CN109382051B - Production system and production process of nano biomedical material - Google Patents
Production system and production process of nano biomedical material Download PDFInfo
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- CN109382051B CN109382051B CN201811365459.6A CN201811365459A CN109382051B CN 109382051 B CN109382051 B CN 109382051B CN 201811365459 A CN201811365459 A CN 201811365459A CN 109382051 B CN109382051 B CN 109382051B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B5/00—Other centrifuges
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Abstract
The invention discloses a production system and a production process of a nano biomedical material, belonging to the technical field of medical material production. The production system and the production process of the nano biomedical material not only can produce the nano biomedical material safely and reliably, but also can effectively meet the requirement that the corresponding nano biomedical material cannot be produced at home at present.
Description
Technical Field
The invention relates to the technical field of medical material production, in particular to a production system and a production process of a nano biomedical material.
Background
At present, the nano biomedical material has very obvious effect on auxiliary biological detection and diagnosis. However, there is no related industrial production system and production process thereof in the market of nano biomedical materials, so there is a need for a production system and production process thereof in the market.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In view of the above, the present invention is directed to a system and a process for producing a biomedical nanomaterial, which can solve the problem that no system and process for producing a biomedical nanomaterial exist in the market.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a production system of nano biomedical materials comprises a reaction kettle, an electromagnetic separator, a tubular centrifuge, a first membrane separator, a second membrane separator and a reduced pressure distillation tower;
the reaction kettle is used for preparing magnetic particles, finely processing the magnetic particles and organically coating the finely processed magnetic particles;
the electromagnetic separator is used for separating magnetic particles prepared in the reaction kettle from reaction liquid;
the tube centrifuge is: the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of particle size after fine processing;
the first membrane separator: the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of molecular weight after fine processing;
the second membrane separator: used for removing the magnetic particles which do not meet the molecular weight requirement after organic coating;
the reduced pressure distillation column: the magnetic particle concentrator is used for concentrating magnetic particles meeting the particle size requirement and the molecular weight requirement after organic coating.
Further, a first liquid outlet of the reaction kettle is respectively connected with a liquid inlet of the electromagnetic separator, a liquid inlet of the tubular centrifuge and a liquid inlet of the second membrane separator; a liquid outlet of the electromagnetic separator is connected with a second liquid inlet of the reaction kettle;
a liquid outlet of the tubular centrifuge is connected with a liquid inlet of the first membrane separator, and a liquid outlet of the first membrane separator is connected with any liquid inlet of the reaction kettle; the liquid outlet of the second membrane separator is connected with the liquid inlet of the reduced pressure distillation tower.
Furthermore, a spraying device is arranged at the top of the electromagnetic separator and used for washing the magnetic particles.
Further, the electromagnetic separator also comprises an adjustable electromagnetic intensity device.
The production process of the production system for nano biomedical materials comprises the following steps:
s1, adding the raw materials to be prepared into a reaction kettle according to a certain proportion, and reacting the raw materials in the reaction kettle to prepare a reaction solution containing nano-scale magnetic particles;
s2, the reaction kettle sends the reaction liquid containing the nano-scale magnetic particles to an electromagnetic separator, the magnetic separation of the liquid and the nano-scale magnetic particles is carried out, and the separated liquid is discharged; the electromagnetic separator continuously washes all the nanoscale magnetic particles by washing liquid;
s3, after the washed washing liquid is discharged completely by the electromagnetic separator, the electrification is stopped, the backflushing liquid is introduced, the nanoscale magnetic particles are eluted from the wall of the electromagnetic separator, the reaction liquid containing the magnetic particles after elution is returned to the reaction kettle, and the fine treatment is carried out;
s4, sending the reaction liquid containing the refined magnetic nanoparticles to a tubular centrifuge, and centrifuging to remove the magnetic nanoparticles which do not meet the size of the particle size specification;
s5, the tubular centrifuge sends the residual magnetic nanoparticle reaction liquid meeting the particle size requirement to a first membrane separator, and removes the magnetic nanoparticles not meeting the molecular weight requirement;
s6, returning the residual magnetic nanoparticle reaction solution meeting the molecular weight requirement to the reaction kettle by the first membrane separator, and coating with a high polymer material;
s7, the reaction kettle sends the coated magnetic nano-particle reaction liquid to a second membrane separator to remove the magnetic nano-particles which do not meet the molecular weight requirement;
and S8, sending the residual magnetic nanoparticle reaction liquid meeting the molecular weight requirement to a reduced pressure distillation tower by the second membrane separator, concentrating, and finishing production after reaching the specified concentration.
