producer and start limit stirring paddle and emulsifying head, after operating 15 ~ 30min, glue A is delivered in ultrasound wave homogenizing still by certain flow rate, the rotating speed of limit stirring paddle and emulsifying head will be adjusted after glue A conveying, start to be cooled to 25 DEG C with the speed of 1 ~ 10 DEG C/min after running 30 ~ 120min；(3) feed liquid in ultrasound wave homogenizing still is transported in oil water separator, in oil water separator, adds suitable alcohols breakdown of emulsion, and open mid-frequency ultrasonic ripple acceleration breakdown of emulsion, obtain oil water two phase system；(4) oil-water separating function of oil water separator is opened, obtain aqueous phase and enter microsphere washer, to cleanout fluid preparing tank be transported in microsphere washer containing in the washing liquid of finite concentration ethanol and salt by certain flow rate, open low-frequency ultrasonic waves and remove the little oil droplet of the microsphere surface attachment in aqueous phase；(5) 20% alcoholic solution of configuration in Agitation Tank is transported in vortex mixer, more clean microsphere is transported in vortex mixer, be transported to metering and separate loading machine after mix homogeneously and carry out metering packing.
Further, after the oil phase entrance oil product separation purifier apparatus that in step (4), the separation of oil water separator obtains is easily separated purification, then it is transported in premix heating kettle standby；Cleanout fluid after cleaning in step (1) is transported in cleanout fluid preparing tank after entering the regeneration of cleanout fluid purifying regeneration equipment and recycles.
Further, in step (1), the mass ratio of agarose and ultra-pure water is 1 50～8 25, it is preferable that 1 25～4 25, and light oil described in step (1) is one or more in light diesel fuel, heavy diesel fuel, No. 98 gasoline, isobutyltrimethylmethane. and glycerol；Described mink cell focus is the mixed oil phase viscosity of one or more in Camellia oil, Petiolus Trachycarpi oil, Oleum Cocois, lanoline, Adeps Sus domestica and Cera Flava, light oil and mink cell focus is 30～580mPa s.
Further, the ultrasonic frequency of the homogeneous froth breaking still of step (1) ultrasound wave is 30～50KHz；In step (2), the ultrasonic frequency of ultrasound wave homogenizing still is 80～120KHz；In step (3), the mid-frequency ultrasonic wave frequency of oil water separator is 40～60KHz；In step (4), the low frequency ultrasound wave frequency of microsphere washer is 20～28KHz.
Further, in step (2), ultrasound wave homogenizing still is 200～1500r/Min at the rotating speed of the time internal emulsification head of operating 15 ~ 30min, and limit rotating speed of agitator is 20～150r/min；Glue A is delivered to the flow speed control in ultrasound wave homogenizing still at 0.5～50L/min, and the time of conveying glue A controls at 2～10min；Carry after the adjustment of rotational speed of all emulsifying head and limit stirring paddle after glue respectively 2000～18000r/min and 50～200r/min.
Compared with prior art, the method have the advantages that (1) achieves that uniform particle diameter, ball-type be round and smooth, free from admixture agarose gel microsphere large-scale production；(2) by real-time detector data and video monitor live feedback, adjust and control each systematic parameter and not only reached safety, automatization, and intelligent produced but also save cost of labor；(3) technique mode of heating be designed to microwave heating reach energy-conservation and shorten technique consuming time achieve high-efficiency cleaning produce；Achieve recycling of technical process waste liquid；(4) the scientific and reasonable design of production technology, production system and technological process layout solves homogeneous agarose gel microsphere and produces a difficult problem, realize uniform particle diameter agarose gel microsphere safe, energy-conservation, cleaning, efficiently, intelligent produce continuously, development for China's Bio-pharmaceutical Industry has certain impetus, has good social and economic benefits.
For making the purpose of the present invention, technical scheme and advantage clearly understand, below by specific embodiment and relevant drawings, the present invention will be described in further detail.
