CN113262762B - Adsorption material for blood perfusion and preparation method thereof - Google Patents
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Abstract
The invention discloses an adsorption material for blood perfusion and a preparation method thereof, which adopts a suspension polymerization mode to mix pure water, a dispersing agent and an aqueous phase polymerization inhibitor, and dissolve and prepare an aqueous phase; mixing a monomer, an initiator and a pore-forming agent, and stirring until the mixture is completely dissolved to prepare an oil phase; placing the prepared oil phase into the prepared water phase, standing, heating after the oil phase and the water phase are completely layered, regulating the stirring rotation speed to control the granularity, continuing to perform heating and heat preservation reaction, extracting resin after the reaction is finished, recovering a pore-forming agent, washing with water, and screening white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm; purifying the resin to remove the pore-forming agent and the organic solvent, thereby obtaining the adsorption material for blood perfusion. The invention has simple reaction process, energy conservation and environmental protection, and can obtain the high molecular adsorption material for blood perfusion, which has higher intensity, good adsorption performance on beta-microglobulin, low hemolysis rate and high safety.
Description
Technical Field
The invention belongs to the technical fields of chemical industry and medicine, and particularly relates to an adsorption material for blood perfusion and a preparation method thereof.
Background
Blood perfusion refers to the process of purifying blood by extracorporeal circulation through an adsorbent device with broad-spectrum detoxification effect or immobilized specific ligand, and removing endogenous or exogenous pathogenic substances in blood. Blood perfusion is currently limited mainly to adsorption and is therefore also called blood adsorption. The adsorbents commonly used in blood perfusion at present are mainly activated carbon, synthetic resin-based materials and the like, which are generally called blood perfusion adsorbent materials.
Blood perfusion can effectively remove creatinine, uric acid, medium molecular substances, phenols, guanidine, indole, organic acids and various medicines in blood, but can not remove urea, phosphate, water and electrolyte, so that the blood perfusion can be generally combined with HD (hemodialysis) in treating uremia, namely a combined artificial kidney treatment mode (HD+HP, namely hemodialysis+hemodiayer).
The blood perfusion adsorption material applied clinically still has the advantages of improving the mechanical strength of the resin and improving the blood compatibility of the resin. The blood compatibility means that the material does not cause coagulation, adhesion and aggregation of platelets, and hemolysis that damages the physical components of blood when in contact with blood. According to the characteristics of the adsorption material and the contact mode with extracorporeal blood perfusion, the research of the adsorption material is particularly important for the high-strength adsorption material which is not easy to fall off.
In view of the increasingly strict requirements of the current state on environmental protection, the pore-forming agent and a large amount of organic solvents used in the resin production process cause serious environmental pollution and increase the production cost.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art, and provides an adsorption material for blood perfusion and a preparation method thereof, which solve the problems of complex production process, high environmental protection cost, high strength requirement of the adsorption material for blood perfusion and good blood compatibility of the existing adsorption material.
The invention adopts the following technical scheme:
the preparation method of the adsorption material for blood perfusion comprises the following steps:
s1, mixing pure water, a dispersing agent and an aqueous phase polymerization inhibitor in a suspension polymerization mode, and dissolving to prepare an aqueous phase;
s2, mixing the monomer, the initiator and the pore-forming agent, and stirring until the mixture is completely dissolved to prepare an oil phase;
s3, putting the oil phase prepared in the step S2 into the water phase prepared in the step S1, standing, heating after the oil phase and the water phase are completely layered, adjusting the stirring rotation speed to control the granularity, continuously performing temperature rising and heat preservation reaction, extracting the resin after the reaction is finished, recovering the pore-foaming agent, washing with water, and screening the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm;
s4, purifying the resin obtained in the step S3, and removing the pore-forming agent and the organic solvent to obtain the adsorbing material for blood perfusion.
Specifically, in step S1, pure water: dispersing agent: the mass ratio of the aqueous phase polymerization inhibitor is 100: (0.5-1.5): (0.0005-0.0015).
Further, the dispersing agent is gelatin or sodium carboxymethyl cellulose, and the aqueous phase polymerization inhibitor is methylene blue.
Specifically, in step S2, monomers: and (3) an initiator: the mass ratio of the pore-forming agent is 100: (0.5-1.5): (100-250).
Further, the monomer includes divinylbenzene and one or more of styrene, methylstyrene, methyl acrylate, methyl methacrylate, acrylic acid, acrylonitrile, etc.
