CN102489716B - Preparation method for lignosulfonate nano-silver colloid - Google Patents
Preparation method for lignosulfonate nano-silver colloid Download PDFInfo
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- CN102489716B CN102489716B CN 201110422447 CN201110422447A CN102489716B CN 102489716 B CN102489716 B CN 102489716B CN 201110422447 CN201110422447 CN 201110422447 CN 201110422447 A CN201110422447 A CN 201110422447A CN 102489716 B CN102489716 B CN 102489716B
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- lignosulfonate
- nano
- silver
- silver colloid
- colloid
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229920001732 Lignosulfonate Polymers 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- 238000006722 reduction reaction Methods 0.000 claims abstract description 5
- 229920005610 lignin Polymers 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000009938 salting Methods 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 3
- 238000006277 sulfonation reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000000084 colloidal system Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the field of fine chemical industry, and particularly relates to a method for preparing nano-silver colloid by using lignosulfonate. The method for preparing nano-silver colloid by using lignosulfonate disclosed by the invention comprises the following steps of: (1) taking a certain amount of silver nitrate, adding the silver nitrate in lignosulfonate solution, and uniformly mixing, wherein the concentration of the lignosulfonate solution is 0.001-30 wt%, and the amount of the silver nitrate occupies 0.001-10 wt% of the mass of the whole solution; and (2) adding a certain amount of reducing agent in the solution obtained in the step (1), performing a reduction reaction, and then obtaining lignosulfonate nano-silver colloid after the reaction is finished, wherein the amount of the reducing agent occupies 0.01-20 wt% of the mass of the whole solution. The method for preparing nano-silver colloid by using lignosulfonate disclosed by the invention is simple and practicable; the grain size of the obtained nano-silver is about 20 nanometres; and the colloid has no precipitation after being placed in half a year and is a stable nano-silver colloid. The method for preparing nano-silver colloid by using lignosulfonate disclosed by the invention can turn waste into wealth and reduce environmental pollution; and the nano-silver colloid is a new functional material prepared based on lignosulfonate.
Description
Technical field
The invention belongs to field of fine chemical, be specifically related to a kind of method of utilizing lignosulfonates to prepare nano silver colloidal sol.
Background technology
Nano Silver all has broad application prospects in fields such as anti-biotic material, effective catalyst, lubricant, light absorbing material, coating, sensor, electrocondution slurry, high performance electrode materials, nano-Ag particles is reunited easily, for obtaining high degree of dispersion, stable nano silver colloidal sol, some high molecular polymers are prepared nano silver colloidal sol by used as stabilizers, such as polyvinylpyrrolidone, polyvinyl alcohol etc.Lignosulfonates are a kind of soluble in water, derive from the three-dimensional netted high molecular polymer of lignin, contain sulfonic group in the molecule, hydroxyl, carbonyl, wherein sulfonic group can be by electrostatic interaction and silver ion combination, and contained lone pair electrons energy and the silver ion of the oxygen atom in hydroxyl and the carbonyl produces coordination, therefore silver ion can be dispersed in the network structure of lignosulfonates preferably, add suitable reducing agent and just can prepare nano-Ag particles by local reduction way this moment, thereby obtain the nano silver colloidal sol of good dispersion, energy stable existence.Lignosulfonates are cheap, and are nontoxic, have biodegradable and biocompatibility, and the nano silver colloidal sol that therefore uses it as the stabilizing agent preparation is expected to become a kind of than the lower antibiotic material in medical use of chitosan nano silver sol price.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of difference lignosulfonate nano-silver colloid in the past.
The inventive method comprises the step of following order:
(1) get a certain amount of silver nitrate and join in the lignin sulfonic acid salting liquid and mix, wherein, the concentration of lignin sulfonic acid salting liquid is 0.001-30wt%, and the amount of silver nitrate accounts for the 0.001-10wt% of whole solution quality;
(2) a certain amount of reducing agent is joined in step (1) the gained solution, carry out reduction reaction, react and namely obtain lignosulfonate nano-silver colloid after complete, wherein, the amount of reducing agent accounts for the 0.01-20wt% of whole solution quality.
More particularly, described lignosulfonates are sulphite pulping process accessory substance or the lignosulfonates that prepared after sulfonation by other lignin.
Described reducing agent is a kind of in sodium borohydride, ethylene glycol and the ascorbic acid.
The present invention utilizes the energy and the interactional chemical group of silver ion that contain in the network structure of lignosulfonates and the molecule thereof that silver ion is fixed, and then adds suitable reducing agent prepares stable dispersion by in-situ reducing nano silver colloidal sol.The inventive method is simple, and gained Nano Silver particle diameter is about 20 nanometers, and colloidal sol is placed half a year without Precipitation, is a kind of more stable nano silver colloidal sol.The present invention can be turned waste into wealth, and environmental contamination reduction is a kind of new functional material based on the lignosulfonates preparation.
Description of drawings
Fig. 1 is the TEM image of the Nano Silver of the embodiment of the invention 1 preparation.
Fig. 2 is the SEM image of the Nano Silver of the embodiment of the invention 1 preparation.
The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1:
It is in the 0.5 wt% lignin sulfonic acid sodium solution that 0.1 gram silver nitrate is joined 200 ml concns, stirred 10 minutes, the sodium borohydride solution room temperature lower magnetic force that adds 4 ml concns again and be 1M stirred one hour, namely made particle diameter and be the ball shaped nano silver sol about 20 nanometers.The TEM image of the nano silver colloidal sol that it makes as shown in Figure 1, its SEM image is as shown in Figure 2.