Accompanying drawing explanation
Fig. 1 is the system diagram of the embodiment of the present invention 1 production system；
Fig. 2 is microwave heating still organigram in the embodiment of the present invention 1；
Fig. 3 is the homogeneous froth breaking still organigram of ultrasound wave in the embodiment of the present invention 1；
Fig. 4 is ultrasound wave homogenizing still organigram in the embodiment of the present invention 1；
Fig. 5 is that embodiment 1 produces the agarose gel microsphere microphotograph obtained；
Fig. 6 is that embodiment 1 produces the agarose gel microsphere grain size distribution obtained；
Fig. 7 is that embodiment 2 produces the agarose gel microsphere microphotograph obtained；
Fig. 8 is that embodiment 2 produces the agarose gel microsphere grain size distribution obtained；
Fig. 9 is that embodiment 3 produces the agarose gel microsphere microphotograph obtained；
Figure 10 is that embodiment 3 produces the agarose gel microsphere grain size distribution obtained；
Number in the figure illustrates: 100-production district, 110-microwave heating still, 111-full-view camera, 112-microwave heating equipment, 113-limit stirring paddle, 114-dispersion wheel, the homogeneous froth breaking still of 120-ultrasound wave, 121-emulsifying head, the generation of 122-high-frequency ultrasonic, 130-ultrasound wave homogenizing still, 200-control zone, 210-visit passage, 300-glass partition.
Detailed description of the invention
Embodiment 1:As shown in Fig. 1 ~ 4, a kind of agarose gel microsphere production system of uniform particle diameter, including producing district 100 and being positioned at the control zone 200 producing district's side, rubber mill and premix heating kettle it is provided with in described production district 100, described premix heating kettle is the premix still with heating function, described rubber mill and a microwave heating still 110 are connected, described premix heating kettle and the homogeneous froth breaking still 120 of a ultrasound wave are connected, described microwave heating still 110 is all connected with a ultrasound wave homogenizing still 130 with the homogeneous froth breaking still 120 of ultrasound wave, described high frequency ultrasound homogenizing still and an oil water separator are connected, the aqueous phase outlet of described oil water separator is connected with a microsphere washer, described microsphere washer and a vortex mixer are connected, described vortex mixer and a metering and separate loading machine are connected.
In the present embodiment, described oil water separator is vacuum type oil water separator, oil water separator is provided with vacuum pump, utilizes negative pressure to be transported in oil water separator by the feed liquid in ultrasound wave homogenizing still, it is ensured that feed liquid will not damage agarose gel microsphere because of machinery conveying.
In the present embodiment, described vortex mixer is also equipped with vacuum pump, utilizes pressure differential to be transported in vortex mixer by the microsphere in microsphere washer.
In the present embodiment, the cleanout fluid preparing tank being connected with described microsphere washer it is additionally provided with in described production district, described microsphere washer is also connected with a cleanout fluid purifying regeneration equipment, and described cleanout fluid purifying regeneration equipment is also connected with described cleanout fluid preparing tank；Described vortex mixer is also associated with an Agitation Tank.
In the present embodiment, the oil phase outlet of described oil water separator separates purifier apparatus with oil product and is connected, and described oil purification equipment is also connected with described premix heating kettle.
In the present embodiment, the control station of production line panorama screen it is provided with in described control zone 200, it is provided with glass partition 300 between described control zone and production district, the visit passage 210 being close to glass partition 300 it is provided with in control zone, control each equipment by control station, feed back to the data of control station again through each equipment and real-time panoramic video monitoring is grasped whole production system working order technique and carried out degree.
In the present embodiment, the kettle inner top of the homogeneous froth breaking still of described microwave heating still, ultrasound wave and ultrasound wave homogenizing still three is provided with full-view camera 111, it is beneficial to and grasps agarose dissolving situation in microwave heating still completely, in ultrasound wave homogeneous froth breaking still, in oil phase, bubble eliminates situation and the homogeneous situation of solution, ultrasound wave homogenizing still internal emulsification droplet size situation and whirlpool production；The kettle peripheral part of three is provided with microwave heating equipment 112, not only largely reduces technique power consumption but also shortens the process time and improve production efficiency.
