CN112358654B - Preparation method of konjac gel carrier - Google Patents
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention provides a preparation method of a konjac gel carrier, wherein the rapid gel carrier comprises the following raw materials in parts by weight: 83-91 parts of hydroxypropyl methyl cellulose, 9-17 parts of konjac flour and 1-5 parts of iodine solution. The viscosity range of the hydroxypropyl methyl cellulose is 1000-2000mPa.s, the viscosity range of the konjac powder is 300-900mPa.s, the particle size of the konjac powder is less than 3 mu m, and the molar concentration of I in the iodine solution is 0.05-1 mol/L. The iodine solution comprises any one of lecithin complex iodine, polyvinylpyrrolidone iodine, alkyl glycoside complex iodine, iodine modified titanium dioxide and MOF-I. By adopting the technical scheme of the invention, the formed gel carrier can be obtained after 1-3 seconds, and is convenient for the operation of factory workshops.
Description
Technical Field
The invention relates to a konjak gel carrier and a preparation method thereof, belonging to the technical field of biological materials.
Background
Hydroxypropyl methylcellulose is a white to off-white fibrous powder or granule that is soluble in water and certain organic solvent systems and insoluble in ethanol. The gel is dispersed in cold water, the aqueous solution has surface activity, a film is formed after drying, and the gel solution has unique reversible thermal gel property. The hydroxypropyl methyl cellulose can be used as a thickening agent, a dispersing agent, an adhesive, an excipient, an oil-resistant coating, a filler, an emulsifier and a stabilizer, and is widely applied to the industries of synthetic resin, textile industry, petrochemical industry, ceramics, papermaking, leather, medicine, food, cosmetics and the like.
The invention patent with the Chinese patent number of CN200510016449.8 discloses a preparation method of a calcium carbonate/hydroxypropyl methyl cellulose compound thermal gel template, which utilizes the reversible thermal gel property of hydroxypropyl methyl cellulose to solve the defects of high price and rejection reaction of preparing an organic template by utilizing natural biological macromolecules.
The invention patent with Chinese patent number CN201710923947.3 discloses an iodine-containing tincture antibacterial gel and a preparation method thereof, the iodine tincture and chitosan/chitin derivative are complexed in the antibacterial gel, hydroxypropyl methylcellulose is added as a thickening agent, the antibacterial gel obtained by operations of low-speed stirring for 2-6 hours at a certain temperature, high-speed stirring for 30-60 minutes and the like can effectively reduce the irritation, the skin is not dyed, the antibacterial time is longer, but the antibacterial gel has the defect of long time consumption of the production process.
Disclosure of Invention
The invention provides a preparation method of a konjac gel carrier, which can solve the problems of low gelling speed and long time consumption by gelling hydroxypropyl methylcellulose and iodine at normal temperature. The specific scheme is as follows:
the rapid gelling carrier comprises the following raw materials in parts by weight: 83-91 parts of hydroxypropyl methyl cellulose, 9-17 parts of konjac flour and 1-5 parts of iodine solution.
The preferable scheme is 88 parts of hydroxypropyl methyl cellulose, 12 parts of konjac flour and 3 parts of iodine solution.
The viscosity range of the hydroxypropyl methyl cellulose is 1000-2000mPa.s, the viscosity range of the konjac powder is 300-900mPa.s, the particle size of the konjac powder is less than 3 mu m, the molar concentration of I in the iodine solution is 0.05-1mol/L, and in the preferred scheme, the molar concentration of I in the iodine solution is 0.5 mol/L.
The iodine solution comprises any one of lecithin complex iodine, polyvinylpyrrolidone iodine, alkyl glycoside complex iodine, iodine modified titanium dioxide and MOF-I.
The lecithin complexed iodine is a composite material of soybean lecithin and iodine elementary substance or potassium iodate at the temperature of 90-120 ℃. Adding soybean lecithin into a mixing reactor, adding water, introducing nitrogen, stirring uniformly at 90-120 ℃, adding an iodine simple substance or potassium iodate, and reacting for 2-3h to obtain the lecithin complexed iodine. Wherein the mass ratio of soybean lecithin, water, iodine simple substance or potassium iodate is 0.2-1: 20-28: 0.1-5.
In the soybean lecithin and iodine complex material, the soybean lecithin is a high-permeability solvent, and can quickly permeate into a cellulose material when being mixed with a high-molecular material, namely hydroxypropyl methyl cellulose and konjac flour containing glucomannan, so that a carried complex iodine material quickly reacts with the hydroxypropyl methyl cellulose and the konjac flour containing the glucomannan to promote quick gelation.
