CN103142550A - 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
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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, and as forming calcium alginate gel bead with the calcium ion reaction, 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 that uses about the slow releasing carrier of medication of calcium alginate gel bead is a lot, and its preparation method commonly used 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, namely forms the thin film of polycondensation product after a few minutes, until monomer exhausts fully.Participate in monomer poly-and reaction two classes are arranged: 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 prepare 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.
Summary of the invention
The present invention will solve the problem that existing interface polycondensation can not prepare the microcapsule of slightly solubility solid drugs, and a kind of microcapsule based on interface polycondensation preparation and preparation method thereof is provided.
A kind of microcapsule based on the interface polycondensation preparation prepares by interface polycondensation; Wherein, described interface polycondensation, specifically complete 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of coating medicine is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the 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, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, namely based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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 several mixture wherein.
Described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.
Described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
A kind of preparation method of the microcapsule based on interface polycondensation preparation, specifically complete 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of coating medicine is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the 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, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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 several mixture wherein.
Described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.
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 based on interface polycondensation preparation of the present invention, be based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up the slightly solubility solid drugs, what overcome the traditional interface condensation methods only can wrap up the deficiency of oil-soluble medicine and water soluble drug;
Two, the microcapsule for preparing of the preparation method of a kind of microcapsule based on interface polycondensation preparation of the present invention, have good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reached more than 3 months;
Three, in the preparation method of a kind of microcapsule based on interface polycondensation preparation 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, comparing with traditional microcapsule preparation technology does not simultaneously need to add firming agent, has reduced production cost.
Description of drawings
Fig. 1 is the microscope figure of 160 times for the amplification of testing a microcapsule that obtains;
Fig. 2 is the drug release curve of test one microcapsule that obtains.
The specific embodiment
The specific embodiment one: present embodiment is a kind of microcapsule based on the interface polycondensation preparation, and it prepares by interface polycondensation; Wherein said interface polycondensation, specifically complete 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of coating medicine is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the 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, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, namely based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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.
Add medicine to be covered in the present embodiment step 3 in calcium chloride water, the saturated solution that is made into medicine is to be sprayed in step 4 when forming microcapsule in the solution II that step 3 obtains in order to make, and the medicine in microcapsule can not be penetrated in solution.
Adding diamine in the present embodiment step 3 in calcium chloride water is to be sprayed in step 4 when forming microcapsule in the solution II that step 3 obtains in order to make, and diamine can not penetrate into microcapsule from the solution II, can not be exuded to from microcapsule in the solution II yet.
The purpose that adds diisocyanate compound in the present embodiment step 5 is that the 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 based on interface polycondensation preparation of present embodiment, be based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up the slightly solubility solid drugs, what overcome the traditional interface condensation methods only can wrap up the deficiency of oil-soluble medicine and water soluble drug; Two, the microcapsule for preparing of the preparation method of a kind of microcapsule based on interface polycondensation preparation of present embodiment, have good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reached more than 3 months; Three, in the preparation method of a kind of microcapsule based on interface polycondensation preparation of present embodiment, preparation technology is simple and convenient, response speed is fast, effective, do not need expensive equipment, can react at normal temperatures, comparing with traditional microcapsule preparation technology does not simultaneously need to add firming agent, has reduced production cost.
The specific embodiment two: the difference of present embodiment and the specific embodiment one is: described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.Other is identical with the specific embodiment one.
When the medicine to be covered of present embodiment was water soluble drug or oiliness medicine, in the step 3 of the specific embodiment one, identical the getting final product of drug level of the drug level of described solution II and solution I do not need to reach capacity.
When the medicine to be covered described in present embodiment was water soluble drug, medicine to be covered was dissolving at the state of solution I and solution II; When described medicine to be covered was the slightly solubility solid drugs, medicine to be covered was to form suspension with the solid granule Uniform Dispersion at the state of solution I and solution II; When described medicine to be covered was the oiliness medicine, medicine to be covered was that form Uniform Dispersion with little oil droplet forms suspension at the state of solution I and solution II.
The specific embodiment three: present embodiment and the specific embodiment one or twos' difference is: described diamine is ethylenediamine, 1,3-propane diamine, 1, a kind of in 6-hexamethylene diamine, methylene diamine and toluenediamine or several mixture wherein.Other is identical with the specific embodiment one or two.
Each component in the described mixture of present embodiment be arbitrarily than.
The specific embodiment four: the difference of one of present embodiment and specific embodiment one to three is: described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.Other is identical with the specific embodiment one to three.
Each component in the described mixture of present embodiment be arbitrarily than.
The specific embodiment five: the difference of one of present embodiment and specific embodiment 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 the specific embodiment one to four.
Solvent described in present embodiment can not dissolve or micro dissolution medicament purpose to be covered is to prevent that pulverulent solids that step 4 obtains from separating out and be dissolved in solvent in order to make, and makes the microcapsule bag not live medicine; Simultaneously, solvent can dissolve diisocyanate compound again, makes polycondensation reaction can occur, and has formed polyurea film on the microcapsule surface.