In the present embodiment, the limit stirring paddle 113 being positioned at week side and the dispersion wheel 114 being centrally located it is provided with in the kettle of described microwave heating still 110, microwave heating still 11 combines whipped form by designing limit stirring paddle 113 and dispersion wheel 114, being conducive to stirring to solve the difficult problems of dissolution in the preparation of high concentration agarose gel microsphere fully simultaneously, also solving the problem of the deep and viscous wall of color that agarose excessively occurs because of local heating thus affecting product quality；It is provided with centrally located emulsifying head 121 in the kettle of described ultrasound wave homogeneous froth breaking still 120, autoclave body bottom is provided with high frequency ultrasound wave producer 122, the homogeneous oil phase environment prepared needed for homogeneous microsphere is realized mutually by the homogeneous just oil emulsion of emulsifying head 121, bubble is driven again through high frequency ultrasound wave producer 122, achieve the oil phase zero homogeneous state of bubble, solve and cause that a defect difficult problem occurs in agarose gel microsphere product；The limit stirring paddle 113 being positioned at week side and the emulsifying head 121 being centrally located it is provided with in the kettle of described ultrasound wave homogenizing still 130, autoclave body bottom is provided with high frequency ultrasound wave producer 122, by the reverse rate controlling stirring of limit stirring paddle 113 and emulsifying head 121 high speed emulsifying, this design prevents the whirlpool produced because of high speed emulsifying thus eliminating the inhomogenous impact of microsphere that whole still emulsion emulsifying environment difference causes；The high-frequency ultrasonic synergistic function sent again through high frequency ultrasound wave producer 122 reduces the distribution of agarose gel microsphere particle diameter further.
A kind of agarose gel microsphere high-efficient production technology of uniform particle diameter, agarose gel microsphere production system including a kind of uniform particle diameter as above, and sequentially include the following steps: (1) agarose is joined in ultra-pure water by certain ratio, and it is delivered in microwave heating still and quickly fully dissolves forms glue A after being transported in rubber mill to process 10min；Light oil as solvent and the mink cell focus as surfactant are joined in premix heating kettle after Hybrid Heating with certain ratio simultaneously, be transported to and ultrasound wave homogeneous froth breaking still carries out process form the homogeneous B of phase without scald in warm oil；(2) the homogeneous B of phase without scald in warm oil is transported in ultrasound wave homogenizing still it is heated to 100 DEG C, open high frequency ultrasound wave producer and start limit stirring paddle and emulsifying head, emulsifying head rotating speed is 500r/min, emulsifying head rotating speed is 20r/min, after operating 15min, glue A is delivered in ultrasound wave homogenizing still by 10L/min flow velocity, the time of conveying glue A controls at 5min, the rotating speed of limit stirring paddle and emulsifying head will be adjusted after glue A conveying, respectively 8000r/min and 80r/min after the adjustment of rotational speed of emulsifying head and limit stirring paddle, start to be cooled to 25 DEG C with the speed of 5 DEG C/min after running 30min；(3) feed liquid in ultrasound wave homogenizing still is transported in oil water separator, in oil water separator, adds suitable alcohols breakdown of emulsion, and open mid-frequency ultrasonic ripple acceleration breakdown of emulsion, obtain oil water two phase system；(4) oil-water separating function of oil water separator is opened, obtain aqueous phase and enter microsphere washer, to cleanout fluid preparing tank be transported in microsphere washer containing in the washing liquid of finite concentration ethanol and salt by certain flow rate, open low-frequency ultrasonic waves and remove the little oil droplet of the microsphere surface attachment in aqueous phase；(5) 20% alcoholic solution of configuration in Agitation Tank is transported in vortex mixer, more clean microsphere is transported in vortex mixer, be transported to metering and separate loading machine after mix homogeneously and carry out metering packing.
