CN110105759A - A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application - Google Patents
A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application Download PDFInfo
- Publication number
- CN110105759A CN110105759A CN201910428980.8A CN201910428980A CN110105759A CN 110105759 A CN110105759 A CN 110105759A CN 201910428980 A CN201910428980 A CN 201910428980A CN 110105759 A CN110105759 A CN 110105759A
- Authority
- CN
- China
- Prior art keywords
- titanium carbide
- aeroge
- preparation
- liquid
- polyamic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
Abstract
A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application, is related to aeroge and its preparation field.Polyamic acid and triethylamine are added separately in titanium carbide dispersion liquid, liquid nitrogen frozen is used after agitated dissolution, successively being made after vacuum freeze drying and high temperature imidization has tridimensional network, polyimides/titanium carbide the aeroge formed in polyimide matrix is dispersed in by titanium carbide nanometer sheet, there is the aeroge excellent mechanical property, flame retardancy, hydrophobicity and excellent organic liquid waste to be separated by solid-liquid separation performance.
Description
Technical field
The present invention relates to aeroge and its preparation fields, are specifically related to a kind of hydrophobic polyimide/titanium carbide airsetting
Glue, preparation method and application.
Background technique
With the rapid development of modern industry, all kinds of organic solvents have obtained a large amount of application, but resulting organic
Waste liquid is difficult to be effectively addressed, and causes huge threat to the life security of environment and the people, and beneficial in waste liquid
The un-extracted recycling of ingredient, also results in huge waste.
It generallys use the processing modes such as filtering or absorption to handle industrial organic waste liquid, but due to used filtering
That there are filter efficiencies is low for material and adsorbent material, adsorption rate is poor, the low disadvantage of selectivity, causes these processing methods can not be to having
Beneficial ingredient carries out high efficiente callback and realizes the recycling of organic solvent.
Aeroge has the characteristics that density is low, porosity is big and large specific surface area because of its unique tridimensional network,
The fields such as absorption, water-oil separating and particulate filter are with a wide range of applications.Polyimide aerogels have high mechanical strength,
High temperature resistant and the characteristics such as fire-retardant, have obtained extensive concern.Titanium carbide is a kind of novel two-dimentional transition metal carbide, is had
Excellent structural stability and electric conductivity is shown huge in the fields such as energy storage and power generation, water purification, gas separation, absorption
Application potential.But polyimides/titanium carbide aeroge preparation and its in organic liquid waste separation of solid and liquid field using fresh
It appears in the newspapers.
Summary of the invention
In order to overcome drawbacks described above existing in the prior art, it is sub- that one of the objects of the present invention is to provide a kind of polyamides
Amine/titanium carbide aeroge is dispersed in group in polyimide matrix by titanium carbide nanometer sheet with tridimensional network
At there is excellent mechanical property, flame retardancy, hydrophobicity and excellent organic liquid waste to be separated by solid-liquid separation performance for it.
Meanwhile the present invention also provides a kind of preparation methods of aeroge, specifically by polyamic acid and triethylamine point
It is not added in titanium carbide dispersion liquid, liquid nitrogen frozen is used after agitated dissolution, then in turn through vacuum freeze drying and high temperature
Polyimides/titanium carbide aeroge is made after imidization.
As the preferred technical solution of the present invention, in the preparation method of above-mentioned aeroge, titanium carbide nanometer sheet dispersion liquid
Concentration is 0.3~3.5mg/ml, and the mass ratio of polyamic acid and titanium carbide is 2.5~60:1, the matter of polyamic acid and triethylamine
Amount is than being 2:1.Mixed solution is transferred in mold, through liquid nitrogen frozen 30~after sixty minutes, it is done in vacuum freeze drier
Dry 96~144h finally carries out imidization in tube furnace under nitrogen protection.Imidization condition be from room temperature with 8 DEG C/
Sample segmentally heating is continuously kept the temperature 1 hour to 80 DEG C, 150 DEG C and 250 DEG C, and at every section by the rate of min, obtains polyamides Asia
Amine/titanium carbide aeroge.
