Back to results
US 9,764,964 B2Granted
Application of lactam as solvent in nanomaterial preparation
AssigneeShanghai Genius Advanced Material (Group) Co., Ltd.
InventorsHousheng Xia, Guisheng Yang
Life of this patent
Estimating the term…
Abstract
The present invention disclosed use of lactam as a solvent in the preparation of nanomaterials by precipitation method, sol-gel method or high temperature pyrolysis. These methods are able to recycle lactam solvent, which meet requirements of environmental protection.
Claims19
A precipitation method for synthesis of nanomaterials, comprising the following steps:
- adding 0.01-100 weight parts of precursor and 100 weight parts of lactam solvent into a reactor to form a mixture;
- stirring the mixture at 80-200° C. for 0.1-2 hr wherein the lactam solvent becomes a molten lactam solvent in which the precursor is fully dissolved or dispersed, when stirring, adding 0.05-50 weight parts of precipitant, at a temperature of 80-250° C. and a time of 0.1-200 hr to obtain precipitate;
- washing the precipitate with water to obtain washed precipitate;
- centrifuging the washed precipitate to obtain centrifuged precipitate;
- and
- drying the centrifuged precipitate to obtain synthesized nanomaterials;
- wherein the precursor is selected from the group consisting of soluble inorganic metal salts of halogen, nitrate, nitrite, sulfate, sulfite or carbonate anions and organic compounds of metals or metalloids;
- wherein the lactam contained in the lactam solvent is one or more substances selected from cyclic amides or cyclic amide derivatives;
- wherein the general structural formula of the cyclic amides is:
- wherein the general structural formula of the cyclic amide derivatives is:
- wherein R is a substance selected from the group consisting of hydrogen, halogen, alkyl, hydroxy, alkoxy and acyl;
- wherein the precipitant is selected from the group consisting of alkali metals, alkali metal oxides, alkali metal hydroxides, alkali metal organic salts, ammonia, compounds able to release ammonia by pyrolysis, soluble inorganic salts formed by metal elements and halogen elements, soluble inorganic salts formed by metal elements and chalcogens, soluble inorganic salts formed by metal elements and carbonate, and soluble inorganic salts formed by metal elements and sulfate;
- and
- wherein the nanomaterials are substances containing inorganic particles having a particle size of greater than 1 nm and less than or equal to 100 nm;
- the content of the inorganic particles is no less than 0.01% of the substance;
- the inorganic particles are mixtures composed of one or more substances selected from the group consisting of hydroxides, oxides, sulfides, metals and inorganic salts.
13 more elements
A sol-gel method for synthesis of nanomaterials with lactam as the solvent comprising the steps:
- adding 0.01-100 weight parts of hydrolyzable precursor and 100 weight parts of lactam solvent into a reactor to form a mixture;
- stirring the mixture at 80-150° C. for 0.1-2 hr to make the lactam solvent molten and to fully dissolve and disperse the hydrolysable precursor in the molten lactam solvent, and adding 0.01-50 weight parts of water for hydrolysis with the hydrolysis temperature of 80˜250° C. and hydrolysis time of 0.01-48 hr to obtain sol;
- performing gelatinization on the sol in the reactor at 80˜270° C. for 0.01-96 hr to obtain a gelatinized mixture;
- washing the gelatinized mixture with absolute alcohol to obtain a washed mixture;
- and
- drying the washed mixture to obtain synthesized nanomaterials;
- wherein the hydrolyzable precursor is selected from the group consisting of inorganic metal salts of halogen, nitrate, sulfate or acetate anions and metal organics,
- wherein the lactam contained in the lactam solvent is one or more substances selected from the group consisting of cyclic amides and cyclic amide derivatives,
- wherein the general structural formula of the cyclic amide is:
- the general structural formula of the cyclic amide derivatives is:
- wherein R is a substance selected from hydrogen, halogen, alkyl, hydroxy, alkoxy or acyl;
- and
- wherein the nanomaterials are substances containing inorganic particles having a particle size of greater than 1 nm and less than or equal to 100 nm;
- the content of the inorganic particles is no less than 0.01% of the substance;
- the inorganic particles are mixtures composed of one or more substances selected from the group consisting of hydroxides, oxides, sulfides, metals and inorganic salts.
12 more elements
A high temperature pyrolysis method for synthesis of nanomaterials with lactam as the solvent comprising the steps:
- adding 0.01-100 weight parts of pyrolyzable precursor and 100 weight parts of lactam solvent into a reactor to form a mixture;
- stirring the mixture at 80-150° C. for 0.1-2 hr to create a molten lactam solvent from the lactam solvent and to fully dissolve or disperse the pyrolyzable precursor in the molten lactam solvent;
- performing pyrolysis on the molten lactam solvent by raising the temperature to 100˜270° C. for 0.1-20 hr whereby a pyrolysis product is formed;
- washing the pyrolysis product with absolute alcohol;
- and
- drying the washed pyrolysis product to obtain synthesized nanomaterials,
- wherein the pyrolyzable precursor is selected from soluble inorganic salts pyrolyzable in solvent at a temperature of no higher than 280° C. or from metal organics pyrolyzable in solvent at a temperature of no higher than 280° C.,
- wherein the lactam contained in the lactam solvent is one or more of the substances selected from cyclic amides or cyclic amide derivatives,
- wherein the general structural formula of the cyclic amide is:
- wherein the general structural formula of the cyclic amide derivatives is:
- wherein R is a substance selected from hydrogen, halogen, alkyl, hydroxy, alkoxy or acyl, and
- wherein the nanomaterials are substances containing inorganic particles having a particle size of greater than 1 nm and less than or equal to 100 nm;
- the content of the inorganic particles is no less than 0.01% of the substance;
- the inorganic particles are mixtures composed of one or more substances selected from hydroxides, oxides, sulfides, metals or inorganic salts.
11 more elements
Dependencies are inferred from the claim text.