The specific embodiment six: present embodiment is a kind of preparation method of the microcapsule based on interface polycondensation preparation, 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of coating medicine is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the 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, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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.
Add medicine to be covered in the present embodiment step 3 in calcium chloride water, the saturated solution that is made into medicine is to be sprayed in step 4 when forming microcapsule in the solution II that step 3 obtains in order to make, and the medicine in microcapsule can not be penetrated in solution.
Adding diamine in the present embodiment step 3 in calcium chloride water is to be sprayed in step 4 when forming microcapsule in the solution II that step 3 obtains in order to make, and diamine can not penetrate into microcapsule from the solution II, can not be exuded to from microcapsule in the solution II yet.
The purpose that adds diisocyanate compound in the present embodiment step 5 is that the 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 based on interface polycondensation preparation of present embodiment, be based on interface polycondensation, it not only can wrap up oil-soluble medicine and water soluble drug, can also wrap up the slightly solubility solid drugs, what overcome the traditional interface condensation methods only can wrap up the deficiency of oil-soluble medicine and water soluble drug; Two, the microcapsule for preparing of the preparation method of a kind of microcapsule based on interface polycondensation preparation of present embodiment, have good controlled-release effect, and cyst wall is thicker, discharges slowlyer, and the sustained release time reached more than 3 months; Three, in the preparation method of a kind of microcapsule based on interface polycondensation preparation of present embodiment, preparation technology is simple and convenient, response speed is fast, effective, do not need expensive equipment, can react at normal temperatures, comparing with traditional microcapsule preparation technology does not simultaneously need to add firming agent, has reduced production cost.
The specific embodiment seven: the difference of present embodiment and the specific embodiment six is: described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.Other is identical with the specific embodiment six.
When the medicine to be covered of present embodiment was water soluble drug or oiliness medicine, in the step 3 of the specific embodiment six, identical the getting final product of drug level of the drug level of described solution II and solution I do not need to reach capacity.
When the medicine to be covered described in present embodiment was water soluble drug, medicine to be covered was dissolving at the state of solution I and solution II; When described medicine to be covered was the slightly solubility solid drugs, medicine to be covered was to form suspension with the solid granule Uniform Dispersion at the state of solution I and solution II; When described medicine to be covered was the oiliness medicine, medicine to be covered was that form Uniform Dispersion with little oil droplet forms suspension at the state of solution I and solution II.
The specific embodiment eight: the difference of present embodiment and the specific embodiment 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 several mixture wherein.Other is identical with the specific embodiment six to seven.
Each component in the described mixture of present embodiment be arbitrarily than.
The specific embodiment nine: the difference of one of present embodiment and specific embodiment six to eight is: described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.Other is identical with the specific embodiment six to eight.
Each component in the described mixture of present embodiment be arbitrarily than.
The specific embodiment ten: the difference of one of present embodiment and specific embodiment 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 the specific embodiment six to nine.
Solvent described in present embodiment can not dissolve or micro dissolution medicament purpose to be covered is to prevent that pulverulent solids that step 4 obtains from separating out and be dissolved in solvent in order to make, and makes the microcapsule bag not live medicine; Simultaneously, solvent can dissolve diisocyanate compound again, makes polycondensation reaction can occur, and has formed polyurea film on the microcapsule surface.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of the microcapsule based on interface polycondensation preparation, specifically complete 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, add Imidacloprid 2g and ethylenediamine 5mL in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I;
Three, add Imidacloprid that it is reached capacity in the mass percent concentration of 500mL is 10% calcium chloride water, then add the 25mL ethylenediamine, be stirred to mix homogeneously, obtain the solution II;
Four, the solution I that step 2 is obtained is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL dimethylbenzene, stir speed (S.S.) dispersed with stirring with 400r/min, obtain suspension, then, add the 5g hexamethylene diisocyanate in suspension, after reaction 40min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation.
Imidacloprid in this test is the slightly solubility solid drugs.
Fig. 1 is the microscope figure of test one microcapsule that obtains, and wherein, microscopical amplification is 160 times.Can see clearly the chondritic of microcapsule from Fig. 1, illustrate and adopt the preparation method of test one to prepare microcapsule.
Carry out drug release studies to testing a microcapsule that obtains, get Fig. 2.The sustained drug releasing effect of as can be seen from Figure 2 testing a microcapsule that obtains can reach more than 90 days; Illustrate that the microcapsule that test one adopts interface polycondensation to coat the preparation of slightly solubility solid drugs still has higher drug release effect.
