CN112774622A - Diatomite-based hierarchical pore composite humidity-controlling material and preparation method thereof - Google Patents
Diatomite-based hierarchical pore composite humidity-controlling material and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Abstract
The invention relates to a diatomite-based hierarchical pore composite humidity-controlling material and a preparation method thereof, wherein diatomite is used as a silicon source and a carrier, a partial alkali dissolution-hydrothermal forming method is adopted, and diatomite and sodium hydroxide are subjected to alkali dissolution at 50-80 ℃ for 10-40 min to prepare mixed ore pulp of sodium silicate and diatomite according to the mass ratio of 1.5-3.5; adding 30-60% by mass of weak-corrosiveness oxalic acid solution into the mixed ore pulp, carrying out acid precipitation to generate white carbon black, adding crystalline aluminum chloride and sodium hydroxide according to a molar ratio of 1: 3-1: 1, aging for 30-150 min, uniformly stirring, transferring into a reaction kettle, carrying out hydrothermal reaction at 100-150 ℃ for 6-12 h, filtering, washing and drying. The main components of the material are amorphous silicon dioxide and hydroxy alumina; the nitrogen adsorption specific surface area is 110m2/g, the pore volume is 0.15cm3/g, and the average pore diameter is 10-40 nm; the maximum moisture absorption amount reaches more than 25% and 20% respectively at the ambient temperature of 10-30 ℃ and the relative humidity of 95% and 85%; the maximum moisture release capacity reaches more than 15% and 10% respectively at the ambient temperature of 10-30 ℃ and the relative humidity of 45% and 35%, and is improved by more than 3 times compared with diatomite, so that the diatomite has a good application prospect.
Description
Technical Field
The invention relates to a diatomite-based hierarchical pore composite humidity controlling material and a preparation method thereof, belonging to the field of deep processing of mineral materials and non-metallic mineral resources.
Background
With the improvement of the living standard of people, people seek comfortable living environment more and more. Humidity is an important index affecting indoor comfort and is related to people's health. Research shows that excessively high or low humidity has adverse effects on life, study and work of people. As a main means for adjusting the relative humidity of indoor air at present, mechanical humidity control devices such as air conditioners and humidifiers consume a large amount of electric energy, and do not meet the requirements for building resource-saving and environment-friendly society. At present, the building energy consumption occupies a large proportion of the energy consumption of China, so that the development of a novel efficient environment-friendly energy-saving humidifying functional material is urgently needed.
Natural inorganic porous mineral materials such as diatomite and the like have the characteristics of developed porous structure, large specific surface area and strong adsorption capacity. The special pore channel structure and the larger pore volume of the porous mineral material provide a storage space for regulating the indoor air humidity, so that the natural inorganic porous mineral is an ideal raw material for preparing the humidity regulating material. The humidity conditioning material prepared from natural nonmetallic ore is used for reasonably regulating and controlling indoor humidity, and non-renewable energy sources such as power and the like are not needed, so that the carbon emission is reduced, and the requirements of energy conservation and environmental protection in the current society are met. However, the diatomite which is not processed has a single pore structure, large proportion of macropores, relatively insufficient content of micro mesopores, small specific surface area, insufficient surface active groups, small balance moisture absorption and release capacity and humidity regulation performance which can not meet the requirement of people on high moisture absorption and release performance of the novel building humidity regulation material.
The white carbon black is a chemical raw material with wide application, and has the characteristics of large specific surface area, rich microporous structure, strong adsorption capacity and the like. The white carbon black prepared by using inorganic nonmetallic ore as a silicon source and adopting a liquid phase method has the characteristics of low cost, reliable technology and the like, the aluminum oxyhydroxide is widely used as an adsorbent due to larger specific surface area and proper nanopore distribution, and the abundant micro-mesoporous structure and surface activity of the white carbon black and the aluminum oxyhydroxide are beneficial to making up the defects of the structure and the performance of a single diatomite humidity-controlling material.
Aiming at the characteristics that the single diatomite humidity-controlling material has weak moisture absorption and desorption capacity and the traditional diatomite-based material has unreasonable pore channel mechanism, the invention provides a diatomite-based hierarchical pore composite humidity-controlling material which is prepared by taking diatomite as a silicon source and oxalic acid which has weak corrosion to instruments and equipment as an acid precipitation raw material and performing partial alkali dissolution-hydrothermal forming.
