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CN109046309B - Macroporous SiO for soot combustion2One-pot synthesis method of material and product thereof - Google Patents

Macroporous SiO for soot combustion2One-pot synthesis method of material and product thereof Download PDF

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CN109046309B
CN109046309B CN201810915784.9A CN201810915784A CN109046309B CN 109046309 B CN109046309 B CN 109046309B CN 201810915784 A CN201810915784 A CN 201810915784A CN 109046309 B CN109046309 B CN 109046309B
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sio
silicate
macroporous
alkali metal
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王卉
陈丹丹
曹莹莹
陈泽文
邓兴宇
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Hangzhou Dianzi University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • B01J23/04—Alkali metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material

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Abstract

The invention discloses a macroporous SiO for soot combustion2A one-pot synthesis method of the material and a product thereof. The invention adopts specific silicate as silicon source, sodium aluminate as aluminum source, specific silicate cation as active center, inorganic acid as pH regulator, water as solvent, silicate and sodium aluminate are hydrolyzed under the catalysis of inorganic acid to prepare SiO with macroporous structure2Simultaneously with the carrier, alkali metal and Al are mixed2O3The isoactive center is highly dispersed in SiO2The catalyst prepared finally on the surface of the carrier has high catalytic activity on soot combustion reaction, and the preparation process flow of the catalyst is simple and is convenient for industrial production.

