CN112062149A - Preparation method of nano copper sulfide - Google Patents
Preparation method of nano copper sulfide Download PDFInfo
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- CN112062149A CN112062149A CN202010975578.4A CN202010975578A CN112062149A CN 112062149 A CN112062149 A CN 112062149A CN 202010975578 A CN202010975578 A CN 202010975578A CN 112062149 A CN112062149 A CN 112062149A
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- copper
- hair
- copper sulfide
- nano copper
- sulfide
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- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 150000001879 copper Chemical class 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 241000282414 Homo sapiens Species 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000002699 waste material Substances 0.000 claims abstract description 7
- 239000012620 biological material Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 4
- 241000272525 Anas platyrhynchos Species 0.000 claims abstract description 3
- 241000287828 Gallus gallus Species 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 210000003746 feather Anatomy 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000003917 TEM image Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 102000011782 Keratins Human genes 0.000 description 1
- 108010076876 Keratins Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 229910001779 copper mineral Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a preparation method of nano copper sulfide, which comprises the steps of cutting waste biological materials such as human hair, pig hair, chicken feather, duck hair and the like into fine crushed materials, drying, sequentially adding the crushed materials into ethylene glycol together with copper salt, carrying out magnetic stirring for a period of time, adding a certain amount of sodium hydroxide, uniformly stirring, transferring the mixture into a polytetrafluoroethylene tank, carrying out heating reaction for a certain period of time, filtering, and cleaning with ethanol to obtain the nano copper sulfide. The method for synthesizing the copper sulfide by using the hair as the sulfur source has the advantages of simple process, low cost, safety, no toxicity, environmental friendliness, wide material source and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of nano copper sulfide.
Background
Copper sulfide accounts for 80% of copper ore resources, and has been attracting attention as a main copper mineral. The nano copper sulfide has been widely applied in the fields of photocatalysis, capacitors, semiconductors, lithium batteries and the like. Meanwhile, in recent years, copper sulfide has attracted a great deal of interest in tumor diagnosis and treatment due to its strong near infrared absorption plasmon resonance absorption effect and low toxicity. If the copper sulfide is used for treating tumors by a photothermal method, high-concentration active oxygen clusters can be generated to kill tumor cells according to the characteristics of high photothermal conversion and near infrared light induced photodynamic of copper sulfide nanocrystals.
At present, most of the synthesis methods of nano copper sulfide use toxic chemical reagents, such as a method for preparing nano copper sulfide by adding sodium sulfide or thioacetamide into a copper salt solution. Sodium sulfide is easily deliquesced in the air, and the released hydrogen sulfide gas can generate toxic effect on human bodies. Thioacetamide itself belongs to carcinogen, and acidic conditions used in the process of preparing the nano copper sulfide can also release hydrogen sulfide gas which is harmful to human bodies. Therefore, how to make the synthesis process safer and more environment-friendly is a problem that relevant researchers are continuously working on.
Hair from human and animals is a sulfur-containing material (containing about 5% of sulfur) which is produced in enormous quantities and is often treated as waste by human beings, and mainly comprises 19 to 22 kinds of amino acids (keratin), and the amino acids are naturally combined into a sulfur chain, and a disulfide bond in the sulfur chain is broken under high temperature, high pressure and strong alkali conditions to generate a mercapto group, which can be further combined with copper ions under strong alkali conditions to form nuclei to generate nano copper sulfide. Therefore, the animal hair can be used as a novel sulfur source to replace the traditional toxic sulfur source to prepare the copper sulfide, which is an important innovation for preparing the nano copper sulfide.
Disclosure of Invention
The invention aims to provide a preparation method of green and nontoxic nano copper sulfide aiming at the current situation and technical defects of copper sulfide synthesis.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of nano copper sulfide comprises the following steps:
(1) cutting the waste biological materials into small crushed materials, and drying for later use;
(2) taking 0.5-10 g of crushed materials and 5-50 mmol of copper salt, sequentially adding the crushed materials and the 5-50 mmol of copper salt into 10-100 ml of ethylene glycol, and magnetically stirring for 30 min;
(3) adding 0.05-0.50 g of sodium hydroxide, and uniformly stirring;
(4) transferring the mixed solution obtained in the step (3) into a polytetrafluoroethylene tank, and heating and reacting for a certain time;
(5) and (4) filtering the reaction liquid obtained in the step (4), and cleaning the precipitate with ethanol to obtain the nano copper sulfide.