Natural inorganic porous mineral materials such as diatomite and the like have the characteristics of developed porous structure, large specific surface area and strong adsorption capacity. The special pore channel structure and the larger pore volume of the porous mineral material provide a storage space for regulating the indoor air humidity, so that the natural inorganic porous mineral is an ideal raw material for preparing the humidity regulating material. The humidity conditioning material prepared from natural nonmetallic ore is used for reasonably regulating and controlling indoor humidity, and non-renewable energy sources such as power and the like are not needed, so that the carbon emission is reduced, and the requirements of energy conservation and environmental protection in the current society are met. However, the diatomite which is not processed has a single pore structure, large proportion of macropores, relatively insufficient content of micro mesopores, small specific surface area, insufficient surface active groups, small balance moisture absorption and release capacity and humidity regulation performance which can not meet the requirement of people on high moisture absorption and release performance of the novel building humidity regulation material.
The white carbon black is a chemical raw material with wide application, and has the characteristics of large specific surface area, rich microporous structure, strong adsorption capacity and the like. The white carbon black prepared by using inorganic nonmetallic ore as a silicon source and adopting a liquid phase method has the characteristics of low cost, reliable technology and the like, the aluminum oxyhydroxide is widely used as an adsorbent due to larger specific surface area and proper nanopore distribution, and the abundant micro-mesoporous structure and surface activity of the white carbon black and the aluminum oxyhydroxide are beneficial to making up the defects of the structure and the performance of a single diatomite humidity-controlling material.
Aiming at the characteristics that the single diatomite humidity-controlling material has weak moisture absorption and desorption capacity and the traditional diatomite-based material has unreasonable pore channel mechanism, the invention provides a diatomite-based hierarchical pore composite humidity-controlling material which is prepared by taking diatomite as a silicon source and oxalic acid which has weak corrosion to instruments and equipment as an acid precipitation raw material and performing partial alkali dissolution-hydrothermal forming.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention aims to provide the diatomite-based hierarchical pore composite humidity controlling material with large moisture absorbing and releasing capacity and reasonable pore structure distribution and the preparation method of the composite humidity controlling material.
The diatomite-based hierarchical pore composite humidity controlling material provided by the invention has the following main technical characteristics:
the main components are amorphous silicon dioxide and hydroxy alumina; the nitrogen adsorption specific surface area is more than or equal to 110m2Per g, pore volume is more than or equal to 0.15cm3(ii)/g, the average pore diameter is 10-40 nm.
The invention further provides a method for preparing the diatomite-based hierarchical pore composite humidity controlling material, namely, diatomite is used as a silicon source and a carrier, a partial alkali dissolution-hydrothermal forming method is adopted, and the preparation process comprises the following steps:
(1) dissolving diatomite and sodium hydroxide in an alkali solution at 50-80 ℃ for 10-40 min according to the mass ratio of 1.5-3.5 to prepare mixed ore pulp containing sodium silicate and diatomite;
(2) adding 30-60% mass percent of oxalic acid solution into the uniformly mixed ore pulp in the step (1) to acidify the sodium silicate to produce precipitated white carbon black.
(3) Adding crystalline aluminum chloride and sodium hydroxide into the suspended matters in the step (2) according to a molar ratio of 1: 3-1: 1, aging the mixed ore pulp for 30-150 min, uniformly stirring, and then transferring the mixed ore pulp into a reaction kettle to perform hydrothermal reaction for 6-12 h at 100-150 ℃.
(4) And (4) filtering and washing the product obtained in the step (3) to be neutral, and drying to obtain the diatomite-based hierarchical porous composite humidity-controlling material.
The diatomite in the step (1) is raw diatomite ore or concentrated diatomite with the granularity of 97 percent to 80m (the screen residue of a standard sieve with 200 meshes is less than or equal to 5 percent) and the amorphous SiO2 content of more than or equal to 75 percent.
The preparation principle of the diatomite-based hierarchical pore composite humidity controlling material is as follows: the following chemical reactions of diatomite, sodium hydroxide, oxalic acid and crystalline aluminum chloride occur:
（1）mSiO2+2NaOH+H2O Na2O·mSiO2+2H2O
（2）Na2O·mSiO2 + H2SO4 +2H2O→mSiO2＋Na2SO4＋3H2O
（3）AlCl3·6H2O + 3NaOH → AlOOH＋3NaCl＋7H2O
wherein m is the modulus of sodium silicate.