The polyvinylpyrrolidone iodine is a composite material of polyvinylpyrrolidone and iodine simple substance or potassium iodate at the temperature of 90-120 ℃. The specific technical scheme is that polyvinylpyrrolidone is added into a mixing reactor, nitrogen is introduced after water is added, the mixture is uniformly stirred at 90-120 ℃, an iodine simple substance or potassium iodate is added, and the polyvinylpyrrolidone complex iodine can be prepared after reaction for 2-3 hours. Wherein the mass ratio of polyvinylpyrrolidone, water, iodine simple substance or potassium iodate is 0.2-1: 20-28: 0.1-5.
Polyvinylpyrrolidone is a nonionic surfactant, and forms a nonionic surfactant containing iodine materials after complexing with iodine simple substance or iodide ions. The hydrophilicity of the material can quickly emulsify the hydroxypropyl methylcellulose as a high molecular material and the konjac containing glucomannan, and the surface activation energy of the material is improved, so that the konjac can be quickly gelled.
The alkyl glycoside complex iodine is a composite material of alkyl glycoside and iodine simple substance or potassium iodate at the temperature of 90-120 ℃. Adding alkyl glycoside into a mixing reactor, adding water, introducing nitrogen, stirring uniformly at 90-120 ℃, adding iodine simple substance or potassium iodate, and reacting for 2-3h to obtain alkyl glycoside complex iodine. Wherein the mass ratio of alkyl glycoside, water, iodine simple substance or potassium iodate is 0.2-1: 20-28: 0.1-5.
The alkyl glycoside has strong wettability and good water solubility, and can be compounded with the I simple substance or iodide ions to enhance the effect of the I simple substance and iodide ions. Meanwhile, in the process of catalyzing and promoting the gel by I, the thickening effect is good.
The iodine modified titanium dioxide is a composite material prepared by carrying out hydrothermal reaction on tetrabutyl titanate and an iodine simple substance at the temperature of 180-220 ℃.
The specific technical scheme is that anhydrous ethanol, isopropyl titanate or tetrabutyl titanate are mixed and stirred uniformly at room temperature, a mixed solution of a simple substance iodine and water is dripped, and the mixture is stirred uniformly and then reacts for 8 to 12 hours at the temperature of 220 ℃ in a hydrothermal reaction kettle at 180 ℃ to prepare the iodine modified titanium dioxide. Wherein the mass ratio of isopropyl titanate or tetrabutyl titanate, iodine simple substance and water is as follows: 0.2-1: 0.1-5: 20-28. The ethanol is a mixed solvent of isopropyl titanate or tetrabutyl titanate, and is completely dissolved.
The iodine modified titanium dioxide material has high catalytic activity, and after the titanium dioxide is compounded with I, the energy provided by the titanium dioxide can promote the catalytic activity of I. Meanwhile, the particle size of the iodine modified titanium dioxide is a nano-grade material, the preparation method can reach within 50nm, and the iodine modified titanium dioxide can quickly permeate into the high polymer material hydroxypropyl methyl cellulose and the konjac material containing glucomannan after atomization spraying, so that the gelation is quick.
The MOF-I is a composite material prepared by carrying out a hydrothermal reaction on MOF and an iodine simple substance at the temperature of 180-220 ℃.
The specific technical scheme is that absolute ethyl alcohol and MOF are mixed at room temperature and then are uniformly stirred, a mixed solution of iodine simple substance and water is dripped, and the mixture is uniformly stirred and then reacts in a hydrothermal reaction kettle at the temperature of 180-220 ℃ for 8-12h to obtain the MOF-I. Wherein the mass ratio of the MOF to the iodine to the water is as follows: 0.2-1: 0.1-5: 20-28.
The MOF is a macroporous material and can adsorb iodine simple substances in pores to form a nano submicron grade material, and then is sprayed into high molecular materials of hydroxypropyl methyl cellulose and konjac material containing glucomannan, the metal framework composite I material is pulled by gaps to enter the gaps of the high molecular materials, and can quickly release I to promote the formation of gel.
A preparation method of a rapid gel carrier comprises the following steps:
(1) adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(2) and (2) after the mixture in the step (1) is tiled, spraying iodine solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m.
By adopting the technical scheme of the invention, the formed gel carrier can be obtained after 1-3 seconds, and is convenient for the operation of factory workshops.
Drawings
Fig. 1 is an effect diagram of a product obtained in embodiment 4 of the present invention.
