CN1259352C - Preparation process and device for superparamagnetism polymer microsphere - Google Patents
Preparation process and device for superparamagnetism polymer microsphere Download PDFInfo
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- CN1259352C CN1259352C CN 03149190 CN03149190A CN1259352C CN 1259352 C CN1259352 C CN 1259352C CN 03149190 CN03149190 CN 03149190 CN 03149190 A CN03149190 A CN 03149190A CN 1259352 C CN1259352 C CN 1259352C
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Abstract
The present invention relates to a method for preparing superparamagnetism polymer microspheres and a device thereof. In the preparing method, the breaking dispersion and the polyreaction of liquid drops are respectively carried out; oil phase liquid drops with a large viscosity are uniformly broken by two kinds of same-intensity normal force generated by the vibration of wire-mesh sieve plates; the obtained matter enters a reaction still for reaction under the condition of the existence of a stabilizing agent; the device comprises a reaction still, an oil phase storing tank and a water phase storing tank. The present invention is characterized in that the device also comprises a dispersing tower; the oil phase storing tank and the water phase storing tank are respectively communicated with the bottom inlet of the dispersing tower; the reaction still is communicated with the top of the dispersing tower; a vibrating shaft is arranged on the centerline of the dispersing tower; the upper end of the vibrating shaft is connected with an eccentric wheel positioned above the dispersing tower; 2 to 50 wire-mesh sieve plates are arranged on the vibrating shaft. The present invention is mainly used for preparing a carrier of superparamagnetism polymer microspheres with the uniform micrometre dimensions and sizes and has potential application value for the separation of biomolecules.
Description
Technical field
The present invention relates to the preparation method and the isolated plant of magnetic microsphere carrier, particularly a kind of preparation method of microballs of super-paramagnetic polymer and device thereof.
Background technology
The application of magnetic microsphere carrier in bioseparation more and more is subject to people's attention.Compare with other biochemical isolation technique and to have many potential advantages, be applied to fields such as cellular segregation, immobilized enzyme, immunodetection and protein purification gradually.Adopt the macroporous type or the non-pass magnetic carrier of micron-scale at present mostly about the biomolecules magnetic resolution.Magnetic microsphere requires to have higher magnetic property, particle size is little, narrow particle size distribution, chemical stability is good and preparation technology simple, low price.Suspension polymerization is a kind of important method of current preparation micron order magnetic microsphere.Existing magnetic polymer microsphere preparation facilities generally comprises oil phase storage tank, water storage tank and reactor, after oil phase and water mix by a certain percentage, adds in the reactor.But in reaction process, owing to adopt the mechanical stirring slurry to mix, the velocity field of paddle is different and different with the distance of axle syneresis leaf, the each several part drop is stressed also different in the reactor, cause drop not of uniform size, the final magnetic microsphere granularity that generates distributes wide, and magnetic property is widely different between the different microballoons, influences practical effect.
Suspension polymerization related to the present invention (referring to U.S. Pat 4,339,337) is the magnetic Fe of oleophylic processing
3O
4The oil phase that particle, lipophilicity vinyl monomer and oil-soluble initiator are formed is dispersed in aqueous phase, and under mechanical stirring and function of stabilizer, oil phase is the drop state and is dispersed in aqueous phase, temperature reaction.Experimental result shows, because dispersion effect is poor in the reaction, and nano-scale magnetic Fe especially
3O
4Particle is easily reunited in polymerization process and is separated with vinyl monomer, and there are some defectives in the synthetic polymer microballoon on performance, as magnetic Fe
3O
4Content is low, and magnetic-particle easily accumulates in the ball periphery, and different ball magnetic content are big, homogeneity is poor.Cocker etc. adopt the inverse suspension polymerization method (referring to Biotechnology and Bioengineering, vol.53:79-87,1997) prepare the magnetic polyacrylamide microsphere, and obtain the microballoon of particle diameter, but particle size distribution is wide at 60-600 μ m with the method for screening.Official's moon equality is improved the suspension polymerization device, makes suspension polymerization carry out (referring to Chinese invention patent CN98124516.1) in the cylindrical stirring reactor with vertical flow-stopping plate.Another kind method be by SPG (the Shirasu Porous Glass) method of exploitation such as Omi (referring to Journal of Applied Polymer Science, vol.51:1-11,1994; Colloids Surface A:Physicochemical Engineering Aspects, vol.109:97-107,1996).Its concrete operation is to adopt the SPG glass pore membrane with big or small homogeneous aperture to replace traditional mechanical stirring, and the filtration by fenestra generates uniform drop, thereby temperature reaction obtains uniform microballoon then.But because glassy membrane is hydrophilic and is fixed on the hollow tube that it is short grained microsphere supported to make this device can't be used for preparation band solid magnetic, reason is that the magnetic particle easily stops up fenestra, and is difficult to wash off.
