CN110724278A - Method for preparing soluble compound based on polyelectrolyte - Google Patents
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Abstract
The invention discloses a method for preparing a soluble compound based on polyelectrolyte, which uses a multi-channel mixer to mix polyelectrolyte A solution and polyelectrolyte B solution or multivalent salt ion solution with different molar concentrations under the condition of rapid solution injection and mixing to obtain the soluble compound based on polyelectrolyte. The method is simple and convenient, has high mixing efficiency and good repeatability, avoids the problems of the occurrence of insoluble colloidal compounds and large-particle aggregates caused by the local over-saturation of solution mixing, has poor reproducibility and the like, enables the polyelectrolyte with opposite charges or the polyelectrolyte and the counter ions to be subjected to electrostatic compounding to obtain the soluble compound, provides a new thought and method for preparing the soluble compound based on the polyelectrolyte, and is beneficial to the research and utilization of the soluble compound based on the polyelectrolyte so as to be applied to the fields of biological materials, medical engineering and the like.
Description
Technical Field
The invention relates to a method for preparing a soluble compound based on polyelectrolyte by a multichannel rapid mixing method, belonging to the fields of polymer chemistry and materials.
Background
Polyelectrolyte refers to a polymer having an electrolyte group on a repeating unit, which includes a large amount of natural macromolecules (such as alginic acid, chitosan, nucleic acid, etc.) and artificially synthesized macromolecules (such as polyallylamine hydrochloride, polyacrylic acid, etc.). When the polyelectrolyte is mixed with multivalent counter ion solution with opposite charges or polyelectrolyte solution with opposite charges, the polyelectrolyte can generate soluble compound, liquid aggregate, hydrogel, precipitate and ion crosslinking micro-nano particles with the diameter of tens of nanometers to several micrometers through electrostatic compounding and self-assembly. The preparation method is simple and easy to operate, and the preparation conditions are mild, so that the product is widely applied to controlled release carriers, adsorbents, flocculating agents, thickening agents and the like in the fields of food industry and scientific research. For example, chitosan is the only natural polycationic sugar, and can form a complex with multiple negatively charged molecules such as sodium tripolyphosphate or alginic acid, and is widely used in various fields due to its biodegradability, biocompatibility, bioadhesion, antimicrobial activity and film-forming property. For another example, polyallylamine hydrochloride is a typical synthetic polymeric polyelectrolyte and is widely used in research based on polyelectrolyte complexes. However, the kinetics of such electrostatic complexing processes are extremely rapid, and local supersaturation, precipitation and particle generation are prone to occur during mixing, resulting in the inability or difficulty of preparing soluble polyelectrolyte-based complexes using traditional mixing methods. Therefore, the development of a simple, convenient and highly reproducible method for preparing a soluble polyelectrolyte-based complex is of great significance.
Disclosure of Invention
The invention aims to provide a simple and convenient method for preparing a soluble compound based on polyelectrolyte with high mixing efficiency and good repeatability aiming at the defects of the research in the field.
In order to realize the purpose, the following technical scheme is adopted:
the invention uses a multi-channel rapid mixing method to prepare a soluble compound based on polyelectrolyte, which comprises the following steps:
(1) preparation of the solution: respectively dissolving polyelectrolyte A, polyelectrolyte B with charges opposite to those of polyelectrolyte A or multivalent salt ions (counter ions) in water to obtain corresponding aqueous solutions.
(2) And (3) quickly mixing the solution: and (2) introducing a solution of the polyelectrolyte A into one or more channels of the multi-channel mixer, introducing a solution of the polyelectrolyte B or multivalent salt ions into inlets of the other channels, and quickly injecting and mixing the solution to obtain the soluble compound when the ratio of the molar quantity of the polyelectrolyte B or the counter ions to the molar concentration of the charges of the polyelectrolyte A is lower than a certain specific ratio (the ratio is determined by the types of the polyelectrolyte A, B and the counter ions).
Further, the multi-channel mixer is a mixer containing two or more solution channels.