Compared with prior art, beneficial effects of the present invention are shown:
1), polyimides prepared by the present invention/titanium carbide aeroge method is simple, can effectively control the shape of aeroge
Shape.
2), polyimides prepared by the present invention/titanium carbide aeroge needs not move through surface treatment, that is, has hydrophobicity.
3), there is polyimides prepared by the present invention/titanium carbide aeroge excellent organic liquid waste to be separated by solid-liquid separation performance.
Detailed description of the invention
Fig. 1 is polyimides/titanium carbide aeroge stereoscan photograph prepared by embodiment 1；
Fig. 2 is polyimides/titanium carbide aeroge contact angle test figure prepared by embodiment 2；
Fig. 3 is polyimides/titanium carbide aeroge separation organic liquid waste effect contrast figure prepared by embodiment 3.
Specific embodiment
The present invention is made with attached drawing with reference to embodiments and being discussed further.
Embodiment 1
The polyamic acid for weighing 50mg is added in the titanium carbide dispersion liquid that 6ml concentration is 3.2mg/ml, is then added
0.035ml triethylamine, stirring is until polyamic acid is completely dissolved.Wherein, the mass ratio of polyamic acid and titanium carbide is 2.6:1,
The mass ratio of polyamic acid and triethylamine is 2:1.Mixed solution is transferred in mold, is placed in liquid nitrogen and freezes 40 minutes, is turned
Move in vacuum freeze drier and handle 120 hours, sample is placed in tube furnace after taking-up, under nitrogen protection, with 8 DEG C/
Sample is continuously kept the temperature 1 hour in 80 DEG C, 150 DEG C and 250 DEG C difference by the heating rate of minute, and products therefrom is polyamides Asia
Amine/titanium carbide aeroge.
Fig. 1 is polyimides/titanium carbide aeroge scanning electron microscope (SEM) photograph prepared by embodiment 1.As can be seen from the figure sample
Product have tridimensional network.
Embodiment 2
The polyamic acid for weighing 400mg is added in the titanium carbide dispersion liquid that 6ml concentration is 3.2mg/ml, is then added
0.28ml triethylamine, stirring is until polyamic acid is completely dissolved.Wherein, the mass ratio of polyamic acid and titanium carbide is 20.8:1,
The mass ratio of polyamic acid and triethylamine is 2:1.Mixed solution is transferred in mold, is placed in liquid nitrogen and freezes 30 minutes, is turned
Move in vacuum freeze drier and handle 140 hours, sample is placed in tube furnace after taking-up, under nitrogen protection, with 8 DEG C/
Sample is continuously kept the temperature 1 hour in 80 DEG C, 150 DEG C and 250 DEG C difference by the heating rate of minute, and products therefrom is polyamides Asia
Amine/titanium carbide aeroge.
Fig. 2 is polyimides/titanium carbide aeroge contact angle figure prepared by embodiment 2.As can be seen from the figure sample
With excellent hydrophobicity, contact angle is 125.5 °.
Embodiment 3
The polyamic acid for weighing 100mg is added in the titanium carbide dispersion liquid that 6ml concentration is 0.3mg/ml, is then added
0.07ml triethylamine, stirring is until polyamic acid is completely dissolved.Wherein, the mass ratio of polyamic acid and titanium carbide is 55.6:1,
The mass ratio of polyamic acid and triethylamine is 2:1.Mixed solution is transferred in mold, is placed in liquid nitrogen and freezes 60 minutes, is turned
Move in vacuum freeze drier and handle 100 hours, sample is placed in tube furnace after taking-up, under nitrogen protection, with 8 DEG C/
Sample is continuously kept the temperature 1 hour in 80 DEG C, 150 DEG C and 250 DEG C difference by the heating rate of minute, and products therefrom is polyamides Asia
Amine/titanium carbide aeroge.