Further, the stirring speed of the reaction kettle in the steps S1 and S3 is: 500-: 30-360min, and the temperature range is as follows: from room temperature to 80 ℃.
Further, the magnetic field strength range in the electromagnetic separator in the step S2 is: 2000 + 10000 gauss.
Further, the rotation speed range of the tube centrifuge in the step S4 is: 4000-6000 rpm.
Further, the stirring speed of the reaction kettle in the step S6 is: 200-1000 rpm, stirring time 30-360min, temperature range: from room temperature to 80 ℃.
Further, the temperature range of the vacuum distillation column in the step S8 is: 60-70 ℃.
Compared with the prior art, the invention has the beneficial effects that: the production system and the production process of the nano biomedical material not only can produce the nano biomedical material safely and reliably, but also can effectively meet the requirement that the corresponding nano biomedical material cannot be produced at home at present. 2, the production system of the nano biomedical material is simple and easy to control; the cost of enterprises or users can be effectively reduced. 3, the production system and the production process of the nano biomedical material not only can accurately realize refined treatment, but also can effectively improve the quality qualification rate of the produced material.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below.
FIG. 1 is a schematic view of a production system according to an embodiment of the present invention;
the figures in the drawings represent:
1. reaction kettle 2, electromagnetic separator 3, tubular centrifuge 4, first membrane separator 5, second membrane separator 6, reduced pressure distillation tower
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Example 1
As shown in figure 1, the production system of the nano biomedical material comprises a reaction kettle 1, an electromagnetic separator 2, a tubular centrifuge 3, a first membrane separator 4, a second membrane separator 5 and a reduced pressure distillation tower 6.
The reaction kettle 1 is used for preparing magnetic particles (magnetic particles), finely processing the magnetic particles and organically coating the finely processed magnetic particles;
the electromagnetic separator 2: used for separating the magnetic particles prepared in the reaction kettle 1 from the reaction liquid;
a tube centrifuge 3: the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of particle size after fine processing; the method is mainly used for removing the magnetic nano particles larger than 12 nm.
First membrane separator 4: the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of molecular weight after fine processing; mainly removes the magnetic nano-particles with the molecular weight less than 3500.
The second membrane separator 5: used for removing the magnetic particles which do not meet the molecular weight requirement after organic coating; mainly removes magnetic nano particles with molecular weight more than 10000.
Vacuum distillation column 6: the magnetic particle concentrator is used for concentrating magnetic particles meeting the particle size requirement and the molecular weight requirement after organic coating.
The liquid outlet of the reaction kettle 1 is respectively connected with the liquid inlet of the electromagnetic separator 2, the liquid inlet of the tubular centrifuge 3 and the liquid inlet of the second membrane separator 5, but the liquid inlets of the three are not simultaneously fed with liquid; when the liquid inlet of the electromagnetic separator 2 or the liquid inlet of the tubular centrifuge 3 or the liquid inlet of the second membrane separator 5 is opened, the other two liquid inlets are in a closed state.
The liquid outlet of the electromagnetic separator 2 is connected with the second liquid inlet of the reaction kettle 1; the positions of the liquid inlet and the liquid outlet of the electromagnetic separator 2 can be self-set according to actual requirements; can be moved up and down, and can be moved down and up.
The liquid outlet of the tubular centrifuge 3 is connected with the liquid inlet of the first membrane separator 4, and the liquid outlet of the first membrane separator 4 is connected with any liquid inlet of the reaction kettle 1.
