CN115651274B - Preparation method of clay-based composite hydrogel for solar seawater desalination - Google Patents
Preparation method of clay-based composite hydrogel for solar seawater desalination Download PDFInfo
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- CN115651274B CN115651274B CN202211342135.7A CN202211342135A CN115651274B CN 115651274 B CN115651274 B CN 115651274B CN 202211342135 A CN202211342135 A CN 202211342135A CN 115651274 B CN115651274 B CN 115651274B
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 78
- 239000004927 clay Substances 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000010612 desalination reaction Methods 0.000 title claims abstract description 10
- 239000013535 sea water Substances 0.000 title claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 49
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000499 gel Substances 0.000 claims abstract description 41
- 239000000661 sodium alginate Substances 0.000 claims abstract description 41
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 41
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 41
- 238000010257 thawing Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- PHOQVHQSTUBQQK-SQOUGZDYSA-N D-glucono-1,5-lactone Chemical compound OC[C@H]1OC(=O)[C@H](O)[C@@H](O)[C@@H]1O PHOQVHQSTUBQQK-SQOUGZDYSA-N 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 8
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 7
- 230000008014 freezing Effects 0.000 claims description 40
- 238000007710 freezing Methods 0.000 claims description 40
- 229960000892 attapulgite Drugs 0.000 claims description 18
- 229910052625 palygorskite Inorganic materials 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 11
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 11
- 239000006229 carbon black Substances 0.000 claims description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000001506 calcium phosphate Substances 0.000 claims description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 3
- 235000011010 calcium phosphates Nutrition 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004113 Sepiolite Substances 0.000 claims description 2
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 claims description 2
- 235000010261 calcium sulphite Nutrition 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229910003472 fullerene Inorganic materials 0.000 claims description 2
- 229910052900 illite Inorganic materials 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- -1 mxene Chemical compound 0.000 claims description 2
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 2
- 229910052624 sepiolite Inorganic materials 0.000 claims description 2
- 235000019355 sepiolite Nutrition 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 57
- 238000001704 evaporation Methods 0.000 abstract description 31
- 230000008020 evaporation Effects 0.000 abstract description 31
- 239000011148 porous material Substances 0.000 abstract description 29
- 230000008569 process Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 9
- 230000031700 light absorption Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012267 brine Substances 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 235000012209 glucono delta-lactone Nutrition 0.000 description 12
- 229960003681 gluconolactone Drugs 0.000 description 12
- 238000005259 measurement Methods 0.000 description 12
- 239000013505 freshwater Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
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- 230000009286 beneficial effect Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 230000004807 localization Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
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- 230000006835 compression Effects 0.000 description 1
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- 229920000547 conjugated polymer Polymers 0.000 description 1
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- 238000007791 dehumidification Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
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Classifications
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- 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
-
- 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
- Y02A20/138—Water desalination using renewable energy
- Y02A20/142—Solar thermal; Photovoltaics
-
- 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
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention relates to the field of hydrogel material preparation, and discloses a preparation method of clay-based solar composite hydrogel for solar sea water desalination, which comprises the following specific steps: dissolving sodium alginate in aqueous solution, adding a proper amount of clay and carbon-based material to disperse uniformly, slowly adding calcium salt, stirring uniformly, adding glucolactone aqueous solution or powder, stirring uniformly continuously, pouring into a mold, and standing for gel; and (3) performing directional freeze thawing on the aged gel for multiple times to obtain the clay-based hydrogel with the vertical pore canal structure. The clay-based composite hydrogel prepared by the method has the advantages of simple process, green and pollution-free raw materials, low price and contribution to industrial production. The obtained clay-based composite hydrogel has good light absorption efficiency, good water evaporation efficiency, rich pore channel structures and good hydrophilicity, and can be used in the fields of sewage treatment, sea water desalination, brine concentration and the like.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a preparation method of clay-based composite hydrogel for solar sea water desalination.