Summary of the invention
Purpose of the present invention: overcome existing suspension polymerization process and conventional stirring-type suspension polymerization device when the preparation magnetic polymer microsphere, the defective that the made polymer microballoon that can not generate the magnetic microsphere of homogeneous and cause exists on performance, and the SPG method can't prepare the problem of magnetic microballoon, thereby a kind of preparation method of microballs of super-paramagnetic polymer is provided.
Another object of the present invention: a kind of device for preparing microballs of super-paramagnetic polymer is provided.
The object of the present invention is achieved like this: the preparation method of microballs of super-paramagnetic polymer provided by the invention may further comprise the steps:
(1) be after oil phase that 100: 1: 0.5 to 100: 10: 20 oil-soluble polymers monomer, oil-soluble initiator and oil base magnetic nanoparticle are formed mixes, to add in the oil phase storage tank weight part ratio; Described oil-soluble initiator is benzoyl peroxide or azo isobutyronitrile; Described oil base magnetic nanoparticle is Z 250, the Z 250 of capric acid coating or the ferric oxide that citric acid coats that oleic acid coats;
(2) be 100 with weight part ratio in the water storage tank: 0.5-100: 5 water and stablizer mix the water that forms and add in the scattered tower, and described stablizer is polyvinyl alcohol or polyvinylpyrrolidone;
(3) again oil phase is added scattered tower from the bottom of scattered tower, and and scattered tower in water mix and form emulsion, the weight part ratio of oil phase and water is 1: 0.5 to 1: 100;
(4) open the motor drive eccentric wheel, drive vibrating shaft and make it to do vibration up and down reciprocatingly, carry out swing crushing under the effect of emulsion silk screen sieve plate on the vibrating shaft in scattered tower, and rise;
(5) emulsion in the scattered tower continues to rise to the top, finely dispersed monomer droplet overflows in the reactor that is equipped with the identical water of step (2) and reacts, its temperature of reaction is 60 ℃-80 ℃, obtain the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution, the volume of the water in the reactor accounts for the 1/3-2/3 of reactor volume.
Described oil-soluble polymers monomer is that weight part ratio is 10: 0.5: 1-10: the mixture of 1: 6 vinylbenzene, divinylbenzene and glycidyl methacrylate or weight part ratio are 10: 0.5: 1-10: the mixture of 1: 6 methyl methacrylate, divinylbenzene and glycidyl methacrylate.
A kind of prepare microballs of super-paramagnetic polymer reaction unit, this device comprises a reactor, oil phase storage tank and water storage tank, it is characterized in that, also comprises a scattered tower; Described oil phase storage tank is communicated with nitrogengas cylinder, and be connected with the scattered tower bottom inlet through the first flow meter, the water storage tank is connected with another inlet of scattered tower bottom through the peristaltic pump and second under meter, reactor is connected with the scattered tower top, one vibrating shaft is installed on the medullary ray of described scattered tower, and the upper end of vibrating shaft is connected with the eccentric wheel that is positioned at the scattered tower top; 2-50 silk screen sieve plate is installed on the described vibrating shaft.
The silk screen sieve plate of described silk screen sieve plate for making by stainless steel, tetrafluoroethylene, steel wire, polyvinyl chloride, polyethylene, plastics or nylon.
The circle that the mesh of described silk screen sieve plate is evenly distributed, square or rhombus.
The circular net bore dia of described silk screen sieve plate is between 0.1 micron to 20 millimeters.
The aperture of the square or diamond-shaped meshes of described silk screen sieve plate is between 0.1 micron to 20 millimeters.
