CN117326615B - Three-dimensional isomerism evaporator and preparation method and application thereof - Google Patents
Three-dimensional isomerism evaporator and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 117
- 230000008020 evaporation Effects 0.000 claims abstract description 106
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 98
- 150000003839 salts Chemical class 0.000 claims abstract description 80
- 230000005540 biological transmission Effects 0.000 claims abstract description 31
- 238000010146 3D printing Methods 0.000 claims abstract description 25
- 239000013535 sea water Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910021389 graphene Inorganic materials 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 14
- 238000010612 desalination reaction Methods 0.000 claims description 13
- 239000013505 freshwater Substances 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 8
- -1 graphene metal compound Chemical class 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 150000002736 metal compounds Chemical class 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000006317 isomerization reaction Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 2
- 229920001983 poloxamer Polymers 0.000 claims description 2
- 150000003609 titanium compounds Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 31
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 26
- 239000011780 sodium chloride Substances 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 10
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract description 8
- 238000012546 transfer Methods 0.000 abstract description 8
- 239000012267 brine Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000011033 desalting Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 32
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 11
- 238000012360 testing method Methods 0.000 description 8
- 230000004907 flux Effects 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- 238000009825 accumulation Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000031700 light absorption Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
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- 229960005070 ascorbic acid Drugs 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
- 235000020188 drinking water Nutrition 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000008520 organization Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 238000004299 exfoliation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
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- 230000008569 process Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Classifications
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- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Hydrology & Water Resources (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention discloses a three-dimensional isomerism evaporator and a preparation method and application thereof. The present solar sea water desalting evaporator can only operate at a lower evaporation rate, and the present invention prepares a new three-dimensional isomerism evaporator for the first time through the present 3D printing technology, and the new three-dimensional isomerism evaporator is composed of two parts, namely rGO-TiN and rGO-F127 serving as an evaporation interface and rGO serving as a water transmission passage, and the difference of the two parts in mass transfer capacity finally leads to stable water salt co-production. The evaporator of the invention can be 8.75 kg m ‑2 ·h ‑1 The evaporation rate of the catalyst is stabilized to fade 20 wt percent of NaCl, and the salt production rate reaches 1.02 kg.m ‑2 ·h ‑1 This work provides a new method for zero liquid discharge of solar driven high concentration brine (within 1 hour).
Description
Technical Field
The invention belongs to the sea water desalination technology, and particularly relates to a three-dimensional isomerism evaporator and a preparation method and application thereof.
Background
Desalination of sea water using abundant sea water or brackish water is widely used to solve the increasingly serious problem of water resource shortage. Reverse osmosis is currently the technology of sea water desalination with the largest installed capacity, and occupies 65% of water treatment capacity worldwide. However, reverse osmosis requires high energy consumption and large centralized equipment, and generates a large amount of high-concentration brine (> 7 wt% NaCl) during operation, and direct discharge to the environment causes ecological pollution, and a method for treating the high-concentration brine is urgently sought.
Solar-driven interface photo-thermal sea water desalination is an emerging technology which is eco-friendly, high in cost performance, sustainable and fast in development, and can efficiently convert solar energy into heat energy to produce fresh water from sea water through evaporation. In order to realize continuous operation of solar interface sea water desalination, most evaporators utilize a salt ion diffusion reflux mode to perform salt accumulation resistance. However, the diffusion of salt ions back into the evaporating water wastes mineral resources to some extent (adv. Mater. 2022, 34, 2203137; ACS Nano 2022, 16, 2, 2511-2520). Therefore, more and more evaporators achieve both fresh water and salt production by regulating the water transport path. However, these operations can only be operated at lower evaporation rates, and once the evaporation rate is increased, the salt-accumulating zone of these evaporators continues to spread to the water-producing zone, resulting in a decrease in evaporation performance (Energy environment. Sci.2019, 12, 1840; nano-Micro lett. 2022, 14, 10). Until now, it has been a challenge to develop evaporators that can achieve stable water and salt co-production at high evaporation rates.
