CN101585088B - Method for preparing nano-silver thread - Google Patents
Method for preparing nano-silver thread Download PDFInfo
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- CN101585088B CN101585088B CN2008101121915A CN200810112191A CN101585088B CN 101585088 B CN101585088 B CN 101585088B CN 2008101121915 A CN2008101121915 A CN 2008101121915A CN 200810112191 A CN200810112191 A CN 200810112191A CN 101585088 B CN101585088 B CN 101585088B
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Abstract
The invention discloses a method for preparing a nano-silver thread, which comprises the operation steps of: preparing 1 mmol of silver nitrate solution and 2 mmols of sodium borohydride solution respectively, then preparing the two solutions into a nano-silver colloid solution, then preparing the nano-silver colloid solution into a nano-silver gelatin solution, performing heating and concentration on the nano-silver mixed gelatin solution, then performing water bath heat preservation on the concentrated nano-silver mixed gelatin solution to ensure that the mixed gelatin solution is in a melted state, then soaking a suture which can be absorbed by human bodies into the nano-silver gelatin solution for a period of time, then uniformly drawing out of the suture at a preset rate, and naturally drying thesuture; and thus ensuring that the nano-silver gelatin mixed solution with corresponding viscosity forms a layer of thin glue film on the suture to obtain the nano-silver thread. The method has simple and easy operation steps; used instruments are commonly used experimental vessels; and the prepared nano-silver wire has the surface silver content of between 15 and 300 ng/cm, is used as a novel thread body for catgut embedding therapy, can play roles in infection resistance, sterilization, inflammation diminishing and the promotion of wound healing of surface element-silver, and can increase the therapeutic effect, repair and stimulate the regeneration of organisms when embedded into tissues for a long time.
Description
Technical field
The present invention relates to a kind of preparation method of nano-silver thread, exactly, relate to a kind of manufacture method that is used to not have the nano-silver thread of creating catgut embedding for treatment, belong to medical instruments or medical compounding ingredient technical field.
Background technology
At present, often adopt catgut embedding therapy in clinical treatment: the line body is imbedded the method that human acupoint carries out physical treatment, and it is to substitute traditional acupuncture and moxibustion therapy with imbedding the lasting spread effect of line body to the acupuncture point.The medical practice of recent decades proves: catgut embedding therapy is a kind of medical procedure that good efficacy is arranged.Because traditional catgut embedding therapy has certain traumatic, do not developed so enough pay attention to, now seldom application clinically.Yet in recent years, because the appearance of novel needle set; " make to make this nothing create the welcome and the attention of sunkening cord and obtaining numerous doctor and patients by the medical domain that present catgut embedding therapy has entered does not have wound or minimally-invasive treatment simultaneously, become the new direction of acupuncture medicine development.
Except continuing to improve the needle set of catgut embedding therapy, do not have and create the more wide development space in addition of sunkening cord: the improvement of heeling-in wire rod and development.Now, use medical stitching catgut as sunkening cord material usually.Though medical stitching catgut belongs to absorbable medical bio albumen, the line body of imbedding behind the human body can both be absorbed gradually by health.But catgut is mainly used in surgery stitching operation, is not special heeling-in industrial siding.And it also is the foreign matter in the human body after all, and the back human body of sunkening cord produces rejection, allergic reaction to it easily or meets talent for swimming and dye, and is to cause the part to produce situations such as hyperplasia furuncle joint.Moreover most widely used common medical stitching catgut is the physical stimulation that only substitutes acupuncture in the main medical mechanism of carrying out catgut embedding therapy at present, and curative effect is single, does not have other expansion result of treatment.Although the low price of catgut is drawn materials conveniently, many shortcomings such as it is poor also to have an absorbability, and infiltration rate that tissue reaction is big, body is interior and stimulus intensity are restive can not satisfy clinical requirement fully.Therefore how the employed line body of catgut embedding therapy material is improved,,, just become the new problem of healthcare givers's concern in the industry to substitute existing common medical stitching catgut according to the new material of sunkening cord of the clinical needs development of acupuncture.