Fig. 3 is polyimides/titanium carbide aeroge separation organic liquid waste effect contrast figure prepared by embodiment 3.From figure
It can be seen that it is limpid thorough by organic solvent obtained after separation, show that the aeroge has excellent separating effect.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (8)
1. a kind of hydrophobic polyimide/titanium carbide aeroge, which is characterized in that there is tridimensional network, received by titanium carbide
Rice piece, which is dispersed in polyimide matrix, to be formed.
2. a kind of prepare polyimides as described in claim 1/titanium carbide aeroge method, which is characterized in that by polyamide
Acid and triethylamine are added separately in titanium carbide dispersion liquid, and liquid nitrogen frozen is used after agitated dissolution, cold then in turn through vacuum
Polyimides/titanium carbide aeroge is made after dry and high temperature imidization is lyophilized.
3. preparation method as claimed in claim 2, which is characterized in that the concentration of titanium carbide dispersion liquid is 0.3~3.5mg/ml.
4. preparation method as claimed in claim 2, which is characterized in that the mass ratio of polyamic acid and titanium carbide is 2.5~60:
1, the mass ratio of polyamic acid and triethylamine is 2:1.
5. preparation method as claimed in claim 2, which is characterized in that handled the time 30~60 minutes using liquid nitrogen frozen.
6. preparation method as claimed in claim 2, which is characterized in that sample is placed in freeze drier after liquid nitrogen frozen
96~144h of middle progress vacuum freeze drying.
7. preparation method as claimed in claim 2, which is characterized in that high temperature imidization condition is under nitrogen protection in tubular type
In furnace, sample segmentally heating is continuously kept the temperature 1 to 80 DEG C, 150 DEG C and 250 DEG C, and at every section from room temperature with the rate of 8 DEG C/min
Hour.
8. application of the hydrophobic polyimide as described in claim 1/titanium carbide aeroge in organic liquid waste separation of solid and liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910428980.8A CN110105759A (en) | 2019-05-22 | 2019-05-22 | A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910428980.8A CN110105759A (en) | 2019-05-22 | 2019-05-22 | A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110105759A true CN110105759A (en) | 2019-08-09 |
Family
ID=67491494
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910428980.8A Pending CN110105759A (en) | 2019-05-22 | 2019-05-22 | A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110105759A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021031306A1 (en) * | 2019-08-16 | 2021-02-25 | 武汉华星光电半导体显示技术有限公司 | Hydrophobic polyimide material, preparation method therefor and organic electroluminescent diode |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050131163A1 (en) * | 2002-07-22 | 2005-06-16 | Wendell Rhine | Aerogel metallic compositions |
| CN103467986A (en) * | 2013-10-01 | 2013-12-25 | 哈尔滨理工大学 | Nano titanium carbide/polyimide composite material modified by small organic molecules |
| CN107955167A (en) * | 2017-12-07 | 2018-04-24 | 黑龙江科技大学 | A kind of preparation method of high-performance polyimide titanium carbide nanosheet composite material |
-
2019
- 2019-05-22 CN CN201910428980.8A patent/CN110105759A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050131163A1 (en) * | 2002-07-22 | 2005-06-16 | Wendell Rhine | Aerogel metallic compositions |
| CN103467986A (en) * | 2013-10-01 | 2013-12-25 | 哈尔滨理工大学 | Nano titanium carbide/polyimide composite material modified by small organic molecules |
| CN107955167A (en) * | 2017-12-07 | 2018-04-24 | 黑龙江科技大学 | A kind of preparation method of high-performance polyimide titanium carbide nanosheet composite material |
Non-Patent Citations (2)
| Title |
|---|
| JI LIU ET AL.: "Multifunctional, Superelastic, and Lightweight MXene/Polyimide Aerogels", 《SMALL》 * |