Detailed Description
Example 1
A preparation method of konjak gel carrier comprises the following steps:
(1) adding soybean lecithin into a mixing reactor, adding water, introducing nitrogen, stirring uniformly at 110 ℃, adding an iodine simple substance or potassium iodate, and reacting for 2-3h to obtain the lecithin complexed iodine. Wherein the mass ratio of soybean lecithin, water and iodine is 0.38: 24: 0.15. (ii) a
(2) Adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(3) and (3) after the mixture in the step (2) is spread flatly, spraying lecithin-iodine complex solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m. The molecular weight of the obtained gel carrier was 1.0X 105-2.0×106Da. Cut into 1cm by 1cm pieces, and the degradation rate in 10ml of PBS buffer is 15-20 days per piece. Cut into 1cm × 1cm pieces, and the liquid absorption in 50ml of PBS buffer solution was 42.8-50.5 (mass of liquid absorbed per 1g of gel carrier). The storage modulus (G ') and the loss modulus (G') of the gel in the example 1 at 25 ℃ and different shear frequencies are measured by an RS6000 rheometer (Thermo-Fisher company), and the in-situ hydrogel in the example 1 has higher storage modulus between 360 and 450Pa and viscosity within 10 mPas.
Example 2
A preparation method of konjak gel carrier comprises the following steps:
(1) adding polyvinylpyrrolidone into a mixing reactor, adding water, introducing nitrogen, stirring uniformly at 90 ℃, adding an iodine simple substance, and reacting for 2-3h to obtain the polyvinylpyrrolidone complex iodine. Wherein the mass ratio of polyvinylpyrrolidone to water to iodine is 0.62: 25: 3.2;
(2) adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(3) after the mixture of the step (2) is laid flatSpraying a polyvinylpyrrolidone complex iodine solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m. The molecular weight of the obtained gel carrier was 1.0X 105-2.0×106Da. Cut into 1cm by 1cm pieces, and the degradation rate in 10ml of PBS buffer was 17-22 days per piece. The gel was cut into 1cm X1 cm pieces, and the liquid absorption in 50ml of PBS buffer was 46.7 to 53.4 (mass of liquid absorbed per 1g of gel carrier). The storage modulus (G ') and the loss modulus (G') of the gel in the example 1 at 25 ℃ and different shear frequencies are measured by an RS6000 rheometer (Thermo-Fisher company), and the in-situ hydrogel in the example 1 has higher storage modulus between 500 and 600Pa and viscosity within 10 mPas.
Example 3
A preparation method of konjak gel carrier comprises the following steps:
(1) adding alkyl glycoside into a mixing reactor, adding water, introducing nitrogen, stirring uniformly at 120 ℃, adding potassium iodate, and reacting for 2-3h to obtain the alkyl glycoside complex iodine. Wherein the mass ratio of alkyl glycoside, water, iodine simple substance or potassium iodate is 0.8: 27: 4.4;
(2) adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(3) and (3) after the mixture in the step (2) is tiled, spraying an alkyl glycoside complex iodine solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m. The molecular weight of the obtained gel carrier was 1.0X 106-4.0×106Da. Cut into 1cm by 1cm pieces, and the degradation rate in 10ml of PBS buffer is 15-20 days per piece. The gel was cut into 1cm X1 cm pieces, and the liquid absorption in 50ml of PBS buffer was 47.8.7-55.6 (mass of liquid absorbed per 1g of gel carrier). The storage modulus (G ') and loss modulus (G') of the gel of example 1 were measured at 25 ℃ and different shear frequencies using an RS6000 rheometer (Thermo-Fisher Co., Ltd.), and it was found that the storage modulus of the in situ hydrogel of example 1 wasHigher, between 300-400Pa, the viscosity is within 10 mPas.
Example 4
A preparation method of konjak gel carrier comprises the following steps:
(1) mixing absolute ethyl alcohol and tetrabutyl titanate at room temperature, uniformly stirring, dropwise adding a mixed solution of an iodine simple substance and water, uniformly stirring, and reacting in a hydrothermal reaction kettle at 200 ℃ for 10 hours to prepare the iodine-modified titanium dioxide. Wherein the mass ratio of isopropyl titanate or tetrabutyl titanate, iodine simple substance and water is as follows: 0.35: 1.5: 22. the ethanol is a mixed solvent of isopropyl titanate or tetrabutyl titanate, and is completely dissolved;
(2) adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(3) and (3) after the mixture in the step (2) is tiled, spraying iodine-doped titanium dioxide solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m. The molecular weight of the obtained gel carrier was 1.0X 106-3.5×106Da. Cut into 1cm by 1cm pieces, and the degradation rate in 10ml of PBS buffer is 17-26 days per piece. The gel was cut into 1cm X1 cm pieces, and the liquid absorption in 50ml of PBS buffer was 50.8 to 55.5 (mass of liquid absorbed per 1g of gel carrier). The storage modulus (G ') and the loss modulus (G') of the gel in the example 1 at 25 ℃ and different shear frequencies are measured by an RS6000 rheometer (Thermo-Fisher company), and the in-situ hydrogel in the example 1 has a higher storage modulus between 320 and 400Pa and a viscosity within 10 mPas.