Background
Fresh water is an indispensable resource for human beings and all ecosystems to survive, and plays a vital role. In the case of ever-increasing population, environmental changes and pollution of fresh water resources, how to achieve safe fresh water supply is a new challenge. The available water resource of the earth only accounts for 3% of the total water quantity, and in the few fresh water resources, more than 70% of the fresh water resources are frozen in ice covers of south poles and north poles, and less than 1% of the fresh water resources can be utilized by human beings. In addition, global fresh water resources are not only in shortage but also are extremely unbalanced in regional distribution. By 2025, 30 million people in the world are expected to face water shortage, and 40 countries and regions are severely deficient in fresh water.
To solve this problem, various seawater and freshwater technologies are endlessly layered. Such as Reverse Osmosis (RO), multi-effect sea water desalination (MED), thermal Vapor Compression (TVC), humidification Dehumidification (HDH), hybrid systems, and multi-stage flash (MSF). However, these techniques are difficult to be widely popularized and applied due to the expensive running cost. Solar energy is an almost inexhaustible renewable resource in nature, and the solar energy driven freshwater technology is superior to other technologies with low cost and high photo-thermal conversion efficiency, and becomes one of effective ways for relieving the shortage of water resources, such as (CN 112108084A, CN 113735208A) but under natural light (the solar intensity is less than or equal to 1 KW.m) -2 The low utilization efficiency of sunlight leads to the fact that the existing solar water purification technology cannot reach the commercial expectation yet. In order to improve the evaporation efficiency, the current work mainly focuses on the following three problems: (1) the photo-thermal conversion efficiency is improved; (2) continuously and stably supplying water in the evaporation process; (3) anti-theft deviceSalting out is stopped to block the pore canal. Based on the above requirements, solar evaporation new materials such as plasma nanoparticles, conjugated polymers, carbon-based materials and the like, and solar evaporation devices such as thermal localization films, bionic nanostructures, mushroom bionics and the like are highly valued and rapidly developed.
The hydrogel is a three-dimensional network structure formed by mutually stacking and polymerizing polymer long chains or colloid particles with water as a medium, and can keep a large amount of water without dissolving. Because of their highly tunable physicochemical properties, they have gained wide attention and application in the fields of inclusive artificial organizations, sanitary products, contact lenses, drug delivery, and agricultural fertilizers. Hydrogels, one of the most important materials in water evaporation and desalination processes, have higher water evaporation rates and efficiencies due to thermal localization at the air-water interface; the weak interactions between water molecules and polymer chains can form intermediate water, thereby reducing the energy requirements for water vaporization. Hu et al prepared a vapor rate of 1.582 kg m -2 h -1 Is a double layer cellulose hydrogel (Carbohydrate Polymer,2020, 243, 116480). Zhao et al utilized a one-step crosslinking process to prepare a novel hydrogel-based solar evaporator. Sodium alginate and PEDOT-PSS composite hydrogel are used as a photo-thermal layer to realize 1.23 kg.m -2 h -1 Is described (Desalinatio, 2020, 482, 114385). Song et al prepared a polymer having a physical/chemical cross-linking of 1.41 kg.m -2 h -1 High content attapulgite aerogel with evaporation rate (Journal of Materials Chemistry A,2021,9, 23117-23126). But in practical application, the problems of unstable salt deposition and evaporation performance are faced.
Disclosure of Invention
The invention aims to: aiming at the problems existing in the prior art, the invention provides a preparation method of clay-based composite hydrogel for solar sea water desalination, which is characterized in that a super-hydrophilic water delivery channel is constructed based on the characteristics of clay materials, and the clay-based hydrogel with a vertical micro-pore structure is obtained by utilizing directional freezing to adjust the pore diameter and performing multiple directional freezing and thawing. The clay-based composite hydrogel prepared by the invention has good light absorption efficiency and water evaporation efficiency,rich pore canal structure and good hydrophilicity, and the evaporation rate can reach 3.78 kg.m at maximum -2 h -1 。
The technical scheme is as follows: the invention provides a preparation method of clay-based composite hydrogel for solar sea water desalination, which comprises the following steps:
adding sodium alginate into the aqueous solution to dissolve to obtain an aqueous sodium alginate solution, and adding clay and a carbon-based material into the aqueous sodium alginate solution to mix;
wherein the addition amount of the sodium alginate in the sodium alginate aqueous solution is 0.5-4wt% and the addition amount of the clay in the sodium alginate aqueous solution is 0-15wt%;
step (2), slowly adding calcium salt into the mixed solution in the step (1), and stirring to obtain a mixed suspension;
step (3), adding glucolactone into the mixed suspension in the step (2), uniformly stirring, pouring into a mould, and standing for gel;
step (4), aging the gel, and performing directional freeze thawing for multiple times to obtain clay-based composite hydrogel; the mass ratio of the sodium alginate to the clay in the clay-based composite hydrogel is 1:1-1:4.
