CN110327894A - A kind of blood purification polymer microsphere of high adsorption capacity and preparation method thereof - Google Patents
A kind of blood purification polymer microsphere of high adsorption capacity and preparation method thereof Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
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Abstract
The invention discloses blood purification polymer microspheres of a kind of high adsorption capacity and preparation method thereof, comprising the following steps: prepares dispersant solution: methyl blue aqueous solution being added in polyvinyl alcohol water solution；Prepare organic phase: by benzoyl peroxide and pore-foaming agent, divinylbenzene mixing；The dispersant solution of above-mentioned preparation and organic phase are stirred, polymerization reaction is carried out using gradient increased temperature, obtains polymer；Polymer is dispersed in water, system solid content 10% ~ 30% is made, modifying agent is added, insulation reaction obtains the blood purification polymer microsphere of high adsorption capacity.A kind of blood purification polymer microsphere of obtained high adsorption capacity is the smooth regular spherical in surface, it has been provided simultaneously with the biocompatibility layer of large specific surface area, big pore property, high absorption capacity, material surface, the security performance of material is greatly improved, it is higher for the adsorption rate of protein substance in blood.
Description
Technical field
The present invention relates to blood purification polymer microspheres of a kind of high adsorption capacity and preparation method thereof, belong to polymer microsphere
Preparation technical field.
Background technique
Carrying out purification to blood is conventional rescue means, is divided into haemodialysis and blood purification.Haemodialysis is mainly led to
Dialysis membrane is crossed to realize, small molecule venomous injurant can only be removed in dialysis procedure, is mainly used for the balance of electrolyte, such as
The small-molecule substances such as sodium, potassium.Blood purification mainly passes through adsorbent material, such as active carbon, macromolecule resin, mainly by blood
Small molecular or macromolecular, which adsorb, in liquid achievees the purpose that treatment.The blood purification material of early stage lays particular emphasis on hypnotic, agriculture
The small-molecule substances such as medicine.Currently with the increase of human longevity, after the organ agings such as kidney, liver, a large amount of rubbish is produced,
The venomous injurant in blood is increased, the protein substance of mainly some macromoleculars, representative is beta-2 microglobulin.
Excessively accumulation will lead to death to these wastes, therefore how effectively remove the direction that these protein-based wastes are current researches.
The patent of invention of notification number CN104587979B discloses a kind of efficient blood-purifying adsorbing agent and its preparation side
Method, adsorbent are made of carrier and aglucon, and carrier is chloromethylated polystyrene microballoon, and aglucon includes styrene derivative and second
The polystyrene dissaving polymer that alkenyl halide monomer copolyreaction generates, synthesizes to obtain using one-step method or two-step method.
In the dissaving polymer of the surface grafting relative specificity of polystyrene neutrality macroporous absorbent resin, in conjunction with macroporous absorbent resin
Wide absorption spectrum and dissaving polymer high specific, can be used for the absorption to morbid substances such as cell factors, it can also be used to
Absorption to other hydrophobic protein, small molecular can adjust reaction condition according to the target substance of design, generate not
The polymer of the same degree of branching, different branch lengths provides specifically absorption change ligand structure, can satisfy in blood perfusion
It is a kind of high-efficiency adsorbent novel, absorption spectrum is controllable to the isolation of purified of various hydrophobicity morbid substances.Although of the invention
By preparing hyperbranched compound adsorption capacity is increased, still, preparation process is complicated, and for adsorbance
It is required that higher situation, is still not achieved adsorption entails.
In order to expand adsorbance, existing technology is mainly by forming high specific surface micro-sphere material or large aperture material.Greatly
Pore size material is suitble to the protein absorption of macromolecular, is a kind of effective adsorbent material, but existing large aperture material biology is simultaneous
Capacitive difference will lead to blood clotting, so secondary embedding is needed to form biocompatibility layer.During secondary embedding, it will lead to
Original duct is also blocked or changes chemical property, adsorbance decline.Meanwhile secondary embedding reaction increases the system of material
Standby cost and uncontrollable type increase biological safety risk.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of existing technologies, the blood for providing a kind of high adsorption capacity is net
Change polymer microsphere and preparation method thereof, has obtained that large specific surface area, spatial capacity are big, adsorbance is high with biocompatibility layer
Micro-sphere absorption material.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, comprising the following steps:
(1) it prepares dispersant solution: methyl blue aqueous solution being added in polyvinyl alcohol water solution；
(2) it prepares organic phase: benzoyl peroxide, pore-foaming agent, styrene, divinylbenzene is mixed；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, polymerization reaction is carried out using gradient increased temperature, is gathered
Close object；
(4) polymer is dispersed in water, makes system solid content 10% ~ 30%, modifying agent is added, insulation reaction obtains high suction
The blood purification polymer microsphere of attached amount.