The moisture-adjusting performance of the diatomite-based hierarchical pore composite moisture-adjusting material prepared by the method is obviously improved compared with that of pure diatomite, and the maximum moisture absorption amounts of the diatomite-based hierarchical pore composite moisture-adjusting material are respectively more than 25% and 20% under the conditions of the environmental temperature of 10-30 ℃, the relative humidity of 95% and 85%; the maximum moisture release capacity reaches more than 15% and 10% under the conditions of the environmental temperature of 10-30 ℃, the relative humidity of 45% and 35%, the maximum moisture release capacity is improved by more than 3 times compared with that of pure diatomite, and the preparation method is simple, low in production cost and good in application prospect.
Drawings
FIG. 1 shows an SEM image of diatomaceous earth.
Fig. 2 is an SEM image of the diatomaceous earth-based hierarchical pore composite humidity control material.
Fig. 3 is a partially enlarged SEM image of the diatomaceous earth-based hierarchical pore composite humidity control material.
Detailed Description
The diatomaceous earth-based hierarchical pore composite humidity controlling material of the present invention will be further described.
As can be seen from fig. 1, the surface of the diatomite is smooth, only a small amount of clastic diatomite is attached to the surface, and the pore channels on the diatomite disc are mainly macroporous and assisted by a small amount of mesopores; as can be seen from fig. 2 and fig. 3, white carbon black with a flocculent structure and hydroxy alumina with a needle-like structure are generated in the diatomite-based hierarchical porous composite humidity control material, and the diatomite carrier, the flocculent white carbon black and the needle-like hydroxy alumina form three-dimensional network cross-linking to form a hierarchical porous structure, so that the proportion of micro-mesopores in the pore structure is significantly increased compared with diatomite.
The following will further describe the preparation method of the diatomite-based hierarchical pore composite humidity controlling material according to the present invention with reference to specific examples.
Example 1:
introduction of raw materials: the diatomite concentrate is from diatomite Limited company of North Peak Yangjiang, and has main chemical components and content of SiO2 86.97%，Al2O3 3.76%，Fe2O32.13 percent, 0.23 percent of MgO, 0.35 percent of CaO, and less than 2.0 percent of the residue of a 200-mesh sieve in granularity; the sodium hydroxide is from Chengdu Jinshan chemical reagent GmbH, analytically pure; oxalic acid is from Douglas chemical Co., Ltd and crystalline aluminum chloride is from Douglas chemical Co., Ltd.
The preparation process comprises the following steps:
mixing diatomite and sodium hydroxide according to the mass ratio of 1.75, and preparing mixed ore pulp containing sodium silicate and diatomite by alkali dissolution for 30min at the temperature of 80 ℃; adding an oxalic acid solution with the mass fraction of 60% into the mixed ore pulp, carrying out acid precipitation on sodium silicate to generate precipitated white carbon black, adding crystalline aluminum chloride and sodium hydroxide according to the molar ratio of 1:1, aging the mixed ore pulp for 90min, uniformly stirring, and then transferring the mixed ore pulp into a reaction kettle to carry out hydrothermal reaction for 12h at the temperature of 120 ℃. .
The samples of the examples were tested for moisture absorption and desorption properties using a constant temperature and humidity test chamber. The test procedure was as follows:
(1) sample pretreatment: weighing 10g of sample, soaking the sample in distilled water, shaking up, putting the sample into a drying oven at 105 ℃, drying the sample until the change of the sample mass is less than 0.1 percent after the sample mass is weighed continuously for one hour, cooling the sample in a dryer to room temperature, weighing the sample, and recording the mass;
(2) test preparation: the program target humidity was adjusted under constant 20 ℃ (protection temperature 50 ℃). Opening a control software system of the electronic balance, and setting port parameters;
(3) and (3) testing: and (3) carrying out a moisture absorption test on the sample under a set temperature and humidity environment, when the mass of the sample is not changed for one hour continuously, the sample reaches saturated moisture absorption, ending the moisture absorption process, reducing the humidity in the constant-temperature constant-humidity box by 50%, carrying out a moisture release test, when the mass of the sample is not changed for one hour continuously, the sample reaches saturated moisture release, and ending the moisture release process.
The calculation formula of the moisture absorption and release amount of the material is as follows:
in the formula: wa-the amount of moisture absorbed at the end of the moisture absorption process, in%;
Wb-the amount of dewetting at the end of the dewetting process, in%;
ma-the mass of the sample at the end of the hygroscopic course in g;
mb-the mass of the sample at the end of the dewetting process, in g;
m0initial mass of sample in g.
