CN109793916A - A kind of preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter - Google Patents
A kind of preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter Download PDFInfo
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- CN109793916A CN109793916A CN201910044629.9A CN201910044629A CN109793916A CN 109793916 A CN109793916 A CN 109793916A CN 201910044629 A CN201910044629 A CN 201910044629A CN 109793916 A CN109793916 A CN 109793916A
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Abstract
The present invention relates to a kind of preparation methods of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter, belong to medical macromolecular materials technical field.Its in microchannel tubing by water phase material under the action of oil phase material shearing force, cut into small liquid pearl, form the structure of Water-In-Oil, while initiator being dissolved in oil phase material, pass through crosslinking curing and aging and prepare uniform particle diameter Polyvinyl Alcohol Embolization microballoon.The present invention prepares uniform particle diameter Polyvinyl Alcohol Embolization microballoon by microchannel tubing, further simplifies production operation, reduces production cost, greatly reduce the generation of pollutant, so that production technology is more economically environmentally friendly.
Description
Technical field
The present invention relates to a kind of preparation methods of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter, belong to medical macromolecular materials
Technical field.
Background technique
Treatment of the Polyvinyl Alcohol Embolization microballoon for tumor disease has been very common clinical treatment means, and principle is
By the blood vessel of microballoon embolism patient part, the nutrition supply of tumour cell being cut off, tumour cell being made to wither because cannot get nutrition
Zero death, and then have the function that treatment.
The microspherulite diameter that the embolism of different region tumors blood vessels needs is different, requires to the size of partial size.At present
The microspheres product partial size of market supply in a certain range, such as 100-300 μm, 300-500 μm, 500-700um etc., in technique
The mixture of microspheres that a variety of partial sizes are first prepared using " one kettle way " is produced by the microballoon that sub-sieve process obtains certain particle size range
Product.
Polyvinyl Alcohol Embolization microballoon is widely used in the treatment of tumor disease, there is the very big market demand.It is currently marketed
Similar product particle diameter distribution it is wider, such as 100-300 μm, 300-500 μm can satisfy most bolt in therapeutic effect
Plug treatment needs, if it is possible to keep the partial size of product more uniform, then be capable of forming better embolotherapy effect；If can be from system
Standby technically innovation, invents a kind of method for preparing uniform particle diameter microballoon, then can be further simplified production operation, reduction is produced into
This, greatly reduces the generation of pollutant, so that production technology is more economically environmentally friendly.
The document and patent report for thering are some uniform particle diameter microballoons to prepare at present, such as patent CN104857576B,
CN102895927A, CN101342472A, use is all microchannel or similar preparation process, is being crossed by two-phase liquid
Place forms shearing, or is sprayed by tip, forms target grain size and uniform drop, and then form the microballoon of uniform particle diameter.
This method can prepare the microballoon of uniform particle diameter, can be with by adjusting the internal diameter of microchannel and the flowing velocity of two-phase liquid
Adjust the particle size of microballoon.It is also in the scientific research stage at present, there are industrial difficulties, such as microchannel is continuous
Production problem, the pressure coordination problem of oil phase and water phase.
Summary of the invention
The purpose of the present invention is overcoming above-mentioned shortcoming, a kind of system of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter is provided
The partial size of Preparation Method, product is more uniform, is capable of forming better embolotherapy effect.
Technical solution of the present invention, a kind of preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter, in micro-channel tubes
In road by water phase material under the action of oil phase material shearing force, small liquid pearl is cut into, the structure of Water-In-Oil is formed, by being crosslinked
Solidification and aging prepare uniform particle diameter Polyvinyl Alcohol Embolization microballoon.
Further, the water phase material is polyvinyl alcohol and its derivative, water, crosslinking agent and water phase material initiator；
Preferably, the polyvinyl alcohol derivative: water: crosslinking agent: water phase material initiator quality ratio is 100:30-400:10-
80:1-6。
Further, the oil phase material is butyl acetate and oil phase material initiator；
Preferably, it is 0.1%-5% that the oil phase material initiator, which accounts for the mass ratio of butyl acetate,.
Further, the microchannel tubing is cross, Y type and/or T-type microchannel tubing.
Further, the oily phase tubing internal diameter of cross, the Y type and/or T-type microchannel tubing is 60-2000 μm, water
Phase tubing internal diameter is 20-1000 μm.
Further, the aging temperature is 40-80 DEG C, ageing time 1-6h.
Further, the Oil phase flow rate is 100-50000 μ L/min, and aqueous phase flow rate is 0.1-100 μ L/min.