The liquid outlet of the second membrane separator 5 is connected with the liquid inlet of the reduced pressure distillation tower 6.
The reaction kettle 1, the electromagnetic separator 2, the tubular centrifuge 3, the first membrane separator 4, the second membrane separator 5 and the reduced pressure distillation tower 6 are all provided with liquid discharge ports, and the positions of the liquid discharge ports can be adjusted automatically according to actual needs.
The nano biological material produced by the production system of the nano biological medical material is safe and reliable, and can effectively meet the requirement that the corresponding nano medical biological material cannot be produced at home at present.
Example 2
The top of the electromagnetic separator 2 is also provided with a spraying device for washing the magnetic particles; the spraying device can accurately wash all magnetic particles comprehensively, can save washing liquid used in washing, and effectively reduces the cost of enterprises or users.
Example 3
The electromagnetic separator 2 further comprises an adjustable electromagnetic intensity device. The user adjusts the electromagnetic intensity according to actual needs. The adjustable electromagnetic intensity effectively meets the requirement of a user for automatically setting the electromagnetic intensity, so that the whole system is convenient and quick to use.
Example 4
The process utilizing the production system of the nano biomedical material in the embodiment comprises the following steps:
s1, adding the raw materials to be prepared into a reaction kettle 1 according to a certain proportion, and reacting in the reaction kettle 1 to prepare a reaction solution containing nano-scale magnetic particles;
specifically, after the raw materials were added, the reaction vessel 1 was stirred under normal pressure.
Preferably, the stirring speed of the reaction kettle 1 is as follows: 500-: 30-360min, and the temperature range is as follows: from room temperature to 80 ℃.
S2, the reaction kettle 1 sends the prepared reaction liquid containing the nano-scale magnetic particles to a feed inlet of an electromagnetic separator 2 for magnetic separation of the liquid and the nano-scale magnetic particles, and the separated liquid is discharged from a liquid discharge port; the electromagnetic separator 2 continuously washes all the nanometer magnetic particles by washing liquid;
specifically, after the reaction liquid containing the nano-scale magnetic particles prepared by the reaction kettle 1 enters the electromagnetic separator 2, the electromagnetic separator 2 is electrified, the reaction liquid containing the nano-scale magnetic particles is separated by the electromagnetic separator 2, so that the nano-scale magnetic particles are adsorbed on the inner wall of the electromagnetic separator 2, and the residual reaction liquid is discharged from a liquid discharge port of the electromagnetic separator 2. Preferably, the electromagnetic separator 2 sets the magnetic field strength as follows: 2000 gauss to 10000 gauss.
The reaction liquid passes through the electromagnetic separator 2, after the magnetic particles are adsorbed, the spraying device at the top of the electromagnetic separator is started to wash the magnetic particles until the PH value of the discharged liquid reaches 7.
S3, discharging the cleaning solution in the electromagnetic separator 2, stopping electrifying the electromagnetic separator 2, introducing the backflushing solution, eluting the nanoscale magnetic particles from the wall of the electromagnetic separator 2, returning the reaction solution containing the magnetic particles after elution to the second feeding hole of the reaction kettle 1, and refining.
Preferably, the backflushing liquid is: a backwash liquid mixed with nitrogen.
Specifically, a catalyst is added into the reaction kettle 1 for stirring, and the reaction solution containing the magnetic nanoparticles is subjected to refining treatment; the catalyst added to the reaction vessel 1 and the reaction solution containing the magnetic nanoparticles undergo an oxidation-reduction reaction. Preferably, under the normal pressure condition, the stirring speed of the reaction kettle 1 is as follows: 500-: 30-360min, and the temperature range is as follows: from room temperature to 80 ℃.
And S4, sending the reaction liquid containing the refined magnetic nanoparticles to a tubular centrifuge 3, centrifuging to remove the magnetic nanoparticles which do not meet the specification size, and discharging from a liquid outlet of the tubular centrifuge.
