CN110898798A - Amorphous composite oxide adsorbent and preparation method thereof - Google Patents
Amorphous composite oxide adsorbent and preparation method thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—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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- B01J20/06—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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Abstract
The invention provides an amorphous composite oxide adsorbent, which comprises 10-90% of silicon dioxide and 10-90% of amorphous oxide by mass. The silica gel dehumidification rotating wheel has high desorption temperature and poor dehumidification capability under the condition of medium and low humidity (RH is less than 40 percent). The silicon-containing amorphous composite oxide is used as an adsorbent instead of silica gel, so that the deep dehumidification capability under medium and low humidity is improved; the desorption energy consumption is reduced, the desorption regeneration rate is improved, and the running stability of the rotating wheel is improved.
Description
Technical Field
The invention relates to a preparation method of a dehumidifying material, in particular to an amorphous composite oxide adsorbent used in the dehumidifying field and a preparation method thereof.
Background
The air humidity has important influence on human life and industrial production, and the significance of ensuring the indoor proper humidity or the low humidity required by industrial production is great. Common dehumidification methods include freeze dehumidification, compression dehumidification, and adsorption dehumidification. The rotary wheel dehumidification is the best method for treating fresh air to achieve low dew point humidity, and the core component of the rotary wheel dehumidification is a dehumidification material. Through decades of development, the dehumidification materials used by the dehumidification rotary wheel mainly comprise silica gel type and molecular sieve type. A secondary dehumidification rotating wheel is needed in a low dew point scene, namely, the front rotating wheel is a silica gel type dehumidification rotating wheel and is responsible for greatly reducing the moisture content of fresh air; the rear rotating wheel is a molecular sieve type dehumidifying rotating wheel and is responsible for generating low-dew-point fresh air. The invention relates to a silicon-containing amorphous oxide which is used for replacing silica gel and is used for a dehumidifying rotary wheel.
At present, the process for preparing the silica gel dehumidification rotating wheel mainly comprises water glass immersion acidification. The inorganic fiber carrier containing corrugated pore channels is soaked in water glass with proper concentration, preliminarily dried, then subjected to in-situ reaction with acid, washed to remove impurity ions, and dried to complete the loading of the silica gel.
Disclosure of Invention
The dehumidifying rotary wheel of the invention loads the composite material on a carrier by a loading method, wherein the carrier can be an inorganic fiber carrier such as a glass fiber carrier, a ceramic fiber carrier and the like. Through the synthesis optimization of the composite material, the rotating wheel has higher adsorption capacity, and the energy consumption of the rotating wheel for desorption is reduced. The rotating wheel is mainly used in a low dew point and ultra-low dew point dehumidifying unit singly or in series with a molecular sieve dehumidifying rotating wheel.
The invention provides an amorphous composite oxide adsorbent, which comprises 10-90% of silicon dioxide and 10-90% of amorphous oxide by mass.
Wherein the amorphous oxide is at least one of aluminum oxide, titanium oxide, magnesium oxide, lanthanum oxide, cerium oxide, cobalt oxide, boron oxide and vanadium oxide.
Wherein the amorphous oxide is prepared by an acid-base neutralization method.
The invention provides a preparation method of an amorphous composite oxide adsorbent, which comprises the following steps: a) preparing a metal oxide precursor, namely introducing one or more metal salt solutions and an alkaline precipitator into a reaction container, and precipitating under the stirring condition to prepare a metal oxide precursor solution;
b) adding water to dilute the silicon source to a certain concentration;
c) fully mixing the diluted silicon source with a metal oxide precursor solution and aging;
d) adding an acid solution into the mixed solution to adjust the pH value, and stirring and aging;
e) and filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material.
The metal salt solution in the step a) is at least one solution of aluminum source, titanium source, magnesium source, lanthanum source, cerium source, nickel source, cobalt source, boron source and vanadium source which can be selected from corresponding sulfate, chloride and nitrate; the alkaline precipitator is at least one of sodium hydroxide, ammonia water, potassium hydroxide, sodium carbonate and sodium bicarbonate; the reaction time of the step a) is 0.5-2h, and the temperature is 20-90 ℃.
The silicon source in the step b) is at least one of water glass, silica sol and sodium silicate; the content of silicon dioxide in the diluted silicon source is 10-200 g/L;
the aging reaction temperature in the step c) is 20-90 ℃, and the aging reaction time is 1-72 h; the added mass of the metal oxide precursor accounts for 1-50% of the composite oxide calculated by the solid content of the oxide.
In the step d), the acid solution is at least one of hydrochloric acid, sulfuric acid, nitric acid, citric acid, acetic acid, formic acid, malic acid, oxalic acid, maleic acid, phosphoric acid and tartaric acid; the pH value of the aging reaction is 3-9; the aging time is 0.5-3h, and the aging reaction temperature is 20-90 ℃.