Embodiment 2:
To join 200 ml concns be in the 0.2 wt% lignin sulfonic acid sodium solution with 0.1 gram silver nitrate, stirred 10 minutes, adds 20 milliliters of ethylene glycol again, and 80 ℃ of lower magnetic forces stirrings one hour namely make particle diameter and be the ball shaped nano silver sol about 20 nanometers.
Embodiment 3:
To join 200 ml concns be in the 0.2 wt% lignin sulfonic acid sodium solution with 0.1 gram silver nitrate, stirred 10 minutes, adds 0.7 gram ascorbic acid again, and 30 ℃ of lower magnetic forces stirrings one hour namely make particle diameter and be the ball shaped nano silver sol about 20 nanometers.
Used lignin sulfonic acid sodium solution is sulphite pulping process accessory substance or the lignosulfonates that prepared after sulfonation by other lignin in above-described embodiment.
Claims (3)
1. the preparation method of a lignosulfonate nano-silver colloid is characterized in that comprising the step of following order:
(1) get a certain amount of silver nitrate and join in the lignin sulfonic acid salting liquid and mix, wherein, the concentration of lignin sulfonic acid salting liquid is 0.001-30wt%, and the amount of silver nitrate accounts for the 0.001-10wt% of whole solution quality;
(2) a certain amount of reducing agent is joined in step (1) the gained solution, carry out reduction reaction, react and namely obtain lignosulfonate nano-silver colloid after complete, wherein, the amount of reducing agent accounts for the 0.01-20wt% of whole solution quality.
2. the preparation method of lignosulfonate nano-silver colloid according to claim 1 is characterized in that: described lignosulfonates are sulphite pulping process accessory substance or the lignosulfonates that prepared after sulfonation by other lignin.
3. the preparation method of lignosulfonate nano-silver colloid according to claim 1 and 2 is characterized in that: described reducing agent is a kind of in sodium borohydride, ethylene glycol and the ascorbic acid.
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| CN 201110422447 CN102489716B (en) | 2011-12-15 | 2011-12-15 | Preparation method for lignosulfonate nano-silver colloid |
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| CN102489716B true CN102489716B (en) | 2013-03-13 |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104277468A (en) * | 2013-07-10 | 2015-01-14 | 石家庄铁道大学 | Composite material of lignin/metal nanoparticles and preparation method of composite material |
| CN103749535B (en) * | 2013-12-26 | 2015-11-04 | 西南大学 | Nano-silver/lignin composite antibacterial material and preparation method thereof |
| CN103769604B (en) * | 2014-01-25 | 2016-03-02 | 华南理工大学 | A kind of green fast preparation method of lignin-nano silver colloidal sol |
| CN108436099A (en) * | 2018-04-04 | 2018-08-24 | 吉林化工学院 | A kind of preparation method of the nano silver with anti-microbial property |
| CN108620604A (en) * | 2018-06-11 | 2018-10-09 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of high-purity nano silver paste |
| CN110860695A (en) * | 2019-11-25 | 2020-03-06 | 天津科技大学 | Preparation method of silver nanoparticles with adjustable size and distribution |
| CN112221520B (en) * | 2019-12-10 | 2024-03-29 | 天津科技大学 | Preparation method of silver/silver chloride composite nanocube |
| CN112221436B (en) * | 2019-12-10 | 2022-08-12 | 天津科技大学 | Preparation method of silver/silver chloride composite cubic nanoparticle self-assembled microspheres |
| CN113884458A (en) * | 2020-07-03 | 2022-01-04 | 吉林化工学院 | Method for detecting mercury ions by nano silver particles based on green synthesis |
| CN113960021A (en) * | 2020-07-03 | 2022-01-21 | 吉林化工学院 | Test paper for rapidly detecting mercury ions by nano silver particles based on green synthesis |
| CN112191861B (en) * | 2020-09-29 | 2022-12-20 | 湖南中伟新银材料科技有限公司 | Preparation method of conductive silver powder, prepared conductive silver powder and application of conductive silver powder |
| RU2756226C1 (en) * | 2020-12-02 | 2021-09-28 | Федеральное государственное автономное образовательное учреждение высшего образования «Северный (Арктический) федеральный университет имени М. В. Ломоносова» | Method for obtaining a solution of colloidal silver |
| CN113512209B (en) * | 2021-08-10 | 2022-04-15 | 吉林大学 | Preparation method of high-conductivity and high-sensitivity polyvinyl alcohol-based conductive hydrogel |
| CN113679881A (en) * | 2021-08-30 | 2021-11-23 | 中南大学湘雅医院 | Medical dressing with antibacterial property and preparation method thereof |
| CN114062347B (en) * | 2021-11-12 | 2024-02-02 | 福州大学 | Flexible hydrogel SERS chip of aggregation state silver nano particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1704843A (en) * | 2004-05-31 | 2005-12-07 | 中国科学院理化技术研究所 | Silver sulfide nano particle sensibilizer, its preparing method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010043337A (en) * | 2008-08-18 | 2010-02-25 | Sumitomo Metal Mining Co Ltd | Silver powder and its manufacturing method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1704843A (en) * | 2004-05-31 | 2005-12-07 | 中国科学院理化技术研究所 | Silver sulfide nano particle sensibilizer, its preparing method and use |
Non-Patent Citations (2)
| Title |
|---|
| JP特开2010-43337A 2010.02.25 |
| 向育君等.木质素磺酸盐研究及其主要应用最新进展.《高分子通报》.2010,(第9期), * |
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