Further, the initiator comprises one or more of benzoyl peroxide, azobisisobutyronitrile and azobisisovaleronitrile.
Further, the pore-forming agent comprises any one or more of saturated alkane, toluene, xylene and tetramethylbenzene.
Specifically, in the step S3, the oil phase is put into the water phase for 5 minutes, and then the temperature rise and the heat preservation reaction are carried out twice, and the resin is extracted by using steam at 100-110 ℃.
Further, the two-time heating and heat preserving reaction specifically comprises: heating to 65-75 ℃ at a speed of 5 ℃/10min, preserving heat for 3-6 hours, heating to 80-95 ℃ and preserving heat for 10-15 hours.
The invention also provides an adsorption material for blood perfusion prepared according to the preparation method of the adsorption material for blood perfusion.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention relates to a preparation method of an adsorption material for blood perfusion, which comprises the steps of mixing pure water, a dispersing agent and a water phase polymerization inhibitor, stirring and dissolving the mixture to prepare a water phase, adding divinylbenzene or styrene monomer and a pore-foaming agent, dispersing the monomer into liquid beads with proper size by adopting a suspension polymerization mode under proper stirring, polymerizing the liquid beads into an adsorption material by adopting a series of different temperatures, removing the pore-foaming agent by adopting a steam extraction mode, and purifying the liquid beads to obtain the adsorption material for blood perfusion. The steam extraction reduces the use of a large amount of organic solvents, and the types and the dosage of pore-forming agents adjust the pore structure so as to be beneficial to optimizing each performance of the hemoperfusion adsorption material.
Further, pure water: dispersing agent: the mass ratio of the aqueous phase polymerization inhibitor is 100: (0.5-1.5): (0.0005-0.0015).
The adjustment of a certain proportion is beneficial to the conduction of polymerization heat, reduces the aggregation of spheres, can improve the sphere forming rate and obtain the adsorption material for blood perfusion with proper pore structure.
Further, the dispersant gelatin or carboxymethyl cellulose has the function of reducing the surface tension of water, so that the monomer is easier to disperse into small liquid beads and is adsorbed on the surfaces of the liquid beads, and the liquid beads are prevented from being combined and aggregated and adhered when touching each other. So as to ensure higher white ball yield. Methylene blue is an aqueous phase polymerization inhibitor, and the effect of adding methylene blue into a monomer is to prevent emulsion polymerization of the monomer in water, remove oxygen dissolved in the water through oxidation-reduction reaction, and shorten the induction period of polymerization. The amount of the polymer can influence the polymerization speed, the solution emulsification can be caused to a small extent, the white ball molding is influenced, and the bursting phenomenon can be caused to a large extent.
Further, monomer: and (3) an initiator: the mass ratio of the pore-forming agent is 100: (0.5-1.5): (100-250). The white ball crosslinking degree and the pore-forming agent dosage are adjusted to obtain a proper pore structure, and the adsorption material for blood perfusion with high strength and good adsorption performance is obtained.
Further, divinylbenzene is used as a crosslinking agent, and the diene monomer can be copolymerized with styrene, methyl acrylate, methyl methacrylate, acrylic acid and acrylonitrile to enable the polymer chains to be in a cross-linked network structure.
Furthermore, different initiators are selected according to different pore-forming agents, the decomposition rate of benzoyl peroxide is related to the solvent, the decomposition rates of other two azo initiators are not related to the solvent, and the reaction speed of suspension polymerization is controlled by adjusting the temperature and selecting the types and the dosage of the initiators, so that the white balls with high yield are obtained.
Further, the nature, amount and crosslinking degree of the porogen have a significant effect on the pore structure of the adsorption material for hemoperfusion. In view of environmental protection situation requirements, a pore-forming agent which is easy to recycle and has good performance on the hemoperfusion adsorption material should be selected.
Further, the oil phase solution is added into the water phase solution, and the mixture is kept stand for 5 minutes, so that the oil phase and the water phase are completely layered, and the granularity of the white balls can be adjusted. When the steam extraction is adopted, the proper temperature is selected between 100 ℃ and 110 ℃ according to the extraction effect, so that the porogen is ensured to be extracted cleanly, the steam extraction replaces the traditional organic solvent extraction, a large amount of organic solvents can be avoided, and the production process of the adsorption material for blood perfusion is more energy-saving and environment-friendly.