Disclosure of Invention
The invention prepares a new three-dimensional isomerism evaporator for the first time through the prior 3D printing technology, and can be 8.75 kg m -2 ·h -1 The evaporation rate of the catalyst is stabilized to fade 20 wt percent of NaCl, and the salt production rate reaches 1.02 kg.m -2 ·h -1 . The isomerism evaporator is composed of two parts, namely rGO-TiN and rGO-F127 serving as an evaporation interface and rGO serving as a water transmission passage. Wherein rGO-TiN is used as a water producing region in the evaporation interface, and rGO-F127 is used as a salt producing region in the evaporation interface. The rGO-TiN can ensure that the evaporator has good photo-thermal capability, and the rGO-F127 not only blocks the aperture of the rGO, but also ensures that the rGO-TiN has certain hydrophilic capability, thereby being beneficial to the self-shedding of crystalline salt. The isomerised evaporator exhibited good performance over a long test period of 10 hoursGood stability and the collected fresh water meets the drinking water requirement of the world health organization. The work provides a new method for treating high-concentration brine and also provides a new strategy for designing the solar interface seawater desalination evaporator.
The invention adopts the following technical scheme:
a three-dimensional heterogeneous evaporator comprises a water transmission layer, and an evaporation water-producing layer and an evaporation salt-producing layer are arranged above the water transmission layer. Preferably, the evaporation salt-producing layer is located around the evaporation salt-producing layer.
In the invention, the water transmission layer is a graphene material layer; the evaporation water-producing layer is a graphene metal compound composite material layer; the evaporation salt-producing layer is a graphene polymer composite layer. Preferably, the graphene is reduced graphene oxide; in the graphene metal compound composite material layer, the mass ratio of graphene to metal compound is (2-5) to 1; in the graphene polymer composite material layer, the mass ratio of graphene to polymer is (1-3) to 1.
The invention discloses a preparation method of the three-dimensional isomerism evaporator, which comprises the following steps of preparing a water transmission layer, evaporating a water producing layer and evaporating a salt producing layer to obtain the three-dimensional isomerism evaporator. Further, a 3D printing is adopted to sequentially prepare a water transmission layer, an evaporation water-producing layer and an evaporation salt-producing layer, and then a three-dimensional isomerism evaporator is obtained through freeze drying and reduction treatment. Specifically, a three-dimensional heterogeneous evaporator water transmission passage layer is prepared by 3D printing through Pr-GO (partially reduced graphene oxide) ink; then preparing an evaporation water-producing layer of the three-dimensional isomerism evaporator by 3D printing through Pr-GO-metal compound ink above the water transmission channel layer of the three-dimensional isomerism evaporator; then preparing an evaporation salt-producing layer of the three-dimensional isomerism evaporator by 3D printing through Pr-GO-polymer ink around the evaporation water-producing layer of the three-dimensional isomerism evaporator; the evaporation water-producing layer of the three-dimensional isomerism evaporator and the evaporation salt-producing layer of the three-dimensional isomerism evaporator form an evaporation interface of the three-dimensional isomerism evaporator.
In the invention, partially reduced graphene oxide is a conventional product, and is mixed with a metal compound to obtain Pr-GO-metal compound ink; mixing the ink with a polymer to obtain Pr-GO-polymer ink. Preferably, the metal compound is a titanium compound; the polymer is pluronic; specifically, the metal compound is TiN, and the Pr-GO-metal compound ink is Pr-GO-TiN ink; the polymer is F127, and the Pr-GO-polymer ink is PrGO-F127 ink.
The invention discloses application of the three-dimensional isomerism evaporator in water evaporation or sea water desalination. In particular, the three-dimensional isomerism evaporator is applied to producing fresh water and salt, in particular to the application to simultaneously producing fresh water and salt.
The invention also discloses a method for desalting the sea water, which is characterized in that the three-dimensional isomerism evaporator is placed into the sea water, and the sea water is desalted by illumination, and particularly, the simultaneous fresh water and salt production are realized.
