CN105617956A - Molybdenum disulfide nanosheet/polyimide based composite aerogel and preparation method thereof - Google Patents
Molybdenum disulfide nanosheet/polyimide based composite aerogel and preparation method thereof Download PDFInfo
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- CN105617956A CN105617956A CN201610059510.5A CN201610059510A CN105617956A CN 105617956 A CN105617956 A CN 105617956A CN 201610059510 A CN201610059510 A CN 201610059510A CN 105617956 A CN105617956 A CN 105617956A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention belongs to the technical field of aerogel and particularly relates to molybdenum disulfide nanosheet/polyimide based composite aerogel and a preparation method thereof. The composite aerogel is prepared by compounding molybdenum disulfide nanosheets with good water dispersibility, prepared by a solvothermal method, with polyimide, and from molybdenum salt, sulfosalt and one or more of water-soluble polyimide precursor, and polyamide acid. The preparation process comprises the steps of preparing molybdenum disulfide nanosheets with good water dispersibility by the one-step solvothermal method, compounding the molybdenum disulfide nanosheets with polyamide acid, and performing sol-gel preparation, freezing-drying and amidation to obtain the molybdenum disulfide nanosheet/polyimide based composite aerogel. The composite aerogel has the characteristics that internal pores are uniformly distributed and the limit oxygen index is obviously higher than relative performance of macromolecule based aerogel in other documents or patents, and thus the composite aerogel can be taken as an ideal flame retardant material, heat insulation material and noise reduced material.
Description
Technical field
The invention belongs to aeroge technical field, be specifically related to a kind of polymer-based composite aerogel and preparation method thereof.
Background technology
Polymer aerogel is a kind of porous light-weight material with three-dimensional net structure, has that cost is low, easy-formation, porosity high (80 ~ 99.8%) and a specific surface area (200 ~ 1000m greatly2g-1) etc. advantage. The loose structure of its uniqueness makes polymer aerogel have broad application prospects in heat insulation, fire-retardant, sound insulation etc. Current polymer aerogel generally with polyvinyl alcohol, phenolic macromolecular material for matrix, nanoclay (such as montmorillonite, Kaolin and galapectite), carbon nanomaterial and SiO2Deng for filler, preparing through sol-gel process and special dry technology (such as Freeze Drying Technique, Supercritical Drying Technology). But, the problem such as these polymer-based aeroges ubiquity poor mechanical property (modulus of compressibility is generally 0.1 ~ 6.0MPa), heat decomposition temperature low (150 ~ 300 DEG C), fire resistance poor (limited oxygen index, LOI < 30), thus its application is restricted. Trace it to its cause, be by the mechanical property of macromolecule matrix material own is not high and heat decomposition temperature is low on the one hand; It is owing to Nano filling itself is easily reunited on the other hand, dispersion inequality in macromolecule matrix. Thus, the macromolecule matrix material how synthesizing excellent in mechanical performance, high decomposition temperature and high flame resistance and self agglomeration traits how solving Nano filling and scattering problem in the base thereof are scientific research and industrial key.
Polyimides, as a kind of conventional engineering plastics, because it has the mechanical property of excellence, hot property and fire resistance, is widely used in the every field of national economy. In the research that we are conventional (patent CN104355302A), it is successfully prepared the imido precursor-polyamic acid of water-soluble poly, and successfully prepares polyimide aerogels base carbon aerogels. Therefore, in the present invention, we select polyimides to be macromolecule matrix, prepare polyimide-based composite aerogel.
