CN107902700B - A kind of preparation method of molybdenum disulfide aeroge - Google Patents

A kind of preparation method of molybdenum disulfide aeroge Download PDF

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CN107902700B
CN107902700B CN201711058035.0A CN201711058035A CN107902700B CN 107902700 B CN107902700 B CN 107902700B CN 201711058035 A CN201711058035 A CN 201711058035A CN 107902700 B CN107902700 B CN 107902700B
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aeroge
molybdenum disulfide
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CN107902700A (en
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金一铭
金亚妮
支明佳
洪樟连
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Zhejiang University ZJU
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    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
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Abstract

The invention discloses a kind of molybdenum disulfide (MoS2) aeroge preparation method.The preparation feature of the preparation method of the molybdenum disulfide aeroge includes: 1) with Ammonium Molybdate Tetrahydrate (molecular formula: (NH4)6Mo7O24·4H2It O) is molybdenum presoma；2) with dimercaptosuccinic acid (molecular formula: C4H6O4It S) is sulphur presoma；3) it takes water as a solvent；4) using polyacrylic acid as additive；5) using propylene oxide as gel promotor；6) molybdenum disulfide aeroge is obtained by Supercritical Drying Technology.The characteristics of preparation method of molybdenum disulfide aeroge of the invention is easy to get with raw material, simple process.The specific surface area of obtained molybdenum disulfide aeroge is in 200-500m2/ g, porosity can be applied to catalyst and catalyst carrier, lithium sulphur battery electrode material etc. between 99%-99.5%.