In the present embodiment, after the oil phase entrance oil product separation purifier apparatus that in step (4), the separation of oil water separator obtains is easily separated purification, then it is transported in premix heating kettle standby；Cleanout fluid after cleaning in step (1) is transported in cleanout fluid preparing tank after entering the regeneration of cleanout fluid purifying regeneration equipment and recycles.
In the present embodiment, in step (3), the feed liquid in ultrasound wave homogenizing still is to utilize the negative pressure produced in oil water separator to be drawn in oil water separator；(5) microsphere cleaned in sucks in vortex mixer also with the negative pressure produced in vortex mixer；Guarantee that feed liquid will not be damaged because of machinery conveying.
In the present embodiment, in step (1), after agarose and ultra-pure water mixing, the concentration of agarose is 2%, and light oil described in step (1) is glycerol；Described mink cell focus is the mixed oil phase viscosity of Camellia oil and Adeps Sus domestica, light oil and mink cell focus is 60mPa s.
In the present embodiment, the ultrasonic frequency of the homogeneous froth breaking still of step (1) ultrasound wave is 32KHz；In step (2), the ultrasonic frequency of ultrasound wave homogenizing still is 90KHz；In step (3), the mid-frequency ultrasonic wave frequency of oil water separator is 45KHz；In step (4), the low frequency ultrasound wave frequency of microsphere washer is 23KHz.
The present embodiment produce the microsphere optical microphotograph that obtains as it is shown in figure 5, particle size distribution as shown in Figure 6, the particle size distribution coefficient of microsphere is 15%, uniform particle diameter.
Embodiment 2:A kind of agarose gel microsphere high-efficient production technology of uniform particle diameter, agarose gel microsphere production system including uniform particle diameter as described in Example 1, and sequentially include the following steps: (1) agarose is joined in ultra-pure water by certain ratio, and it is delivered in microwave heating still and quickly fully dissolves forms glue A after being transported in rubber mill to process 10min；Light oil as solvent and the mink cell focus as surfactant are joined in premix heating kettle after Hybrid Heating with certain ratio simultaneously, be transported to and ultrasound wave homogeneous froth breaking still carries out process form the homogeneous B of phase without scald in warm oil；(2) the homogeneous B of phase without scald in warm oil is transported in ultrasound wave homogenizing still it is heated to 200 DEG C, open high frequency ultrasound wave producer and start limit stirring paddle and emulsifying head, emulsifying head rotating speed is 600r/min, emulsifying head rotating speed is 80r/min, after operating 20min, glue A is delivered in ultrasound wave homogenizing still by 10L/min flow velocity, the time of conveying glue A controls at 6min, the rotating speed of limit stirring paddle and emulsifying head will be adjusted after glue A conveying, respectively 6000r/min and 100r/min after the adjustment of rotational speed of emulsifying head and limit stirring paddle, start to be cooled to 25 DEG C with the speed of 5 DEG C/min after running 50min；(3) feed liquid in ultrasound wave homogenizing still is transported in oil water separator, in oil water separator, adds suitable alcohols breakdown of emulsion, and open mid-frequency ultrasonic ripple acceleration breakdown of emulsion, obtain oil water two phase system；(4) oil-water separating function of oil water separator is opened, obtain aqueous phase and enter microsphere washer, to cleanout fluid preparing tank be transported in microsphere washer containing in the washing liquid of finite concentration ethanol and salt by certain flow rate, open low-frequency ultrasonic waves and remove the little oil droplet of the microsphere surface attachment in aqueous phase；(5) 20% alcoholic solution of configuration in Agitation Tank is transported in vortex mixer, more clean microsphere is transported in vortex mixer, be transported to metering and separate loading machine after mix homogeneously and carry out metering packing.
In the present embodiment, after the oil phase entrance oil product separation purifier apparatus that in step (4), the separation of oil water separator obtains is easily separated purification, then it is transported in premix heating kettle standby；Cleanout fluid after cleaning in step (1) is transported in cleanout fluid preparing tank after entering the regeneration of cleanout fluid purifying regeneration equipment and recycles.