Molybdenum bisuphide is a kind of typical Transition-metal dichalcogenide, has the lamellar structure being similar to graphite, and lamella combines with covalent bond between inside, then interacts by weak Van der Waals force between lamella. And the molybdenum bisuphide of monolayer is a kind of " sandwich " structure, one layer of molybdenum atom of folder in the middle of two-layer sulphur atom, form sandwich structure, interlamellar spacing is about 0.65nm. Research shows, the molybdenum disulfide nano sheet of lamellar structure equally has good heat stability and gas barrier property with laminar nano clay and is widely used in the industries such as macromolecular material. But, molybdenum bisuphide bulk material is easily generated stacking due to respective interlayer strong interaction, it is difficult to dispersion. Therefore, in the present invention, utilize solvent thermal process, preparation can in water homodisperse molybdenum disulfide nano sheet, and it can be used as filler to join in polyimide-based aeroge, prepare heat stability height, molybdenum disulfide nano sheet/polyimide-based composite aerogel that fire resistance is good.
Summary of the invention
It is an object of the invention to provide molybdenum disulfide nano sheet/polyimide-based composite aerogel that a kind of preparation process is simple, preparation cost is cheap and preparation method thereof.
Molybdenum disulfide nano sheet provided by the invention/polyimide-based composite aerogel, it is prepared raw material composition and includes: molybdenum salt, sulfosalt and one or more water solublity polyimide precursor-polyamic acid; Its preparation process includes: prepare the good molybdenum disulfide nano sheet of water dispersible by a step solvent-thermal method; Molybdenum disulfide nano sheet and polyamic acid are carried out compound, is prepared into molybdenum disulfide nano sheet/polyimide-based composite aerogel by sol-gel, lyophilization and sub-amidatioon.
The preparation method of molybdenum disulfide nano sheet provided by the invention/polyimide-based composite aerogel, concretely comprises the following steps:
(1) molybdenum salt, sulfur source are dissolved in deionized water, obtain molybdenum saline solution;
(2) by obtained molybdenum saline solution by solvent thermal reaction, by deionized water, washing with alcohol 3-5 time, dry, obtain molybdenum disulfide nano sheet;
(3) being scattered in deionized water by obtained molybdenum disulfide nano sheet, supersound process obtains the molybdenum disulfide nano sheet aqueous dispersions of stable dispersion;
(4) prior art (as used the patent CN104355302A of inventor) is adopted to prepare polyimides water-soluble precursor-polyamic acid;
(5) prepared water-soluble polyamic acid is dissolved in the stable dispersions that step (3) obtains, by sol-gel process, obtains molybdenum disulfide nano sheet/polyamic acid hydrogel;
(6) it is solid by the freezing in refrigerator or liquid nitrogen of molybdenum disulfide nano sheet/polyamic acid hydrogel, then lyophilization in freezer dryer, obtain molybdenum disulfide nano sheet/polyamic acid aeroge;
(7) it is carried out the sub-amidatioon of heat by temperature programming by molybdenum disulfide nano sheet/polyamic acid aeroge, obtain molybdenum disulfide nano sheet/polyimide-based composite aerogel.
In step of the present invention (1), described molybdenum salt is selected from ammonium molybdate, sodium molybdate and ammonium thiomolybdate, it is preferable that amine molybdate; Described sulfosalt is selected from thiourea, thioacetamide and sodium sulfide, it is preferable that thiourea; The consumption of described molybdenum salt is 0.5-2mmol, and the consumption in sulfur source is 7-28mmol.
In step of the present invention (2), described solvent thermal reaction temperature is 200-230 DEG C, and the response time is 10-15h.
In step of the present invention (3), the solubility of described molybdenum disulfide nano sheet ranges for 0.5-9mgmL-1��
In step of the present invention (5), the mass ratio of described molybdenum disulfide nano sheet and water-soluble polyamic acid is 2:100-8:100, and the described sol-gel process time is 5-10h.
In step of the present invention (6), described sublimation drying is 36-48h.
In step of the present invention (7), the sub-amidated process of described heat is: obtained molybdenum disulfide nano sheet/polyamic acid aeroge controls temperature programming in tube furnace in nitrogen atmosphere, i.e. room temperature to 280-300 DEG C, insulation 1-5h, preferably segmented heating and thermal insulation, namely 80-100 DEG C, 180-200 DEG C and 280-300 DEG C is incubated 0.5 to 2h respectively.