Test two: a kind of preparation method of the microcapsule based on interface polycondensation preparation, specifically complete 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, add dimehypo 5g and 1,6-hexamethylene diamine 6mL in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I;
Three, add the 25g dimehypo to make it consistent with the drug level in the solution I in the mass percent concentration of 500mL is 10% calcium chloride water, then add 1 of 30mL, the 6-hexamethylene diamine is stirred to mix homogeneously, obtains the solution II;
Four, the solution I that step 2 is obtained is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL dimethylbenzene, stir speed (S.S.) dispersed with stirring with 400r/min, obtain suspension, then, add the 6g hexamethylene diisocyanate in suspension, after reaction 40min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation;
Dimehypo in this test is water soluble drug.
Test three: a kind of preparation method of the microcapsule based on interface polycondensation preparation, specifically complete 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, add Acetochlor 5g and 1,3-propane diamine 6mL in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I;
Three, add the 25g Acetochlor to make it consistent with the drug level in the solution I in the mass percent concentration of 500mL is 10% calcium chloride water, then add 1 of 30mL, the 3-propane diamine is stirred to mix homogeneously, obtains the solution II;
Four, the solution I that step 2 is obtained is sprayed in the solution II that step 3 obtains by sprayer unit, after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in 500mL kerosene, stir speed (S.S.) dispersed with stirring with 400r/min, obtain suspension, then, add the 6g hexamethylene diisocyanate in suspension, after reaction 40min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation;
Acetochlor in this test is oil-soluble medicine.
Claims (10)
1. the microcapsule based on the interface polycondensation preparation, is characterized in that preparing by interface polycondensation based on the microcapsule of interface polycondensation preparation, and wherein said interface polycondensation is specifically completed 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of medicine to be covered is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the 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, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, namely based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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.
2. a kind of microcapsule based on the interface polycondensation preparation according to claim 1, is characterized in that described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.
3. a kind of microcapsule based on interface polycondensation preparation according to claim 1 and 2, 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 several mixture wherein.
4. a kind of microcapsule based on interface polycondensation preparation according to claim 1 and 2, it is characterized in that described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.
5. a kind of microcapsule based on the interface polycondensation preparation according to claim 1 and 2, is characterized in that described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
6. the preparation method of a kind of microcapsule based on interface polycondensation preparation as claimed in claim 1 is characterized in that a kind of preparation method of the microcapsule based on the interface polycondensation preparation is completed 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, add medicine to be covered and diamine in the sodium alginate aqueous solution that obtains to step 1, be stirred to mix homogeneously, obtain the solution I; Wherein, in the solution I, the mass percent concentration of coating medicine is 0.05%～10%; In the solution I, the mass percent concentration of diamine is 2%～30%;
Three, add medicine to be covered and diamine in calcium chloride water, be stirred to mix homogeneously, obtain the solution II; Wherein, the mass percent concentration of described calcium chloride water is 1%～40%; The volume ratio of calcium chloride water and solution I (1～100): 1, described solution II is the saturated solution of medicine to be covered; In the solution II in the mass percent concentration of diamine and solution I the ratio of the mass percent concentration of diamine be (0.95～1.05): 1;
Four, the solution I that step 2 is obtained by sprayer unit, is sprayed in the solution II that step 3 obtains, and after sucking filtration, gets the calcium alginate microsphere filter cake;
Five, taking the calcium alginate microsphere filter cake that step 4 obtains joins in solvent, stir speed (S.S.) dispersed with stirring with 100r/min～500r/min, obtain dispersion liquid, then, add diisocyanate compound in dispersion liquid, after reaction 20min～60min, filter to get solid, drying obtains pulverulent solids, has namely completed the preparation based on the microcapsule of interface polycondensation; Wherein, the ratio of the described quality that takes the calcium alginate microsphere filter cake that step 4 obtains and 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.
7. a kind of microcapsule based on the interface polycondensation preparation according to claim 6, is characterized in that described medicine to be covered is water soluble drug, slightly solubility solid drugs or oiliness medicine.
8. according to claim 6 or 7 described a kind of microcapsules based on interface polycondensation preparation, 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 several mixture wherein.
9. according to claim 6 or 7 described a kind of microcapsules based on interface polycondensation preparation, it is characterized in that described diisocyanate compound is toluene di-isocyanate(TDI), hexamethylene diisocyanate, XDI, dimethyl diphenyl vulcabond, two pairs of phenyl diisocyanate of methylene, 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 several mixture wherein.
10. according to claim 6 or 7 described a kind of microcapsules based on the interface polycondensation preparation, is characterized in that described solvent is for can dissolve diisocyanate compound and can not dissolve or micro dissolution medicine to be covered.
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Citations (2)
| 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 |
| WO2012071248A1 (en) * | 2010-11-23 | 2012-05-31 | Dow Agrosciences Llc | Herbicidal capsule suspensions of acetochlor containing reduced amounts of safener |
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Patent Citations (2)
| 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 |
| WO2012071248A1 (en) * | 2010-11-23 | 2012-05-31 | Dow Agrosciences Llc | Herbicidal capsule suspensions of acetochlor containing reduced amounts of safener |
Non-Patent Citations (1)
| Title |
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| 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》 * |
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