In the present embodiment, in step (3), the feed liquid in ultrasound wave homogenizing still is to utilize the negative pressure produced in oil water separator to be drawn in oil water separator；(5) microsphere cleaned in sucks in vortex mixer also with the negative pressure produced in vortex mixer；Guarantee that feed liquid will not be damaged because of machinery conveying.
In the present embodiment, in step (1), after agarose and ultra-pure water mixing, the concentration of agarose is 6%, and light oil described in step (1) is light diesel fuel and glycerol；Described mink cell focus is the mixed oil phase viscosity of Oleum Cocois, Petiolus Trachycarpi oil, light oil and mink cell focus is 100mPa s.
In the present embodiment, the ultrasonic frequency of the homogeneous froth breaking still of step (1) ultrasound wave is 35KHz；In step (2), the ultrasonic frequency of ultrasound wave homogenizing still is 92KHz；In step (3), the mid-frequency ultrasonic wave frequency of oil water separator is 45KHz；In step (4), the low frequency ultrasound wave frequency of microsphere washer is 24KHz.
The present embodiment produce the microsphere optical microphotograph that obtains as it is shown in fig. 7, particle size distribution as shown in Figure 8, the particle size distribution coefficient of microsphere is 10%, uniform particle diameter.
Embodiment 3:A kind of agarose gel microsphere high-efficient production technology of uniform particle diameter, agarose gel microsphere production system including uniform particle diameter as described in Example 1, and sequentially include the following steps: (1) agarose is joined in ultra-pure water by certain ratio, and it is delivered in microwave heating still and quickly fully dissolves forms glue A after being transported in rubber mill to process 20min；Light oil as solvent and the mink cell focus as surfactant are joined in premix heating kettle after Hybrid Heating with certain ratio simultaneously, be transported to and ultrasound wave homogeneous froth breaking still carries out process form the homogeneous B of phase without scald in warm oil；(2) the homogeneous B of phase without scald in warm oil is transported in ultrasound wave homogenizing still it is heated to 300 DEG C, open high frequency ultrasound wave producer and start limit stirring paddle and emulsifying head, emulsifying head rotating speed is 800r/min, emulsifying head rotating speed is 100r/min, after operating 30min, glue A is delivered in ultrasound wave homogenizing still by 5L/min flow velocity, the time of conveying glue A controls at 8min, the rotating speed of limit stirring paddle and emulsifying head will be adjusted after glue A conveying, respectively 10000r/min and 150r/min after the adjustment of rotational speed of emulsifying head and limit stirring paddle, start to be cooled to 25 DEG C with the speed of 10 DEG C/min after running 120min；(3) feed liquid in ultrasound wave homogenizing still is transported in oil water separator, in oil water separator, adds suitable alcohols breakdown of emulsion, and open mid-frequency ultrasonic ripple acceleration breakdown of emulsion, obtain oil water two phase system；(4) oil-water separating function of oil water separator is opened, obtain aqueous phase and enter microsphere washer, to cleanout fluid preparing tank be transported in microsphere washer containing in the washing liquid of finite concentration ethanol and salt by certain flow rate, open low-frequency ultrasonic waves and remove the little oil droplet of the microsphere surface attachment in aqueous phase；(5) 20% alcoholic solution of configuration in Agitation Tank is transported in vortex mixer, more clean microsphere is transported in vortex mixer, be transported to metering and separate loading machine after mix homogeneously and carry out metering packing.
In the present embodiment, after the oil phase entrance oil product separation purifier apparatus that in step (4), the separation of oil water separator obtains is easily separated purification, then it is transported in premix heating kettle standby；Cleanout fluid after cleaning in step (1) is transported in cleanout fluid preparing tank after entering the regeneration of cleanout fluid purifying regeneration equipment and recycles.
In the present embodiment, in step (3), the feed liquid in ultrasound wave homogenizing still is to utilize the negative pressure produced in oil water separator to be drawn in oil water separator；(5) microsphere cleaned in sucks in vortex mixer also with the negative pressure produced in vortex mixer；Guarantee that feed liquid will not be damaged because of machinery conveying.