By using above-mentioned technical proposal, the high adsorption capacity that large specific surface area, spatial capacity are big, adsorbance is high is prepared
Blood purification polymer microsphere.
Preferably, the pore-foaming agent be include component A, B component；The component A is in liquid alcohol of the carbon atom number greater than 6
One kind, the B component is one of n-butyl ether, normal hexane, normal heptane or phthalic acid ester.
Preferably, the mass ratio of the component A and B component be 4:1.
Preferably, the gradient increased temperature is to rise to 60 DEG C by 0.5h, keeps the temperature 1h；Using 0.5h, 70 DEG C are risen to, is protected
Warm 2h；80 DEG C are risen to finally by 0.5h, keeps the temperature 6h.
By using above-mentioned technical proposal, gathered using the heating mode of mitigation so that polymerization reaction progress is more complete
It is right higher, it is more advantageous to the preparation of subsequent material.
Preferably, the modifying agent is one of hydroxy-ethyl acrylate or vinyl pyrrolidone.
Preferably, the insulation reaction temperature is 70 ~ 90 DEG C, and the insulation reaction time is 3 ~ 5h.
The present invention also provides a kind of blood purification polymer microspheres of high adsorption capacity, by a kind of above-mentioned high adsorption capacity
The preparation method of blood purification polymer microsphere obtains.
Preferably, the microspherulite diameter is 300 μm ~ 1.2 mm.
In conclusion the invention has the following advantages:
(1) a kind of blood purification polymer microsphere of high adsorption capacity of the invention is the smooth regular spherical in surface, is had simultaneously
For large specific surface area, the biocompatibility layer of big pore property, high absorption capacity, material surface, the safety of material is greatly improved
Performance is higher for the adsorption rate of protein substance in blood；
(2) preparation method of the blood purification polymer microsphere of a kind of high adsorption capacity of the invention, preparation process is simple, is not necessarily to two
Secondary embedding, reduces processing step, saves the preparation cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the blood purification polymer microsphere of high adsorption capacity of the invention；
Fig. 2 is the microscope figure of the blood purification polymer microsphere of high adsorption capacity of the invention.
Specific embodiment
The invention will be further described below.Following embodiment is only used for clearly illustrating technical side of the invention
Case, and not intended to limit the protection scope of the present invention.
A kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, comprising the following steps:
(1) it prepares dispersant solution: methyl blue aqueous solution being added in polyvinyl alcohol water solution；
(2) organic phase is prepared: by benzoyl peroxide and pore-foaming agent, divinylbenzene mixing；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, polymerization reaction is carried out using gradient increased temperature, is gathered
Close object；
(4) polymer is dispersed in water, makes system solid content 10% ~ 30%, modifying agent is added, insulation reaction obtains high suction
The blood purification polymer microsphere of attached amount.
The structural schematic diagram of the blood purification polymer microsphere of obtained high adsorption capacity is as shown in Figure 1.
The microscope figure of the blood purification polymer microsphere of obtained high adsorption capacity as shown in Fig. 2, it can be seen from the figure that
Obtained microballoon is the smooth regular spherical in surface.
