CN111097344A - Equipment and method for preparing hydrogel microspheres - Google Patents

Equipment and method for preparing hydrogel microspheres Download PDF

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Publication number
CN111097344A
CN111097344A CN202010014079.9A CN202010014079A CN111097344A CN 111097344 A CN111097344 A CN 111097344A CN 202010014079 A CN202010014079 A CN 202010014079A CN 111097344 A CN111097344 A CN 111097344A
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CN
China
Prior art keywords
conveyor belt
driven roller
hydrogel microspheres
roller
micro
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010014079.9A
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Chinese (zh)
Inventor
石志军
陈坤
龙笑
杨光
汪茂旭
叶伟亮
潘博
刘昊
杨跃梅
周颖
贾冰寒
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Weige Stem Cell Technology Co.,Ltd.
Original Assignee
Beijing Zhicheng Biomedical Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing Zhicheng Biomedical Technology Co ltd filed Critical Beijing Zhicheng Biomedical Technology Co ltd
Priority to CN202010014079.9A priority Critical patent/CN111097344A/en
Publication of CN111097344A publication Critical patent/CN111097344A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052Preparation of gels
    • B01J13/0065Preparation of gels containing an organic phase
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/04Alginic acid; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/08Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof

Abstract

The invention discloses a device and a method for preparing hydrogel microspheres, wherein the device comprises: the bracket comprises a first end and a second end, wherein the first end is provided with a driving roller and the second end is provided with a driven roller; the transmission belt is arranged on the driving roller and the driven roller to connect the driving roller and the driven roller, and the outer side surface of the transmission belt is coated with super-hydrophobic paint; the quick-freezing box is arranged between the first end and the second end and is positioned above the material bearing section of the conveying belt, the lower part of the quick-freezing box is provided with a channel for the material bearing section of the conveying belt to pass through, and a gap for allowing a conveyed object to pass through is reserved between the conveying belt and the upper surface of the channel; the spray head is close to the first end and arranged above the conveyor belt towards the conveyor belt; and a collecting box disposed at a side where the second end where a portion of the conveyor belt is guided by the driven roller to protrude into the collecting box. The method can automatically produce the hydrogel microspheres, and improves the preparation efficiency of the hydrogel microspheres.

