CN103142550B - Microcapsule prepared based on interfacial polycondensation method and preparation method thereof - Google Patents
Microcapsule prepared based on interfacial polycondensation method and preparation method thereof Download PDFInfo
- Publication number
- CN103142550B CN103142550B CN201310099464.8A CN201310099464A CN103142550B CN 103142550 B CN103142550 B CN 103142550B CN 201310099464 A CN201310099464 A CN 201310099464A CN 103142550 B CN103142550 B CN 103142550B
- Authority
- CN
- China
- Prior art keywords
- solution
- diamine
- microcapsule
- diisocyanate
- medicine
- 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.)
- Active
Links
Abstract
The invention discloses a microcapsule prepared based on an interfacial polycondensation method and a preparation method thereof, and relates to the field of microcapsules and the preparation method thereof. The preparation method disclosed by the invention is used for solving the problem that microcapsules of slightly soluble solid medicines cannot be prepared by current interfacial polycondensation method. The microcapsule prepared based on the interfacial polycondensation method is prepared through the interfacial polycondensation method. The preparation method comprises the following steps of: 1, preparing a sodium alginate aqueous liquid; 2, preparing a liquid I; 3, preparing a liquid III; 4, spraying the liquid I to the liquid II, and filtering to obtain sodium alginate microspherical filter cakes; and 5, preparing the capsule by nterfacial polycondensation. According to the microcapsule prepared based on an interfacial polycondensation method provided by the invention, slightly soluble solid medicines can be wrapped, and the preparation process is simple and low in cost. The capsule prepared is good in controlled release effect, and the sustainable release time reaches over 3 months. The microcapsule provided by the invention is suitable for the field of pesticide and medicine slow release.
Description
Technical field
The present invention relates to the field of microcapsule and preparation method thereof.
Background technology
Sodium alginate has the characteristic that forms gel with polyvalent cation generation gelling reaction, forms calcium alginate gel bead as reacted with calcium ion, and electron-microscope scanning is tridimensional network, is called visually ＂ egg box ＂ structure.Therefore be widely used in pharmacy, food and biological technical field, as the fixture of food additive, pharmaceutical carrier and living cells and enzyme.The report using about the slow releasing carrier of medication of calcium alginate gel bead is a lot, and its conventional preparation method has dropping preparation method, soaks stagnant method, anti-dropping preparation method, microencapsulation and complex coacervation.Interface polymerization reaction is two kinds of monomers that contain difunctional, is dissolved in respectively in two kinds of not miscible liquid, and polycondensation reaction is carried out on two-phase interface, forms the thin film of polycondensation product after a few minutes, until monomer exhausts completely.Participate in monomer poly-and reaction and have two classes: a class is oil-soluble monomer; Another kind of is water-soluble monomer.They lay respectively at the inside and outside of core drop and form polymer thin film on the surfaces of core drop.But existing interface polycondensation can only be prepared the microcapsule of parcel oil-soluble medicine and water soluble drug, and slightly solubility solid particle medicine is difficult to adopt interface polycondensation to make microcapsule.
CN102413683A discloses a kind of formulation of insecticides, and the method for the synthetic microcapsule with insecticidal property, said method comprising the steps of: organophosphorus compounds insecticide and at least one monomer are provided; Described organophosphorus ester insecticides is mixed with at least one monomer, form microcapsule; Wherein said monomer forms polymer, described polymer formation wall, and wherein said wall surrounds a part of described insecticide at least partly, thereby forms microcapsule.
Summary of the invention
The present invention will solve the problem that existing interface polycondensation can not be prepared the microcapsule of slightly solubility solid drugs, and a kind of microcapsule of preparing based on interface polycondensation and preparation method thereof is provided.
A microcapsule of preparing based on interface polycondensation, prepares by interface polycondensation; Wherein, described interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of coating medicine is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of the solution I described in calcium chloride water and step 2: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, i.e. the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1.
Described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.
Described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.
Described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.
Described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
A preparation method for the microcapsule of preparing based on interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of coating medicine is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of the solution I described in calcium chloride water and step 2: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1.
Described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.
Described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.
Described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.