Description

A kind of preparation method of molybdenum disulfide aeroge
Technical field
The invention belongs to aerogel material preparation technical fields, and in particular to a kind of side for preparing molybdenum disulfide aeroge Method.
Technical background
Molybdenum disulfide has emphatically in terms of solid lubrication, micro-nano as a kind of important sulfide material The purposes wanted.Especially Recent study person have found molybdenum disulfide electrochemical energy storage performance with higher and electrolysis water The catalytic performance for producing hydrogen, can be used for high performance lithium ion battery and photoelectric chemical electrode material.
In the applications described above, it improves the specific surface area of molybdenum disulfide material and optimizes its pore structure, have for increasing There is the active surface site of electrochemical reaction, so that further promoting material property has extremely important effect.Airsetting glue material Material theoretically can satisfy above requirement as a kind of intrinsic material with bigger serface and controllable pore structure. If it is possible to molybdenum disulfide aerogel material be prepared using sol-gel technology, for further widening it in electrification Learn having great significance for energy storage and catalytic field.
In document report at home and abroad, at present about molybdenum sulfide (MoSx) aeroge preparation method can be mainly divided into Two classes: the first kind is in 2015, and directly with the metal salt of sulfur-bearing, (ingredient is (NH to Worsley et al.4)2(MS4), wherein M is Metal ion) be presoma, by freeze-drying and later period heat-treating methods in hydrogen, be prepared for MoS2And WS2Airsetting Glue, and have studied its as adsorbent and electrochemical catalysis produce hydrogen catalyst performance (ACS Nano, 2015,9,4698- 4705).Obtained molybdenum disulfide/graphene composite aerogel has high-specific surface area (323m2/ g) structure feature.Second class It is the oxidation-reduction method that the Kanatzidis research group of Northwestern Univ USA is invented, using I2(NH4)2(MoS4) directly It is reacted in formamide, wherein I2With Mo6+Redox reaction in situ occurs between ion and generates wet gel, then passes through dioxy Change carbon Supercritical Drying Technology and obtains MoSxAeroge (J.Am.Chem.Soc.2015,137,13943-13948).Both the above Method has been all made of ammonium thiomolybdate while being used as molybdenum source and sulphur source.In addition, Ma Jie et al. is in Chinese invention patent (application number 201610362513.6) in propose the preparation method of the aerogel carried molybdenum disulfide nano sheet hybrid material of three-dimensional grapheme, And report its application in dye sensitization solar battery electrode.Liu Tianxi etc. is in Chinese invention patent (application number 201510444473.5) in report a kind of molybdenum disulfide nano sheet/carbon aerogels hybrid material and preparation method thereof, and think Its electrode material that can be used for the new energy devices such as high performance catalyst material, lithium ion battery or solar battery.Lv Bin Et al. graphene aerogel/molybdenum disulfide/polyaniline is proposed in Chinese invention patent (application number 201510066222.8) Tri compound electrode material for super capacitor and preparation and application, by the way that molybdenum disulfide/polyaniline material is supported on graphene On aeroge, the aerogel composite with good chemical property is obtained.
It is summarized from above data it is found that the molybdenum disulfide aerogel material reported at present is using expensive and not Stable ammonium thiomolybdate is as presoma, or by supporting molybdenum disulfide on the aeroge of the carbon-based material prepared Form prepare composite aerogel.Currently, not being incorporated in overcritical in ethyl alcohol fluid directly with sol-gel process still Drying process prepares the report of molybdenum disulfide aeroge.
The present patent application discloses one kind using Ammonium Molybdate Tetrahydrate as molybdenum source, and dimercaptosuccinic acid is sulphur source, and polyacrylic acid is Additive, propylene oxide are gel promotor, prepare molybdenum disulfide wet gel using the method for sol-gel.
Summary of the invention
The purpose of the present invention is to provide one kind with Ammonium Molybdate Tetrahydrate, and dimercaptosuccinic acid and propylene oxide are colloidal sol- Gel reaction raw material, polyacrylic acid are additive, and the preparation method of disulphide aeroge is prepared in conjunction with supercritical drying.
A kind of preparation method of molybdenum disulfide aeroge, comprising the following steps:
(1) with Ammonium Molybdate Tetrahydrate (molecular formula: (NH4)6Mo7O24·4H2It O is) molybdenum presoma, water is solvent, configures molybdenum Sour ammonium/aqueous solution, wherein Mo6+Total concentration is 0.01M-1M.
(2) dimercaptosuccinic acid (C is configured4H6O4S)/aqueous solution is as sulphur presoma, the wherein concentration of dimercaptosuccinic acid 0.02M-2M；
(3) molybdenum precursor solution above-mentioned and dimercaptosuccinic acid solution are mixed, is calculated with volume ratio, molybdenum precursor solution And the ratio of dimercaptosuccinic acid solution is between 1:5-5:1.Meanwhile suitable polyacrylic acid is added as additive, additive amount It is calculated with volume ratio, the polyacrylic acid of addition is the 1-3% of overall solution volume；
(4) colloidal sol is configured, propylene oxide (molecular formula: C is added dropwise in the above solution3H6O it) is used as gel promotor, is added Volume be overall solution volume 20-50%, obtain colloidal sol.
(5) above-mentioned colloidal sol is put into closed mold, carries out gel reaction, obtain wet gel；
(6) above-mentioned wet gel is put into dehydrated alcohol and carries out aging process, the wet gel after obtaining aging；
(7) wet gel after above-mentioned aging is put into supercritical drying device, uses dehydrated alcohol for dried medium, risen Temperature keeps the temperature 60-120 minutes to 260 DEG C -280 DEG C, carries out supercritical drying, dry to complete to obtain molybdenum disulfide aeroge.
Wherein: sol gel reaction can carry out in 40 DEG C of -80 DEG C of environment, and ageing time may be configured as 3-7 days, super to face Heating rate may be configured as 2 DEG C/min in boundary's drying process.
The standby molybdenum disulfide aeroge of the present invention has raw material cheap, the material porosity height (99%- of acquisition 99.5%), large specific surface area (200-500m2/ g), the good characteristic such as microscopic structural units are controllable, can be used for catalyst and Catalyst carrier, lithium ion battery and electrode material of supercapacitor etc..
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of molybdenum disulfide aeroge prepared in embodiment 1.
Fig. 2 is the scanning electron microscope diagram piece of molybdenum disulfide aeroge prepared in embodiment 2.
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and examples.
Embodiment 1
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.25M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 25ml water being stirred mixed It closes, keeps dimercaptosuccinic acid soluble in water, wherein the concentration of dimercaptosuccinic acid in the solution is 0.5M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while is added dropwise 1ml's in the solution Polyacrylic acid.
5) propylene oxide of 15ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 3 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 7 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 260 DEG C, when autoclave pressure reaches 10MPa, system reaches overcritical State；It maintains 60 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.07g/cm3, specific surface area 360m2/ g, porosity It is 98.5%.
Embodiment 2
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.50M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 25ml water being stirred mixed It closes, keeps dimercaptosuccinic acid soluble in water, wherein the concentration of dimercaptosuccinic acid in the solution is 1.0M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while is added dropwise 1ml's in the solution Polyacrylic acid.
5) propylene oxide of 20ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 2 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 7 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 280 DEG C, when autoclave pressure reaches 15MPa, system reaches overcritical State；It maintains 120 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.08g/cm3, specific surface area 392m2/ g, porosity It is 98.3%.
Embodiment 3
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.50M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 25ml water being stirred mixed It closes, keeps dimercaptosuccinic acid soluble in water, wherein the concentration of dimercaptosuccinic acid in the solution is 1.0M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while 0.5ml is added dropwise in the solution Polyacrylic acid.
5) propylene oxide of 20ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 2 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 3 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 280 DEG C, when autoclave pressure reaches 15MPa, system reaches overcritical State；It maintains 120 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.08g/cm3, specific surface area 392m2/ g, porosity It is 98.3%.
Embodiment 4
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.10M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 2.5ml water being stirred mixed It closes, keeps dimercaptosuccinic acid soluble in water, wherein the concentration of dimercaptosuccinic acid in the solution is 2M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while 0.25ml is added dropwise in the solution Polyacrylic acid.
5) propylene oxide of 15ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 3 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 7 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 270 DEG C, when autoclave pressure reaches 12MPa, system reaches overcritical State；It maintains 90 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.10g/cm3, specific surface area 251m2/ g, porosity It is 97.9%.
Embodiment 5
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.01M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 12.5ml water being stirred Mixing, keeps dimercaptosuccinic acid soluble in water, and wherein the concentration of dimercaptosuccinic acid in the solution is 0.08M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while 0.5ml is added dropwise in the solution Polyacrylic acid.
5) propylene oxide of 10ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 3 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 7 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 275 DEG C, when autoclave pressure reaches 11MPa, system reaches overcritical State；It maintains 60 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.04g/cm3, specific surface area 251m2/ g, porosity It is 99.2%.
Embodiment 6
The molybdenum disulfide aeroge preparation method of the present embodiment successively comprises the following steps:
1) Ammonium Molybdate Tetrahydrate ((NH is taken4)6Mo7O24·4H2O), dimercaptosuccinic acid (C4H6O4S), polyacrylic acid ((C3H4O2)n, molecular weight~30,000), propylene oxide, water, dehydrated alcohol is reaction raw materials.
2) Ammonium Molybdate Tetrahydrate aqueous solution is configured: under the conditions of 25 DEG C of waters bath with thermostatic control, by Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O it) is stirred with 25ml water, makes Ammonium Molybdate Tetrahydrate ((NH4)6Mo7O24·4H2O) soluble in water, wherein Mo6 +The concentration of ion in the solution is 0.02M.
3) it configures dimercaptosuccinic acid solution: under the conditions of 25 DEG C of waters bath with thermostatic control, dimercaptosuccinic acid and 25ml water being stirred mixed It closes, keeps dimercaptosuccinic acid soluble in water, wherein the concentration of dimercaptosuccinic acid in the solution is 0.04M.
4) dimercaptosuccinic acid solution is added rapidly in Ammonium Molybdate Tetrahydrate solution, while 1.5ml is added dropwise in the solution Polyacrylic acid.
5) propylene oxide of 10ml is added dropwise in the above solution, forms colloidal sol.
6) colloidal sol being put into closed mold, gel is immersed in dehydrated alcohol after 1 hour and carries out aging by gel to be formed, Dehydrated alcohol dosage is 3 times of gel volume, and every the dehydrated alcohol of replacement in 24 hours, ageing time is 3 days.
7) it by after the Ageing solution removal in gel, is put into the autoclave of supercritical drying device, and nothing is added Water-ethanol.When the temperature of autoclave reaches 265 DEG C, when autoclave pressure reaches 11MPa, system reaches overcritical State；It maintains 60 minutes；After drying, the dehydrated alcohol in autoclave is released, molybdenum disulfide aeroge is obtained.
The molybdenum disulfide aeroge density for using the technique to prepare is 0.11g/cm3, specific surface area 302m2/ g, porosity It is 97.9%.