Table 1 shows the maximum moisture absorption of the sample of example 1 at 20 ℃ and 95% relative humidity and 85% ambient temperature and the maximum moisture release at 20 ℃ and 45% relative humidity and 35% ambient temperature.
Example 2:
the method is the same as the raw materials and the process steps in the example 1, except that the diatomite and the sodium hydroxide are mixed according to the mass ratio of 2.0, and the mixture is subjected to alkali dissolution at the temperature of 60 ℃ for 20min to prepare mixed ore pulp containing sodium silicate and the diatomite; adding 50% oxalic acid solution in percentage by mass into the mixed ore pulp, carrying out acid precipitation on sodium silicate to generate precipitated white carbon black, adding crystalline aluminum chloride and sodium hydroxide according to the molar ratio of 1:2, aging the mixed ore pulp for 120min, uniformly stirring, and then transferring the mixed ore pulp into a reaction kettle to carry out hydrothermal reaction for 9h at 150 ℃. The conditioning performance of the samples of examples was measured in the same manner as in example 1, and the results are shown in Table 1.
Example 3:
the method is the same as the raw materials and the process steps in the example 1, except that the diatomite and the sodium hydroxide are mixed according to the mass ratio of 2.5, and the mixture is subjected to alkali dissolution at the temperature of 50 ℃ for 40min to prepare mixed ore pulp containing sodium silicate and the diatomite; adding oxalic acid solution with the mass fraction of 40% into the mixed ore pulp, carrying out acid precipitation on sodium silicate to generate precipitated white carbon black, adding crystalline aluminum chloride and sodium hydroxide according to the molar ratio of 1:3, aging the mixed ore pulp for 60min, uniformly stirring, and then transferring the mixed ore pulp into a reaction kettle to carry out hydrothermal reaction for 6h at the temperature of 100 ℃. The method for measuring the humidity control performance of the sample of example was the same as in example 1.
The results are shown in Table 1.
TABLE 1 conditioning performance and pore structure characteristics of the samples of the examples
Finally, although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that changes and modifications may be made to the embodiments without departing from the spirit of the present invention as defined by the appended claims.
Claims (3)
1. A diatomite-based hierarchical pore composite humidity controlling material is characterized in that: the main components are amorphous silicon dioxide and hydroxy alumina; the nitrogen adsorption specific surface area is more than or equal to 110m2/g, the pore volume is more than or equal to 0.15cm3/g, and the average pore diameter is 10-40 nm; the maximum moisture absorption amount reaches more than 25% and 20% respectively at the ambient temperature of 10-30 ℃ and the relative humidity of 95% and 85%; the maximum moisture release rate is respectively up to 15% and 10% at the ambient temperature of 10-30 ℃ and the relative humidity of 45% and 35%.
2. The preparation method of the diatomite-based hierarchical pore composite humidity controlling material of claim 1, which uses natural porous mineral diatomite as a silicon source and a carrier, adopts a partial alkali dissolution-hydrothermal forming method, and comprises the following steps:
(1) and (2) carrying out alkali dissolution on the diatomite and sodium hydroxide for 10-40 min at the temperature of 50-80 ℃ according to the mass ratio of 1.5-3.5 to prepare mixed ore pulp consisting of sodium silicate and diatomite.
(2) Adding 30-60% by mass of oxalic acid solution into the mixed ore pulp obtained in the step (1), and carrying out acid precipitation with sodium silicate to generate precipitated white carbon black.
(3) Adding crystalline aluminum chloride and sodium hydroxide into the mixture obtained in the step (2) in a molar ratio of 1: 3-1: 1, aging the mixed ore pulp for 30-150 min, uniformly stirring, placing the mixture into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 6-12 h at 100-150 ℃.
(4) And (4) filtering and washing the product obtained in the step (3) to be neutral, and drying to obtain the diatomite-based hierarchical porous composite humidity controlling material.
3. The diatomite-based hierarchical porous composite humidity controlling material and the preparation method thereof as claimed in claims 1 to 2, wherein: the diatomite is raw diatomite ore or concentrated diatomite with the granularity of 97 percent to 80m (the screen residue of a standard sieve with 200 meshes is less than or equal to 5 percent) and the amorphous SiO2 content of more than or equal to 75 percent.
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