In the present embodiment, in step (1), after agarose and ultra-pure water mixing, the concentration of agarose is 30%, and light oil described in step (1) is light diesel fuel and heavy diesel fuel；Described mink cell focus is the mixed oil phase viscosity of Cera Flava, light oil and mink cell focus is 200mPa s.
In the present embodiment, the ultrasonic frequency of the homogeneous froth breaking still of step (1) ultrasound wave is 40KHz；In step (2), the ultrasonic frequency of ultrasound wave homogenizing still is 100KHz；In step (3), the mid-frequency ultrasonic wave frequency of oil water separator is 50KHz；In step (4), the low frequency ultrasound wave frequency of microsphere washer is 26KHz.
The present embodiment produce the microsphere optical microphotograph that obtains as it is shown in figure 9, particle size distribution as shown in Figure 10, the particle size distribution coefficient of microsphere is 8%, uniform particle diameter.
Above-listed preferred embodiment; the object, technical solutions and advantages of the present invention have been further described; it is it should be understood that; the foregoing is only presently preferred embodiments of the present invention; not in order to limit the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. the agarose gel microsphere production system of a uniform particle diameter, it is characterized in that: include producing district and being positioned at the control zone producing district's side, rubber mill and premix heating kettle it is provided with in described production district, described rubber mill and a microwave heating still are connected, described premix heating kettle and the homogeneous froth breaking still of a ultrasound wave are connected, described microwave heating still is all connected with a ultrasound wave homogenizing still with the homogeneous froth breaking still of ultrasound wave, described high frequency ultrasound homogenizing still and an oil water separator are connected, the aqueous phase outlet of described oil water separator is connected with a microsphere washer, described microsphere washer and a vortex mixer are connected, described vortex mixer and a metering and separate loading machine are connected.
2. the agarose gel microsphere production system of uniform particle diameter according to claim 1, it is characterized in that: in described production district, be additionally provided with the cleanout fluid preparing tank being connected with described microsphere washer, described microsphere washer is also connected with a cleanout fluid purifying regeneration equipment, and described cleanout fluid purifying regeneration equipment is also connected with described cleanout fluid preparing tank；Described vortex mixer is also associated with an Agitation Tank.
3. the agarose gel microsphere production system of uniform particle diameter according to claim 2, it is characterised in that: the oil phase outlet of described oil water separator separates purifier apparatus with oil product and is connected, and described oil purification equipment is also connected with described premix heating kettle.
4. the agarose gel microsphere production system of uniform particle diameter according to claim 1, it is characterized in that: in described control zone, be provided with the control station of production line panorama screen, it is provided with glass partition between described control zone and production district, in control zone, is provided with the visit passage being close to glass partition.
5. the agarose gel microsphere production system of uniform particle diameter according to claim 1, it is characterized in that: the kettle inner top of the homogeneous froth breaking still of described microwave heating still, ultrasound wave and ultrasound wave homogenizing still three is provided with full-view camera, and the kettle peripheral part of three is provided with microwave heating equipment；The limit stirring paddle being positioned at week side and the dispersion wheel being centrally located it is provided with in the kettle of described microwave heating still；Being provided with centrally located emulsifying head in the kettle of described ultrasound wave homogeneous froth breaking still, autoclave body bottom is provided with high frequency ultrasound wave producer；Being provided with the limit stirring paddle being positioned at week side and the emulsifying head being centrally located in the kettle of described ultrasound wave homogenizing still, autoclave body bottom is provided with high frequency ultrasound wave producer.