Preferably, in the step (1), the clay is one or a combination of more than two of nano attapulgite, bentonite, kaolin, illite, diatomite or sepiolite.
Preferably, in the step (1), the addition amount of the carbon-based material in the sodium alginate aqueous solution is 0.1-10wt%.
Preferably, in the step (1), the carbon-based material is one or a combination of two or more of graphite, graphene, carbon black, mxene, fullerene, activated carbon, carbon nanotube, and carbon fiber.
Preferably, in the step (2), the addition amount of the calcium salt in the mixed suspension is 0.1-1wt%;
and/or the calcium salt is one or the combination of more than two of calcium carbonate, calcium sulfate, calcium sulfite, hydroxyapatite and calcium phosphate.
Preferably, in the step (3), the addition amount of the glucolactone in the mixed suspension is 0.1-1wt%.
Preferably, the total solid content of the sodium alginate and the clay in the clay-based composite hydrogel is 4% -8%.
Preferably, in the step (4), the thickness of the clay-based composite hydrogel is 0.5-1.1 cm.
Preferably, in the step (4), the number of directional freeze thawing is 6-8;
and/or the directional freezing temperature in the directional freezing and thawing is-20 ℃ to-70 ℃.
The beneficial effects are that: the invention constructs super-hydrophilic water delivery channel based on the characteristics of clay material, and adjusts aperture by directional freezing, and the prepared clay-based composite hydrogel has good light absorption efficiency and water evaporation efficiency, rich pore channel structure and good hydrophilicity, and has the following specific beneficial effects:
1. the invention utilizes the self characteristics of clay materials, and has good hydrophilicity and low heat conductivity;
2. the super-hydrophilic clay material and sodium alginate are combined, the concentration proportion is regulated, the thickness of the hydrogel is regulated, the directional freeze thawing technology is utilized to expand the pore canal for a plurality of times to construct vertical micro-scale macropores (the pore diameter range is 50-380 mu m), the flux of water vapor can be effectively improved under the combined action of the mesoporous structure (2-45 nm) built by the pore wall clay, and the evaporation rate can reach 3.78 kg.m at most -2 h -1 ；
3. The preparation method has the advantages of simple preparation process, green and pollution-free raw materials and low price, and is beneficial to industrial production.
Drawings
FIG. 1 is an external view of the diatomaceous earth-based hydrogel prepared in example 3;
FIG. 2 is an SEM photograph of a freeze-dried attapulgite-based hydrogel prepared in example 2;
FIG. 3 is an SEM image of the freeze-dried bentonite-based hydrogel prepared in example 5;
FIG. 4 is a mesoporous structure built with attapulgite clay;
FIG. 5 is an adsorption/desorption curve of a clay-based hydrogel after freeze-drying;
FIG. 6 is a pore size distribution of a clay-based hydrogel after lyophilization;
fig. 7 is a diagram of a water evaporation experimental apparatus.
Description of the embodiments
In order that those skilled in the art will fully understand the technical scheme and the advantages of the present invention, the following description is given with reference to the accompanying drawings and specific embodiments, which are meant to illustrate the invention, but not to limit the invention.
Example 1:
dissolving 0.5g sodium alginate in 49.5ml deionized water, adding 0.5g active carbon powder, and dispersing at high speed for 30min until the active carbon is completely dispersed; slowly adding 0.1g of hydroxyapatite in the stirring process, continuously stirring for 10min, then adding 0.5g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; the gel was aged overnight and subjected to directional freeze thawing treatment 6 times to obtain hydrogels. The directional freezing temperature is-20 ℃, and the specific surface area of the hydrogel reaches 20.72m through measurement 2 And/g, wherein the directional freezing pore diameter range is 320-360 mu m, and the gel thickness is 1cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 2.53kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 87.3%.