Using sedimentation experiment, x-ray diffractometer, scanning electron microscope (SEM), thermogravimetric analyzer (TGA) and oxygen index instrument to characterize the molybdenum disulfide nano sheet/structure and morphology of polyimide-based composite aerogel, thermal stability and the fire resistance that the present invention obtains, its result is as follows:
(1) sedimentation experiment test (accompanying drawing 1A) result shows: the present invention, by the molybdenum disulfide nano sheet prepared by solvent-thermal method, can be stably dispersed in deionized water after supersound process. By sol-gel process, molybdenum disulfide nano sheet/polyamic acid can form stable hydrogel (accompanying drawing 1B). By the sub-amidatioon of heat, molybdenum disulfide nano sheet/polyimides composite aerogel (accompanying drawing 1C) can be prepared;
(2) XRD test result (accompanying drawing 2) shows, the present invention is by actually molybdenum bisuphide really prepared by solvent-thermal method, it is in 2 ��=14.2 ��, 33.8 �� and 59.3 �� all have stronger diffraction maximum, correspond respectively to (002), (100) and (110) crystal face of molybdenum bisuphide, meanwhile, all there is more weak diffraction maximum 2 ��=39.8 �� and 69.8 ��, correspond respectively to (103) and (201) crystal face of molybdenum bisuphide;
(3) test result (accompanying drawing 3) of SEM shows: pure polyimide aerogels and molybdenum disulfide nano sheet/polyimides composite aerogel prepared by the present invention are porous material, its inner void size is homogeneous, but after addition molybdenum disulfide nano sheet, the hole dimension of molybdenum disulfide nano sheet/polyimides composite aerogel is less than the hole dimension of pure polyimide aerogels, and quantity is many. More than these, little hole is conducive to the obstruct to oxygen, therefore can improve the fire resistance of composite aerogel;
(4) TGA test result (accompanying drawing 4) shows, pure polyimide aerogels and molybdenum disulfide nano sheet/polyimides composite aerogel prepared by the present invention are respectively provided with higher heat stability, and when its weight loss is 95%, its heat decomposition temperature is above 575 DEG C. Show additionally, TGA tests data, after adding molybdenum disulfide nano sheet, it is possible to improve the heat stability of polyimide aerogels. Be embodied in, along with the increase of molybdenum disulfide nano sheet addition, when the thermal weight loss amount of material is 95%, the heat decomposition temperature of polyimide aerogels from improve 576.0 DEG C to 604.7 DEG C, namely pure polyimide aerogels, MoS2/PI-2��MoS2/ PI-5 and MoS2When the thermal weight loss of/PI-8 is 95%, its heat decomposition temperature respectively 576.0 DEG C, 580.7 DEG C, 595.2 DEG C and 604.7 DEG C;
(5) oxygen index (OI) result (subordinate list 1) is analyzed and is shown, pure polyimide aerogels and molybdenum disulfide nano sheet/polyimides composite aerogel prepared by the present invention are respectively provided with higher oxygen index (OI), and along with the increase of molybdenum disulfide nano sheet consumption, the oxygen index (OI) of composite is also gradually increased.
Compared with prior art, its remarkable advantage is as follows for the present invention:
(1) molybdenum disulfide nano sheet prepared in the present invention needs not move through other surface treatment, only ultrasonic just can evenly spread in deionized water. Additionally, the molybdenum disulfide nano sheet productivity prepared by the present invention is higher, can be mass (molybdenum disulfide nano sheet that the solvent thermal reaction of 30mL can produce more than 2g);
(2) the composite aerogel preparation process of the present invention is simple and environmentally-friendly, easily operated, is a kind of Green Chemistry preparation method. The preparation of the N doping cellulose base carbon aerogels in this present invention is only had only to high temperature cabonization, without time-consuming sol-gel process, relatively costly dry (supercritical carbon dioxide dries or lyophilization) process;
(3) stratified pieces layer material molybdenum bisuphide and engineering plastics polyimides are carried out compound effectively by the present invention, have prepared the composite aerogel of heat stability and the fire resistance with excellence.