Develop as early as possible and a kind ofly both can keep the strong point that catgut can be absorbed by the body as medical bio albumen, can remedy again its curative effect single, be easy to generate rejection and meet the novel implant material of the weak point that talent for swimming dyes, (sunken cord as the swimmer then can dive, swim) just becomes the exploration problem that healthcare givers in the industry seek assiduously.
Summary of the invention
In view of this, the preparation method who the purpose of this invention is to provide a kind of nano-silver thread, so that can make the nano-silver thread of its surperficial silver content in 15～300ng/cm scope, new molded lines body as catgut embedding therapy, it not only can keep the various advantages of medical catgut, more can bring into play simple substance silver sterilization that is had and the long-acting spread effect that promotes the regeneration of tissue repair and human body, can also be anti-infective and antibiotic, promote wound healing, improve and expand the curative effect of catgut embedding therapy greatly.
In order to achieve the above object, the invention provides a kind of preparation method of nano-silver thread, it is characterized in that: prepare 1 mM liquor argenti nitratis ophthalmicus and 2 mM sodium borohydride solutions respectively, again these two kinds of solution are mixed with nano-class silver colloidal solution, after being formulated as the nano silver gelatin mixed liquor then and heating, concentrate, the nano silver gelatin mixed liquor that concentrates is carried out water bath heat preservation, make this nano silver gelatin mixed liquor be in molten state, after the more absorbable suture of human body being soaked wherein a period of time, at the uniform velocity pull out to set speed, dry naturally; Just make nano silver gelatin mixed liquor on suture, form the skim glued membrane, make nano-silver thread with corresponding viscosity.
Described method comprises following operating procedure:
(1) preparation 1 mM liquor argenti nitratis ophthalmicus: take by weighing silver nitrate AgNO with electronic balance
30.170 the gram, be positioned in 100 milliliters of volumetric flasks after, add purified water and jolting again, make it the dissolving, be settled to 100 milliliters with purified water then;
(2) preparation 2 mM sodium borohydride solutions: take by weighing sodium borohydride NaBH with electronic balance
40.0760 gram is positioned in 1000 ml beakers, measures after purified water adds this beaker to again, uses glass bar to stir and makes it dissolving;
(3) preparation of nano silver colloidal solution: all dropwise splash in the 2 mM sodium borohydride solutions that prepare with the 1 mM liquor argenti nitratis ophthalmicus that the speed of 3 ml/min will prepare with dropper, in the process of splashing into, ceaselessly stir simultaneously and make transparent glassy yellow colloidal solution;
(4) preparation and concentrated nano silver gelatin mixed liquor: take by weighing gelatin 16 grams with electronic balance, put into 1000 ml beakers, add purified water and soaked 30 minutes, prevent to produce a large amount of foams, on the 1000w electric furnace, heat then, stir with glass bar simultaneously, make after the gelatin fusing evenly, the above-mentioned nano-class silver colloidal solution for preparing is poured in the beaker, continue heating, stirring and boiling again, when making mixed liquor be concentrated into about 100 milliliters, get one 250 ml beaker and weigh and count and be M
1, again mixed liquor is poured in this beaker, continue heating, stir and concentrate, and the numeration of weighing is M
2, as the weight of mixed liquor, i.e. M
2-M
1Stop heating when being 85 ± 3 grams;
(5) be coated with line: the nano silver gelatin mixed liquor for preparing is placed 65～70 ℃ of water bath heat preservations, make this nano silver gelatin mixed liquor be in the state of fusing, again the absorbable suture of human body is immersed wherein, after soaking for 10～20 seconds, speed with 0.2～0.6 cel is at the uniform velocity pulled out, and dries naturally; Just make that the nano silver gelatin mixed liquor with corresponding viscosity has formed the skim Thread with rubberized film on suture, finish the preparation of nano-silver thread.
The various glasswares that use in the described preparation process all will clean cleaning: each glass container that will need earlier to use is immersed in and was not less than in the washing lotion of being made up of the potassium bichromate and the concentrated sulfuric acid 5 minutes, take out glass container then, carried out ultrasonic 3～6 minutes with purified water, wash with purified water again, the dry back of nature airing is standby, so that the nano-class silver colloidal solution that is mixed with can long-term stability be deposited in the glass apparatus of cleaning.