Device of the present invention, disperseing to substitute the mechanical stirring slurry with the vibration of net formula sieve plate disperses, the breakup of drop is disperseed and polyreaction is separately carried out, provide the energy of the breakup of drop, the oil phase breakup of drop that viscosity is bigger by the silk screen sieve plate up-down vibration that has even mesh; Vibrating shaft is driven by the eccentric wheel of scattered tower top, and the amplitude of vibration and frequency can be regulated, and the waveform of vibration can be sinusoidal wave or other waveform; The size of drop and degree of scatter can be controlled by the frequency and the amplitude of silk screen aperture and vibrating shaft; Dexterously drop suffered shearing force not of uniform size in mechanical stirring is changed in the vibration of net formula disperses and form normal force of the same size by the silk screen up-down vibration, the size of wire mesh screens panel vibration intake directly influences droplet dia size, mass transfer character and tower processing power, and the vibrational frequency of silk screen sieve plate and amplitude directly influence the stirring intensity in the tower.
Because mesh diameter is less, and size evenly, driving vibrating shaft at hotwire makees up and down reciprocatingly in the vibration processes silk screen sieve plate, emulsion is subjected to the swing crushing of silk screen sieve plate in uphill process, under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, is fractured into the even small droplets of certain particle size through the big drop of multi-layer silk screen sieve plate, less drop directly by mesh, enters reactor at last and directly carries out next step polyreaction in the presence of stablizer.
The diameter Distribution of drop is relevant with the vibration intensity of silk screen sieve plate.When the energy of vibration input hour, droplet diameter distribution broad, and the multimodal phenomenon is arranged.When vibration intensity was higher, droplet diameter distribution was narrower, was unimodal distribution.In use can be according to the size of required microballoon, the factors such as viscosity of what and reactant of magnetic content are come the number of required silk screen sieve plate in the true fixed net type sieve plate vibration scattered tower, the size of mesh etc. in the microballoon.For the dispersion effect that guarantees drop can be installed a plurality of silk screen sieve plates on central shaft, form multistage diverting device, oil phase and water separately enter the vibration scattered tower simultaneously, by regulating under meter separately, can guarantee that oil phase and water react according to a certain percentage.The ratio of oil phase and water can be regulated between 1: 0.5 to 1: 100.
The invention has the advantages that: the preparation method of magnetic polymer microsphere of the present invention and device thereof, the magnetic polymer microsphere of preparation size homogeneous has that higher magnetic property, particle size are little, narrow particle size distribution, chemical stability be good; And preparation technology is simple, low price.
Correspondingly, net formula sieve plate vibration suspension polymerization device of the present invention has following characteristics:
(1) flux is big and efficient is higher.
(2), thereby be easy to handle and contain the solid material because vibrational state can be selected and be in the aperture of mesh.
(3) since vibrational frequency and amplitude can regulate, and on the tower cross section external energy distribution uniform, thereby be suitable for handling easy emulsifying system.
(4) simple in structure, amplify easily.
(5) maintenance and process cost are low.
Suspension polymerization device provided by the invention has advantages such as simple in structure, that cost is low, and controllability is good.This device is not only applicable to prepare the non magnetic polymer microballoon that uniform magnetic polymer microsphere also is applicable to the preparation homogeneous.
Description of drawings
Fig. 1 the present invention prepares the structural representation of the reaction unit of magnetic polymer microsphere
The accompanying drawing sign
1, oil phase storage tank 2, water storage tank 3, scattered tower
4, reactor 5, peristaltic pump 6, vibrating shaft
7, silk screen sieve plate 8, nitrogengas cylinder 9, first flow meter
10, second under meter 11, eccentric wheel
Embodiment
Embodiment 1
Make the suspension polymerization device of a preparation magnetic polymer microsphere.
The oil phase storage tank 1 of this device is communicated with nitrogengas cylinder 8, and be connected with scattered tower 3 bottom inlets through first flow meter 9, water storage tank 2 is connected with another inlet of scattered tower 3 bottoms through the peristaltic pump 5 and second under meter 10, reactor 4 is communicated with scattered tower 3 tops, vibrating shaft 6 is installed on the central axis of described scattered tower 3, and vibrating shaft 6 is driven by the eccentric wheel 11 of cat head; 10 silk screen sieve plates of being made by Stainless Steel Wire 7 are installed on the described vibrating shaft, and the mesh diameter of silk screen sieve plate is 20 microns, is equally distributed circle; Vibrating shaft 6 is done vibration up and down reciprocatingly under the drive of eccentric wheel 11, the waveform of its vibration is sinusoidal wave.
Embodiment 2
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix by the oil phase that the Z 250 that 67ml vinylbenzene, 5ml divinylbenzene, the composite oil-soluble polymers monomer of 30ml glycidyl methacrylate, 3g benzoyl peroxide and 10g oleic acid coat is formed after, adding oil phase storage tank 1.