Accompanying drawing explanation
Fig. 1: place the digital photograph (A) of 5h, molybdenum disulfide nano sheet/polyimide-based composite aquogel (B) and molybdenum disulfide nano sheet/polyimide-based composite aerogel (C) after molybdenum disulfide nano sheet supersound process prepared in the present invention.
Fig. 2: the XRD figure of the molybdenum disulfide nano sheet prepared by the present invention.
Fig. 3: polyimide aerogels (A-B) prepared in the present invention and molybdenum disulfide nano sheet/polyimide-based composite aerogel (C-D) low power and high power SEM are schemed.
Fig. 4: polyimide aerogels prepared in the present invention and the TGA curve of molybdenum disulfide nano sheet/polyimide-based composite aerogel.
Detailed description of the invention
The present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention below in conjunction with instantiation. In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various change or amendment by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1, the present embodiment comprises the following steps:
(1) the good molybdenum disulfide nano sheet of water dispersible is prepared. 1mmol Ammonium Molybdate Tetrahydrate and 14mmol thiourea are dissolved in 30mL deionized water, then this solution are transferred in 40mL water heating kettle, react 12h in 200 DEG C. After reaction terminates, with deionized water cyclic washing sample 3-5 time, dry. Then being disperseed in deionized water by dried molybdenum disulfide nano sheet, its concentration is 8mgmL-1��
(2) step patent CN104355302A with us of water-soluble polyamic acid is prepared.
(3) 8mgmL prepared of 2.5mL is taken-1Molybdenum disulfide nano sheet aqueous dispersions, add 8.5mL deionized water and 0.5g triethylamine, ultrasonic 0.5h. Being put into by 1g water-soluble polyamic acid fiber containing in the aqueous dispersions of the molybdenum disulfide nano sheet of triethylamine, stirring makes it dissolve, and is then placed 6h and completes sol-gel process. It is transferred in the container that diameter is 2cm, putting into and making its quick freeze in liquid nitrogen is solid, is finally putting in freezer dryer lyophilization 36h and can obtain molybdenum disulfide nano sheet and molybdenum disulfide nano sheet/polyamic acid aeroge that polyamic acid ratio is 2:100.
(4) obtained molybdenum disulfide nano sheet/polyamic acid aeroge is controlled in tube furnace in nitrogen atmosphere temperature programming, i.e. room temperature to 100 DEG C intensification 30min, be incubated 1h; 100 DEG C to 200 DEG C, intensification 30min, it is incubated 1h; 200 DEG C to 300 DEG C, intensification 30min, it is incubated 1h, molybdenum disulfide nano sheet/polyimide-based composite aerogel can be obtained, be denoted as MoS2/PI-2��
Embodiment 2, the present embodiment comprises the following steps:
Change the ratio of molybdenum disulfide nano sheet and polyamic acid into 5:100, namely take the 6.25mL 8mgmL prepared-1Molybdenum disulfide nano sheet aqueous dispersions, add 4.75mL deionized water and 0.5g triethylamine, ultrasonic 0.5h, all the other are with implementing 1, and final prepared molybdenum disulfide nano sheet/polyimide-based composite aerogel is denoted as MoS2/PI-5��
Embodiment 3, the present embodiment comprises the following steps:
Change the ratio of molybdenum disulfide nano sheet and polyamic acid into 8:100, namely take the 10mL 8mgmL prepared-1Molybdenum disulfide nano sheet aqueous dispersions, add 1mL deionized water and 0.5g triethylamine, ultrasonic 0.5h, all the other are with implementing 1, and final prepared molybdenum disulfide nano sheet/polyimide-based composite aerogel is denoted as MoS2/PI-8��
Embodiment 4, matched group is tested, and the present embodiment comprises the following steps:
The process prepare aeroge is not added with molybdenum disulfide nano sheet, prepares pure polyimide aerogels. Concretely comprising the following steps, take 11.5mL deionized water and 0.5g triethylamine, ultrasonic 0.5h, all the other are with implementing 1, final prepared polyimide aerogels note PI.