When the preparation nano-class silver colloidal solution, be to AgNO
3And NaBH
4Accurately weigh strict control AgNO
3And NaBH
4Mol ratio be 1: 2; Require simultaneously to pick and place chemical example rapidly in the operating process, avoid its deliquescence, decomposition, sex change in air, and the nano-class silver colloidal solution that is made into should put into gelatin solution immediately, join the glue reaction.
With AgNO
3Solution dropwise splashes into NaBH
4In the process of the beaker of solution, keep the rate of addition set, will constantly stir glue simultaneously, assemble to avoid colloidal particle.
In the operating process of described step (4) preparation and concentrated nano silver gelatin mixed liquor, must be after gelatin melt fully, the nano-class silver colloidal solution that step (3) is prepared is poured in the beaker that holds gelatin again, on one side and stirring constantly when adding.
Described step (4) heats at the mixed liquor that described nano-class silver colloidal solution is added gelatin solution, in the operating process of stirring and boiling, the concentrated point of this mixed liquor depends on the minimum viscosity that can be coated with line, want the final concentrating degree of strict control, can make the silver content of the Nano Silver silk thread that coats in 15～200ng/cm scope to guarantee prepared gelatin concentration.
Described purified water is commercially available drinking pure water.
The absorbable suture of described human body is the synthetic suture of operation, slowly-releasing macromolecule operation synthetic thread or the poly-synthetic suture of operation that two oxygen cyclohexanone materials are made that medical operation catgut, medical polymer biological degradable material are made.
The present invention is the preparation method of nano-silver thread, and the operating procedure of this method is simple, realization is easy, and the instrument of use all is an experimental ware commonly used.Use this method and can make the nano-silver thread of surperficial silver content in 15～300ng/cm scope, as the new molded lines body of catgut embedding therapy.This novel nano silver material of sunkening cord not only keeps the various advantages of medical catgut, can bring into play more that the chance water that its simple substance silver that shows had is anti-infective, the effect of sterilization, anti-inflammatory and promotion wound healing, promote in the tissue if imbed for a long time, have the long-acting that increases curative effect, repairs and stimulate human body regeneration, improve and expand the curative effect of catgut embedding therapy greatly.
In addition, the medical polymer biological degradable material that its center line body has adopted development in recent years to get up, this wire rod can decompose in vivo, and catabolite can be absorbed by the body, metabolism, finally excretes.At present, the application of Biodegradable material aspect surgery medical science is quite ripe, the present invention just selects one or more different novel high polymer biodegradation materials to improve, or carry out functionalization, as the material that does not have the wound point catgut-embedding therapy for treating, to reduce the misery and the prescription on individual diagnosis number of times of patient's acupuncture, catgut embedding for treatment, reach convenient, do not have wound, effective and controlled requirement.Therefore, the present invention has good popularization and application prospect.
Description of drawings
Fig. 1 is preparation method's operating process schematic diagram of nano-silver thread of the present invention.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, the present invention is described in further detail below in conjunction with accompanying drawing.
Referring to Fig. 1, introduce the preparation method of nano-silver thread of the present invention, earlier the various glasswares that will use in the preparation process are all cleaned cleaning: each glass container that will need to use was immersed in the washing lotion of being made up of the potassium bichromate and the concentrated sulfuric acid above 5 minutes, take out glass container then, carried out ultrasonic 3～6 minutes with purified water, with the purified water flushing, the dry back of natural airing is standby, so that the nano-class silver colloidal solution that is mixed with can long-term stability be deposited in the glass apparatus of cleaning again.And prepare the absorbable suture of human body: the synthetic suture of the operation that can select for use medical operation catgut, medical polymer biological degradable material to make, slowly-releasing macromolecule operation synthetic thread or the poly-synthetic suture of operation that two oxygen cyclohexanone Absorbable suture materials are made.With commercially available drinking pure water as purified water.