Further, the crosslinking agent in the water phase material is acrylates, is specifically included: sodium acrylate, metering system
Sour sodium, 2- acrylamide-2-methylpro panesulfonic acid sodium etc., initiator are peroxide initiator, including hydrogen peroxide, persulfuric acid
Sodium, potassium peroxydisulfate, ammonium persulfate etc..Further, the initiator in the oil phase material is tertiary amine compounds, including tetramethyl
Base ethylenediamine, triethylamine, triethanolamine, N, N- dimethylaniline, N, N- dimethyl-p-toluidine etc..
Further, the specific steps are as follows:
(1) preparation of water phase material: water phase material initiator is dissolved in the water, and crosslinking agent is added, stirs evenly, poly- second is added
Enol and its derivative, stir evenly, spare as water phase material；Control polyvinyl alcohol derivative: water: crosslinking agent: initiator
Mass ratio is 100:30-400:10-80:1-6；
(2) preparation of oil phase material: oil phase material initiator is added in butyl acetate, is stirred evenly, as oil phase material
It is spare；The mass concentration for controlling oil phase material initiator is 0.1%-5%.
(3) device is set up: the water phase material of preparation being sucked syringe pump, and by syringe pump discharge port and microchannel tubing
Water phase pipeline is connected；The feeding pipe of constant-flux pump is inserted into prepared oil phase material, by discharging pipeline and microchannel
The oily phase pipeline of pipeline is connected；The discharge port of microchannel tubing is connect with aging equipment；
(4) it prepares uniform particle diameter microballoon: opening constant-flux pump, oil phase material is pumped into pipeline, opens simultaneously syringe pump for water phase
Material is pumped into pipeline, and the flow velocity of oil phase material is 100-50000 μ L/min, the flow velocity of water phase material be 0.1-100 μ L/
Min, after microchannel tubing, water phase material cuts into small liquid pearl by oil phase material, mutually flows out with oily, into aging equipment,
The aging 1-6h at 40-80 DEG C；Microballoon is cooled into room temperature, uses butyl acetate, ethyl acetate, acetone washing respectively, it is dry, i.e.,
Obtain the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter.The particle size range of Polyvinyl Alcohol Embolization microballoon is to be less than etc. more than or equal to 30um
In 1400um.
The present invention uses microchannel tubing, by the unique texture of Water-In-Oil, by causing institute in liquid pearl in liquid bead surface
Cross-linked polymeric comprising polymerizable molecular ultimately forms crosslinking closely, the round microballoon of regular shape；It is representated by the present invention
The preparation process of a whole set of uniform particle diameter Polyvinyl Alcohol Embolization microballoon reaches rather than just a certain component such as microchannel tubing
Effect be also not only form liquid pearl, but will in channel cross-linked polymeric, form the microballoon of uniform particle diameter.
According to hydromechanical design principle, when two-phase liquid converges in the duct, the big liquid meeting of flow velocity big flow
The liquid small to the small flow of flow velocity forms shearing, forms Water-In-Oil or oil-in-water liquid, passes through the flow velocity of fixed two-phase liquid
Etc. factors, while the mode of fixed microchannel tubing internal diameter and shearing obtain the liquid pearl of uniform particle diameter, generated by crosslinking curing
Uniform particle diameter microballoon.
Beneficial effects of the present invention: the present invention prepares uniform particle diameter Polyvinyl Alcohol Embolization microballoon by microchannel tubing, into
One step simplifies production operation, reduces production cost, greatly reduces the generation of pollutant, so that production technology is more economical
Environmental protection.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1
For the cross micro-channel tubes road binders phase tubing internal diameter that the present embodiment uses for 60 μm, water phase tubing internal diameter is 20 μm.Such as Fig. 1
It is shown, the specific steps are as follows:
(1) it the preparation of water phase material: weighs 0.1 gram of sodium peroxydisulfate and 3 grams of water is added, 1 gram of Sodium methacrylate is added in stirring and dissolving
It is added, stirs evenly, 10 grams of polyvinyl alcohol derivatives are added, stir evenly, it is spare as water phase material.
(2) preparation of oil phase material: 1mL triethanolamine being added in 1000mL butyl acetate solution, is stirred evenly, and is made
It is spare for oil phase material.
(3) device is set up: the water phase material of preparation being sucked syringe pump, and by syringe pump discharge port and microchannel tubing
Water phase pipeline is connected；The feeding pipe of constant-flux pump is inserted into prepared oil phase material, by discharging pipeline and microchannel
The oily phase pipeline of pipeline is connected；The discharge port of microchannel tubing is connect with aging equipment.