Specifically, the size of the removed magnetic nanoparticles can be automatically adjusted according to the actual needs of a user; preferably, the magnetic nanoparticles larger than 12nm are removed; the rotating speed of the centrifuge is 4000-6000rpm, and magnetic nano particles larger than 12nm are removed.
S5, the tubular centrifuge 3 sends the residual magnetic nanoparticle reaction liquid meeting the particle size requirement to the first membrane separator 4 for removing the small molecular magnetic nanoparticles which do not meet the specification; and discharged from the liquid discharge port of the first membrane separator 4.
Specifically, the removal molecular weight can be changed adaptively according to the user's setting. Preferably, the reaction solution containing magnetic nanoparticles with a molecular weight less than 3500 is introduced into the first membrane separator 4 for removing the magnetic nanoparticles with a molecular weight less than 12 nm.
S6, returning the residual magnetic nanoparticle reaction solution meeting the molecular weight requirement to the reaction kettle 1 by the first membrane separator 4, and coating the high molecular material.
Specifically, the residual magnetic nanoparticle reaction solution (with the particle size of 1nm-12 nm) with the molecular weight of more than 3500 is returned to the reaction kettle 1, and the high polymer material is added into the reaction kettle 1 to coat the magnetic nanoparticles with the high polymer material.
Preferably, under the normal pressure condition, the stirring speed of the reaction kettle 1 is 200-1000 rpm, the stirring time is 30min to 360min, and the temperature range is room temperature to 80 ℃; the high polymer materials added into the reaction kettle 1 are hydrophilic high polymer auxiliary materials and stabilizing agents.
The magnetic nano particles are wrapped by the polymer material, so that the hydrophilicity and the stability are improved, the nonspecific adsorption of the magnetic nano particles in human body application is reduced, and the toxicity of the nano biological material is reduced.
Therefore, the magnetic nano-particles coated with the organic polymer material can reduce the rejection and harm to human bodies when in use.
S7, the reaction kettle 1 sends the coated magnetic nano-particle reaction liquid to a second membrane separator 5, removes the magnetic nano-particles which do not meet the molecular weight requirement, and discharges the magnetic nano-particles from a liquid discharge port of the second membrane separator 5.
Specifically, removing magnetic nanoparticles with molecular weight greater than 10000; removing impurities with molecular weight more than 10000; and the molecular weight of the nano biomaterial is increased after the polymer is coated, so that the aim is to remove the non-coated biomaterial with the molecular weight of more than 10000 polymers.
S8, the second membrane separator 5 sends the residual magnetic nano-particle reaction liquid meeting the molecular weight requirement to the reduced pressure distillation tower 6 for concentration, and after reaching the specified concentration, the production is completed, and finally the nano biomedical material is obtained.
Preferably, the temperature range of the vacuum distillation tower 6 is as follows: 60-70 ℃.
The production process of the nano biomedical material can not only accurately realize refined treatment, but also ensure that the produced nano biomedical material is nontoxic and improve the safety of users; the invention can also effectively improve the quality qualification rate of the produced material.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A production system of nano biomedical materials is characterized by comprising a reaction kettle (1), an electromagnetic separator (2), a tubular centrifuge (3), a first membrane separator (4), a second membrane separator (5) and a reduced pressure distillation tower (6);
the reaction kettle (1) is used for preparing magnetic particles, finely processing the magnetic particles and organically coating the finely processed magnetic particles;
the electromagnetic separator (2): used for separating the magnetic particles prepared in the reaction kettle (1) from the reaction liquid;
the tube centrifuge (3): the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of particle size after fine processing;
the first membrane separator (4): the magnetic particle removing device is used for removing magnetic particles which do not meet the requirement of molecular weight after fine processing;
the second membrane separator (5): used for removing the magnetic particles which do not meet the molecular weight requirement after organic coating;
the reduced pressure distillation column (6): the magnetic particle concentrator is used for concentrating magnetic particles meeting the particle size requirement and the molecular weight requirement after organic coating;
a liquid outlet of the reaction kettle (1) is respectively connected with a liquid inlet of the electromagnetic separator (2), a liquid inlet of the tubular centrifuge (3) and a liquid inlet of the second membrane separator (5); a liquid outlet of the electromagnetic separator (2) is connected with a second liquid inlet of the reaction kettle (1);
a liquid outlet of the tubular centrifuge (3) is connected with a liquid inlet of the first membrane separator (4), and a liquid outlet of the first membrane separator (4) is connected with any liquid inlet of the reaction kettle (1); the liquid outlet of the second membrane separator (5) is connected with the liquid inlet of the reduced pressure distillation tower (6).