The preparation process of Nano Silver silk thread of the present invention is: prepare 1 mM liquor argenti nitratis ophthalmicus and 2 mM sodium borohydride solutions respectively, again these two kinds of solution are mixed with nano-class silver colloidal solution, after being formulated as the nano silver gelatin mixed liquor then and heating, concentrate, the nano silver gelatin mixed liquor that concentrates is carried out water bath heat preservation, make the colloid mixed liquor be in molten state, after the more absorbable suture of human body being soaked wherein a period of time, at the uniform velocity pull out, dry naturally to set speed; Just make nano silver gelatin mixed liquor on suture, form the skim glued membrane, make nano-silver thread with corresponding viscosity.This method comprises following operating procedure;
(1) preparation 1 mM liquor argenti nitratis ophthalmicus: take by weighing silver nitrate AgNO with electronic balance
30.170 the gram, be positioned in 100 milliliters of volumetric flasks after, add purified water and jolting again, make it the dissolving, be settled to 100 milliliters with purified water then.
(2) preparation 2 mM sodium borohydride solutions: take by weighing sodium borohydride NaBH with electronic balance
40.0.0760 gram is positioned in 1000 ml beakers, measures after purified water adds this beaker to again, uses glass bar to stir and makes it dissolving.
(3) preparation of nano silver colloidal solution: all dropwise splash in the 2 mM sodium borohydride solutions that prepare with the 1 mM liquor argenti nitratis ophthalmicus that the speed of 3 ml/min will prepare with dropper, in the process of splashing into, ceaselessly stir simultaneously and make transparent glassy yellow colloidal solution.It should be noted that: with AgNO
3Solution dropwise splashes into NaBH
4In the solution process, keep the rate of addition set, and constantly stir glue simultaneously, assemble to avoid colloidal particle.
(4) preparation and concentrated nano silver gelatin mixed liquor: take by weighing gelatin 16 grams with electronic balance, put into 1000 ml beakers, adding purified water soaked 30 minutes, prevent to produce a large amount of foams, on the 1000w electric furnace, heat then, stir with glass bar simultaneously, after making that gelatin melts evenly fully, the above-mentioned nano-class silver colloidal solution for preparing is poured in the beaker, again while continuing heating, stirring and boiling constantly, when making mixed liquor be concentrated into about 100 milliliters, get one 250 ml beaker and weigh and count and be M
1, again mixed liquor is poured in this beaker, continue heating, stir and concentrate, and the numeration of weighing is M
2, as the weight of mixed liquor, i.e. M
2-M
1Stop heating when being 85 ± 3 grams.It should be noted that: nano-class silver colloidal solution is heated, in the operating process of stirring and boiling, the concentrated point of mixed liquor depends on the minimum viscosity that can be coated with line, want the final concentrating degree of strict control, can make the silver content of the Nano Silver silk thread that coats in 15～300ng/cm scope to guarantee prepared gelatin concentration.
(5) be coated with line: the nano silver gelatin mixed liquor for preparing is placed 65～70 ℃ of water bath heat preservations, make the colloid mixed liquor be in the state of fusing, the more absorbable suture of human body immersed wherein, soaked for 10～20 seconds after, speed with 0.2～0.6 cel is at the uniform velocity pulled out, and dries naturally; Just make that the nano silver gelatin mixed liquor with corresponding viscosity has formed the skim Thread with rubberized film on suture, finish the preparation of nano-silver thread.
This method it should be noted that in operating process: when the preparation nano-class silver colloidal solution, and be to AgNO
3And NaBH
4Accurately weigh strict control AgNO
3And NaBH
4Mol ratio be 1: 2; Require simultaneously to pick and place chemical example rapidly in the operating process, avoid its deliquescence, decomposition, sex change in air, and two parts of solution that are made into should put into gelatin solution immediately, join the glue reaction.
The present invention has carried out implementing test according to above-mentioned steps, and the sample of making have 100cm, and employing standard method and condition determination, and every centimetre silver content on the absorbable suture that coats sodium rice Gelatin is measured, and adheres to specification fully.Then, carry out the catgut embedding for treatment test with these wire rods again, also realized goal of the invention.