Described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
Advantage of the present invention:
One, the preparation method of a kind of microcapsule of preparing based on interface polycondensation of the present invention, based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up slightly solubility solid drugs, overcome the deficiency that only can wrap up oil-soluble medicine and water soluble drug of traditional interface condensation methods;
Two, the microcapsule that the preparation method of a kind of microcapsule of preparing based on interface polycondensation of the present invention prepares, has good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reaches more than 3 months;
Three, in the preparation method of a kind of microcapsule of preparing based on interface polycondensation of the present invention, preparation technology is simple and convenient, response speed is fast, effective, do not need expensive equipment, can react at normal temperatures, simultaneously not need to add firming agent compared with traditional microcapsule preparation technology, reduce production cost.
Brief description of the drawings
Fig. 1 is that the amplification of test one microcapsule obtaining is the microscope figure of 160 times;
Fig. 2 is the drug release curve of test one microcapsule obtaining.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of microcapsule of preparing based on interface polycondensation, and it prepares by interface polycondensation; Wherein said interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of coating medicine is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of the solution I described in calcium chloride water and step 2: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, i.e. the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1.
In present embodiment step 3, in calcium chloride water, add medicine to be covered, the saturated solution that is made into medicine is that the medicine in microcapsule can not be penetrated in solution in order to make to be sprayed in step 4 while forming microcapsule in the solution II that step 3 obtains.
In present embodiment step 3, in calcium chloride water, adding diamine is that diamine can not penetrate into microcapsule from solution II, also can from microcapsule, not be exuded in solution II in order to make to be sprayed in step 4 while forming microcapsule in the solution II that step 3 obtains.
The object that adds diisocyanate compound in present embodiment step 5 is that microcapsule surface has formed polyurea film, makes it have better controlled-release effect.
The advantage of present embodiment: one, the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment, based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up slightly solubility solid drugs, overcome the deficiency that only can wrap up oil-soluble medicine and water soluble drug of traditional interface condensation methods; Two, the microcapsule that the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment prepares, has good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reaches more than 3 months; Three, in the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment, preparation technology is simple and convenient, response speed is fast, effective, do not need expensive equipment, can react at normal temperatures, simultaneously not need to add firming agent compared with traditional microcapsule preparation technology, reduce production cost.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.Other is identical with detailed description of the invention one.
When the medicine to be covered of present embodiment is water soluble drug or oiliness medicine, in the step 3 of detailed description of the invention one, the drug level of described solution II is identical with the drug level of solution I, does not need to reach capacity.
When medicine to be covered described in present embodiment is water soluble drug, medicine to be covered is to dissolve at the state of solution I and solution II; When described medicine to be covered is slightly solubility solid drugs, medicine to be covered is with the dispersed formation suspension of solid granule at the state of solution I and solution II; When described medicine to be covered is oiliness medicine, medicine to be covered is the dispersed formation suspension of form with little oil droplet at the state of solution I and solution II.
Detailed description of the invention three: the difference of present embodiment and detailed description of the invention one or two is: described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.Other is identical with detailed description of the invention one or two.
Each component in mixture described in present embodiment be arbitrarily than.
Detailed description of the invention four: the difference of one of present embodiment and detailed description of the invention one to three is: described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.Other is identical with detailed description of the invention one to three.
Each component in mixture described in present embodiment be arbitrarily than.
Detailed description of the invention five: the difference of one of present embodiment and detailed description of the invention one to four is: described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.Other is identical with detailed description of the invention one to four.
Solvent described in present embodiment can not dissolve or micro dissolution medicament purpose to be covered is to be dissolved in solvent in order to make to prevent that pulverulent solids that step 4 obtains from separating out, and makes microcapsule bag not live medicine; Meanwhile, solvent can dissolve diisocyanate compound again, makes polycondensation reaction can occur, and has formed polyurea film on microcapsule surface.
Detailed description of the invention six: present embodiment is a kind of preparation method of the microcapsule of preparing based on interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of coating medicine is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of the solution I described in calcium chloride water and step 2: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1.
In present embodiment step 3, in calcium chloride water, add medicine to be covered, the saturated solution that is made into medicine is that the medicine in microcapsule can not be penetrated in solution in order to make to be sprayed in step 4 while forming microcapsule in the solution II that step 3 obtains.