Description

Macroporous SiO for soot combustion2One-pot synthesis method of material and product thereof
Technical Field
The invention relates to the field of material preparation, in particular to macroporous SiO for carbon smoke combustion2A one-pot synthesis method of the material and a product thereof.
Background
Soot is a primary particulate matter produced by the combustion of coal and oil, which is itself non-toxic, but it is often entrained with SO2And other hydrocarbons, such as carcinogenic polycyclic aromatic hydrocarbons, can cause serious pollution to the atmospheric environment. Nowadays, the soot control technology is generally a catalytic combustion method, and the principle of the soot control technology is that soot is adsorbed on the inner surface of a catalyst to promote the combustion reaction of soot and oxygen. However, the diameter of the soot particles is generally large (usually larger than 25nm), while the pore diameter of the ordinary catalyst is usually much smaller than 25nm, so the soot particles are difficult to enter the catalyst pore channels for reaction and only contact with the outer surface of the catalyst, resulting in small effective active surface area of the catalyst. Therefore, a catalyst material with reasonable structure and high activity is needed to be found to improve the efficiency of soot catalytic combustion.
At present, the catalyst for the catalytic combustion of soot mainly comprises noble metal catalyst in industryTransition metal oxide catalysts, alkali metal and alkaline earth metal catalysts, and multiple metal composite oxide catalysts. The noble metal catalyst is a catalyst system in which a noble metal (Pt, Pd, etc.) is supported on an oxide carrier. Noble metal catalyst can synergistically remove NO in tail gasxAnd soot particles. Although the noble metal catalyst has high catalytic activity and wide application range, the noble metal is rare in resource, expensive in price and high in cost, and is not suitable for large-scale industrial application. In recent years, hot research on carbon smoke catalytic combustion catalysts in academia has focused on three-dimensional ordered macroporous materials, such as 3DOMCe0.7Zr0.3O2、 3DOMLaCoO3、3DOMLaFeO3. The pore size distribution range of the catalyst is about 50-300nm, which is far larger than the particle size of soot particles, so the soot particles are easy to enter the inside of the pore channels of the catalyst. However, the synthesis of such catalysts requires a large amount of organic template, which must be removed by calcination at high temperature, resulting in complex process and high cost.
The invention takes cheap silicate as raw material, and directly prepares alkali metal-doped macroporous SiO by an improved sol-gel method and a one-pot method2The catalytic material has low price and simple operation process.
Disclosure of Invention
An object of the present invention is to overcome the disadvantages and shortcomings of the prior art by providing an alkali metal-doped macroporous SiO2A method for preparing a catalyst system. The method can realize the preparation of the carbon smoke catalytic combustion catalyst with low cost, high yield and high efficiency, and the prepared catalyst material has the characteristics of high dispersion degree of active components, large aperture and the like.
The purpose of the invention is realized by the following scheme:
the invention provides alkali metal doped macroporous SiO2The preparation method of the catalyst system comprises the following steps: the method comprises the following steps of sequentially carrying out the following steps of using specific silicate as a silicon source, sodium aluminate as an aluminum source, specific silicate cations as an active center, inorganic acid as a pH regulator and water as a solvent:
(1) mixing a proper amount of silicate with water, and stirring until the silicate is completely dissolved;
(2) adding a small amount of sodium aluminate in a certain proportion until the sodium aluminate is completely dissolved;
(3) adding inorganic acid to the required pH value, and standing and aging for a period of time at a certain temperature to obtain the required mixed colloid;
(4) soaking the mixed colloid in the step (3) in deionized water to release excessive cations (at least one of lithium, sodium and potassium cations, which are determined by metal cations in silicate, and sodium ions in sodium aluminate);
(5) drying the colloid soaked in the step (4), and roasting at high temperature to ensure that active centers (at least one of lithium, sodium and potassium cations, which are determined by metal cations in silicate and sodium and aluminum ions in sodium aluminate) in the colloid and SiO carrier2Better combining to finally obtain the needed alkali metal doped macroporous SiO2A catalyst.
In the step (1), the silicate is at least one of lithium silicate, sodium silicate and potassium silicate; the mass ratio of the silicate to the water is (0.05-0.25) to 1;
in the step (2), the mass ratio of the sodium aluminate to the silicate is (0-0.1): 1
In the step (3), the inorganic acid is HCl or HNO3、CH3At least one of COOH; the pH value is 5.5-10.
The aging treatment in the step (3) is carried out at 70-150 ℃ for 12-36 h;
the soaking time in the step (4) is about 6-18 h, and the quantity of the released cation is controlled by using the soaking time;
the high-temperature roasting in the step (5) refers to treatment for 6 hours at 400-600 ℃.
Another object of the present invention is to obtain alkali metal-doped macroporous SiO by the above-mentioned preparation method2A catalyst. The carrier of the catalyst is SiO with a macroporous structure2The average pore diameter is generally more than 70nm, and the macroporous structure is mainly realized by accurately regulating and controlling the pH value, the aging temperature and the like in the sol-gel process; the aluminum ion can be directly doped due to the close valence state with SiInto SiO2The content of the skeleton structure can also be regulated and controlled by the feeding ratio, and finally the skeleton structure is highly dispersed in an oxide form by a high-temperature roasting mode; alkali metal ion (Li)+、Na+、K+) Dispersed in colloid, but because the relative content is too high, excessive ions must be released first, and then the ions are highly dispersed in oxide form in macroporous SiO by high-temperature roasting2In the duct.
Compared with the prior art, the invention has the following advantages and beneficial effects: the alkali metal doped macroporous SiO prepared by the invention2In the process of catalyzing the material, silicate and sodium aluminate are hydrolyzed under the catalysis of inorganic acid to prepare SiO with a macroporous structure2Simultaneously with the carrier, alkali metal and Al are mixed2O3The isoactive center is highly dispersed in SiO2The catalyst prepared finally on the surface of the carrier has high catalytic activity on soot combustion reaction, and the preparation process flow of the catalyst is simple and is convenient for industrial production.