Furthermore, the purpose of the suspension polymerization is to control the reaction speed at first, so as to avoid the severe reaction process and further explosion polymerization, the high-temperature reaction improves the polymerization degree, the reaction is complete, and the white balls are further solidified.
In conclusion, the reaction process is simple, energy-saving and environment-friendly, and the high-molecular adsorption material for blood perfusion, which has the advantages of higher strength, good adsorption performance on beta-microglobulin, low hemolysis rate and high safety, can be obtained.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
The invention provides a preparation method of an adsorption material for blood perfusion, which is characterized by simple process, environmental protection and high-strength adsorption material for blood perfusion, and can realize the green and environmental protection production of macroporous adsorption resin, and simultaneously realize the characteristics of safe use, high mechanical strength, good blood compatibility and good adsorption performance on beta-microglobulin of the adsorption material for blood perfusion by a suspension polymerization method.
The invention relates to a preparation method of an adsorption material for blood perfusion, which comprises the following steps:
s1, adopting a suspension polymerization mode, specifically adding a certain amount of pure water into a reaction kettle, adding a dispersing agent and an aqueous phase polymerization inhibitor, and completely dissolving all components at 45 ℃ to prepare an aqueous phase;
pure water: dispersing agent: the mass ratio of the aqueous phase polymerization inhibitor is 100: (0.5-1.5): (0.0005-0.0015), wherein the dispersing agent is gelatin or sodium carboxymethyl cellulose, and the aqueous phase polymerization inhibitor is methylene blue.
S2, preparing a monomer, an initiator and a pore-forming agent according to the process requirement, and stirring until the monomer, the initiator and the pore-forming agent are completely dissolved to prepare an oil phase;
monomer (C): and (3) an initiator: the mass ratio of the pore-forming agent is 100: (0.5-1.5): (100-250).
The monomer comprises divinylbenzene and one or more of styrene, methyl acrylate, methyl methacrylate, acrylic acid, acrylonitrile and the like.
The initiator comprises one or more of benzoyl peroxide, azodiisobutyronitrile and azodiisovaleronitrile.
The pore-forming agent comprises any one or more of saturated alkane, toluene, xylene and tetramethylbenzene.
S3, putting the oil phase into the water phase, standing for 5 minutes, controlling the granularity by adjusting the stirring rotation speed when the oil phase and the water phase are completely layered, heating to 60-75 ℃ at the speed of 5 ℃/10 minutes, preserving heat for 3-6 hours, heating to 80-95 ℃ and preserving heat for 10-15 hours, extracting the resin by using steam at 100-110 ℃ after the reaction is finished, recovering the pore-foaming agent, washing with a large amount of water, and screening the resin with the thickness of 0.5-1.25 mm;
s4, purifying again to remove the residual pore-forming agent and the organic solvent in the adsorption material, so as to ensure the use safety of the adsorption material for blood perfusion.
The method can not only prepare the adsorption material with high strength and good blood compatibility, but also recycle the pore-forming agent in the process of preparing the adsorption material, the recycling rate of the pore-forming agent can reach more than 95%, and the recycled pore-forming agent can be used as a new pore-forming agent for preparing other types of macroporous adsorption resins.
The specific surface area of the adsorption material for blood perfusion is 800-900 m 2 Per gram, the pore volume is 1.0-1.4 ml/g, the average pore diameter is 4-6 nm, the detection intensity of an intensity meter is 7-8N, the ball rate after grinding is more than or equal to 95%, the adsorption of beta-microglobulin is more than or equal to 88%, the adsorption of albumin is less than or equal to 5%, and the hemolysis rate is less than or equal to 5%.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. The components of the embodiments of the invention generally illustrated herein can be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the invention, as provided, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing an oil phase in a beaker: 80g of divinylbenzene (content 80%), 5g of methyl acrylate, 15g of styrene, 100g of n-heptane and 0.5g of benzoyl peroxide.
500ml of water, 3g of gelatin, 0.5g of sodium carboxymethylcellulose and 5ml of 0.1% methylene blue solution are added into a 1 liter three-neck flask to completely dissolve each component at 45 ℃ to prepare an aqueous phase solution, an oil phase solution is added into the aqueous phase solution, standing is carried out for 5 minutes, stirring is started, the stirring speed is adjusted to control the granularity, the temperature is increased to 65 ℃ at 5 ℃/10 minutes, and the reaction is carried out for 3 hours at 85 ℃.