Polyimide aerogels prepared by the present embodiment, its sol-gel time is longer, and its inner void is than the hole of the polyimide-based aeroge after addition molybdenum disulfide nano sheet. In addition, its oxygen index (OI) and heat decomposition temperature all low than molybdenum disulfide nano sheet/polyimide-based aeroge, after addition molybdenum disulfide nano sheet is described, it is possible to improve the pore space structure of polyimide aerogels, improve fire resistance and the heat stability of polyimide aerogels.
The oxygen index (OI) (LOI) of table 1, molybdenum disulfide nano sheet/polyimide-based composite aerogel
��
Claims (10)
1. a preparation method for molybdenum disulfide nano sheet/polyimide-based composite aerogel, specifically comprises the following steps that
(1) molybdenum salt, sulfur source are dissolved in deionized water, obtain molybdenum saline solution;
(2) by obtained molybdenum saline solution by solvent thermal reaction, by deionized water, washing with alcohol 3-5 time, dry, obtain molybdenum disulfide nano sheet;
(3) being scattered in deionized water by obtained molybdenum disulfide nano sheet, supersound process obtains the molybdenum disulfide nano sheet aqueous dispersions of stable dispersion;
(4) polyimides water-soluble precursor-polyamic acid is prepared;
(5) prepared water-soluble polyamic acid is dissolved in the stable dispersions of step (3), by sol-gel process, obtains molybdenum disulfide nano sheet/polyamic acid hydrogel;
(6) it is solid by the freezing in refrigerator or liquid nitrogen of molybdenum disulfide nano sheet/polyamic acid hydrogel, then lyophilization in freezer dryer, obtain molybdenum disulfide nano sheet/polyamic acid aeroge;
(7) it is carried out the sub-amidatioon of heat by temperature programming by molybdenum disulfide nano sheet/polyamic acid aeroge, obtain molybdenum disulfide nano sheet/polyimide-based composite aerogel.
2. the preparation method of molybdenum disulfide nano sheet according to claim 1/polyimide-based composite aerogel, it is characterised in that the molybdenum salt described in step (1) is selected from ammonium molybdate, sodium molybdate and ammonium thiomolybdate; Described sulfosalt is selected from thiourea, thioacetamide and sodium sulfide; The consumption of described molybdenum salt is 0.5-2mmol, and the consumption in sulfur source is 7-28mmol.
3. the preparation method of molybdenum disulfide nano sheet according to claim 1 and 2/polyimide-based composite aerogel, it is characterised in that the solvent thermal reaction temperature described in step (2) is 200-230 DEG C, the response time is 10-15h.
4. the preparation method of molybdenum disulfide nano sheet according to claim 3/polyimide-based composite aerogel, it is characterised in that the solubility of the molybdenum disulfide nano sheet described in step (3) ranges for 0.5-9mgmL-1��
5. the preparation method of molybdenum disulfide nano sheet according to claim 4/polyimide-based composite aerogel, it is characterized in that the mass ratio of the molybdenum disulfide nano sheet described in step (5) and water-soluble polyamic acid is 2:100-8:100, the described sol-gel process time is 5-10h.
6. the preparation method of the molybdenum disulfide nano sheet/polyimide-based composite aerogel according to claim 1,2,4 or 5, it is characterised in that the sublimation drying described in step (6) is 36-48h.
7. the preparation method of the molybdenum disulfide nano sheet/polyimide-based composite aerogel according to claim 1,2,4 or 5, it is characterized in that the sub-amidation process of the heat described in step (7) is: obtained molybdenum disulfide nano sheet/polyamic acid aeroge is controlled in tube furnace in nitrogen atmosphere temperature programming, i.e. room temperature to 280-300 DEG C, is incubated 1-5h.