In present embodiment step 3, in calcium chloride water, adding diamine is that diamine can not penetrate into microcapsule from solution II, also can from microcapsule, not be exuded in solution II in order to make to be sprayed in step 4 while forming microcapsule in the solution II that step 3 obtains.
The object that adds diisocyanate compound in present embodiment step 5 is that microcapsule surface has formed polyurea film, makes it have better controlled-release effect.
The advantage of present embodiment: one, the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment, based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up slightly solubility solid drugs, overcome the deficiency that only can wrap up oil-soluble medicine and water soluble drug of traditional interface condensation methods; Two, the microcapsule that the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment prepares, has good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reaches more than 3 months; Three, in the preparation method of a kind of microcapsule of preparing based on interface polycondensation of present embodiment, preparation technology is simple and convenient, response speed is fast, effective, do not need expensive equipment, can react at normal temperatures, simultaneously not need to add firming agent compared with traditional microcapsule preparation technology, reduce production cost.
Detailed description of the invention seven: the difference of present embodiment and detailed description of the invention six is: described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.Other is identical with detailed description of the invention six.
When the medicine to be covered of present embodiment is water soluble drug or oiliness medicine, in the step 3 of detailed description of the invention six, the drug level of described solution II is identical with the drug level of solution I, does not need to reach capacity.
When medicine to be covered described in present embodiment is water soluble drug, medicine to be covered is to dissolve at the state of solution I and solution II; When described medicine to be covered is slightly solubility solid drugs, medicine to be covered is with the dispersed formation suspension of solid granule at the state of solution I and solution II; When described medicine to be covered is oiliness medicine, medicine to be covered is the dispersed formation suspension of form with little oil droplet at the state of solution I and solution II.
Detailed description of the invention eight: the difference of present embodiment and detailed description of the invention six to seven is: described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.Other is identical with detailed description of the invention six to seven.
Each component in mixture described in present embodiment be arbitrarily than.
Detailed description of the invention nine: the difference of one of present embodiment and detailed description of the invention six to eight is: described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.Other is identical with detailed description of the invention six to eight.
Each component in mixture described in present embodiment be arbitrarily than.
Detailed description of the invention ten: the difference of one of present embodiment and detailed description of the invention six to nine is: described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.Other is identical with detailed description of the invention six to nine.
Solvent described in present embodiment can not dissolve or micro dissolution medicament purpose to be covered is to be dissolved in solvent in order to make to prevent that pulverulent solids that step 4 obtains from separating out, and makes microcapsule bag not live medicine; Meanwhile, solvent can dissolve diisocyanate compound again, makes polycondensation reaction can occur, and has formed polyurea film on microcapsule surface.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of the microcapsule of preparing based on interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 2% sodium alginate aqueous solution 100mL;
Two, in the sodium alginate aqueous solution obtaining to step 1, add Imidacloprid 2g and ethylenediamine 5mL, be stirred to mix homogeneously, obtain solution I;
Three, in the calcium chloride water that is 10% at the mass percent concentration of 500mL, add Imidacloprid that it is reached capacity, then add 25mL ethylenediamine, be stirred to mix homogeneously, obtain solution II;
Four, solution I step 2 being obtained, is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL dimethylbenzene, with the stir speed (S.S.) dispersed with stirring of 400r/min, obtain suspension, then, in suspension, add 5g hexamethylene diisocyanate, after reaction 40min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation.
Imidacloprid in this test is slightly solubility solid drugs.
Fig. 1 is the microscope figure of test one microcapsule obtaining, and wherein, microscopical amplification is 160 times.From Fig. 1, can see clearly the chondritic of microcapsule, illustrate and adopt the preparation method of test one to prepare microcapsule.
Carry out drug release studies to testing a microcapsule obtaining, obtain Fig. 2.As can be seen from Figure 2 the sustained drug releasing effect of testing a microcapsule obtaining can reach more than 90 days; Illustrate that the microcapsule that test one adopts the coated slightly solubility solid drugs of interface polycondensation to prepare still has higher drug release effect.