6. the agarose gel microsphere high-efficient production technology of a uniform particle diameter, it is characterized in that: include the agarose gel microsphere production system of any one uniform particle diameter as described in claim 1 ~ 5, and sequentially include the following steps: (1) agarose is joined in ultra-pure water by certain ratio, and it is delivered in microwave heating still and quickly fully dissolves forms glue A after being transported in rubber mill to process 10 ~ 20min；Light oil as solvent and the mink cell focus as surfactant are joined in premix heating kettle after Hybrid Heating with certain ratio simultaneously, be transported to and ultrasound wave homogeneous froth breaking still carries out process form the homogeneous B of phase without scald in warm oil；(2) the homogeneous B of phase without scald in warm oil is transported in ultrasound wave homogenizing still it is heated to predetermined temperature, open high frequency ultrasound wave producer and start limit stirring paddle and emulsifying head, after operating 15 ~ 30min, glue A is delivered in ultrasound wave homogenizing still by certain flow rate, the rotating speed of limit stirring paddle and emulsifying head will be adjusted after glue A conveying, start to be cooled to 25 DEG C with the speed of 1 ~ 10 DEG C/min after running 30 ~ 120min；(3) feed liquid in ultrasound wave homogenizing still is transported in oil water separator, in oil water separator, adds suitable alcohols breakdown of emulsion, and open mid-frequency ultrasonic ripple acceleration breakdown of emulsion, obtain oil water two phase system；(4) oil-water separating function of oil water separator is opened, obtain aqueous phase and enter microsphere washer, to cleanout fluid preparing tank be transported in microsphere washer containing in the washing liquid of finite concentration ethanol and salt by certain flow rate, open low-frequency ultrasonic waves and remove the little oil droplet of the microsphere surface attachment in aqueous phase；(5) 20% alcoholic solution of configuration in Agitation Tank is transported in vortex mixer, more clean microsphere is transported in vortex mixer, be transported to metering and separate loading machine after mix homogeneously and carry out metering packing.
7. the agarose gel microsphere high-efficient production technology of uniform particle diameter according to claim 6, it is characterized in that: after the oil phase entrance oil product separation purifier apparatus that in step (4), the separation of oil water separator obtains is easily separated purification, then be transported in premix heating kettle standby；Cleanout fluid after cleaning in step (1) is transported in cleanout fluid preparing tank after entering the regeneration of cleanout fluid purifying regeneration equipment and recycles.
8. the agarose gel microsphere high-efficient production technology of uniform particle diameter according to claim 6, it is characterised in that: in step (1), agarose is 1 50～8 25 with the mass ratio of ultra-pure water；Light oil described in step (1) is one or more in light diesel fuel, heavy diesel fuel, No. 98 gasoline, isobutyltrimethylmethane. and glycerol；Described mink cell focus is the mixed oil phase viscosity of one or more in Camellia oil, Petiolus Trachycarpi oil, Oleum Cocois, lanoline, Adeps Sus domestica and Cera Flava, light oil and mink cell focus is 30～580mPa s.
9. the agarose gel microsphere high-efficient production technology of uniform particle diameter according to claim 6, it is characterised in that: the ultrasonic frequency of the homogeneous froth breaking still of step (1) ultrasound wave is 30～50KHz；In step (2), the ultrasonic frequency of ultrasound wave homogenizing still is 80～120KHz；In step (3), the mid-frequency ultrasonic wave frequency of oil water separator is 40～60KHz；In step (4), the low frequency ultrasound wave frequency of microsphere washer is 20～28KHz.
10. the agarose gel microsphere high-efficient production technology of uniform particle diameter according to claim 6, it is characterized in that: in step (2), ultrasound wave homogenizing still is 200～1500r/Min at the rotating speed of the time internal emulsification head of operating 15 ~ 30min, and limit rotating speed of agitator is 20～150r/min；Glue A is delivered to the flow speed control in ultrasound wave homogenizing still at 0.5～50L/min, and the time of conveying glue A controls at 2～10min；Carry after the adjustment of rotational speed of all emulsifying head and limit stirring paddle after glue respectively 2000～18000r/min and 50～200r/min.
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| CN108690202A (en) * | 2018-06-21 | 2018-10-23 | 福建省天源兴达食品有限公司 | A kind of manufacture craft of low-temperature instant agar |
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