The invention breaks through the method for preparing the macroporous catalytic material by the conventional template method, takes a specific silicon source, sodium aluminate and inorganic acid which are low in price as raw materials, and innovatively provides that the catalyst with high dispersion of active centers and macroporosity of a carrier is synchronously prepared by regulating and controlling the gelling process (step 3, aging temperature and ph environment). The key technology for preparing the catalyst lies in the selection of an active center, the regulation and control of dispersion degree and the control of a silica gel forming process.
The specific principle is as follows:
silicate anions are continuously hydrolyzed and separated out in the form of silicate molecules, and the solubility of orthosilicic acid and the condensation degree of Si-OH are controlled by regulating and controlling the pH value, the temperature and the anions, so that the SiO carrier is realized2The macroporosity of (2). Sodium aluminate hydrolysate and silicate cation are used as catalyst active centers, are uniformly dispersed in a gel system through a gel aging process, and are finally promoted to be in contact with a carrier SiO through roasting2Better combination is carried out, thus preparing the high-quality soot combustion catalyst.
Detailed Description
The present invention is further analyzed with reference to the following specific examples.
Example 1
Mixing 20g of silicate with 200g of water, and stirring until the silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C for 12 hr until pH is 5.5; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalytic material. Mass ratio of different silicates to water alkali metal doped macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 1
TABLE 1 silicate species vs. alkali metal doped macroporous SiO2Influence of catalytic Properties of
Figure GDA0003081481120000031
Figure GDA0003081481120000041
Example 2
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding inorganic acid until pH is 5.5, and aging at 70 deg.C for 12 hr; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Different inorganic acids to alkali metal doped macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 2
TABLE 2 different inorganic acids vs. alkali metals doped macroporous SiO2Influence of catalytic Properties of
Inorganic acid Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
HCl 485 76
HNO3 475 80
CH3COOH 480 78
HCl、HNO3 475 80
HCl、HNO3、CH3COOH 478 80
Example 3
Mixing 20g of lithium silicate with a certain amount of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C for 12 hr until pH is 5.5; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better.Finally preparing the alkali metal doped macroporous SiO2A catalyst. Different mass ratios of lithium silicate to water for alkali metal-doped macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 3
TABLE 3 mass ratio of lithium silicate to water alkali metal doped macroporous SiO2Influence of catalytic Properties of
Mass ratio of lithium silicate to water Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
0.05 475 84
0.1 475 80
0.15 477 78
0.25 480 75
Example 4
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; adding a certain amount of sodium aluminate till the sodium aluminate is completely dissolved; adding HNO3To a pH of 5.5 at 70 deg.CPlacing and aging for 12 h; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Different mass ratios of sodium aluminate to lithium silicate and alkali metal doped macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 4
TABLE 4 Mass ratio of different sodium aluminates to lithium silicate alkali metal-doped macroporous SiO2Effect of catalytic Properties of materials
Figure GDA0003081481120000051
Example 5
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C for 12 hr to reach a certain pH; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Different pH for alkali metal doping macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 5
TABLE 5 different pH vs. alkali metal doped macroporous SiO2Influence of catalytic Properties of
pH Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
5.5 475 80
7.5 470 93
10 468 94
Example 6
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at certain temperature for 12h until pH is 5.5; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Alkali metal doped macroporous SiO under different aging conditions2The effect of the catalytic properties of the materials is shown in Table 6
TABLE 6 different aging temperatures for alkali metal doped macroporous SiO2Influence of catalytic Properties of
Aging temperature (. degree.C.) Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
70 475 80
110 480 74
150 485 60
Example 7
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C until pH is 5.5; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Alkali metal doped macroporous SiO under different aging conditions2The effect of the catalytic properties of the materials is shown in Table 7
TABLE 7 different aging temperatures for alkali metal doped macroporous SiO2Influence of catalytic Properties of
Aging time (h) Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
12 475 80
24 470 92
36 475 78
Example 8
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C for 12 hr until pH is 5.5; soaking the mixed colloid in deionized water for a period of time to release excessive cations; drying the soaked colloid, and roasting at 400 deg.C for 6h to make the active center and the carrier combined better. Finally preparing the alkali metal doped macroporous SiO2A catalyst. Different soaking time for doping alkali metal with macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 8
TABLE 8 different soaking times for alkali metal doped macroporous SiO2Influence of catalytic Properties of
Figure GDA0003081481120000061
Figure GDA0003081481120000071
Example 9
Mixing 20g of lithium silicate with 200g of water, and stirring until the lithium silicate is completely dissolved; then adding 1g of sodium aluminate till complete dissolution; adding HNO3Aging at 70 deg.C for 12 hr until pH is 5.5; soaking the mixed colloid in deionized water for 6h to release excessive cations; drying the soaked colloid, and roasting at high temperature for 6h to make the active center and the carrier combined better. Final preparation ofObtaining alkali metal doped macroporous SiO2A catalyst. Different roasting temperatures for doping alkali metal with macroporous SiO2The effect of the catalytic properties of the materials is shown in Table 9
TABLE 9 different calcination temperatures for alkali metal doped macroporous SiO2Influence of catalytic Properties of
Calcination temperature (. degree.C.) Soot complete catalytic combustion temperature (. degree. C.) Average pore diameter (nm)
400 475 80
500 470 80
600 480 75
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.