Filtering mother liquor after the reaction is finished, adding macroporous adsorption resin into an extraction column, introducing 100 ℃ steam to recover pore-forming agent n-heptane until the outlet condensate almost does not contain oily matters, stopping steam feeding, cooling, washing with a large amount of water, screening, and discharging to obtain the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm.
Example 2
Preparing an oil phase in a beaker: 80g of divinylbenzene (content 80%), 5g of methyl acrylate, 15g of methylstyrene, 150g of tetramethylbenzene and 1.0g of benzoyl peroxide.
500ml of water, 5g of gelatin and 10ml of 0.1% methylene blue solution are added into a 1 liter three-neck flask to completely dissolve each component at 45 ℃ to prepare aqueous phase solution, oil phase solution is added into aqueous phase solution, standing is carried out for 5 minutes, stirring is started, the stirring speed is adjusted to control the granularity, the temperature is increased to 65 ℃ at 5 ℃/10 minutes, the reaction is carried out for 6 hours at 80 ℃, and the reaction is carried out for 10 hours at 80 ℃, so that the tetramethylbenzene is recovered.
Filtering mother liquor after the reaction is finished, adding macroporous adsorption resin into an extraction column, introducing 105 ℃ steam to recover pore-forming agent tetramethylbenzene until the outlet condensate almost does not contain oily matters, stopping steam feeding, cooling, washing with a large amount of water, screening, and discharging to obtain the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm.
Example 3
Preparing an oil phase in a beaker: 80g of divinylbenzene (content 80%), 5g of methyl acrylate, 15g of styrene, 100g of n-heptane and 80g of tetramethylbenzene and 1.2g of benzoyl peroxide were stirred uniformly.
500ml of water, 4.5g of gelatin, 2g of sodium carboxymethylcellulose and 15ml of 0.1% methylene blue solution are added into a 1 liter three-neck flask to completely dissolve each component at 45 ℃ to prepare an aqueous phase solution, an oil phase solution is added into the aqueous phase solution, standing is carried out for 5 minutes, stirring is started, the stirring speed is adjusted to control the granularity, the temperature is increased to 65 ℃ at 5 ℃/10 minutes for reaction for 5 hours, and the reaction is carried out at 90 ℃ for 12 hours, so that n-heptane is recovered.
Filtering mother liquor after the reaction is finished, adding macroporous adsorption resin into an extraction column, introducing 105 ℃ steam to recover pore-forming agent tetramethylbenzene until the outlet condensate almost does not contain oily matters, stopping steam feeding, cooling, washing with a large amount of water, screening, and discharging to obtain the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm.
Example 4
Preparing an oil phase in a beaker: 80g of divinylbenzene (content 80%), 5g of methyl acrylate, 15g of styrene, 200g of toluene and 50g of isododecane and 1.0g of benzoyl peroxide.
500ml of water, 6.5g of gelatin and 20ml of 0.1% methylene blue solution are added into a 1 liter three-neck flask to completely dissolve each component at 45 ℃ to prepare an aqueous phase solution, an oil phase solution is added into an aqueous phase solution, the mixture is kept stand for 5 minutes, stirring is started, the stirring speed is adjusted to control the granularity, the mixture is heated to 75 ℃ at 5 ℃/10min for 6 hours, the reaction is carried out at 95 ℃ for 12 hours, and toluene is recovered.
Filtering mother liquor after the reaction is finished, adding macroporous adsorption resin into an extraction column, introducing 110 ℃ steam to recover residual pore-forming agent isododecane until the outlet condensate almost does not contain oily matters, stopping steam feeding, cooling, washing with a large amount of water, screening, and discharging to obtain the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm.
Example 5
Preparing an oil phase in a beaker: 90g of divinylbenzene (content 80%), 10g of methyl acrylate, 100g of toluene and 80g of isododecane and 1.5g of benzoyl peroxide were stirred uniformly.
500ml of water, 5g of gelatin, 2.5g of sodium carboxymethyl cellulose and 25ml of 0.1% methylene blue solution are added into a 1-liter three-neck flask to completely dissolve each component at 45 ℃ to prepare an aqueous phase solution, an oil phase solution is added into the aqueous phase solution, standing is carried out for 5 minutes, stirring is started, the stirring speed is adjusted to control the particle size, the temperature is increased to 60 ℃ at 5 ℃/10 minutes for 6 hours, the reaction is carried out at 95 ℃ for 12 hours, and toluene is recovered.