The waste biological materials in the step (1) comprise human hair, hair materials such as pig hair, chicken hair, duck hair and the like; the length of the obtained crushed aggregates is 0.1-0.5 cm; the drying temperature is 60-90 ℃, and the drying time is 3-8 h.
The copper salt in the step (2) is copper nitrate, copper sulfate, copper chloride or copper acetate.
In the step (4), the heating temperature is 120-200 ℃, and the time is 8-24 h.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the nano copper sulfide provided by the invention is safe, nontoxic, simple in process, low in cost, green and environment-friendly, and wide in raw material source.
Drawings
FIG. 1 is a transmission electron micrograph of the product prepared in example 1.
FIG. 2 is a transmission electron micrograph of the product prepared in example 2.
FIG. 3 is a transmission electron micrograph of the product prepared in example 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described implementation cases are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Cutting waste human hair into crushed materials with the length of 0.1-0.5 cm, drying for 4 hours at 80 ℃, sequentially adding 1.5 g and 0.005 mol of copper nitrate into 30 ml of ethylene glycol, magnetically stirring for 30 minutes, adding 0.1 g of sodium hydroxide, uniformly stirring, transferring into a polytetrafluoroethylene tank, and heating and reacting for 12 hours at 150 ℃; and filtering the mixed solution obtained after the reaction is finished, and cleaning the mixed solution by using ethanol to obtain the nano copper sulfide.
FIG. 1 is a transmission electron micrograph of the product prepared in this example.
Example 2
The procedure of example 1 was repeated except that the copper salt used in example 1 was changed to copper chloride.
FIG. 2 is a transmission electron micrograph of the product prepared in this example.
Example 3
The procedure of example 1 was repeated except that the amount of sodium hydroxide used in example 1 was changed to 0.05 g.
FIG. 3 is a transmission electron micrograph of the product prepared in this example.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (4)
1. The preparation method of the nano copper sulfide is characterized by comprising the following steps of:
(1) cutting the waste biological materials into small crushed materials, and drying for later use;
(2) taking 0.5-10 g of crushed materials and 5-50 mmol of copper salt, sequentially adding the crushed materials and the 5-50 mmol of copper salt into 10-100 ml of ethylene glycol, and magnetically stirring for 30 min;
(3) adding 0.05-0.50 g of sodium hydroxide, and uniformly stirring;
(4) transferring the mixed solution obtained in the step (3) into a polytetrafluoroethylene tank, and heating and reacting for a certain time;
(5) filtering the reaction liquid obtained in the step (4), and cleaning the precipitate with ethanol to obtain nano copper sulfide;
the waste biological materials in the step (1) comprise human hair, pig hair, chicken hair and duck hair.
2. The method for preparing nano copper sulfide as claimed in claim 1, wherein the length of the crushed aggregates obtained in the step (1) is 0.1-0.5 cm; the drying temperature is 60-90 ℃, and the drying time is 3-8 h.
3. The method as claimed in claim 1, wherein the copper salt in step (2) is selected from the group consisting of copper nitrate, copper sulfate, copper chloride and copper acetate.
4. The method for preparing nano copper sulfide as claimed in claim 1, wherein the heating temperature in the step (4) is 120-200 ℃ and the heating time is 8-24 h.
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CN202010975578.4A CN112062149A (en) | 2020-09-16 | 2020-09-16 | Preparation method of nano copper sulfide |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112915104A (en) * | 2021-02-01 | 2021-06-08 | 吉林大学 | Application of copper sulfide, copper sulfide nanocomposite and preparation method and application thereof |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2009109110A1 (en) * | 2008-03-06 | 2009-09-11 | 拜耳技术工程{上海}有限公司 | Copper indium sulfide nanoparticles and a preparation method thereof |
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CN110282652A (en) * | 2019-08-09 | 2019-09-27 | 陕西科技大学 | A kind of flower-shaped copper sulfide of 3D and its hydrothermal preparing process |
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CN111484067A (en) * | 2020-04-15 | 2020-08-04 | 邯郸学院 | Preparation method of solid cubic block copper sulfide |
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2020
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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