Fresh water is produced from seawater through evaporation, and in order to realize continuous operation of solar interface seawater desalination, the existing evaporator utilizes a salt ion diffusion reflux mode to perform salt accumulation resistance. However, the diffusion of salt ions back into the evaporating water wastes mineral resources to some extent. While more and more evaporators achieve both fresh water and salt production by regulating the water transport path, these operations can only be run at lower evaporation rates, once the evaporation rate is increased, the salt accumulation zone of these evaporators continues to spread to the water production zone, resulting in reduced evaporation performance. The invention prepares a new three-dimensional isomerism evaporator for the first time through the prior 3D printing technology, and can be 8.75 kg m -2 ·h -1 The evaporation rate of the catalyst is stabilized to fade 20 wt percent of NaCl, and the salt production rate reaches 1.02 kg.m -2 ·h -1 (within 1 hour). The isomerism evaporator is composed of two parts, namely rGO-TiN and rGO-F127 serving as an evaporation interface and rGO serving as a water transmission passage. Wherein rGO-TiN is used as a water producing region in the evaporation interface, and rGO-F127 is used as a salt producing region in the evaporation interface. The rGO-TiN can ensure that the evaporator has good photo-thermal capability, and the rGO-F127 not only blocks the aperture of the rGO, but also ensures that the rGO-TiN has certain hydrophilic capability, thereby being beneficial to the self-shedding of crystalline salt. The isomerised evaporator exhibits good stability over a long test period of 10 hours andthe collected fresh water meets the drinking water requirement of the world health organization. The work provides a new method for treating high-concentration brine and also provides a new strategy for designing the solar interface seawater desalination evaporator.
Drawings
FIG. 1 is a schematic diagram of a 3D isomerisation evaporator of the invention for efficient water and salt co-production.
FIG. 2 is a morphology characterization of rGO-TiN and rGO-F127. Wherein: (a) is SEM photograph of rGO-TiN, (b) is pore size distribution of rGO-TiN, (c) is SEM photograph of rGO-F127, and (d) is pore size distribution of rGO-F127.
Fig. 3 is a graph of water contact angle and salt mass transfer flux, wherein: (a) Contact angles of rGO-TiN and rGO-F127, and (b) mass transfer flux of rGO-TiN and rGO-F127.
Fig. 4 is a device characterization diagram, wherein: (a) A TEM pattern of rGO-TiN, and (b) XRD patterns of rGO-TiN and rGO.
Fig. 5 is a graph of light absorption for 2D rGO, 2D rGO-TiN and 3D rGO-TiN, wherein: (a) is reflectance, (b) is transmittance, and (c) is absorptivity and solar radiation.
Fig. 6 is a representation of device evaporation, wherein: (a) The evaporation rate and the salt production rate of the heterogeneous evaporators with different heights rGO-F127, and (b) the evaporation phenomenon of the heterogeneous evaporators with different heights rGO-F127.
Fig. 7 is a device evaporation performance graph, wherein: (a) At 1 kW.m for different evaporators -2 Evaporation rate and evaporation phenomenon, (b) evaporation rate, salt production rate and evaporation phenomenon of the isomerism evaporator under different light intensities.
Fig. 8 is a graph of device evaporation results, wherein: (a) At 3 kW.m for isomerisation evaporator -2 Evaporation rate and evaporation phenomenon within 10 hours at the light intensity of (b) is the XRD pattern of the harvested NaCl.
Fig. 9 shows salinity changes before and after sea water desalination at a solar energy interface.
Fig. 10 is a photograph of a 3D heterogeneous evaporator successfully prepared by the ink direct writing 3D printing technique of the present invention.
Detailed Description
The 3D isomerism evaporator is successfully prepared by an ink direct writing 3D printing technology (conventional method) and consists of an evaporation interface and a water transmission channel. In the evaporation interface, three-dimensional grid rGO-TiN is used as a water producing area, rGO-F127 is used as a salt producing area and is stuck to the periphery of the water producing area, and rGO is used as a water transmission passage. Due to the difference of rGO-TiN and rGO-F127 in mass transfer flux, 20 wt% NaCl is quickly desalted in a water producing area under the irradiation of sunlight, and salt crystals are crystallized on the surface of rGO-F127, so that efficient water and salt co-production is realized, and the method is shown in figure 1.
The raw materials used in the invention are existing products, and the specific experimental method and performance test are conventional technologies.
Flake graphite flake (XF 049, 50 mesh) was purchased from xfnno corporation. Concentrated H 2 SO 4 (98%), fuming nitric acid and hydrochloric acid are purchased from Zhongshan specialty Co, and used in a receiving mode. KMnO 4 、P 2 O 5 、H 2 O 2 (30%) solution, K 2 S 2 O 8 NaCl was purchased from national pharmaceutical chemicals Co. Ascorbic Acid (AA) was purchased from Sigma-aldrich. F127 was purchased from Millipore Sigma Co. TiN was purchased from Shanghai Michlin Biochemical technologies Co. Vacuum freeze dryer LABCONCO.