Example 2:
1g of sodium alginate is dissolved in 39.48ml of deionized water, 1g of carbon black powder and 9.52g of dispersed attapulgite clay slurry with the mass fraction of 10.5wt% are added, and the mixture is stirred for 30min to be dispersed; slowly adding 0.15g of calcium carbonate in the stirring process, continuously stirring for 10min, then adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 6 times after the gel is aged for one night to obtain the clay-based composite hydrogel. Fig. 2 is an SEM image under this condition. The directional freezing temperature is-30 ℃, and the specific surface area of the hydrogel reaches 35.14m through measurement 2 Per g, the directional freezing pore diameter range is 260-300 μm, the gel thickness is 0.8cm, the water evaporation efficiency of the hydrogel under the irradiation of a sun is 2.76kg.m -2 ·h -1 The light-heat conversion efficiency was 86.2%.
Example 3:
dissolving 0.75g of sodium alginate in 30.5ml of deionized water, adding 2g of graphene and 18.75g of dispersed diatomite slurry with mass fraction of 8wt%, and stirring for 30min to disperse; slowly adding 0.3g of calcium phosphate in the stirring process, continuously stirring for 10min, then adding 1.5g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; the gel was aged overnight and subjected to directional freeze thawing treatment 8 times to obtain clay-based composite hydrogels, as shown in fig. 1. The directional freezing temperature is-40 ℃, and the specific surface area of the hydrogel reaches 38.62m through measurement 2 And/g, wherein the directional freezing pore diameter range is 210-250 mu m, and the gel thickness is 1.1cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 3.11kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 89.6%.
Example 4:
1g of sodium alginate is dissolved in 19.37ml of deionized water, 3g of carbon black powder and 29.63g of dispersed kaolin slurry with the mass fraction of 13.5wt% are added, and the mixture is stirred for 30min to be dispersed; slowly adding 0.45g of hydroxyapatite in the stirring process, continuously stirring for 10min, then adding 2g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) after aging the gel for one night, performing directional freeze thawing treatment for 7 times to obtain the clay-based composite hydrogel. The directional freezing temperature is-55 ℃, and the specific surface area of the hydrogel reaches 50.54m through measurement 2 And/g, wherein the directional freezing pore diameter range is 60-80 mu m, and the gel thickness is 0.9cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 3.66kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 90.4%.
Example 5:
1g of sodium alginate is dissolved in 49ml of deionized water, 3g of carbon nano tube and 29.63g of dispersed bentonite slurry with the mass fraction of 13.5wt% are added, and the mixture is stirred for 30min to be dispersed; slowly adding 0.12g of hydroxyapatite in the stirring process, continuously stirring for 10min, then adding 1.6g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; gelAnd (5) aging for one night, and performing directional freeze thawing treatment for 7 times to obtain the clay-based composite hydrogel. Fig. 3 is an SEM image under this condition. The directional freezing temperature is-70 ℃, and the specific surface area of the hydrogel reaches 52.28m through measurement 2 And/g, wherein the directional freezing pore diameter range is 30-50 mu m, and the gel thickness is 0.6cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 3.78 kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 92.7%.
Example 6:
2g of sodium alginate is dissolved in 34.67ml of deionized water, 2.25g of carbon black powder and 13.33g of dispersed attapulgite clay slurry with the mass fraction of 7.5wt% are added, and the mixture is stirred for 30min to be dispersed; slowly adding 0.3g of hydroxyapatite in the stirring process, continuously stirring for 10min, then adding 1.5g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 8 times after the gel is aged for one night to obtain the clay-based composite hydrogel. The directional freezing temperature is-70 ℃, and the specific surface area of the hydrogel reaches 36.49m through measurement 2 And/g, wherein the directional freezing pore diameter range is 50-80 mu m, and the gel thickness is 0.5cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 3.06kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 89.1%.