Furthermore, in the final mixture, the molar concentration of the charges of the polyelectrolyte B or the multivalent salt ions (counter ions) is less than that of the polyelectrolyte A, and the ratio of the two is determined by the specific types of the polyelectrolyte A and the polyelectrolyte B or the multivalent salt ions (counter ions), and the specific calculation mode is as follows:
has the advantages that: the multi-channel rapid mixing method is simple and convenient, high in mixing efficiency and good in repeatability, avoids the problems of the occurrence of insoluble colloidal compounds and large-particle aggregates caused by local over-saturation of solution mixing, is poor in reproducibility and the like, enables the polyelectrolytes with opposite charges or the polyelectrolytes and counter ions to be subjected to electrostatic compounding to obtain the soluble compound, provides a new thought and method for preparing the soluble compound based on the polyelectrolytes, and is beneficial to research and utilization of the soluble compound based on the polyelectrolytes so as to be applied to the fields of biological materials, medical engineering and the like.
Drawings
FIG. 1 is a schematic view of multi-channel rapid mixing in example 1;
FIG. 2 is a graph showing the variation of light scattering intensity and particle size for chitosan/tripolyphosphate complex, chitosan/sodium alginate complex, sodium tripolyphosphate/polyallylamine hydrochloride complex, and sodium pyrophosphate/polyallylamine hydrochloride complex at different molar ratios;
FIG. 3 is a transmission electron microscope image of the mixed solution when the charge molar concentration ratio of sodium tripolyphosphate/chitosan is 0.1.
Detailed Description
Example 1
A method of preparing a soluble polyelectrolyte-based complex, comprising the steps of:
the polyelectrolyte A is chitosan, and the polyelectrolyte B is sodium tripolyphosphate; weighing 0.1g of chitosan, dissolving the chitosan in 100ml of 0.1% acetic acid solution, stirring overnight to obtain a dilute chitosan solution, weighing 0.004g, 0.008g, 0.012g, 0.016g, 0.024g, 0.032g, 0.040g, 0.048g, 0.056g, 0.064g, 0.072g, 0.08g, 0.088g and 0.096g of sodium tripolyphosphate, respectively dissolving in 100ml of deionized water, and stirring to obtain sodium tripolyphosphate solutions with different concentrations; then dilute chitosan solution and sodium tripolyphosphate solution with different concentrations are respectively adjusted to pH =4 by HCl solution, dilute chitosan solution is introduced into inlets 1 and 3 of a multi-channel mixer, sodium tripolyphosphate solution with a certain concentration (shown in figure 1) is introduced into inlets 2 and 4, the solutions are mixed in equal volumes, the mixing speed is 30mL/min, and sodium tripolyphosphate/chitosan solution with the charge molar concentration ratio of 0.05, 0.10, 0.15, 0.20, 0.30, 0.40, 0.50, 0.60, 0.70, 0.80, 0.90, 1.00, 1.10 and 1.20 (corresponding to 0.004g, 0.008g, 0.012g, 0.016g, 0.024g, 0.032g, 0.040g, 0.048g, 0.056g, 0.064g, 0.072g, 0.08g, 0.088g and 0.096 g) is obtained after mixing, and the solution is dissolved in 100mL of chitosan solution. When the sodium tripolyphosphate/chitosan charge molar concentration ratio is 0.05, 0.10, 0.15 and 0.20, the light scattering intensity of the mixed solution is not obviously increased and is similar to that of the chitosan solution (as shown in figure 2A), which indicates that the soluble complex is generated. When the charge molar concentration ratio of the sodium tripolyphosphate/chitosan is 0.30, 0.40, 0.50, 0.60, 0.70, 0.80, 0.90, 1.00, 1.10 and 1.20, the light scattering intensity is obviously increased, which indicates that an insoluble complex is formed; the following formula is the calculation formula of the charge molar concentration ratio of sodium tripolyphosphate/chitosan:
example 2
A method of preparing a soluble polyelectrolyte-based complex, comprising the steps of:
the polyelectrolyte A is sodium alginate, and the polyelectrolyte B is chitosan; weighing 0.1g of sodium alginate, dissolving the sodium alginate in 100ml of deionized water, stirring to obtain a diluted sodium alginate solution, weighing 0.009g, 0.018g, 0.027g, 0.036g, 0.045g, 0.054g, 0.063g, 0.072g, 0.081g, 0.090g, 0.108g, 0.126g, 0.144g, 0.162g and 0.180g of chitosan, respectively dissolving in 100ml of 0.1% diluted acetic acid solution, and stirring overnight to obtain chitosan solutions with different concentrations; then dilute sodium alginate solution and chitosan solution with different concentrations are respectively adjusted to pH =4 by HCl solution, dilute sodium alginate solution is introduced into inlets 1 and 3 of a multi-channel mixer, corresponding chitosan solution is introduced into inlets 2 and 4, the solutions are mixed in equal volumes, the mixing speed is 30mL/min, and the chitosan/sodium alginate solution mixed solution with the charge molar concentration ratio of 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.10, 0.12, 0.14, 0.16, 0.18, 0.20 (corresponding to 0.009g, 0.018g, 0.027g, 0.036g, 0.045g, 0.054g, 0.063g, 0.072g, 0.081g, 0.090g, 0.108g, 0.126g, 0.144g, 0.162g and 0.180g is dissolved in 100mL chitosan solution). When the charge molar concentration ratio of the chitosan/sodium alginate is 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08 and 0.09, the light scattering intensity of the mixed solution is not obviously increased and is similar to that of the sodium alginate solution (as shown in figure 3), and the generation of the soluble compound is proved. When the charge molar concentration ratio of chitosan/sodium alginate is 0.10, 0.12, 0.14, 0.16, 0.18 and 0.20, the light scattering intensity is obviously increased, which indicates that an insoluble complex is formed; the following is the calculation formula of the charge molar concentration ratio of chitosan to sodium alginate:
example 3
A method of preparing a soluble polyelectrolyte-based complex, comprising the steps of:
the polyelectrolyte A is polyallylamine hydrochloride and the counter ion is sodium tripolyphosphate; weighing 0.05g of polyallylamine hydrochloride, dissolving the polyallylamine hydrochloride in 100mL of deionized water, stirring to obtain a dilute polyallylamine hydrochloride solution, weighing 0.004g, 0.008g, 0.012g, 0.016g, 0.024g, 0.032g, 0.040g and 0.048g of sodium tripolyphosphate, respectively dissolving the sodium tripolyphosphate in 100mL of deionized water, and stirring to obtain different sodium tripolyphosphate solutions; the pH of the polyallylamine hydrochloride solution and the pH of the sodium tripolyphosphate solution are respectively adjusted to be =7, dilute polyallylamine hydrochloride solutions are introduced into inlets 1 and 3 of a multi-channel mixer, corresponding sodium tripolyphosphate solutions are introduced into inlets 2 and 4, the solutions are mixed in equal volume, the mixing speed is 30mL/min, and a sodium tripolyphosphate/polyallylamine hydrochloride mixed solution with the charge molar concentration ratio of 0.05, 0.10, 0.15, 0.20, 0.30, 0.40, 0.50 and 0.60 (corresponding to 0.004g, 0.008g, 0.012g, 0.016g, 0.024g, 0.032g, 0.040g and 0.048g of sodium tripolyphosphate dissolved in 100 mL) is obtained after mixing. When the soluble complex is characterized by using a malvern particle sizer, the light scattering intensity of the mixed solution is not obviously increased and is similar to that of the polyallylamine hydrochloride solution (as shown in fig. 3) when the charge molar concentration ratio of the sodium tripolyphosphate to the polyallylamine hydrochloride is 0.05 and 0.10, and the generation of the soluble complex is illustrated. When the charge molar concentration ratio of the sodium tripolyphosphate/polyallylamine hydrochloride is 0.15, 0.20, 0.30, 0.40, 0.50 and 0.60, the light scattering intensity is remarkably increased, indicating that an insoluble complex is formed; the following is a calculation formula for the charge molar concentration ratio of sodium tripolyphosphate/polyallylamine hydrochloride:
。
example 4
A method of preparing a soluble polyelectrolyte-based complex, comprising the steps of:
polyelectrolyte A is polyallylamine hydrochloride, polyelectrolyte B is sodium pyrophosphate; 0.05g of polyallylamine hydrochloride is weighed and dissolved in 100mL of deionized water to be stirred to obtain a dilute polyallylamine hydrochloride solution, and 0.0036g, 0.0072g, 0.0108g, 0.0144g, 0.0216g, 0.0288g, 0.0360g and 0.0432g of sodium pyrophosphate are respectively weighed and dissolved in 100mL of deionized water to be stirred to obtain sodium pyrophosphate solutions with different concentrations. The sodium tripolyphosphate solution and the sodium pyrophosphate solution are respectively adjusted to pH = 7; the diluted solution of polyallylamine hydrochloride was fed through the inlets 1 and 3 of the multi-channel mixer, and the corresponding sodium pyrophosphate solution was fed through the inlets 2 and 4, and the solutions were mixed in equal volume at a mixing speed of 30mL/min, thereby obtaining a sodium pyrophosphate/polyallylamine hydrochloride charge molar concentration ratio of 0.05, 0.10, 0.15, 0.20, 0.30, 0.40, 0.50, 0.60, 0.07 (corresponding to 0.0036g, 0.0072g, 0.0108g, 0.0144g, 0.0216g, 0.0288g, 0.0360g, 0.0432g, 0.0504g of sodium pyrophosphate dissolved in 100 mL) mixed solution of sodium pyrophosphate/polyallylamine hydrochloride. When the soluble complex is characterized by using a Malvern particle sizer, the light scattering intensity of the mixed solution is not obviously increased when the charge molar concentration ratio of the sodium pyrophosphate to the polyallylamine hydrochloride is 0.05, 0.10, 0.15 and 0.20, and is similar to that of the polyallylamine hydrochloride solution (as shown in figure 3), which indicates that the soluble complex is generated. When the charge molar concentration ratio of the sodium pyrophosphate to the polyallylamine hydrochloride is 0.30, 0.40, 0.50, 0.60 and 0.07, the light scattering intensity is remarkably increased, indicating that an insoluble complex is formed; the following is a calculation formula of the charge molar concentration ratio of the sodium tripolyphosphate/the polyallylamine hydrochloride;
the above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in the claims of the present invention should be covered by the present invention.
Claims (3)
1. A method for preparing a soluble polyelectrolyte-based complex, characterized in that: the method is to mix a solution of polyelectrolyte A with another solution of polyelectrolyte B or multivalent salt ions with charges opposite to those of polyelectrolyte A by adopting a multichannel rapid mixing method to obtain the soluble compound based on polyelectrolyte.
2. The method for preparing a soluble polyelectrolyte-based complex, according to claim 1, wherein: the method specifically comprises the following steps:
(1) preparation of the solution: respectively dissolving the polyelectrolyte A, the polyelectrolyte B with the charge opposite to that of the polyelectrolyte A or multivalent salt ions in water to obtain corresponding aqueous solutions.
(2) And (3) quickly mixing the solution: and introducing a polyelectrolyte A solution into one or more channels of the multi-channel mixer, introducing a polyelectrolyte B or multivalent salt ion solution into inlets of the other channels, and quickly injecting and mixing the solutions to obtain the soluble compound.
3. The method for preparing a soluble polyelectrolyte-based complex, according to claim 1, wherein: the multi-channel mixer is a mixer containing two or more solution channels.
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| CN112808122A (en) * | 2020-12-28 | 2021-05-18 | 福州大学 | Application of multi-channel mixer and method for continuously preparing liposome in batch |
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| CN109468708A (en) * | 2018-11-27 | 2019-03-15 | 五邑大学 | Calcium alginate-stannic oxide/graphene nano fiber and preparation method and load medicine calcium alginate-stannic oxide/graphene nano fiber |
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| CN109468708A (en) * | 2018-11-27 | 2019-03-15 | 五邑大学 | Calcium alginate-stannic oxide/graphene nano fiber and preparation method and load medicine calcium alginate-stannic oxide/graphene nano fiber |
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| HUANG, YAN ET AL.: ""On the kinetics of chitosan/tripolyphosphate micro- and nanogel aggregation and their effects on particle polydispersity"", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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| CN112808122A (en) * | 2020-12-28 | 2021-05-18 | 福州大学 | Application of multi-channel mixer and method for continuously preparing liposome in batch |
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