(4) it prepares uniform particle diameter microballoon: opening constant-flux pump, oil phase material is pumped into pipeline, opening simultaneously syringe pump will
Water phase material is pumped into pipeline, and the flow velocity of oil phase material is 100 μ L/min, and the flow velocity of water phase material is 0.1 μ L/min, is passed through
After microchannel tubing, water phase material cuts into small liquid pearl by oil phase material, mutually flows out with oily, into aging equipment, at 40 DEG C
Aging 1 hour.Microballoon is cooled into room temperature, uses butyl acetate, ethyl acetate, acetone washing respectively, it is dry to get uniform particle diameter
Polyvinyl Alcohol Embolization microballoon.
By test, the microspherulite diameter range of preparation is 30 ± 15 μm, and preferred scheme is 30 ± 10 μm, more optimal solution
It is 30 ± 5 μm, meets the requirement of uniform particle diameter.
Embodiment 2
For the Y type micro-channel tubes road binders phase tubing internal diameter that the present embodiment uses for 2000 μm, water phase tubing internal diameter is 1000 μm.Such as figure
Shown in 1, the specific steps are as follows:
(1) it the preparation of water phase material: weighs 0.6 gram of potassium peroxydisulfate and 40 grams of water is added, stirring and dissolving is added 8 grams of sodium acrylate and adds
Enter, stir evenly, 10 grams of polyvinyl alcohol derivatives are added, stir evenly, it is spare as water phase material.
(2) preparation of oil phase material: by 50mL N, N- dimethylaniline is added in 1000mL butyl acetate solution, stirring
Uniformly, spare as oil phase material.
(3) device is set up: the water phase material of preparation being sucked syringe pump, and by syringe pump discharge port and microchannel tubing
Water phase pipeline is connected；The feeding pipe of constant-flux pump is inserted into prepared oil phase material, by discharging pipeline and microchannel
The oily phase pipeline of pipeline is connected；The discharge port of microchannel tubing is connect with aging equipment.
(4) it prepares uniform particle diameter microballoon: opening constant-flux pump, oil phase material is pumped into pipeline, opening simultaneously syringe pump will
Water phase material is pumped into pipeline, and the flow velocity of oil phase material is 50000 μ L/min, and the flow velocity of water phase material is 100 μ L/min, warp
After crossing microchannel tubing, water phase material cuts into small liquid pearl by oil phase material, mutually flows out with oily, into aging equipment, at 80 DEG C
Lower aging 6 hours.Microballoon is cooled into room temperature, uses butyl acetate, ethyl acetate, acetone washing respectively, drying is equal to get partial size
One polyethylene embolism microball.
By test, the microspherulite diameter of preparation is 1400 ± 100 μm, and preferred scheme is 1400 ± 75 μm, more preferably side
Case is 1400 ± 50 μm, meets the requirement of uniform particle diameter.
Embodiment 3
For the T-type micro-channel tubes road binders phase tubing internal diameter that the present embodiment uses for 350 μm, water phase tubing internal diameter is 160 μm.Such as Fig. 1
It is shown, the specific steps are as follows:
(1) it the preparation of water phase material: weighs 0.2 gram of ammonium persulfate and 10 grams of water is added, 2 grams of 2- acrylamides are added in stirring and dissolving
Base -2- methyl propane sulfonic acid sodium is added, and stirs evenly, 10 grams of polyvinyl alcohol derivatives are added, stir evenly, standby as water phase material
With.
(2) preparation of oil phase material: 5mL triethylamine being added in 1000mL butyl acetate solution, is stirred evenly, as
Oil phase material is spare.
(3) device is set up: the water phase material of preparation being sucked syringe pump, and by syringe pump discharge port and microchannel tubing
Water phase pipeline is connected；The feeding pipe of constant-flux pump is inserted into prepared oil phase material, by discharging pipeline and microchannel
The oily phase pipeline of pipeline is connected；The discharge port of microchannel tubing is connect with aging equipment.
(4) it prepares uniform particle diameter microballoon: opening constant-flux pump, oil phase material is pumped into pipeline, opening simultaneously syringe pump will
Water phase material is pumped into pipeline, and the flow velocity of oil phase material is 8500 μ L/min, and the flow velocity of water phase material is 15 μ L/min, is passed through
After microchannel tubing, water phase material cuts into small liquid pearl by oil phase material, mutually flows out with oily, into aging equipment, at 60 DEG C
Aging 3 hours.Microballoon is cooled into room temperature, uses butyl acetate, ethyl acetate, acetone washing respectively, it is dry to get uniform particle diameter
Polyethylene embolism microball.
By test, the microspherulite diameter of preparation is 250 ± 30 μm, and preferred scheme is 250 ± 20 μm, and more optimal solution is
250 ± 10 μm of requirements for meeting uniform particle diameter.