| 二维导电纳米复合材料的制备及其性能研究: "刘骥", 《中国博士学位论文全文数据库.工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021031306A1 (en) * | 2019-08-16 | 2021-02-25 | 武汉华星光电半导体显示技术有限公司 | Hydrophobic polyimide material, preparation method therefor and organic electroluminescent diode |
| US11629229B2 (en) | 2019-08-16 | 2023-04-18 | Wuhan China Star Optoelectronics Semiconductor Display Technology Co., Ltd. | Hydrophobic polyimide material and preparation method thereof, and organic electroluminescence light emitting diode |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gokila et al. | Removal of the heavy metal ion chromiuim (VI) using Chitosan and Alginate nanocomposites | |
| Erhayem et al. | Isotherm, kinetic and thermodynamic studies for the sorption of mercury (II) onto activated carbon from Rosmarinus officinalis leaves | |
| Xu et al. | Magnetic solid-phase extraction of protein with deep eutectic solvent immobilized magnetic graphene oxide nanoparticles | |
| Ma et al. | Efficient extraction of trace organochlorine pesticides from environmental samples by a polyacrylonitrile electrospun nanofiber membrane modified with covalent organic framework | |
| CN104761749B (en) | Cellulose nano-fibrous hyperbranched method of modifying | |
| CN113477193B (en) | Preparation and application of sodium alginate-based aerogel | |
| CN110105759A (en) | A kind of hydrophobic polyimide/titanium carbide aeroge, preparation method and application | |
| CN102585221B (en) | Preparation method of porous polyimide microspheres | |
| Moon et al. | Use of curdlan and activated carbon composed adsorbents for heavy metal removal | |
| Zhou et al. | Green preparation and selective permeation of d-Tryptophan imprinted composite membrane for racemic tryptophan | |
| CN109012220A (en) | A kind of preparation of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane | |
| CN103055819B (en) | A kind of heavy metal absorbent and Synthesis and applications thereof | |
| CN101993056A (en) | Graphene-based porous macroscopic carbon material and preparation method thereof | |
| Wang et al. | PEG modified column MIL-101 (Cr)/PVA cryogel as a sorbent in stir bar solid phase extraction for determination of non-steroidal anti-inflammatory drugs in water samples | |
| CN109336100B (en) | Magnetic graphene with core-shell structure, application of magnetic graphene in pesticide residue detection and application method | |
| Liu et al. | Titanate nanotubes-embedded chitosan nanocomposite membranes with high isopropanol dehydration performance | |
| Pisharody et al. | Evaluation of adsorbents and eluents for application in virus concentration and adsorption-desorption isotherms for coliphages | |
| CN110559995A (en) | method for adsorbing polystyrene micro-plastic in water by using three-dimensional graphene | |
| CN105771935B (en) | One kind being used for adsorbed water body 2, porous polyimide/carbon nano tube compound material of 4- chlorophenesic acid | |
| Isa et al. | Different carbonization process of bamboo charcoal using Gigantochloa Albociliata | |
| Zhou et al. | Green preparation of d-tryptophan imprinted self-supported membrane for ultrahigh enantioseparation of racemic tryptophan | |
| Wang et al. | Desalination performance and fouling mechanism of capacitive deionization: effects of natural organic matter | |
| WO2016084945A1 (en) | Particles containing graphene oxide and/or graphite oxide as well as cellulose, composition for nucleic acid extraction, method for extracting nucleic acid, and method for recycling particles or composition for nucleic acid extraction | |
| CN114634229A (en) | Adsorption electrode material with porous microsphere morphology and preparation method and application thereof | |
| CN108905642A (en) | A kind of sodium lignosulfonate being preferentially dehydrated/sodium alginate blending infiltrating and vaporizing membrane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Lu Hongdian Inventor after: Wei Youhao Inventor after: Wang Yuying Inventor after: Wang Ningning Inventor after: Wang Hao Inventor before: Lu Hongdian Inventor before: Wang Yuying Inventor before: Wei Youhao Inventor before: Wang Ningning Inventor before: Wang Hao |
|
| CB03 | Change of inventor or designer information |