Description

Equipment and method for preparing hydrogel microspheres
Technical Field
The invention relates to the technical field of microsphere production, in particular to equipment and a method for preparing hydrogel microspheres.
Background
With the continuous development of the medical industry in China, the medical market is continuously expanded, and the demand of biological medical products is continuously increased. The application of the microspheres in the field of biomedicine is very wide, and the potential of scientific research and clinical application is very huge, but related devices for producing the gel microspheres in the market are not common at present, and related researches are few. For example, the utility model publication No. CN 203639164U discloses "a method for rapidly preparing SiO by using a superhydrophobic surface2Device for conveying gel microspheres' by using conveyor belt2Gel microspheres prepared by scraping with a scraperSiO2Scraping off the gel microspheres, collecting the SiO by a tank2The device can improve the production efficiency, but utilizes the scraper to lead the SiO to be collected2The process of dropping the gel microspheres from the conveyor belt can damage the SiO2The shape of the gel microsphere, and the device is only suitable for preparing SiO2The aerogel microspheres are not suitable for hydrogel microspheres such as calcium alginate, chitosan and the like. At present, the preparation of hydrogel microspheres is still mainly carried out manually, flow line type production is not formed, the production efficiency is low, and the automation degree is insufficient.
In view of the above problems in the prior art, there is a need in the art for an apparatus and method for automatically preparing hydrogel microspheres, which can improve the production efficiency.
Disclosure of Invention
In view of this, an object of the embodiments of the present invention is to provide an apparatus and a method for preparing hydrogel microspheres, which can solve the problems of low production efficiency and insufficient automation degree of hydrogel microspheres.
In view of the above objects, an aspect of the embodiments of the present invention provides an apparatus for preparing hydrogel microspheres, including:
the support comprises a first end and a second end, wherein the first end is provided with a driving roller and the second end is provided with a driven roller;
the conveying belt is arranged on the driving roller and the driven roller to connect the driving roller and the driven roller, and the outer side surface of the conveying belt is coated with super-hydrophobic paint;
the quick-freezing box is arranged between the first end and the second end and is positioned above the material bearing section of the conveying belt, a channel for the material bearing section of the conveying belt to pass through is formed in the lower part of the quick-freezing box, and a gap for allowing conveyed objects to pass through is reserved between the conveying belt and the upper surface of the channel;
a spray head disposed adjacent to the first end and above the conveyor belt toward the conveyor belt; and
a collection box disposed on a side where said second end is located, a portion of said conveyor belt at said second end being guided by said driven roller to project into said collection box.
In the above apparatus for preparing hydrogel microspheres, preferably, the driving roller is connected to a driving device.
The apparatus for preparing hydrogel microspheres as described above, preferably, the second end comprises a pair of tripods symmetrically disposed, one driven roller is installed between each corresponding vertex of three groups of corresponding vertices of the pair of tripods, a first driven roller of the driven rollers is located in the collection box and a second driven roller and a third driven roller are located above the collection box, and the second driven roller and the driving roller are horizontally disposed.
In the above apparatus for preparing hydrogel microspheres, preferably, the conveyor belt forms an obtuse angle at the inflection point after passing through the second driven roller.
The above apparatus for preparing hydrogel microspheres preferably has the obtuse angle of any angle between 110 ° and 150 °.
In the above apparatus for preparing hydrogel microspheres, preferably, the spray head is vertically or obliquely sprayed relative to the conveyor belt.
In view of the above objects, another aspect of the embodiments of the present invention provides a method for preparing hydrogel microspheres using the above apparatus, comprising the steps of:
atomizing the hydrogel microsphere precursor solution prepared in advance into atomized droplets through the spray head at high pressure, and spraying the atomized droplets onto the surface of the conveyor belt coated with the super-hydrophobic coating, wherein the atomized droplets form micro spherical droplets on the surface of the conveyor belt;
conveying the micro-spherical liquid drops through a channel of the quick-freezing box by using the conveyor belt so as to quickly freeze the micro-spherical liquid drops into micro ice balls; and
and conveying the micro ice balls into the collection box filled with a pre-prepared microsphere crosslinking agent by using the conveying belt, wherein the micro ice balls and the microsphere crosslinking agent are subjected to crosslinking reaction to form hydrogel microspheres.
Advantageous effects
The equipment and the method for preparing the hydrogel microspheres can atomize the microsphere precursor solution into micro droplets through the spray head, the micro droplets fall on the surface of a conveyor belt coated with the super-hydrophobic coating, the micro droplets conveyed by the conveyor belt are quickly frozen to form ice balls when passing through a quick-freezing box, and then the ice balls are conveyed into the microsphere crosslinking agent in the collecting box and react with the microsphere crosslinking agent to generate the hydrogel microspheres.
Drawings
FIG. 1 is a schematic perspective view of an apparatus for preparing hydrogel microspheres according to an embodiment of the present invention; and
FIG. 2 is a schematic view showing an operating state of an apparatus for preparing hydrogel microspheres according to an embodiment of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
In view of the above, the present invention provides an embodiment of an apparatus for preparing hydrogel microspheres. FIG. 1 is a schematic perspective view of the apparatus for producing hydrogel microspheres according to this embodiment. As shown in fig. 1, the apparatus for preparing hydrogel microspheres mainly includes a support 10, a plurality of rollers disposed at different positions on the support 10, a conveyor belt 5, a quick-freezing tank 4, a spray head 1, and a collection box 9.
The bracket 10 includes a first end and a second end, the first end is provided with a driving roller 11 and the second end is provided with driven rollers 14, 15, 16, and the driving roller 11 and the driven rollers 14, 15, 16 are connected with the bracket 10 through a rotating shaft. The conveyor belt 5 is disposed on the driving roller 11 and the driven rollers 14, 15, 16 to connect the driving roller 11 and the driven rollers 14, 15, 16, and an outer side surface (i.e., a surface in contact with an object to be conveyed) of the conveyor belt 5 is coated with a superhydrophobic coating which makes the surface of the conveyor belt 5 superhydrophobic. The quick-freeze box 4 is arranged between the first end and the second end and above the material carrying section of the conveyor belt 5, and it is emphasized that the material carrying section is a relative concept, and generally refers to the section of the conveyor belt 5 carrying the transported object during operation, and not specifically refers to a specific section of the conveyor belt 5. A channel 12 for the material carrying section of the conveyor belt 5 to pass through is formed in the lower portion of the quick-freezing box 4, and a gap for allowing conveyed objects to pass through is reserved between the conveyor belt 5 and the upper surface of the channel 12. The spray head 1 is arranged close to the first end and above the conveyor belt 5 towards the conveyor belt 5. A collecting box 9 is placed on the side where the second end is located, at which second end a part of the conveyor belt 5 is guided by the driven rollers into the collecting box 9.
In a preferred embodiment, the driving roller 11 is connected to a driving device, which may be any type of motor. The drive roller 11 and the motor may be connected by a belt or any other known means. The driving device drives the driving roller 11 to rotate, the driving roller 11 drives the conveyor belt 5 to rotate in the direction shown by the arrow in fig. 2, and the conveyor belt 5 drives the driven roller to rotate.
In a preferred embodiment, the second end comprises a pair of tripods 13 symmetrically arranged, one driven roller is mounted between each of three sets of corresponding vertexes of the pair of tripods 13, a first driven roller 14 of the driven rollers is positioned in the collecting box 9, a second driven roller 15 and a third driven roller 16 are positioned above the collecting box 9, and the second driven roller 15 is horizontally arranged with the driving roller 11. The rear inflection point of the conveyor belt 5 passing through the second driven roller 15 forms an obtuse angle, and the obtuse angle is preferably any angle between 110 degrees and 150 degrees. That is, the conveyor belt 5 is horizontally oriented from the first end to the second end, and after reaching the second end, it is guided by the first driven roller 14 and the second driven roller 15, and then slantingly descends at the second driven roller 15, and enters the collecting box 9. It is obvious to those skilled in the art that the number of the driven rollers is not limited by the embodiments described herein, and those skilled in the art can increase or decrease the number of the driven rollers according to actual situations as long as the technical problems described above can be solved.
In a preferred embodiment, the spray head 1 is vertically or obliquely sprayed relative to the conveyor belt 5, and a person skilled in the art can adjust the spray angle of the spray head 1 according to actual conditions.
In view of the above, the present invention also provides an embodiment of a method for preparing hydrogel microspheres. FIG. 2 shows the operation of preparing hydrogel microspheres using the apparatus of the present invention. As shown in figure 2, when the device provided by the invention is used for preparing hydrogel microspheres, a hydrogel microsphere precursor solution is atomized into atomized droplets 2 by a spray head 1 under high pressure and sprayed out to form micro droplets 3 which fall on the surface of a conveyor belt 5, the surface of the conveyor belt 5 is coated with a super-hydrophobic coating, the micro spherical droplets 3 are formed on the conveyor belt 5 coated with the super-hydrophobic coating by using the surface tension of the liquid, the conveyor belt 5 conveys the micro droplets 3 through a channel of a quick freezing box 4 and is rapidly frozen into micro ice balls 6, the conveyor belt 5 conveys the micro ice balls 6 into a collecting box 9, a microsphere crosslinking agent 8 is contained in the collecting box 9 and is subjected to crosslinking reaction with the micro ice balls 6 formed by the hydrogel microsphere precursor solution to form hydrogel microspheres 7, and the hydrogel microspheres 7 leave the conveyor belt 5 under the action of fluid resistance and fall into the microsphere crosslinking agent 8. The equipment provided by the invention can solve the problems that the existing artificial production method of hydrogel microspheres is low in efficiency and insufficient in automation degree, and the existing aerogel microsphere production equipment cannot prepare hydrogel microspheres.
The following illustrates the preparation process of calcium alginate hydrogel microspheres and chitosan hydrogel microspheres by using the apparatus of the present invention.
The process for preparing the calcium alginate hydrogel microspheres by taking sodium alginate as a precursor solution comprises the following steps: preparing a sodium alginate solution with the mass fraction of 2% and a calcium chloride solution with the mass fraction of 5%, spraying and atomizing the sodium alginate solution by a spray head to form tiny sodium alginate drops, dropping the tiny sodium alginate drops on a conveyor belt coated with a super-hydrophobic coating, quickly freezing the sodium alginate drops to ice balls through a quick-freezing box, conveying the ice balls into a collection box filled with the calcium chloride solution along with the conveyor belt, and performing ion crosslinking reaction on the sodium alginate ice balls and calcium ions to form the calcium alginate hydrogel microspheres.
The process for preparing the chitosan hydrogel microspheres by using chitosan as a precursor solution comprises the following steps: preparing 1% of chitosan solution and 5% of sodium hydroxide solution, using acetic acid to assist in dissolving chitosan, then spraying and atomizing the chitosan solution by a spray head to form tiny chitosan drops, dropping the tiny chitosan drops on a conveyor belt coated with super-hydrophobic coating, quickly freezing the chitosan drops into ice balls through a quick-freezing box, conveying the ice balls into a collecting box filled with the sodium hydroxide solution along with the conveyor belt, reacting the sodium hydroxide with the acetic acid of the chitosan assisting in dissolving, neutralizing the acid environment of the chitosan ice balls, and enabling the chitosan to generate self-crosslinking, thereby forming the chitosan hydrogel microspheres.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (7)