Claims (10)
1. the preparation method of the Polyvinyl Alcohol Embolization microballoon of a kind of uniform particle diameter, it is characterized in that: by water phase in microchannel tubing
Material cuts into small liquid pearl, forms the structure of Water-In-Oil, pass through crosslinking curing and aging under the action of oil phase material shearing force
Prepare uniform particle diameter Polyvinyl Alcohol Embolization microballoon.
2. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as described in claim 1, it is characterized in that: the aqueous-phase material
Material is polyvinyl alcohol and its derivative, water, crosslinking agent and water phase material initiator；
Preferably, the polyvinyl alcohol derivative: water: crosslinking agent: water phase material initiator quality ratio is 100:30-400:10-
80:1-6。
3. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as described in claim 1, it is characterized in that: the oil phase thing
Material is butyl acetate and oil phase material initiator；
Preferably, it is 0.1%-5% that the oil phase material initiator, which accounts for the mass ratio of butyl acetate,.
4. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as described in claim 1, it is characterized in that: the microchannel
Pipeline is cross, Y type and/or T-type microchannel tubing.
5. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as claimed in claim 4, it is characterized in that: described cross
The oily phase tubing internal diameter of microchannel tubing is 60-2000 μm, and water phase tubing internal diameter is 20-1000 μm.
6. the preparation method of the polyethylene embolism microball of uniform particle diameter as described in claim 1, it is characterized in that: the aging temperature
It is 40-80 DEG C, ageing time 1-6h.
7. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as claimed in claim 5, it is characterized in that: the oil mutually flows
Speed is 100-50000 μ L/min, and aqueous phase flow rate is 0.1-100 μ L/min.
8. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as claimed in claim 2, it is characterized in that: the aqueous-phase material
Crosslinking agent in material is acrylates, is specifically included: sodium acrylate, Sodium methacrylate, 2- acrylamido -2- methyl-prop sulphur
Sour sodium etc., initiator are peroxide initiator, including hydrogen peroxide, sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate etc..
9. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as claimed in claim 3, it is characterized in that: the oil phase thing
Initiator in material is tertiary amine compounds, including tetramethylethylenediamine, triethylamine, triethanolamine, N, N- dimethylaniline, N, N-
Dimethyl-p-toluidine etc..
10. the preparation method of the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter as described in claim 1, it is characterized in that specific steps are such as
Under:
(1) preparation of water phase material: water phase material initiator is dissolved in the water, and crosslinking agent is added, stirs evenly, poly- second is added
Enol and its derivative, stir evenly, spare as water phase material；Control polyvinyl alcohol derivative: water: crosslinking agent: initiator
Mass ratio is 100:30-400:10-80:1-6；
(2) preparation of oil phase material: oil phase material initiator is added in butyl acetate, is stirred evenly, as oil phase material
It is spare；The mass concentration for controlling oil phase material initiator is 0.1%-5%；
(3) device is set up: the water phase material of preparation being sucked syringe pump, and by the water phase of syringe pump discharge port and microchannel tubing
Pipeline is connected；The feeding pipe of constant-flux pump is inserted into prepared oil phase material, by discharging pipeline and microchannel tubing
Oily phase pipeline be connected；The discharge port of microchannel tubing is connect with aging equipment；
(4) it prepares uniform particle diameter microballoon: opening constant-flux pump, oil phase material is pumped into pipeline, opens simultaneously syringe pump for water phase
Material is pumped into pipeline, and the flow velocity of oil phase material is 100-50000 μ L/min, the flow velocity of water phase material be 0.1-100 μ L/
Min, after microchannel tubing, water phase material cuts into small liquid pearl by oil phase material, mutually flows out with oily, into aging equipment,
The aging 1-6h at 40-80 DEG C；Microballoon is cooled into room temperature, uses butyl acetate, ethyl acetate, acetone washing respectively, it is dry, i.e.,
Obtain the Polyvinyl Alcohol Embolization microballoon of uniform particle diameter.
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Cited By (3)
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| CN111298187A (en) * | 2020-02-20 | 2020-06-19 | 山东谷雨春生物科技有限公司 | Method and device for preparing degradable microspheres for embolism treatment |
| CN112569878A (en) * | 2020-01-21 | 2021-03-30 | 苏州恒瑞宏远医疗科技有限公司 | Equipment for preparing polyvinyl alcohol embolism microsphere with uniform grain diameter and production process thereof |
| CN115038517A (en) * | 2020-01-21 | 2022-09-09 | 苏州恒瑞宏远医疗科技有限公司 | Reaction device and processing method thereof, and preparation equipment and preparation method of embolism microsphere |
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