Embodiment 1
A kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, comprising the following steps:
(1) it prepares dispersant solution: 50g polyvinyl alcohol being added in 1L water and stirs to get polyvinyl alcohol water solution, thereto
Addition mass percent concentration is 0.1% methylene blue aqueous solution 16ml；
(2) it prepares organic phase: being 60% diethyl by 0.4g benzoyl peroxide, isooctanol 32g, normal heptane 8g, 40g mass fraction
Alkenyl benzene, 35g styrene, are uniformly mixed；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, rise to 60 DEG C by 0.5h using gradient increased temperature,
Keep the temperature 1h；Using 0.5h, 70 DEG C are risen to, keeps the temperature 2h；80 DEG C are risen to finally by 0.5h, keeps the temperature 6h, carries out polymerization reaction, instead
After answering, product is filtered, and is washed 3 times, is obtained 100g polymer；
(4) it disperses 100g polymer in 900ml water, makes system solid content 10%, 5g hydroxy-ethyl acrylate is added, 70
Insulation reaction 3h at DEG C obtains the blood purification polymer microsphere of high adsorption capacity, and obtaining particle size range is 300 μm ~ 1.2 mm,
Specific surface area can reach 440 m2/ g or more, pore capacities reach 0.8 cm3/g。
After taking 1 ml micro-sphere material to adsorb two hours in blood plasma, beta-2 microglobulin and albumin residual quantity in blood plasma are surveyed,
Data are as shown in table 1.
Table 1
| Title | β protein residue concentration (mg/L) | Adsorption rate (%) | Albumin residual concentration (mg/L) | Loss late (%) |
| Prepare product | 0.39 | 82.8 | 46.2 | 7.4 |
| Commercial product | 0.45 | 80 | 45.9 | 7.6 |
| Blood plasma blank sample | 2.27 | / | 49.7 | / |
Embodiment 2
A kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, comprising the following steps:
(1) it prepares dispersant solution: 50g polyvinyl alcohol being added in 1L water and stirs to get polyvinyl alcohol water solution, thereto
Addition mass percent concentration is 0.1% methylene blue aqueous solution 16ml；
(2) it prepares organic phase: being 60% diethyl by 0.4g benzoyl peroxide, n-heptanol 32g, normal hexane 8g, 40g mass fraction
Alkenyl benzene, 40g styrene, are uniformly mixed；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, rise to 60 DEG C by 0.5h using gradient increased temperature,
Keep the temperature 1h；Using 0.5h, 70 DEG C are risen to, keeps the temperature 2h；80 DEG C are risen to finally by 0.5h, keeps the temperature 6h, carries out polymerization reaction, instead
After answering, product is filtered, and is washed 3 times, is obtained 110g polymer.
(4) it disperses 110g polymer in 500ml water, makes system solid content 18%, 5g hydroxy-ethyl acrylate is added,
The insulation reaction 4h at 80 DEG C obtains the blood purification polymer microsphere of high adsorption capacity, and obtaining particle size range is 300 μm ~ 1.2
Mm, specific surface area can reach 440 m2/ g or more, pore capacities reach 0.9 cm3/g。
After taking 1 ml micro-sphere material to adsorb two hours in blood plasma, beta-2 microglobulin and albumin residual quantity in blood plasma are surveyed,
Data are as shown in table 2.
Table 2
| Title | β protein residue concentration (mg/L) | Adsorption rate (%) | Albumin residual concentration (mg/L) | Loss late (%) |
| Prepare product | 0.36 | 84.1 | 46.8 | 7.2 |
| Commercial product | 0.45 | 80 | 45.9 | 7.6 |
| Blood plasma blank sample | 2.27 | / | 49.7 | / |
Embodiment 3
A kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, comprising the following steps:
(1) it prepares dispersant solution: 50g polyvinyl alcohol being added in 1L water and stirs to get polyvinyl alcohol water solution, thereto
Addition mass percent concentration is 0.1% methylene blue aqueous solution 16ml；
(2) it prepares organic phase: being 60% diethyl by 0.4g benzoyl peroxide, n-nonyl alcohol 32g, n-butyl ether 8g, 40g mass fraction
Alkenyl benzene, 55g styrene, are uniformly mixed；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, rise to 60 DEG C by 0.5h using gradient increased temperature,
Keep the temperature 1h；Using 0.5h, 70 DEG C are risen to, keeps the temperature 2h；80 DEG C are risen to finally by 0.5h, keeps the temperature 6h, carries out polymerization reaction, instead
After answering, product is filtered, and is washed 3 times, is obtained 115g polymer；
(4) it disperses 115g polymer in 270ml water, makes system solid content 30%, 5g hydroxy-ethyl acrylate is added, 90
Insulation reaction 3h at DEG C obtains the blood purification polymer microsphere of high adsorption capacity, and obtaining particle size range is 300 μm of -1.2 mm,
Specific surface area can reach 440 m2/ g or more, pore capacities reach 1.02 cm3/g。
After taking 1 ml micro-sphere material to adsorb two hours in blood plasma, beta-2 microglobulin and albumin residual quantity in blood plasma are surveyed,
Data are as shown in table 3.