1. An apparatus for preparing hydrogel microspheres, comprising:
the support comprises a first end and a second end, wherein the first end is provided with a driving roller and the second end is provided with a driven roller;
the conveying belt is arranged on the driving roller and the driven roller to connect the driving roller and the driven roller, and the outer side surface of the conveying belt is coated with super-hydrophobic paint;
the quick-freezing box is arranged between the first end and the second end and is positioned above the material bearing section of the conveying belt, a channel for the material bearing section of the conveying belt to pass through is formed in the lower part of the quick-freezing box, and a gap for allowing conveyed objects to pass through is reserved between the conveying belt and the upper surface of the channel;
a spray head disposed adjacent to the first end and above the conveyor belt toward the conveyor belt; and
a collection box disposed on a side where said second end is located, a portion of said conveyor belt at said second end being guided by said driven roller to project into said collection box.
2. The apparatus for preparing hydrogel microspheres according to claim 1, wherein the driving roller is connected to a driving device.
3. The apparatus for preparing hydrogel microspheres according to claim 1, wherein the second end comprises a pair of tripods symmetrically arranged, one driven roller is installed between each of three sets of corresponding vertexes of the pair of tripods, a first driven roller of the driven rollers is located in the collection box and a second driven roller and a third driven roller are located above the collection box, and the second driven roller is horizontally arranged with the driving roller.
4. The apparatus for preparing hydrogel microspheres according to claim 3, wherein the conveyor belt forms an obtuse angle at the inflection point after passing through the second driven roller.
5. The apparatus for preparing hydrogel microspheres according to claim 4, wherein the obtuse angle is any angle between 110 ° and 150 °.
6. The apparatus for preparing hydrogel microspheres according to claim 1, wherein the spray head is vertically or obliquely spraying with respect to the conveyor belt.
7. A method for preparing hydrogel microspheres using the apparatus of any one of claims 1 to 6, comprising the steps of:
atomizing the hydrogel microsphere precursor solution prepared in advance into atomized droplets through the spray head at high pressure, and spraying the atomized droplets onto the surface of the conveyor belt coated with the super-hydrophobic coating, wherein the atomized droplets form micro spherical droplets on the surface of the conveyor belt;
conveying the micro-spherical liquid drops through a channel of the quick-freezing box by using the conveyor belt so as to quickly freeze the micro-spherical liquid drops into micro ice balls; and
and conveying the micro ice balls into the collection box filled with a pre-prepared microsphere crosslinking agent by using the conveying belt, wherein the micro ice balls and the microsphere crosslinking agent are subjected to crosslinking reaction to form hydrogel microspheres.
CN202010014079.9A 2020-01-07 2020-01-07 Equipment and method for preparing hydrogel microspheres Pending CN111097344A (en)