Test two: a kind of preparation method of the microcapsule of preparing based on interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 2% sodium alginate aqueous solution 100mL;
Two, in the sodium alginate aqueous solution obtaining to step 1, add dimehypo 5g and 1,6-hexamethylene diamine 6mL, be stirred to mix homogeneously, obtain solution I;
Three, in the calcium chloride water that is 10% at the mass percent concentration of 500mL, add 25g dimehypo to make it consistent with the drug level in solution I, then add 1 of 30mL, 6-hexamethylene diamine, is stirred to mix homogeneously, obtains solution II;
Four, solution I step 2 being obtained, is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL dimethylbenzene, with the stir speed (S.S.) dispersed with stirring of 400r/min, obtain suspension, then, in suspension, add 6g hexamethylene diisocyanate, after reaction 40min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation;
Dimehypo in this test is water soluble drug.
Test three: a kind of preparation method of the microcapsule of preparing based on interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 2% sodium alginate aqueous solution 100mL;
Two, in the sodium alginate aqueous solution obtaining to step 1, add Acetochlor 5g and 1,3-propane diamine 6mL, be stirred to mix homogeneously, obtain solution I;
Three, in the calcium chloride water that is 10% at the mass percent concentration of 500mL, add 25g Acetochlor to make it consistent with the drug level in solution I, then add 1 of 30mL, 3-propane diamine, is stirred to mix homogeneously, obtains solution II;
Four, solution I step 2 being obtained, is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL kerosene, with the stir speed (S.S.) dispersed with stirring of 400r/min, obtain suspension, then, in suspension, add 6g hexamethylene diisocyanate, after reaction 40min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation;
Acetochlor in this test is oil-soluble medicine.
Claims (6)
1. a microcapsule of preparing based on interface polycondensation, is characterized in that the microcapsule of preparing based on interface polycondensation prepares by interface polycondensation, and wherein said interface polycondensation, specifically completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of medicine to be covered is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of the solution I described in calcium chloride water and step 2: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, i.e. the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1;
Described medicine to be covered is slightly solubility solid drugs; Described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
2. a kind of microcapsule of preparing based on interface polycondensation according to claim 1, is characterized in that described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.
3. a kind of microcapsule of preparing based on interface polycondensation according to claim 1, it is characterized in that described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.
4. the preparation method of a kind of microcapsule of preparing based on interface polycondensation as claimed in claim 1, is characterized in that a kind of preparation method of the microcapsule of preparing based on interface polycondensation completes according to the following steps:
One, take sodium alginate, soluble in water, be made into mass percent concentration and be 0.5%～5% sodium alginate aqueous solution;
Two, in the sodium alginate aqueous solution obtaining to step 1, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution I; Wherein, in solution I, the mass percent concentration of coating medicine is 0.05%～10%; In solution I, the mass percent concentration of diamine is 2%～30%;
Three, in calcium chloride water, add medicine to be covered and diamine, be stirred to mix homogeneously, obtain solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio (1～100) of calcium chloride water and solution I: 1, the saturated solution that described solution II is medicine to be covered; In solution II, in the mass percent concentration of diamine and solution I, the ratio of the mass percent concentration of diamine is (0.95～1.05): 1;
Four, solution I step 2 being obtained, by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, obtains calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, with the stir speed (S.S.) dispersed with stirring of 100r/min～500r/min, obtain dispersion liquid, then, in dispersion liquid, add diisocyanate compound, after reaction 20min～60min, filter to obtain solid, drying, obtains pulverulent solids, has completed the preparation of the microcapsule based on interface polycondensation; Wherein, describedly take the quality of calcium alginate microsphere filter cake that step 4 obtains and the ratio of the volume of solvent is 1g:(1mL～100mL); Described diisocyanate compound is (0.02～0.3) with the mass ratio that takes the calcium alginate microsphere filter cake that step 4 obtains: 1;
Described medicine to be covered is slightly solubility solid drugs; Described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
5. the preparation method of a kind of microcapsule of preparing based on interface polycondensation according to claim 4, it is characterized in that described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or wherein several mixture.