2. The system for producing nano biomedical materials according to claim 1, wherein said system is characterized in that
The top of the electromagnetic separator (2) is also provided with a spraying device for washing the magnetic particles.
3. The system for producing nano biomedical materials according to claim 2, wherein the electromagnetic separator (2) further comprises means for adjusting the electromagnetic intensity.
4. The process for producing a nano biomedical material production system according to any one of claims 1 to 3, comprising the steps of:
s1, adding raw materials to be prepared into a reaction kettle (1) according to a certain proportion, and reacting in the reaction kettle (1) to prepare a reaction solution containing nano-scale magnetic particles;
s2, the reaction kettle (1) sends the prepared reaction liquid containing the nano-scale magnetic particles to an electromagnetic separator (2), the magnetic separation of the liquid and the nano-scale magnetic particles is carried out, and the separated liquid is discharged; the electromagnetic separator (2) continuously washes all the nanometer magnetic particles by washing liquid;
s3, after the washed washing liquid is discharged completely by the electromagnetic separator (2), stopping electrifying and introducing a backflushing liquid, eluting the nanoscale magnetic particles from the wall of the electromagnetic separator (2), returning the reaction liquid containing the magnetic particles after elution to the reaction kettle (1), and performing refinement treatment;
s4, sending the reaction liquid containing the magnetic nanoparticles after the fine treatment to a tubular centrifuge (3), and centrifuging to remove the magnetic nanoparticles which do not meet the size specification of the particle size;
s5, the tubular centrifuge (3) sends the residual magnetic nanoparticle reaction liquid meeting the particle size requirement to a first membrane separator (4) to remove the magnetic nanoparticles not meeting the molecular weight requirement;
s6, returning the residual magnetic nanoparticle reaction solution meeting the molecular weight requirement to the reaction kettle (1) by the first membrane separator (4) for coating with a high polymer material;
s7, the reaction kettle (1) sends the coated magnetic nano-particle reaction liquid to a second membrane separator (5) to remove the magnetic nano-particles which do not meet the molecular weight requirement;
s8, the second membrane separator (5) sends the residual magnetic nanoparticle reaction liquid meeting the molecular weight requirement to a reduced pressure distillation tower (6) for concentration, and the production is finished after the concentration reaches the designated concentration.
5. The production process as claimed in claim 4, wherein the stirring speed of the reaction vessel (1) in the steps S1 and S3 is: 500-: 30-360min, and the temperature range is as follows: from room temperature to 80 ℃.
6. The production process as claimed in claim 4, wherein the magnetic field strength in the electromagnetic separator (2) in the step S2 is in the range of: 2000 + 10000 gauss.
7. The production process as claimed in claim 4, wherein the rotation speed range of the tube centrifuge (3) in the step S4 is: 4000-6000 rpm.
8. The production process as claimed in claim 4, wherein the stirring speed of the reaction tank (1) in the step S6 is: 200-1000 rpm, stirring time 30-360min, temperature range: from room temperature to 80 ℃.
9. The production process as claimed in claim 4, wherein the temperature range of the vacuum distillation column (6) in the step S8 is: 60-70 ℃.
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| CN101445277A (en) * | 2008-11-14 | 2009-06-03 | 东北大学 | Nano-crystalline Fe*O* particles with high absorption capacity and preparation method thereof |
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