2, the water with 2000ml water and 30g PVAC polyvinylalcohol mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 10.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 500ml water and 7.5g PVAC polyvinylalcohol, temperature is risen to 70 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, finely dispersed monomer droplet reacts with 500ml water and 5g PVAC polyvinylalcohol after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Embodiment 3
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix oil phase that Z 250 that the oil-soluble polymers monomer, 6g benzoyl peroxide and the 15g capric acid that form coat forms and mix by 100ml methyl methacrylate, 10ml divinylbenzene and 50ml glycidyl methacrylate after, adding oil phase storage tank 1.
2, the water with 2000ml water and 60g polyvinylpyrrolidone mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 20.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 400ml water and 12g polyvinylpyrrolidone, temperature is risen to 80 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, and finely dispersed monomer droplet reacts after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Embodiment 4
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix by the oil phase that the ferric oxide that 100ml vinylbenzene, 7ml divinylbenzene, the composite oil-soluble polymers monomer of 20ml glycidyl methacrylate, 3g benzoyl peroxide and 10g citric acid coat is formed after, adding storage tank 1.
2, the water with 1000ml water and 40g polyvinylpyrrolidone mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 10.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 100ml water and 4g polyvinylpyrrolidone, temperature is risen to 80 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, and finely dispersed monomer droplet reacts after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Embodiment 5
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix by the oil phase that the Z 250 that 80ml vinylbenzene, 5ml divinylbenzene, the composite oil-soluble polymers monomer of 30ml glycidyl methacrylate, 6g azo isobutyronitrile and 8g oleic acid coat is formed after, adding oil phase storage tank 1.
2, the water with 500ml water and 10g PVAC polyvinylalcohol mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 5.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 100ml water and 1g PVAC polyvinylalcohol, temperature is risen to 80 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, and finely dispersed monomer droplet reacts after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Embodiment 6
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix by the oil phase that the Z 250 that the composite oil-soluble polymers monomer of 100ml methyl methacrylate, 5ml divinylbenzene and 10ml glycidyl methacrylate, 5g azo isobutyronitrile and 10g capric acid coat is formed after, adding oil phase storage tank 1.
2, the water with 1000ml water and 10g PVAC polyvinylalcohol mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 20.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 200ml water and 2g PVAC polyvinylalcohol, temperature is risen to 70 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, and finely dispersed monomer droplet reacts after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Embodiment 7
Utilize the device of embodiment 1 to prepare microballs of super-paramagnetic polymer, its step is as follows:
1, will mix oil phase that ferric oxide that the oil-soluble polymers monomer, 6g azo isobutyronitrile and the 15g citric acid that form coat forms and mix by 100ml methyl methacrylate, 5ml divinylbenzene and 60ml glycidyl methacrylate after, adding oil phase storage tank 1.
2, the water with 1000ml water and 40g polyvinylpyrrolidone mixing formation adds networking formula sieve plate scattered tower 2 by water storage tank 2 by peristaltic pump 5.
3, under the pressure of nitrogengas cylinder, oil phase enters the reactor 4 from the bottom of scattered tower 2, and and water mix to form emulsion, the under meter by separately guarantees that the weight part ratio of oil phase and water is 1: 8.
4, hotwire makes net formula sieve plate do vibration up and down reciprocatingly, and emulsion is subjected to the swing crushing of silk screen in uphill process, and under the effect of homogeneous normal force, big oil phase drop is fractured into tiny liquid pearl, and enters the next stage dispersion, and small droplets then directly passes through.
5, in reactor 4, add 100ml water and 4g polyvinylpyrrolidone, temperature is risen to 60 ℃.
6, the emulsion in the scattered tower 2 continues to rise to the top and overflows in the reactor 4, and finely dispersed monomer droplet reacts after entering reactor 4 immediately, obtains the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution at last.