6. the preparation method of a kind of microcapsule of preparing based on interface polycondensation according to claim 4, it is characterized in that described diisocyanate compound is that toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, methylene two are to phenyl diisocyanate, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, 1, hexamethylene-diisocyanate, 1, a kind of in 5-naphthalene diisocyanate, isophorone diisocyanate and O-phthalic group diisocyanate or wherein several mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310099464.8A CN103142550B (en) | 2013-03-26 | 2013-03-26 | Microcapsule prepared based on interfacial polycondensation method and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310099464.8A CN103142550B (en) | 2013-03-26 | 2013-03-26 | Microcapsule prepared based on interfacial polycondensation method and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103142550A CN103142550A (en) | 2013-06-12 |
| CN103142550B true CN103142550B (en) | 2014-08-20 |
Family
ID=48541066
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310099464.8A Active CN103142550B (en) | 2013-03-26 | 2013-03-26 | Microcapsule prepared based on interfacial polycondensation method and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103142550B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102413683A (en) * | 2009-03-04 | 2012-04-11 | 陶氏益农公司 | Microencapsulated insecticide formulations |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2592851C2 (en) * | 2010-11-23 | 2016-07-27 | ДАУ АГРОСАЙЕНСИЗ ЭлЭлСи | Herbicide suspension of acetochlorine capsules containing reduced amount of antidote |
-
2013
- 2013-03-26 CN CN201310099464.8A patent/CN103142550B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102413683A (en) * | 2009-03-04 | 2012-04-11 | 陶氏益农公司 | Microencapsulated insecticide formulations |
Non-Patent Citations (2)
| Title |
|---|
| 刘书庆等.界面缩聚法维生素C微囊的研究.《山东轻工业学院学报》.2008,第22卷(第2期),第46－47、83页. |
| 界面缩聚法维生素C微囊的研究;刘书庆等;《山东轻工业学院学报》;20080630;第22卷(第2期);第46－47、83页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103142550A (en) | 2013-06-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101591820B1 (en) | Device and Method for Preparing Microparticles | |
| RU2491939C1 (en) | Method for preparing drug microcapsules of cephalosporin in konjac gum in chloroform | |
| CN101940554B (en) | Multi-core adhesive microspheres for loading water soluble low molecular medicament and preparation method thereof | |
| US20170333360A1 (en) | Spray dry method for encapsulation of biological moieties and chemicals in polymers cross-linked by multivalent ions for controlled release applications | |
| JP2003530996A (en) | Temperature-controlled microcapsules exhibiting zero-order release and methods for their preparation | |
| Huang et al. | Microencapsulation based on emulsification for producing pharmaceutical products: A literature review | |
| CN112048080B (en) | Microcapsule-filled sodium alginate-based hydrogel and preparation method thereof | |
| RU2590693C1 (en) | Method of producing nano capsules of adaptogens in pectin | |
| CN1899038A (en) | Method for producing pesticide micro capsule | |
| CN103142550B (en) | Microcapsule prepared based on interfacial polycondensation method and preparation method thereof | |
| JP2004168703A (en) | Microcapsule and method for producing the same | |
| Xue et al. | Physical, structural, and mechanical characterization of calcium–shellac microspheres as a carrier of carbamide peroxide | |
| RU2563618C2 (en) | Method of obtaining microcapsules of biopag-d in pectin | |
| EP3040373B1 (en) | Ionic gelation on solids | |
| EP1866072B1 (en) | Method for encapsulating a liquid | |
| JP2962740B2 (en) | Suspended microcapsule formulation | |
| RU2609824C1 (en) | Method for obtaining nanocapsules of medications of penicillin goup in sodium alginate | |
| RU2599007C1 (en) | Method of producing nanocapsules of ciprofloxacin hydrochloride in sodium alginate | |
| RU2595825C1 (en) | Method of producing potassium iodide nanocapsules in pectin | |
| RU2525158C2 (en) | Method of obtaining microcapsules of medications of cephalosporin group in konjac gum in toluene | |
| PL215011B1 (en) | Method for obtaining monodisperse pectin microgels using micro-flow system | |
| RU2688670C1 (en) | Method for producing nanocapsules of ciprofloxacin hydrochloride in konjac gum | |
| WO2022087680A1 (en) | Microcapsule | |
| CN100411726C (en) | Process for preparing polyhydroxy acid ester micro capsule | |
| RU2619328C2 (en) | Method of producing antibiotic nanocapsules in gellan gum |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180619 Address after: 161005 Feng Tun Village, Taha Township, Fuyu County, Qigihar, Heilongjiang Patentee after: QIQIHAR SHENGZE PESTICIDES CO., LTD. Address before: 150080 74 Xuefu Road, Nangang District, Harbin, Heilongjiang. Patentee before: Heilongjiang University |