Claims (9)
1. the preparation method of a nano-silver thread, it is characterized in that: prepare 1 mM liquor argenti nitratis ophthalmicus and 2 mM sodium borohydride solutions respectively, again these two kinds of solution are mixed with nano-class silver colloidal solution, after being formulated as the nano silver gelatin mixed liquor then and heating, concentrate, the nano silver gelatin mixed liquor that concentrates is carried out water bath heat preservation, make this nano silver gelatin mixed liquor be in molten state, after the more absorbable suture of human body being soaked wherein a period of time, at the uniform velocity pull out to set speed, dry naturally; Just make nano silver gelatin mixed liquor on suture, form the skim glued membrane, make nano-silver thread with corresponding viscosity.
2. the preparation method of nano-silver thread according to claim 1, it is characterized in that: described method comprises following operating procedure:
(1) preparation 1 mM liquor argenti nitratis ophthalmicus: take by weighing silver nitrate AgNO with electronic balance
30.170 the gram, be positioned in 100 milliliters of volumetric flasks after, add purified water and jolting again, make it the dissolving, be settled to 100 milliliters with purified water then;
(2) preparation 2 mM sodium borohydride solutions: take by weighing sodium borohydride NaBH with electronic balance
40.0760 gram is positioned in 1000 ml beakers, measures after purified water adds this beaker to again, uses glass bar to stir and makes it dissolving;
(3) preparation of nano silver colloidal solution: all dropwise splash in the 2 mM sodium borohydride solutions that prepare with the 1 mM liquor argenti nitratis ophthalmicus that the speed of 3 ml/min will prepare with dropper, in the process of splashing into, ceaselessly stir simultaneously and make transparent glassy yellow colloidal solution;
(4) preparation and concentrated nano silver gelatin mixed liquor: take by weighing gelatin 16 grams with electronic balance, put into 1000 ml beakers, add purified water and soaked 30 minutes, prevent to produce a large amount of foams, on the 1000w electric furnace, heat then, stir with glass bar simultaneously, make after the gelatin fusing evenly, the above-mentioned nano-class silver colloidal solution for preparing is poured in the beaker, continue heating, stirring and boiling again, when making mixed liquor be concentrated into about 100 milliliters, get one 250 ml beaker and weigh and count and be M
1, again mixed liquor is poured in this beaker, continue heating, stir and concentrate, and the numeration of weighing is M
2, as the weight of mixed liquor, i.e. M
2-M
1Stop heating when being 85 ± 3 grams;
(5) be coated with line: the nano silver gelatin mixed liquor for preparing is placed 65～70 ℃ of water bath heat preservations, make this nano silver gelatin mixed liquor be in the state of fusing, again the absorbable suture of human body is immersed wherein, after soaking for 10～20 seconds, speed with 0.2～0.6 cel is at the uniform velocity pulled out, and dries naturally; Just make that the nano silver gelatin mixed liquor with corresponding viscosity has formed the skim Thread with rubberized film on suture, finish the preparation of nano-silver thread.
3. the preparation method of nano-silver thread according to claim 1, it is characterized in that: the various glasswares that use in the described preparation process all will clean cleaning: each glass container that will need earlier to use is immersed in and was not less than in the washing lotion of being made up of the potassium bichromate and the concentrated sulfuric acid 5 minutes, take out glass container then, carried out ultrasonic 3～6 minutes with purified water, wash with purified water again, the dry back of nature airing is standby, so that the nano-class silver colloidal solution that is mixed with can long-term stability be deposited in the glass apparatus of cleaning.
4. the preparation method of nano-silver thread according to claim 2 is characterized in that: when the preparation nano-class silver colloidal solution, and be to AgNO
3And NaBH
4Accurately weigh strict control AgNO
3And NaBH
4Mol ratio be 1: 2; Require simultaneously to pick and place chemical example rapidly in the operating process, avoid its deliquescence, decomposition, sex change in air, and the nano-class silver colloidal solution that is made into should put into gelatin solution immediately, join the glue reaction.
5. the preparation method of nano-silver thread according to claim 2 is characterized in that: with AgNO
3Solution dropwise splashes into NaBH
4In the process of the beaker of solution, keep the rate of addition set, will constantly stir glue simultaneously, assemble to avoid colloidal particle.