Claims (4)

1. a kind of preparation method of molybdenum disulfide aeroge, it is characterised in that comprise the steps of:
(1) using Ammonium Molybdate Tetrahydrate as molybdenum presoma, water is solvent, configures ammonium molybdate/aqueous solution, wherein Mo6+Concentration be 0.01M -1M；
(2) using dimercaptosuccinic acid as sulphur presoma, water is solvent, configures dimercaptosuccinic acid/aqueous solution, wherein dimercaptosuccinic acid Concentration is 0.02M -2M；
(3) molybdenum source presoma above-mentioned and sulphur presoma are mixed, is calculated with volume ratio, molybdenum precursor solution and dimercaptosuccinic acid The ratio of solution is between 1:1-5:1；
(4) polyacrylic acid is added in above-mentioned mixed solution as additive, additive amount is the 1-3% of overall solution volume；
(5) propylene oxide is added dropwise in the above solution as gel promotor, the volume of addition is the 20- of overall solution volume 50%, obtain colloidal sol；
(6) above-mentioned colloidal sol is put into closed mold, carries out sol gel reaction, obtain wet gel；
(7) above-mentioned wet gel is put into dehydrated alcohol and carries out aging process, the wet gel after obtaining aging；
(8) wet gel after above-mentioned aging is put into supercritical drying device, uses dehydrated alcohol for dried medium, is warming up to 260 DEG C -280 DEG C, 60-120 minutes are kept the temperature, carries out supercritical drying, it is dry to complete to obtain molybdenum disulfide aeroge.
2. the preparation method of molybdenum disulfide aeroge as described in claim 1, it is characterised in that sol gel reaction is 40 It is carried out in DEG C -80 DEG C of environment.
3. the preparation method of molybdenum disulfide aeroge as described in claim 1, it is characterised in that ageing time is 3-7 days.
4. the preparation method of molybdenum disulfide aeroge as described in claim 1, it is characterised in that risen in supercritical drying process Warm rate is 2 DEG C/min.
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CN106629852A (en) * 2016-12-10 2017-05-10 浙江大学 Preparation method of multilayer molybdenum disulfide material
US9725332B2 (en) * 2013-10-24 2017-08-08 Empire Technology Development Llc Transition metal dichalcogenide aerogels and methods of preparation and use

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US9725332B2 (en) * 2013-10-24 2017-08-08 Empire Technology Development Llc Transition metal dichalcogenide aerogels and methods of preparation and use
CN106629852A (en) * 2016-12-10 2017-05-10 浙江大学 Preparation method of multilayer molybdenum disulfide material

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