The technical problem to be solved by the invention is as follows:
1. the silica gel dehumidification rotating wheel has high desorption temperature and poor dehumidification capability under the condition of medium and low humidity (RH is less than 40 percent). The silicon-containing amorphous composite oxide is used as an adsorbent instead of silica gel, so that the deep dehumidification capability under medium and low humidity is improved; the desorption energy consumption is reduced, the desorption regeneration rate is improved, and the running stability of the rotating wheel is improved.
2. The existing preparation process of the silica gel dehumidification rotating wheel mainly comprises in-situ acidification after dipping a blank body by water glass. The water glass has strong alkalinity and is easy to cause corrosion of the inorganic carrier; the water glass has high viscosity, small single load capacity and poor load uniformity, and the corrugated channel is easy to block; the uniformity degree of the in-situ reaction is poor, and gaps of the inorganic fiber carrier are easy to block the tissue water glass and fully react with acid; hydrated silica gel is dehydrated and shrunk in the drying process of silica gel generated by reaction, so that the rotating core of the rotating wheel is easy to deform, a corrugated channel is blocked, and the wind resistance is easy to cause overlarge. The silicon-containing amorphous composite oxide is used as a dehumidifying agent instead of silica gel, so that the load uniformity and single load capacity of the adsorbent are improved, the dipping/coating process is reduced, the corrosivity of the production process on a fiber carrier is reduced, and the collapse and deformation of corrugated channels are reduced.
Silica gel has poor heat resistance, and high temperature easily causes structural water loss in hydrated silica gel, causes irreversible damage and leads to reduction of adsorption capacity. The silica gel rotary core is desorbed at a high regeneration temperature (more than 120 ℃) for a long time, and the cracking phenomena such as pore canal collapse, core-rotating silica gel melting, cracking and pulverization and the like easily occur, so that the service life is influenced. The silicon-containing amorphous oxide can resist the high temperature of 600 ℃, has good hydrothermal stability, replaces silica gel to be used for the dehumidifying rotating wheel, and can prolong the service life of the dehumidifying rotating wheel.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, which are set forth merely to illustrate the invention and are not intended to limit the scope of the invention.
The dehumidifying rotating wheel adopts the silicon-containing amorphous composite oxide to replace silica gel as an adsorbent, and an M-O-Si bond is formed on the surface of the dehumidifying material through the metal oxide and silicon dioxide composite material, so that the number and the acid strength of acid active centers of B acid and L acid on the surface of the porous dehumidifying material are improved, and the adsorption capacity of the adsorbent to water vapor molecules is enhanced; the composite material has higher specific surface area and pore volume, and the microstructure of composite oxidation is regulated and controlled by the metal oxide and silicon dioxide composite material, so that the pore distribution of the adsorbent is more reasonable, and the adsorption and dehumidification requirements in a larger humidity range are met.
The dehumidifying rotating wheel provided by the invention has the advantages that the dehumidifying rotating core is prepared by coating/impregnating the composite material, acid and alkali corrosion is avoided for a fiber carrier, the impregnating/coating uniformity and the single loading capacity are improved, the deformation of the carrier corrugation is reduced, the wind resistance of the dehumidifying rotating wheel is reduced, the adsorption capacity of the rotating wheel is improved, the desorption energy consumption of the rotating wheel is reduced, and the operation stability and the dehumidifying energy efficiency are improved.
Example 1
1) The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise: preparation of metal oxide precursor2O350g/L of aluminum sulfate and TiO-containing250g/L of titanyl sulfate solution is respectively mixed with 10% ammonia water with a constant pH value of 8.0 in a parallel flow manner, and precipitation is carried out under the stirring condition, so as to respectively prepare metal oxide precursor solutions of alumina and titania, which are marked as A and B. The reaction temperature is 50 ℃, and the reaction time is 2h
2) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
3) According to SiO2:Al2O3:TiO2Adding C into A under the condition of stirring, fully mixing and aging for 1h, continuously adding B into the mixed solution of A and C, and stirring and aging for 1 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-1.
Example 2
6) The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise: preparation of metal oxide precursor2O3Is 50g/L aluminum sulfate and TiO-containing250g/L of titanyl sulfate solution is respectively mixed with 10% ammonia water with a constant pH value of 8.0 in a parallel flow manner, and precipitation is carried out under the stirring condition, so as to respectively prepare metal oxide precursor solutions of alumina and titania, which are marked as A and B. The reaction temperature is 50 ℃, and the reaction time is 2h
7) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
8) According to SiO2:Al2O3:TiO2Adding B into C under the condition of stirring, fully mixing and aging for 1h, continuously adding A into the mixed solution of B and C, and stirring and aging for 1 h.
9) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
10) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-2.