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CN202010014079.9A CN111097344A (en) 2020-01-07 2020-01-07 Equipment and method for preparing hydrogel microspheres

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CN202010014079.9A CN111097344A (en) 2020-01-07 2020-01-07 Equipment and method for preparing hydrogel microspheres

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3423489A (en) * 1966-11-01 1969-01-21 Minnesota Mining & Mfg Encapsulation process
CN203639164U (en) * 2013-12-06 2014-06-11 吴会军 Device for rapid preparation of SiO2 gel microsphere by use of super-hydrophobic surface
CN106964303A (en) * 2017-04-21 2017-07-21 北京健康广济生物技术有限公司 Hydrogel production technology and device
CN107848812A (en) * 2016-02-16 2018-03-27 株式会社Lg化学 For manufacturing the apparatus and method of airsetting film
US20180244029A1 (en) * 2016-02-19 2018-08-30 Lg Chem, Ltd. Apparatus and method for manufacturing composite sheet comprising aerogel sheet
CN209791507U (en) * 2019-01-31 2019-12-17 浙江圣兆药物科技股份有限公司 Rotary disc device for producing microdroplets of liquid material and apparatus for producing microspheres
CN211988544U (en) * 2020-01-07 2020-11-24 北京致成生物医学科技有限公司 Equipment for preparing hydrogel microspheres

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3423489A (en) * 1966-11-01 1969-01-21 Minnesota Mining & Mfg Encapsulation process
CN203639164U (en) * 2013-12-06 2014-06-11 吴会军 Device for rapid preparation of SiO2 gel microsphere by use of super-hydrophobic surface
CN107848812A (en) * 2016-02-16 2018-03-27 株式会社Lg化学 For manufacturing the apparatus and method of airsetting film
US20180244029A1 (en) * 2016-02-19 2018-08-30 Lg Chem, Ltd. Apparatus and method for manufacturing composite sheet comprising aerogel sheet
CN106964303A (en) * 2017-04-21 2017-07-21 北京健康广济生物技术有限公司 Hydrogel production technology and device
CN209791507U (en) * 2019-01-31 2019-12-17 浙江圣兆药物科技股份有限公司 Rotary disc device for producing microdroplets of liquid material and apparatus for producing microspheres
CN211988544U (en) * 2020-01-07 2020-11-24 北京致成生物医学科技有限公司 Equipment for preparing hydrogel microspheres

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