Example 5
A preparation method of konjak gel carrier comprises the following steps:
(1) mixing absolute ethyl alcohol and MOF at room temperature, stirring uniformly, dropwise adding a mixed solution of a simple substance iodine and water, stirring uniformly, and reacting in a hydrothermal reaction kettle at 220 ℃ for 10 hours to obtain MOF-I. Wherein the mass ratio of the MOF to the iodine to the water is as follows: 0.58: 0.45: 27;
(2) adding water into hydroxypropyl methyl cellulose, stirring to dissolve, adding konjac flour, and stirring uniformly at the speed of 150-;
(3) and (3) after the mixture in the step (2) is spread flatly, spraying the MOF-I solution by using an atomizer at normal temperature, and collecting glue after 1-3 seconds to prepare the gel carrier. The particle size of the iodine solution sprayed is less than 0.1 mu m. The molecular weight of the obtained gel carrier was 1.0X 106-4.0×106Da. Cut into 1cm by 1cm pieces, and degrade at a rate of 19-26 days per piece in 10ml of PBS buffer. Cut into 1cm × 1cm pieces, and the liquid absorption in 50ml of PBS buffer solution was 52.1-57.6 (mass of liquid absorbed per 1g of gel carrier). The storage modulus (G ') and the loss modulus (G') of the gel in the example 1 at 25 ℃ and different shear frequencies are measured by an RS6000 rheometer (Thermo-Fisher company), and the in-situ hydrogel in the example 1 has higher storage modulus between 290 and 380Pa and viscosity within 10mPa & s.
Claims (6)
1. The preparation method of the konjac gel carrier is characterized by comprising the following steps:
(1) adding water into hydroxypropyl methyl cellulose, stirring for dissolving, adding konjac flour, and uniformly stirring at 250r/min under 150-;
(2) after the mixture in the step (1) is tiled, spraying iodine solution by using an atomizer, and collecting glue after 1-3 seconds to prepare the gel carrier, wherein the gel carrier comprises the following raw materials in parts by weight: 83-91 parts of hydroxypropyl methyl cellulose, 9-17 parts of konjac flour and 1-5 parts of iodine solution, wherein the iodine solution comprises any one of lecithin complex iodine, polyvinylpyrrolidone iodine, alkyl glycoside complex iodine and MOF-I.
2. The method for preparing a konjac gel carrier as claimed in claim 1, wherein the iodine solution is sprayed to have a particle size of less than 0.1 μm.
3. The method for preparing a konjac gel carrier according to claim 1, wherein the step of preparing the lecithin complexed iodine is to add soybean lecithin into a mixing reactor, add water, introduce nitrogen, stir at 90-120 ℃ uniformly, add iodine or potassium iodate, and react for 2-3 hours to obtain the lecithin complexed iodine, wherein the mass ratio of soybean lecithin, water, iodine or potassium iodate is 0.2-1: 20-28: 0.1-5.
4. The preparation method of the konjac gel carrier according to claim 1, wherein the polyvinylpyrrolidone iodine is prepared by adding polyvinylpyrrolidone into a mixing reactor, adding water, introducing nitrogen, stirring at 90-120 ℃, adding elemental iodine or potassium iodate, and reacting for 2-3 hours to obtain the polyvinylpyrrolidone complex iodine, wherein the mass ratio of polyvinylpyrrolidone to water to elemental iodine or potassium iodate is 0.2-1: 20-28: 0.1-5.
5. The preparation method of the konjac gel carrier according to claim 1, wherein the preparation step of the alkyl glycoside complex iodine is to add the alkyl glycoside into a mixing reactor, add water, introduce nitrogen, stir at 90-120 ℃, add iodine simple substance or potassium iodate, react for 2-3 hours to obtain the alkyl glycoside complex iodine, wherein the mass ratio of the alkyl glycoside, water, iodine simple substance or potassium iodate is 0.2-1: 20-28: 0.1-5.
6. The method for preparing the konjac gel carrier as claimed in claim 1, wherein the MOF-I is a composite material prepared by the hydrothermal reaction of MOF and iodine at 220 ℃ below 180 ℃.
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| Publication number | Publication date |
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| CN112111085B (en) | 2022-02-01 |
| CN112111085A (en) | 2020-12-22 |
| CN109679148A (en) | 2019-04-26 |
| CN112358654A (en) | 2021-02-12 |
| CN109679148B (en) | 2020-11-27 |
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