Example 3
The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise:
1) preparing aluminum sulfate containing Al2O3 of 50g/L, and mixing the aluminum sulfate with 10% ammonia water at a constant pH value of 8.0 in a parallel flow manner, and precipitating under the stirring condition to prepare an aluminum oxide metal oxide precursor solution, which is marked as A. The reaction temperature is 50 ℃, and the reaction time is 2h
2) A solution of SiO2 in 100g/L was prepared by diluting water glass with a modulus of 3.2, and this solution was designated as C.
3) Adding C into A under the stirring condition according to the mass fraction of SiO2 and Al2O3 being 6:4, fully mixing and aging for 2 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-3.
Example 4
The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise:
1) preparation of TiO-containing Metal oxide precursor2A 50g/L titanyl sulfate solution was mixed with 10% ammonia water at a constant pH of 8.0 in parallel, and precipitated under stirring to prepare a metal oxide precursor solution of titanium oxide, which was designated as B. The reaction temperature is 50 ℃, and the reaction time is 2h
2) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
3) According to SiO2:TiO2Adding the C into the B under the stirring condition, fully mixing and aging for 1h, and stirring and aging for 1 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-4.
Example 5
The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise: 1) preparation of metal oxide precursor2O350g/L of aluminum sulfate and TiO-containing250g/L of titanyl sulfate solution is respectively mixed with 10% ammonia water with a constant pH value of 5.0 in a parallel flow manner, and precipitation is carried out under the stirring condition, so as to respectively prepare metal oxide precursor solutions of alumina and titania, which are marked as A and B. The reaction temperature is 50 ℃, and the reaction time is 2h
2) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
3) According to SiO2:Al2O3:TiO2Adding C into A under the condition of stirring, fully mixing and aging for 1h, continuously adding B into the mixed solution of A and C, and stirring and aging for 1 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-5.
Example 6
The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise:
1) preparation of metal oxide precursor2O350g/L of aluminum sulfate and TiO-containing250g/L of titanyl sulfate solution is respectively mixed with 10% ammonia water with a constant pH value of 10.0 in a parallel flow manner, and precipitation is carried out under the stirring condition, so as to respectively prepare metal oxide precursor solutions of alumina and titania, which are marked as A and B. The reaction temperature is 50 ℃, and the reaction time is 2h
2) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
3) According to SiO2:Al2O3:TiO2Adding C into A under the condition of stirring, fully mixing and aging for 1h, continuously adding B into the mixed solution of A and C, and stirring and aging for 1 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-6.
Example 7
The composite adsorbent and the dehumidification rotating wheel are prepared according to the following steps, and the specific steps comprise: 1) preparation of metal oxide precursor2O350g/L of aluminum sulfate and TiO-containing250g/L of titanyl sulfate solution is respectively mixed with 10% ammonia water with a constant pH value of 8.0 in a parallel flow manner, and precipitation is carried out under the stirring condition, so as to respectively prepare metal oxide precursor solutions of alumina and titania, which are marked as A and B. The reaction temperature is 50 ℃, and the reaction time is 2h
2) Taking water glass with the modulus of 3.2 to dilute the water glass into SiO-containing water glass2This is a 100g/L solution and is designated C.
3) According to SiO2:Al2O3:TiO2Adding the C into the mixture under the stirring condition, wherein the mass fraction of the C is 7:2:1And B is continuously added into the mixed solution of A and C, and the mixed solution is stirred and aged for 1 h.
4) To the mixed solution was added a 5% strength sulfuric acid solution to adjust pH 7, and the mixture was aged for 1 hour with stirring.
5) And filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material, namely the composite adsorbent, which is marked as S-7.
Property parameters of the composite materials S-1, S-2, S-3, S-4, S-5, S-6 and S-7 prepared in the above examples 1 to 7 were measured, respectively, and the results are shown in Table 1.
TABLE 1 Properties of the composite materials
The performance parameters of the desiccant wheel made of composite S-1 of example 1 of the present invention were compared with those of the desiccant wheel made of conventional molecular sieve NaX (13X), and the results are shown in table 2.
TABLE 2 comparison of properties of conventional molecular sieve desiccant wheels with composite S-1 desiccant wheels
Note: the thickness of the rotating wheel is 2cm, the rotating speed is 10r/h, the desorption area accounts for 25 percent, the desorption temperature is 150 ℃, and the mass of the rotating wheel is about 170g
In the invention, the silica gel dehumidification rotating wheel has high desorption temperature and poor dehumidification capability under the condition of medium and low humidity (RH is less than 40 percent). The silicon-containing amorphous composite oxide is used as an adsorbent instead of silica gel, so that the deep dehumidification capability under medium and low humidity is improved; the desorption energy consumption is reduced, the desorption regeneration rate is improved, and the running stability of the rotating wheel is improved.