6. the preparation method of nano-silver thread according to claim 2, it is characterized in that: in the operating process of described step (4) preparation and concentrated nano silver gelatin mixed liquor, must be after gelatin melts fully, the nano-class silver colloidal solution that step (3) is prepared is poured in the beaker that holds gelatin again, while and constantly stir when adding.
7. the preparation method of nano-silver thread according to claim 2, it is characterized in that: described step (4) heats at the mixed liquor that described nano-class silver colloidal solution is added gelatin solution, in the operating process of stirring and boiling, the concentrated point of this mixed liquor depends on the minimum viscosity that can be coated with line, want the final concentrating degree of strict control, can make the silver content of the Nano Silver silk thread that coats in 15～300ng/cm scope to guarantee prepared gelatin concentration.
8. the preparation method of nano-silver thread according to claim 2, it is characterized in that: described purified water is commercially available drinking pure water.
9. the preparation method of nano-silver thread according to claim 2 is characterized in that: the absorbable suture of described human body is the synthetic suture of operation, slowly-releasing macromolecule operation synthetic thread or the poly-synthetic suture of operation that two oxygen cyclohexanone materials are made that medical operation catgut, medical polymer biological degradable material are made.
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| CN101585088B true CN101585088B (en) | 2011-07-27 |
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| CN101734617B (en) * | 2009-12-22 | 2013-04-24 | 浙江大学 | A method for preparing tube-network silver nano self-assembled bodies |
| BR112013014066A2 (en) * | 2010-12-07 | 2016-09-13 | Rhodia Operations | electrically conductive nanostructures, method for making such nanostructures, electrically conductive polymer films containing such nanostructures and electronic devices containing such films |
| CN102259190A (en) * | 2011-06-16 | 2011-11-30 | 浙江科创新材料科技有限公司 | Method for quickly preparing nano silver wires with high length-diameter ratio in large batch |
| DE102011052396A1 (en) * | 2011-08-04 | 2013-02-07 | Gelita Ag | Process for the preparation of a stable dispersion of nanoparticles, dispersion prepared and their use |
| CN103446621B (en) * | 2013-05-07 | 2015-06-10 | 哈尔滨工程大学 | Preparation method of nano-silver-containing sodium alginate based antibacterial medical dressing |
| CN104880580A (en) * | 2015-05-11 | 2015-09-02 | 厦门大学 | Method for cleaning surface of silver nanometer needle point by using sodium borohydride aqueous solution |
| CN106178383A (en) * | 2016-07-20 | 2016-12-07 | 宁夏共享生物化工有限公司 | A kind of photocatalyst type formaldehyde scavenger and preparation method thereof |
| CN106474531A (en) * | 2016-11-09 | 2017-03-08 | 泰州市榕兴医疗用品股份有限公司 | A kind of suture containing antiseptic and preparation method |
| CN109930284A (en) * | 2019-01-21 | 2019-06-25 | 杭州丝绸之路文化艺术有限公司 | The real silk fabric of fungus-resistant extremely preparation method |
| CN110354298B (en) * | 2019-07-26 | 2021-08-17 | 南京聚屹新材料有限公司 | Preparation method of in-situ crosslinked silver nanowire/polycaprolactone surgical suture |
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| CN1093004A (en) * | 1993-03-19 | 1994-10-05 | 蒋建华 | Long-acting broad-spectrum antibacterial medical suture |
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| CN1391956A (en) * | 2001-06-20 | 2003-01-22 | 任晓艳 | Medicinal catgut |
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN2734238Y (en) * | 2004-08-25 | 2005-10-19 | 任晓艳 | Nano silver coated suture line |
| CN1810422A (en) * | 2006-02-24 | 2006-08-02 | 中国科学院上海硅酸盐研究所 | Prepn process of nanometer silver sol |
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Patent Citations (6)
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|---|---|---|---|---|
| CN1093004A (en) * | 1993-03-19 | 1994-10-05 | 蒋建华 | Long-acting broad-spectrum antibacterial medical suture |
| CN1306117A (en) * | 2001-01-20 | 2001-08-01 | 南京希科集团有限公司 | Antibacterial flexible material containing nm silver and its preparing process and application |
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