Example 7:
0.75g of sodium alginate is dissolved in 49.25ml of deionized water, 2.4g of graphite is added, and stirring is carried out for 30min until dispersion; slowly adding 0.15g of calcium carbonate in the stirring process, continuously stirring for 10min, then adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; the gel was aged overnight and subjected to directional freeze thawing treatment 8 times to obtain hydrogels. The directional freezing temperature is-40 ℃, and the specific surface area of the hydrogel reaches 21.56m through measurement 2 Per g, the directional freezing pore diameter is 220-250 μm, and the gel thickness is 1cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 2.59kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 88.6%.
Example 8:
2g sodium alginate was dissolved in 96Adding 1g of carbon black and 1.6g of attapulgite powder into 4ml of deionized water, and continuously stirring for 30min to disperse; slowly adding 0.3g hydroxyapatite during stirring, continuously stirring for 10min, adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 6 times after the gel is aged for one night to obtain the clay-based composite hydrogel. By measurement, when the proportion of clay to sodium alginate is 5:4 and the directional freezing temperature is-30 ℃, the specific surface area of the hydrogel reaches 29.37m 2 And/g, wherein the directional freezing pore diameter range is 240-280 mu m, and the gel thickness is 1.5cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 1.74 kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 83.2%.
Example 9:
2g of sodium alginate is dissolved in 88ml of deionized water, 1g of carbon black and 10g of attapulgite powder are added, and stirring is continued for 30min until dispersion; slowly adding 0.3g hydroxyapatite during stirring, continuously stirring for 10min, adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 6 times after the gel is aged for one night to obtain the clay-based composite hydrogel. By measurement, when the proportion of clay to sodium alginate is 5:1 and the directional freezing temperature is-30 ℃, the specific surface area of the hydrogel reaches 33.19m 2 And/g, wherein the directional freezing pore diameter range is 100-120 mu m, and the gel thickness is 1.5cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 1.86 kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 84.9%.
Example 10:
2g of sodium alginate is dissolved in 94ml of deionized water, 1g of carbon black and 4g of attapulgite powder are added, and stirring is continued for 30min until dispersion; slowly adding 0.3g hydroxyapatite during stirring, continuously stirring for 10min, adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 6 times after the gel is aged for one night to obtain the clay-based composite hydrogel. By measurement, when the proportion of clay to sodium alginate is 2:1 and the directional freezing temperature is-30 ℃, the specific surface area of the hydrogel reaches 35.76m 2 And/g, wherein the directional freezing pore diameter range is 120-180 mu m, and the gel thickness is 0.3cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 1.51 kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 82.7%.
Example 11:
2g of sodium alginate is dissolved in 94ml of deionized water, 1g of carbon black and 4g of attapulgite powder are added, and stirring is continued for 30min until dispersion; slowly adding 0.3g hydroxyapatite during stirring, continuously stirring for 10min, adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (5) performing directional freeze thawing treatment for 10 times after the gel is aged for one night to obtain the clay-based composite hydrogel. By measurement, when the proportion of clay to sodium alginate is 2:1 and the directional freezing temperature is-30 ℃, the specific surface area of the hydrogel reaches 36.73m 2 And/g, wherein the directional freezing pore diameter range is 80-120 mu m, and the gel thickness is 0.3cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 1.65kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 84.5%.
Example 12:
2g of sodium alginate is dissolved in 96.4ml of deionized water, 1g of carbon black and 1.6g of attapulgite powder are added, and stirring is continued for 30min until dispersion; slowly adding 0.3g hydroxyapatite during stirring, continuously stirring for 10min, adding 1g of gluconolactone, stirring for 2min, pouring into a mould, and standing for gel; and (3) performing directional freeze thawing treatment for 6 times after the gel is aged for one night to obtain the clay-based composite hydrogel. By measurement, the clay and sea
The ratio of the sodium alginate is 1:1, and the specific surface area of the hydrogel reaches 29.73m when the directional freezing temperature is-90 DEG C 2 And/g, wherein the directional freezing pore diameter range is 130-160 mu m, and the gel thickness is 1.5cm. The hydrogel was tested by the device shown in FIG. 7 to have a water evaporation efficiency of 1.44kg.m under a solar light intensity -2 ·h -1 The light-heat conversion efficiency was 83.8%.