Table 3
| Title | β protein residue concentration (mg/L) | Adsorption rate (%) | Albumin residual concentration (mg/L) | Loss late (%) |
| Prepare product | 0.34 | 85.0 | 47.4 | 7.0 |
| Commercial product | 0.45 | 80 | 45.9 | 7.6 |
| Blood plasma blank sample | 2.27 | / | 49.7 | / |
From 1 ~ table of table 3, it can be seen that the product being prepared increases compared to the absorbability for β albumen of commercial product
By force, and absorptivity improves, and loss late is reduced.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity, characterized in that the following steps are included:
(1) it prepares dispersant solution: methyl blue aqueous solution being added in polyvinyl alcohol water solution；
(2) it prepares organic phase: benzoyl peroxide, pore-foaming agent, styrene, divinylbenzene is mixed；
(3) dispersant solution of above-mentioned preparation and organic phase are stirred, polymerization reaction is carried out using gradient increased temperature, is gathered
Close object；
(4) polymer is dispersed in water, makes system solid content 10% ~ 30%, modifying agent is added, insulation reaction obtains high suction
The blood purification polymer microsphere of attached amount.
2. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity according to claim 1, characterized in that
The pore-foaming agent be include component A, B component；
The component A is one of the liquid alcohol that carbon atom number is greater than 6, and the B component is n-butyl ether, normal hexane, normal heptane
Or one of phthalic acid ester.
3. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity according to claim 2, characterized in that
The mass ratio of the component A and B component be 4:1.
4. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity according to claim 1, characterized in that
The gradient increased temperature is to rise to 60 DEG C by 0.5h, keeps the temperature 1h；Using 0.5h, 70 DEG C are risen to, keeps the temperature 2h；Finally by
0.5h rises to 80 DEG C, keeps the temperature 6h.
5. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity according to claim 1, characterized in that
The modifying agent is one of hydroxy-ethyl acrylate or vinyl pyrrolidone.
6. a kind of preparation method of the blood purification polymer microsphere of high adsorption capacity according to claim 1, characterized in that
The insulation reaction temperature is 70 ~ 90 DEG C, and the insulation reaction time is 3 ~ 5h.
7. the blood purification polymer microsphere of a kind of high adsorption capacity, by a kind of described in any item high adsorption capacities of claim 1 ~ 6
The preparation method of blood purification polymer microsphere obtain.
8. a kind of blood purification polymer microsphere of high adsorption capacity according to claim 7, characterized in that the framboid
Diameter is 300 μm ~ 1.2 mm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111659359A (en) * | 2020-06-24 | 2020-09-15 | 中国人民解放军中部战区总医院 | High-adsorption-capacity blood purification polymer microsphere |
| CN111686704A (en) * | 2020-07-02 | 2020-09-22 | 苏州仝康医疗科技有限公司 | Blood purification adsorbent and preparation method and application thereof |
| CN113372474A (en) * | 2021-06-29 | 2021-09-10 | 西安蓝晓科技新材料股份有限公司 | Blood perfusion resin and preparation method and application thereof |
| CN113967367A (en) * | 2020-07-25 | 2022-01-25 | 苏州仝乾医疗科技有限公司 | Cytokine antibody composition for treating new coronavirus and adsorbent for treatment |
| CN114950383A (en) * | 2022-04-08 | 2022-08-30 | 江苏贝美医疗科技有限公司 | Cytokine adsorbent for blood purification and preparation method thereof |
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| CN114950383A (en) * | 2022-04-08 | 2022-08-30 | 江苏贝美医疗科技有限公司 | Cytokine adsorbent for blood purification and preparation method thereof |
| CN114950383B (en) * | 2022-04-08 | 2024-02-06 | 淄博康贝医疗器械有限公司 | Cytokine adsorbent for blood purification and preparation method thereof |
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