The microstructure and nanostructure of the samples were studied using a Zeiss SUPRA model 55 scanning electron microscope. Porosity and pore size distribution were measured using a mercury porosimeter (large tube Iv 9510). The wettability of the samples was characterized at room temperature using a contact angle meter (JY-82B Kruss DSA, dataPhysics OCA 20). The absorbance (a) was calculated using reflectance (R) and transmittance (T) (a=1-R-T) measured in a wavelength range of 300 to 2500 nm by ultraviolet-visible spectrometer Lambda 35 equipped with an integrating sphere (perkin elmer medical diagnostic product Shanghai limited). XRD patterns were recorded on pamalytical x-ray diffractometer. The salinity of the brine after photothermal desalination of the evaporator was measured by a conductivity meter (mertrer-tolido).
Test method of evaporation experiment: the solar energy-driven water evaporation performance test in the room was carried out using a xenon lamp (HSX-F300, beijing NBet) light source as a solar simulator. Optical power densitometer (CEL-NP 2000, beijing Zhongao optical technology)Limited) measured the intensity of the xenon lamp. Quartz weighing bottles were chosen as the container for the solar evaporation apparatus. Monitoring of mass change (m) using analytical balance (ORUS PR124ZH/E 1 ). In the test process, the indoor temperature is always 25 ℃, and the humidity is always 40-60%.
The calculation method of the evaporation rate comprises the following steps: v=m 1 /S·T
V is the evaporation rate (kg.m) -2 ·h -1 ），m 1 For mass change (kg), S is the evaporator area (m 2 ) T is the test time (h).
The calculation method of the salt production rate comprises the following steps: v=m 2 /S·T
V is the salt production rate (kg.m) -2 ·h -1 ），m 2 For the mass of the collected salt, the collected salt was dried at 60℃for 2 hours and then measured (kg), S being the area of the evaporator (m 2 ) T is the test time (h).
The aqueous GO solution was synthesized by a modified Hummers method according to conventional methods. Then, AA (80 mg.mL) -1 ) Aqueous solution and GO (2 mg. ML) -1 ) Mixing the water solutions in equal volume, and reacting for 30 min at 75 ℃; and then filtering and concentrating to prepare the partially reduced GO (pr-GO) ink.
PrGO-TiN ink is prepared by adding TiN into prGO-GO ink according to the mass ratio of prGO to TiN of 8:2.
PrGO-F127 ink is prepared by adding F127 (40 wt%) aqueous solution into prGO-GO ink according to the mass ratio of prGO to F127 of 7:3.
Before 3D printing, all inks were homogenized to allow uniform mixing, a conventional technique.
As prior art, 3D printers are retrofitted with industrial 3D robotic dispensing systems (fisher F5200N-type) with three-dimensional programmable patterning capability. And a high-precision pressure controller is adopted to provide controllable printing pressure, so that the ink is smoothly extruded. The experiment adopts a 3D printing nozzle (diameter 500 μm), the pressure is controlled to be 150-300 kPa, and the moving speed of the nozzle is 35 mm/s. The target pattern was printed onto a glass substrate in air at room temperature. After printing, the glass was freeze-dried (glass was peeled off at this time), and then heated for reduction, and finally, plasma treatment was performed. The invention discloses a preparation method of the three-dimensional isomerism evaporator, which comprises the following steps of preparing a water transmission layer, evaporating a water producing layer and evaporating a salt producing layer to obtain the three-dimensional isomerism evaporator. The specific size of the three-layer structure meets the requirements of the technical field of water evaporation, and preferably, the contact areas of the water transmission layer and the evaporation water producing layer are consistent, and the height of the evaporation salt producing layer is 0.1-1 times, preferably 0.1-0.8 times of the height of the evaporation water producing layer. The height of the water transport layer is 0.5 to 5 times, preferably 1 to 3 times, the height of the evaporation water-producing layer.