Filtering mother liquor after the reaction is finished, adding macroporous adsorption resin into an extraction column, introducing 110 ℃ steam to recover residual pore-forming agent isododecane until the outlet condensate almost does not contain oily matters, stopping steam feeding, cooling, washing with a large amount of water, screening, and discharging to obtain the white opaque spherical macroporous adsorption resin with the particle size of 0.5-1.25 mm.
Example Performance test data are presented in Table 1
TABLE 1
Examples application experimental test data are shown in Table 2
TABLE 2
As can be seen from tables 1 and 2, the specific surface area of the adsorbent for blood perfusion prepared in the examples of the present invention is 800m 2 And/g, the strength is higher, the KQ-3 particle strength meter is used for detecting that the strength reaches more than 7N, the ball grinding rate reaches more than 97 percent according to GB/12598-2001 detection, the adsorption rate on beta-microglobulin reaches more than 88 percent, the albumin adsorption rate is about 5 percent, and the hemolysis rate is lower.
In summary, the preparation method of the adsorption material for blood perfusion uses a one-time crosslinking method, and in the process of preparing macroporous adsorption resin, not only can single uniform pore-forming agents be recovered, but also mixed pore-forming agents can be respectively recovered, so that the process step of extracting the pore-forming agents by using organic solvents is omitted. Is a simple, efficient, green and environment-friendly process method with low energy consumption. Meanwhile, the high molecular adsorption material for blood perfusion, which has high strength, good adsorption performance on beta-microglobulin, low hemolysis rate and high safety, can be obtained.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (5)
1. The preparation method of the adsorption beta-microglobulin material for blood perfusion is characterized by comprising the following steps:
s1, mixing pure water, a dispersing agent and an aqueous phase polymerization inhibitor in a suspension polymerization mode, dissolving and preparing into an aqueous phase, and pure water: dispersing agent: the mass ratio of the aqueous phase polymerization inhibitor is 100: (0.5 to 1.5): (0.0005 to 0.0015);
s2, mixing the monomer, the initiator and the pore-forming agent, and stirring until the mixture is completely dissolved to prepare an oil phase, wherein the monomer: and (3) an initiator: the mass ratio of the pore-forming agent is 100: (0.5 to 1.5): (100-250), wherein the monomer comprises divinylbenzene, and one or more of styrene, methyl acrylate, methyl methacrylate, acrylic acid and acrylonitrile;
s3, putting the oil phase configured in the step S2 into the water phase configured in the step S1, standing for 5 minutes, heating the oil phase and the water phase after the oil phase and the water phase are completely layered, adjusting the stirring rotation speed to control the granularity, continuously performing heating and heat preservation reactions for two times, extracting resin by using steam at 100-110 ℃, wherein the heating and heat preservation reactions for two times are specifically as follows: heating to 65-75 ℃ at a speed of 5 ℃/10min, preserving heat for 3-6 hours, heating to 80-95 ℃, preserving heat for 10-15 hours, recovering the pore-forming agent, washing with water, and screening white opaque spherical macroporous adsorption resin with a particle size of 0.5-1.25 mm;
s4, purifying the resin obtained in the step S3, and removing the pore-forming agent and the organic solvent to obtain the adsorption beta-microglobulin material for blood perfusion.
2. The method for producing an adsorptive beta-microglobulin material for blood perfusion according to claim 1, wherein in the step S1, the dispersant is gelatin or sodium carboxymethyl cellulose and the aqueous phase polymerization inhibitor is methylene blue.
3. The method for preparing an adsorptive beta-microglobulin material for blood perfusion according to claim 1, wherein in the step S2, the initiator comprises one or more of benzoyl peroxide, azobisisobutyronitrile and azobisisovaleronitrile.
4. The method for preparing the beta-microglobulin adsorbing material for blood perfusion according to claim 1, wherein the pore-forming agent comprises any one or more of saturated alkane, toluene, xylene and tetramethylbenzene.
5. The beta-microglobulin adsorbing material for blood perfusion prepared by the method for preparing the beta-microglobulin adsorbing material for blood perfusion according to claim 1, wherein the specific surface area of the beta-microglobulin adsorbing material for blood perfusion is 800-900 m 2 And/g, wherein the pore volume is 1.0-1.4 ml/g, the average pore diameter is 4-6 nm, the detection intensity of an intensity meter is 7-8N, the ball rate after grinding is more than or equal to 95%, the adsorption of beta-microglobulin is more than or equal to 88%, the adsorption of albumin is less than or equal to 5%, and the hemolysis rate is less than or equal to 5%.
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