8. the preparation method of molybdenum disulfide nano sheet according to claim 7/polyimide-based composite aerogel, it is characterized in that the sub-amidation process of the heat described in step (7) is: obtained molybdenum disulfide nano sheet/polyamic acid aeroge controls temperature programming in tube furnace in nitrogen atmosphere, and namely 80-100 DEG C, 180-200 DEG C and 280-300 DEG C is incubated 0.5 to 2h respectively.
9. prepared molybdenum disulfide nano sheet/polyimide-based composite aerogel by the described preparation method of one of claim 1-8.
10. molybdenum disulfide nano sheet/polyimide-based composite aerogel as claimed in claim 9 is as the application of fire proofing, heat-barrier material and acoustic damping materials.
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| CN106629852A (en) * | 2016-12-10 | 2017-05-10 | 浙江大学 | Preparation method of multilayer molybdenum disulfide material |
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| CN106893323A (en) * | 2017-03-03 | 2017-06-27 | 江苏大学 | A kind of ultra-thin molybdenum disulfide nano sheet/Self-lubrication composite material of polyimide and preparation method thereof |
| CN108054359A (en) * | 2017-12-07 | 2018-05-18 | 同济大学 | A kind of preparation method of molybdenum disulfide hybrid material |
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| CN110240172A (en) * | 2019-07-26 | 2019-09-17 | 沈阳工业大学 | A kind of method that gas phase removing prepares montmorillonite-based nano piece |
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| CN106430310B (en) * | 2016-11-30 | 2018-03-23 | 浙江理工大学 | A kind of preparation method of hollow ball-shape molybdenum disulfide |
| CN106629852A (en) * | 2016-12-10 | 2017-05-10 | 浙江大学 | Preparation method of multilayer molybdenum disulfide material |
| CN106629852B (en) * | 2016-12-10 | 2017-12-12 | 浙江大学 | The preparation method of multilayer molybdenum disulfide material |
| CN106633170A (en) * | 2016-12-14 | 2017-05-10 | 复旦大学 | Nano-diamond filled polyimide based compound aerogel material and preparation method thereof |
| CN106893323A (en) * | 2017-03-03 | 2017-06-27 | 江苏大学 | A kind of ultra-thin molybdenum disulfide nano sheet/Self-lubrication composite material of polyimide and preparation method thereof |
| CN108054359A (en) * | 2017-12-07 | 2018-05-18 | 同济大学 | A kind of preparation method of molybdenum disulfide hybrid material |
| CN108054359B (en) * | 2017-12-07 | 2020-06-26 | 同济大学 | Preparation method of molybdenum disulfide intercalation material |
| CN109179372A (en) * | 2018-10-26 | 2019-01-11 | 华南理工大学 | A kind of high-performance biology cellulose carbon aerogels and its preparation method and application |
| CN109610024A (en) * | 2018-11-20 | 2019-04-12 | 华南理工大学 | A kind of cellulose-molybdenum disulfide aeroge composite fibre and its preparation method and application |
| CN110240172A (en) * | 2019-07-26 | 2019-09-17 | 沈阳工业大学 | A kind of method that gas phase removing prepares montmorillonite-based nano piece |
| CN110240172B (en) * | 2019-07-26 | 2022-06-24 | 沈阳工业大学 | Method for preparing montmorillonite nanosheet through gas phase stripping |
| CN113061286A (en) * | 2021-03-19 | 2021-07-02 | 华南理工大学 | Multifunctional flame-retardant polyimide aerogel and preparation method and application thereof |
| CN114950353A (en) * | 2021-11-05 | 2022-08-30 | 广西师范大学 | High-activity-site molybdenum disulfide/carbon nanofiber aerogel adsorbent and preparation method thereof |
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