Example 1
Three-dimensional heterogeneous evaporator for 3D printing
Firstly, preparing a three-dimensional heterogeneous evaporator water transmission passage layer by 3D printing through pr-GO ink; then preparing an evaporation water-producing layer of the three-dimensional isomerism evaporator by 3D printing through PrGO-TiN ink above the water transmission path layer of the three-dimensional isomerism evaporator; then preparing an evaporation salt-producing layer of the three-dimensional isomerism evaporator by 3D printing through PrGO-F127 ink around the evaporation water-producing layer of the three-dimensional isomerism evaporator; the evaporation water-producing layer of the three-dimensional isomerism evaporator and the evaporation salt-producing layer of the three-dimensional isomerism evaporator form an evaporation interface of the three-dimensional isomerism evaporator, and the interval between grids of the evaporation interface is 2 mm; the mesh spacing of the water transport channels was 0.2cm. The water transmission layer is 1cm multiplied by 1cm, and the height is 1.15cm; the evaporation water-producing layer is 1cm multiplied by 1cm, and the height is 0.9 cm; the evaporation salt-producing layer is distributed around the evaporation salt-producing layer, namely four sides, and is defined as four pieces (the design sizes are consistent), each piece is 0.05 cm multiplied by 0.8 cm, and the height is 0.1cm, 0.3cm, 0.5cm or 0.7cm.
The ink was printed onto a glass substrate in air at room temperature. After printing was completed, 2h was frozen in a-80 ℃ refrigerator and then freeze-dried 12 h. Then, the sample was incubated at 1℃for min -1 The temperature rise rate of (2) is raised from room temperature to 200 ℃, and the heat reduction is carried out for 30 min. Finally, the sample is subjected to O for 3 min 2 And (5) plasma treatment.
Characterization of surface rG by SEMThe surface of O becomes rough and TiN is successfully loaded to the surface of rGO (a in fig. 2). In addition, the introduction of TiN does not have excessive influence on the pore size of rGO, and the density is 0.038 g cm -3 The rGO-TiN has a pore size of mainly 80-150 μm (b in FIG. 2), rGO-F127 has a pore size of mainly 5-15 μm, and a density of 0.151 g cm -3 (c in FIG. 2 and d in FIG. 2). The density is obtained by freeze-drying a printed solid block sample with two materials of ink, and dividing the weight by the volume.
Subsequently, characterization of the hydrophilic angle indicated that rGO-TiN was wettable by water within 31 ms and rGO-F127 was wettable by water within 296 ms (a in fig. 3). The mass transfer flux of rGO-TiN in 20 wt% NaCl aqueous solution is 1.78 kg.m -2 ·h -1 The mass transfer flux of rGO-F127 in 20 wt% NaCl aqueous solution is 0.1 kg.m -2 ·h -1 (b in FIG. 3). The difference of mass transfer flux is beneficial to the co-production of water and salt at the same time of the three-dimensional heterogeneous evaporator, so that the stable salt deposition evaporation resistance of the evaporator can be ensured, and the precipitation of salt crystals can be ensured. Printing an evaporation water-producing layer or an evaporation salt-producing layer sample by using the ink of the two materials, freeze-drying, heating for reduction, and finally performing plasma treatment to obtain rGO-TiN and rGO-F127 respectively.
TEM showed that TiN nanoparticles were uniformly supported on the wall of rGO (a in fig. 4). XRD showed that rGO had only one diffraction peak, and that after TiN was introduced, a significant diffraction peak of TiN appeared, again demonstrating the successful introduction of TiN (b in FIG. 4).
Fig. 5 is a graph of light absorption for 2D rGO, 2D rGO-TiN and 3D rGO-TiN, where (a) is reflectance, (b) is transmittance, and (c) is absorbance and solar radiation in fig. 5. The light absorption of two-dimensional planar rGO in the standard solar spectrum of 300-2500 nm is only 88.29%. After the TiN is introduced, the light absorption of the two-dimensional plane rGO-TiN is improved to 89.61 percent. When rGO-TiN is constructed into a three-dimensional grid structure, the light absorption is improved to 91.69 percent. The two-dimensional plane is the printed thickness of the evaporation layer of 0.1cm on the basis of the water transport path.