The existing preparation process of the silica gel dehumidification rotating wheel mainly comprises in-situ acidification after dipping a blank body by water glass. The water glass has strong alkalinity and is easy to cause corrosion of the inorganic carrier; the water glass has high viscosity, small single load capacity and poor load uniformity, and the corrugated channel is easy to block; the uniformity degree of the in-situ reaction is poor, and gaps of the inorganic fiber carrier are easy to block the tissue water glass and fully react with acid; hydrated silica gel is dehydrated and shrunk in the drying process of silica gel generated by reaction, so that the rotating core of the rotating wheel is easy to deform, a corrugated channel is blocked, and the wind resistance is easy to cause overlarge. The silicon-containing amorphous composite oxide is used as a dehumidifying agent instead of silica gel, so that the load uniformity and single load capacity of the adsorbent are improved, the dipping/coating process is reduced, the corrosivity of the production process on a fiber carrier is reduced, and the collapse and deformation of corrugated channels are reduced.
Silica gel has poor heat resistance, and high temperature easily causes structural water loss in hydrated silica gel, causes irreversible damage and leads to reduction of adsorption capacity. The silica gel rotary core is desorbed at a high regeneration temperature (more than 120 ℃) for a long time, and the cracking phenomena such as pore canal collapse, core-rotating silica gel melting, cracking and pulverization and the like easily occur, so that the service life is influenced. The silicon-containing amorphous oxide can resist the high temperature of 600 ℃, has good hydrothermal stability, replaces silica gel to be used for the dehumidifying rotating wheel, and can prolong the service life of the dehumidifying rotating wheel.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. An amorphous composite oxide adsorbent, characterized in that the adsorbent comprises 10-90% by mass of silica and 10-90% by mass of amorphous oxide.
2. The method according to claim 1, wherein the amorphous oxide is at least one of alumina, titania, magnesia, lanthana, ceria, cobalt oxide, boria, vanadia.
3. The method of claim 2, wherein the amorphous oxide is prepared by acid-base neutralization.
4. A method for preparing an amorphous composite oxide adsorbent is characterized by comprising the following steps: a) preparing a metal oxide precursor, namely introducing one or more metal salt solutions and an alkaline precipitator into a reaction container, and precipitating under the stirring condition to prepare a metal oxide precursor solution;
b) adding water to dilute the silicon source to a certain concentration;
c) fully mixing the diluted silicon source with a metal oxide precursor solution and aging;
d) adding an acid solution into the mixed solution to adjust the pH value, and stirring and aging;
e) and filtering, washing, drying and roasting the aged solution to obtain the silicon-containing amorphous composite oxide material.
5. The method as claimed in claim 4, wherein the metal salt solution in step a) is at least one solution of aluminum source, titanium source, magnesium source, lanthanum source, cerium source, nickel source, cobalt source, boron source, vanadium source selected from their corresponding sulfate, chloride and nitrate; the alkaline precipitator is at least one of sodium hydroxide, ammonia water, potassium hydroxide, sodium carbonate and sodium bicarbonate; the reaction time of the step a) is 0.5-2h, and the temperature is 20-90 ℃.
6. The method according to claim 4, wherein the silicon source in step b) is at least one of water glass, silica sol and sodium silicate; the content of silicon dioxide in the diluted silicon source is 10-200 g/L;
7. the method as claimed in claim 4, wherein the aging reaction temperature in step c) is 20-90 ℃, and the aging reaction time is 1-72 h; the added mass of the metal oxide precursor accounts for 1-50% of the composite oxide calculated by the solid content of the oxide.
8. The method as claimed in claim 4, wherein in the step d), the acid solution is at least one of hydrochloric acid, sulfuric acid, nitric acid, citric acid, acetic acid, formic acid, malic acid, oxalic acid, maleic acid, phosphoric acid and tartaric acid; the pH value of the aging reaction is 3-9; the aging time is 0.5-3h, and the aging reaction temperature is 20-90 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113421617A (en) * | 2021-06-18 | 2021-09-21 | 广东佳纳能源科技有限公司 | Method for calculating solid content in process of preparing solid material by batch method and application thereof |
| WO2024120054A1 (en) * | 2022-12-07 | 2024-06-13 | 江苏苏净集团有限公司 | Method for preparing dehumidification material by using rotating wheel recycled waste, dehumidification material and use thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113421617A (en) * | 2021-06-18 | 2021-09-21 | 广东佳纳能源科技有限公司 | Method for calculating solid content in process of preparing solid material by batch method and application thereof |
| CN113421617B (en) * | 2021-06-18 | 2022-03-11 | 广东佳纳能源科技有限公司 | Method for calculating solid content in process of preparing solid material by batch method and application thereof |
| WO2024120054A1 (en) * | 2022-12-07 | 2024-06-13 | 江苏苏净集团有限公司 | Method for preparing dehumidification material by using rotating wheel recycled waste, dehumidification material and use thereof |
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Application publication date: 20200324 |