Claims (7)
1, a kind of preparation method of microballs of super-paramagnetic polymer, this method may further comprise the steps:
(1) be after oil phase that 100: 1: 0.5 to 100: 10: 20 oil-soluble polymers monomer, oil-soluble initiator and oil base magnetic nanoparticle are formed mixes, to add in the oil phase storage tank weight part ratio; Described oil-soluble initiator is benzoyl peroxide or azo isobutyronitrile; Described oil base magnetic nanoparticle is Z 250, the Z 250 of capric acid coating or the ferric oxide that citric acid coats that oleic acid coats;
(2) be 100 with weight part ratio in the water storage tank: 0.5-100: 5 water and stablizer mix the water that forms and add in the scattered tower, and described stablizer is polyvinyl alcohol or polyvinylpyrrolidone;
(3) again oil phase is added scattered tower from the bottom of scattered tower, and and scattered tower in water mix and form emulsion, the weight part ratio of oil phase and water is 1: 0.5 to 1: 100;
(4) open the motor drive eccentric wheel, drive vibrating shaft and make it to do vibration up and down reciprocatingly, carry out swing crushing under the effect of emulsion silk screen sieve plate on the vibrating shaft in scattered tower, and rise;
(5) emulsion in the scattered tower continues to rise to the top, finely dispersed monomer droplet overflows in the reactor that is equipped with the identical water of step (2) and reacts, its temperature of reaction is 60 ℃-80 ℃, obtain the microballs of super-paramagnetic polymer of micron order, narrow diameter distribution, the volume of the water in the reactor accounts for the 1/3-2/3 of reactor volume.
2, press the preparation method of the described microballs of super-paramagnetic polymer of claim 1, it is characterized in that described capacitive oil polymer monomer is that weight part ratio is 10: 0.5: 1-10: the mixture of 1: 6 vinylbenzene, divinylbenzene and glycidyl methacrylate or weight part ratio are 10: 0.5: 1-10: the mixture of 1: 6 methyl methacrylate, divinylbenzene and glycidyl methacrylate.
3, a kind of reaction unit for preparing the described microballs of super-paramagnetic polymer of claim 1, this device comprise a reactor (4), oil phase storage tank (1) and water storage tank (2), it is characterized in that, also comprise a scattered tower (3); Described oil phase storage tank (1) is communicated with nitrogengas cylinder (8), and be connected with scattered tower (3) bottom inlet through first flow meter (9), water storage tank (2) is connected with another inlet of scattered tower (3) bottom through peristaltic pump (5) and second under meter (10), reactor (4) is connected with scattered tower (3) top, one vibrating shaft (6) is installed on the medullary ray of described scattered tower (3), and the upper end of vibrating shaft (6) is connected with the eccentric wheel (11) that is positioned at scattered tower (3) top; 2-50 silk screen sieve plate (7) is installed on the described vibrating shaft.
4, by the reaction unit of the described preparation microballs of super-paramagnetic polymer of claim 3, it is characterized in that the silk screen sieve plate of described silk screen sieve plate (7) for making by stainless steel, tetrafluoroethylene, steel wire, polyvinyl chloride, polyethylene, plastics or nylon.
5, by the reaction unit of the described preparation microballs of super-paramagnetic polymer of claim 3, it is characterized in that the circle that the mesh of described silk screen sieve plate (7) is evenly distributed, square or rhombus.
6, by the described preparation microballs of super-paramagnetic polymer of claim 7 reaction unit, it is characterized in that the circular net bore dia of described silk screen sieve plate (7) is between 0.1 micron to 20 millimeters.
7, by the described preparation microballs of super-paramagnetic polymer of claim 7 reaction unit, it is characterized in that the aperture of the square or diamond-shaped meshes of described silk screen sieve plate (7) is between 0.1 micron to 20 millimeters.
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| CN 03149190 CN1259352C (en) | 2003-06-20 | 2003-06-20 | Preparation process and device for superparamagnetism polymer microsphere |
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| CN 03149190 CN1259352C (en) | 2003-06-20 | 2003-06-20 | Preparation process and device for superparamagnetism polymer microsphere |
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| CN1298791C (en) * | 2005-07-19 | 2007-02-07 | 吉林大学 | Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method |
| CN102286452B (en) * | 2011-07-19 | 2013-04-24 | 浙江大学 | Method for preparing magnetic covalent immobilized enzyme carriers |
| CN102516563B (en) * | 2011-11-24 | 2013-06-12 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Method for preparing micro magnetic carrier, micro magnetic carrier and active sludge immobilization method |
| CN103111197B (en) * | 2013-01-28 | 2015-07-01 | 西南石油大学 | Swelling device with middle screen guide rod and for accelerating dissolution of polymer |
| CN103554389A (en) * | 2013-09-27 | 2014-02-05 | 华侨大学 | Preparation method of magnetic polymeric microsphere used for immobilized iron reducing bacteria |
| CN113877499A (en) * | 2021-10-08 | 2022-01-04 | 南京大学 | Uniform particle resin production device and use method thereof |
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