First, at 3 kW.m -2 For different height rGO-F127 (evaporating salt producing layer) three-dimensional isomerism evaporator, 20 wt% NaCl water is desalted under the light intensityThe evaporation properties of the solutions were tested. In the test time of 1 hour, along with the elevation of the height, the evaporation rate and the salt production rate of the three-dimensional isomerism evaporator are continuously improved, the highest evaporation rate is reached at 5 mm, and the evaporation rate reaches 8.75 kg m -2 ·h -1 The salt production rate reaches 1.02 kg m -2 ·h -1 (a) in fig. 6), and at a height of 7 mm, the evaporation rate and salt production rate of the three-dimensional isomerised evaporator were reduced. In addition, the evaporator achieved stable co-production of water salts over a test period of 1 hour, with salt only crystallizing on the surface of rGO-F127 (fig. 6 b).
The height of the evaporation water-producing layer in the following three-dimensional isomerism evaporator was 0.9cm, and the height of the salt-producing layer was 0.5cm.
Comparative example one 3D printed three dimensional rGO-TiN evaporator
Firstly, preparing a three-dimensional evaporator water transmission passage layer by 3D printing through pr-GO ink; then preparing an evaporation interface of the three-dimensional evaporator by 3D printing through PrGO-TiN ink above the water transmission path layer of the three-dimensional evaporator, wherein the spacing between grids of the evaporation interface is 2 mm; the mesh spacing of the water transport channels was 0.2cm.
The ink was printed onto a glass substrate in air at room temperature. After printing was completed, 2h was frozen in a-80 ℃ refrigerator and then freeze-dried 12 h. Then, the sample was heated from room temperature to 200℃at a heating rate of 1℃per minute, and thermally reduced for 30 minutes. Finally, for a size of 1.1X1.1 cm 2 (height of water transport layer was 1.15cm; height of evaporating water-generating layer was 0.9. 0.9 cm) for 3 min of O 2 And (5) performing plasma treatment to obtain the three-dimensional rGO-TiN evaporator.
Control example two 3D printing three-dimensional rGO-F127 evaporator
Firstly, preparing a three-dimensional evaporator water transmission passage layer by 3D printing through pr-GO ink; then preparing an evaporation interface of the three-dimensional evaporator by 3D printing through PrGO-F127 ink above the water transmission path layer of the three-dimensional evaporator, wherein the spacing between grids of the evaporation interface is 2 mm; the mesh spacing of the water transport channels was 0.2cm.
At room temperature, the ink is in airPrinted onto a glass substrate. After printing was completed, 2h was frozen in a-80 ℃ refrigerator and then freeze-dried 12 h. Then, the sample was incubated at 1℃for min -1 The temperature rise rate of (2) is raised from room temperature to 200 ℃, and the heat reduction is carried out for 30 min. Finally, for a size of 1.1X1.1 cm 2 (height of water transport layer 1.15cm; height of evaporating salt-generating layer 0.9. 0.9 cm) for 3 min of O 2 And (3) carrying out plasma pretreatment to obtain the three-dimensional rGO-F127 evaporator.
Example two
At 1 kW.m -2 The three-dimensional rGO-TiN evaporator and the three-dimensional isomerism evaporator can stably fade 20 wt percent NaCl aqueous solution under the light intensity, and the evaporation rates respectively reach 2.92 kg.m -2 ·h -1 And 2.95 kg m -2 ·h -1 Salt crystallization did not occur in the rGO-TiN evaporator, whereas the salt of the isomerising evaporator crystallized only on rGO-F127. With the progress of time, the evaporation rate of the rGO-F127 evaporator is continuously reduced, and the evaporation rate after 150min is only 2.24 kg m -2 ·h -1 (a) in FIG. 7), the illustration is a photograph after 150 min. In summary, the heterogeneous evaporator combines the advantages of various evaporators, the evaporation rate and the salt production rate of the heterogeneous evaporator are continuously improved along with the increase of the light intensity, and the salt production area does not spread to the water production area, so that stable water and salt co-production (b in fig. 7) is realized, and the picture is a photograph after 60 minutes.