In the following, examples 8 to 12 are compared, and the influence of freezing temperature, freezing and thawing times and the proportion of clay and sodium alginate on the evaporation efficiency of the clay-based composite hydrogel prepared by the invention is examined, and the results are shown in Table 1:
according to analysis examples 8-12, the pore diameter in the range of 80-380 mu m and the mesoporous structure formed by the attapulgite on the pore wall can be obtained by adjusting the directional freezing temperature, the freezing and thawing times and the proportion of the attapulgite to the sodium alginate, and the mesoporous structure is mainly distributed in 2-50 nm. The attapulgite on the pore wall and the formed mesoporous structure can greatly improve the hydrophilicity of the hydrogel, and realize rapid water absorption, as shown in fig. 4. When the attapulgite content is too high, the growth speed of ice crystals is hindered, the pore size is gradually reduced, the structure becomes compact, and water vapor cannot smoothly pass through a vapor channel of the directional freezing structure. When the attapulgite content is too low, the mesoporous structure built by the attapulgite on the hole wall is reduced, and the water absorption capacity is reduced, so that the water evaporation rate is influenced; with the decrease of the directional freezing temperature, although the growth speed of ice crystals is high and the pore diameter range is gradually reduced, the overall water delivery effect is still poor, and the lower water evaporation rate is shown. And the increase of the freezing and thawing times can construct a larger pore canal structure to enhance the transportation of water, but the water evaporation rate is still not high due to capillary action. Therefore, the selection of proper freezing temperature, freezing and thawing times and the proportion of clay and sodium alginate have important significance for the water evaporation efficiency.
While the invention has been described in terms of specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the equivalent or similar purpose, unless expressly stated otherwise; all of the features disclosed, or all of the steps in a method or process, except for mutually exclusive features and/or steps, may be combined in any manner.
Claims (9)
1. The preparation method of the clay-based composite hydrogel for solar seawater desalination is characterized by comprising the following steps of:
adding sodium alginate into the aqueous solution to dissolve to obtain an aqueous sodium alginate solution, and adding clay and a carbon-based material into the aqueous sodium alginate solution to mix;
wherein the addition amount of the sodium alginate in the sodium alginate aqueous solution is 0.5-4wt% and the addition amount of the clay in the sodium alginate aqueous solution is 0-15wt%;
step (2), slowly adding calcium salt into the mixed solution in the step (1), and stirring to obtain a mixed suspension;
step (3), adding glucolactone into the mixed suspension in the step (2), uniformly stirring, pouring into a mould, and standing for gel;
step (4), aging the gel, and performing directional freeze thawing for a plurality of times to obtain clay-based composite hydrogel with preset thickness; the mass ratio of the sodium alginate to the clay in the clay-based composite hydrogel is 1:1-1:4.
2. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (1), the clay is one or a combination of more than two of nano attapulgite, bentonite, kaolin, illite, diatomite or sepiolite.
3. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (1), the addition amount of the carbon-based material in the sodium alginate aqueous solution is 0.1-10wt%.
4. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (1), the carbon-based material is one or a combination of more than two of graphite, graphene, carbon black, mxene, fullerene, activated carbon, carbon nano tube or carbon fiber.
5. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (2), the addition amount of the calcium salt in the mixed suspension is 0.1-1wt%;
and/or the calcium salt is one or the combination of more than two of calcium carbonate, calcium sulfate, calcium sulfite, hydroxyapatite and calcium phosphate.
6. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (3), the addition amount of the glucolactone in the mixed suspension is 0.1-1wt%.
7. The method for producing a clay-based composite hydrogel according to any one of claims 1 to 6, wherein: the total solid content of the sodium alginate and the clay in the clay-based composite hydrogel is 4% -8%.
8. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (4), the preset thickness is 0.5-1.1 cm.
9. The method for preparing the clay-based composite hydrogel according to claim 1, wherein: in the step (4), the directional freeze thawing times are 6-8 times;
and/or the directional freezing temperature in the directional freezing and thawing is-20 ℃ to-70 ℃.
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