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Nanometer silver aqueous solution with stable macromolecules in closed network structure and preparation method thereof

A network structure, nano-silver technology, applied in the fields of botanical equipment and methods, preservation of human or animal bodies, chemicals for biological control, etc., can solve the problems of easy discoloration, easy oxidation, poor stability, etc. Less impurities, good bacteriostatic effect and high stability

Inactive Publication Date: 2017-04-19
长沙海润生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a nano-silver particle size small Preparation method of nano-silver aqueous solution with narrow distribution and high stability polyamide dendritic macromolecular structure with closed space network structure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 103.2g of diethylenetriamine and place it in a 500ml three-necked flask for cooling in an ice-water bath; use a constant pressure funnel to slowly add a mixed solution of 87.0g of methyl acrylate and 200ml of methanol dropwise under the protection of nitrogen, and react at room temperature for 4 hours after the dropwise addition Generate a light yellow intermediate, transfer the above intermediate to an eggplant-shaped bottle, remove methanol under reduced pressure on a rotary evaporator, then raise the temperature to 120 ° C for 4 hours to react under reduced pressure to obtain a polyamino hyperbranched polymer, add 10 g of succinic anhydride The temperature was raised to 140° C. and the reaction under reduced pressure was continued for 4 hours to obtain a polyamide dendrimer with a closed space network structure.

[0024] 500ml mass fraction of 1% silver nitrate solution is slowly added dropwise to 500ml mass fraction of 1% polyamide dendrimer aqueous solution. A...

Embodiment 2

[0026] Weigh 51.6g of diethylenetriamine and place it in a 250ml three-necked flask to cool in an ice-water bath; use a constant pressure funnel to slowly add a mixed solution of 43.0g of methyl acrylate and 100ml of methanol dropwise under the protection of nitrogen, and react at room temperature for 4 hours after the dropwise addition Generate a light yellow intermediate, transfer the above intermediate to an eggplant-shaped bottle, remove methanol under reduced pressure on a rotary evaporator, then raise the temperature to 140°C for 2 hours under reduced pressure to obtain a polyamino hyperbranched polymer, add 2.5g of maleic acid The temperature of the acid anhydride is raised to 150° C. and the reaction under reduced pressure is continued for 2 hours to obtain a polyamide dendrimer with a closed space network structure.

[0027] 500ml mass fraction of 0.5% silver acetate solution is slowly added dropwise to 500ml of the above-mentioned polyamide dendrimer aqueous solution ...

Embodiment 3

[0029] Weigh 122.6g of tetraethylenepentamine and place it in a 500ml three-necked flask for cooling in an ice-water bath; use a constant pressure funnel to slowly add a mixed solution of 57.5g of methyl acrylate and 200ml of chloroform under the protection of nitrogen, and react at room temperature after the addition is complete A light yellow intermediate was generated in 4 hours, and the above intermediate was transferred to an eggplant-shaped bottle, and the chloroform was removed under reduced pressure on a rotary evaporator, and then the temperature was raised to 140 ° C for 2 hours under reduced pressure to obtain a polyamino hyperbranched polymer. Add 13.4 g of succinic anhydride is heated up to 150° C. and the reaction under reduced pressure is continued for 1 hour to obtain a polyamide dendrimer with a closed space network structure.

[0030] 500ml mass fraction of 1% silver nitrate solution was slowly added dropwise to 500ml mass fraction of 1% polyamide dendrimer aq...

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Abstract

The invention provides a nanometer silver aqueous solution with stable macromolecules in a closed network structure and a preparation method thereof. The preparation method comprises the following steps: cooling a multi-amino monomer to 5 to 10 DEG C in an ice-water bath; then dropwise adding an ethylene monomer and a solvent into the multi-amino monomer through a funnel under the protection of nitrogen gas, after the completion of dropwise addition, carrying out a reaction at normal temperature for 4 hours so as to generate a light-yellow intermediate, placing the intermediate on a rotary evaporator, reducing pressure so as to remove the solvent, carrying out heating to 120 DEG C to 140 DEG C, and carrying out a pressure-reducing reaction for 2 to 4 hours so as to obtain a multi-amino hyperbranched polymer; adding a modifying agent into the multi-amino hyperbranched polymer, carrying out heating to 140 to 150 DEG C, continuing the pressure-reducing reaction for 1 to 4 hours so as to obtain a polyamide dendrimer polymer with the closed space network structure; and adding a silver ion compound solution into the polyamide dendrimer polymer with the closed space network structure, and carrying out complex-reduction so as to obtain a stable nanometer silver solution with a particle size of 5 to 15 nm.

Description

technical field [0001] The invention relates to a disinfectant or bactericide used in the medical and health field, in particular to a method for preparing an aqueous solution of nano-silver with a polyamide tree macromolecular structure. Background technique [0002] Due to its small size and large specific surface area, nano-silver materials have unique optical, electrical, magnetic, thermal, and antibacterial properties, and are widely used in chemical detection, biological imaging, and antibacterial preparations. In addition, nano-silver has extremely strong Nano-activity, showing super-long antibacterial ability, can kill common bacteria, fungi, mycoplasma and other pathogenic microorganisms at extremely low concentrations. Compared with antibiotics, nano-silver has the characteristics of bactericidal effect not affected by pH value, broad-spectrum antibacterial, no drug resistance, long-lasting effect, stronger bactericidal power when exposed to water, safety and envir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N59/16A01N25/22A01N25/04A01P1/00A01P3/00C08G83/00
CPCA01N25/04A01N25/22A01N59/16C08G83/003C08G83/004A01N2300/00
Inventor 史丙华姜志华何杰
Owner 长沙海润生物技术有限公司
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