The three-dimensional isomerism evaporator can realize stable water and salt co-production for 20 wt% NaCl water solution in a long-time test within 10 hours. In addition, the crystalline salt realizes self-shedding in a salt production area, the isomerism evaporator is regenerated after self-shedding, and the salt production rate within 10 hours reaches 1.48 kg m -2 ·h -1 (a in FIG. 8). XRD of the collected NaCl showed no diffraction peaks of other materials due to the effect of salt crystallization from exfoliation (b in fig. 8). The salt on the three-dimensional rGO-F127 evaporator cannot self-fall off.
In addition, the collected fresh water also meets the drinking water requirements of the world health organization (fig. 9).
Compared with the performance of the prior work, the invention has obvious technical progress no matter the salt accumulation resistance rate of 20 wt percent NaCl is compared with the salt production rate.
The existing evaporators can simultaneously realize fresh water and salt production by regulating and controlling a water transmission path, but practical experiments show that the operations can only be operated at a lower evaporation rate, and once the evaporation rate is increased, the salt accumulation areas of the evaporators can continuously spread to a water production area, so that evaporation performance is reduced. The 3D isomerism evaporator is successfully prepared by an ink direct-writing 3D printing technology (conventional method), and consists of an evaporation interface and a water transmission path, and a real object photo of an embodiment is shown in fig. 10. In the evaporation interface, three-dimensional grid rGO-TiN is used as a water producing area, rGO-F127 is used as a salt producing area and is stuck to the periphery of the water producing area, and rGO is used as a water transmission passage. Due to the difference of rGO-TiN and rGO-F127 in mass transfer flux, 20 wt% NaCl is quickly desalted in a water producing area under the irradiation of sunlight, and salt crystals are crystallized on the surface of rGO-F127, so that efficient water and salt co-production is realized.
Claims (9)
1. The three-dimensional heterogeneous evaporator comprises a water transmission layer and is characterized in that an evaporation water-producing layer and an evaporation salt-producing layer are arranged above the water transmission layer; the water transmission layer is a graphene material layer; the evaporation water-producing layer is a graphene metal compound composite material layer; the evaporation salt-producing layer is a graphene polymer composite material layer; the evaporation salt-producing layer is positioned around the evaporation salt-producing layer.
2. The three-dimensional isomerism evaporator according to claim 1, characterized in that the metal compound is a titanium compound; the polymer is pluronic.
3. The three-dimensional heterogeneous evaporator of claim 1, wherein the graphene material layer is a reduced graphene oxide layer; in the graphene metal compound composite material layer, the mass ratio of graphene to metal compound is (2-5) to 1; in the graphene polymer composite material layer, the mass ratio of graphene to polymer is (1-3) to 1.
4. The method for preparing the three-dimensional isomerism evaporator of claim 1, comprising the steps of preparing a water transmission layer, evaporating a water producing layer and evaporating a salt producing layer to obtain the three-dimensional isomerism evaporator.
5. The method for preparing a three-dimensional isomerism evaporator according to claim 4, comprising the steps of preparing a water transmission layer, an evaporation water-producing layer and an evaporation salt-producing layer in sequence by adopting 3D printing, and then performing freeze drying and reduction treatment to obtain the three-dimensional isomerism evaporator.
6. The method for preparing the three-dimensional heterogeneous evaporator according to claim 5, which is characterized by comprising the following steps of preparing a three-dimensional heterogeneous evaporator water transmission passage layer by 3D printing with Pr-GO ink; then preparing an evaporation water-producing layer of the three-dimensional isomerism evaporator by 3D printing through PrGO-metal compound ink above the water transmission channel layer of the three-dimensional isomerism evaporator; then preparing an evaporation salt-producing layer of the three-dimensional isomerism evaporator by 3D printing through PrGO-polymer ink around the evaporation water-producing layer of the three-dimensional isomerism evaporator; the evaporation water-producing layer of the three-dimensional isomerism evaporator and the evaporation salt-producing layer of the three-dimensional isomerism evaporator form an evaporation interface of the three-dimensional isomerism evaporator.
7. Use of the three-dimensional isomerisation evaporator of claim 1 for water evaporation or for sea water desalination.
8. The use of the three-dimensional isomerism evaporator of claim 1 for producing fresh water and salt.
9. A method for desalinating sea water, which is characterized in that the three-dimensional isomerism evaporator of claim 1 is placed into sea water, and illumination is carried out to realize sea water desalination.
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