Claims (5)

1.一种用于碳烟燃烧的大孔SiO2材料的一锅法合成方法，其特征在于该方法包括以下步骤：1. a one - pot synthesis method of macroporous SiO material for soot combustion, characterized in that the method comprises the following steps: (1)取适量硅酸盐与水混合，搅拌直至完全溶解；(1) Mix an appropriate amount of silicate with water, and stir until completely dissolved; (2)再加入一定比例的少量铝酸钠至完全溶解；(2) add a certain proportion of a small amount of sodium aluminate to dissolve completely; (3)加入酸调节pH至5.5～10，在一定温度下放置老化一段时间，得到所需的混合胶体；(3) adding acid to adjust pH to 5.5～10, and aging at a certain temperature for a period of time to obtain the desired mixed colloid; (4)用去离子水浸泡上述步骤(3)混合胶体，以释放出过多的阳离子；(4) soak the mixed colloid in the above step (3) with deionized water to release excessive cations; (5)将步骤(4)浸泡后的胶体干燥，高温焙烧，使胶体内活性中心与载体SiO2更好地结合，最终得到所需的碱金属掺杂大孔SiO2催化剂；其中活性中心是指代硅酸盐中金属阳离子，以及铝酸钠中钠、铝离子；(5) drying the colloid soaked in step (4), and calcining at high temperature, so that the active center in the colloid is better combined with the carrier SiO 2 , and finally the desired alkali metal-doped macroporous SiO 2 catalyst is obtained; wherein the active center is Refers to metal cations in silicates, as well as sodium and aluminum ions in sodium aluminate; 步骤(1)中，硅酸盐为硅酸锂、硅酸钠、硅酸钾中的至少一种；硅酸盐与水的质量比为(0.05～0.25):1；In step (1), the silicate is at least one of lithium silicate, sodium silicate and potassium silicate; the mass ratio of silicate to water is (0.05～0.25):1; 步骤(2)中，铝酸钠与硅酸盐的质量比为(0～0.1):1；In step (2), the mass ratio of sodium aluminate to silicate is (0～0.1):1; 步骤(3)中，老化处理指在70～150℃下处理12～36h；In step (3), the aging treatment refers to treatment at 70-150° C. for 12-36 hours; 步骤(5)中的高温焙烧指在400～600℃下处理6h。The high-temperature calcination in step (5) refers to treatment at 400-600° C. for 6 hours. 2.如权利要求1所述的一种用于碳烟燃烧的大孔SiO2材料的一锅法合成方法，其特征在于步骤(3)中，酸为HCl、HNO3、CH3COOH中的至少一种。 2. a kind of one-pot synthesis method of macroporous SiO material for soot combustion as claimed in claim 1, is characterized in that in step (3), acid is in HCl, HNO 3 , CH 3 COOH at least one. 3.如权利要求1所述的一种用于碳烟燃烧的大孔SiO2材料的一锅法合成方法，其特征在于步骤(4)中浸泡时间为6～18h。3 . The one-pot synthesis method of a macroporous SiO 2 material for soot combustion according to claim 1 , wherein the soaking time in step (4) is 6-18 h. 4 . 4.一种碱金属掺杂大孔SiO2催化剂，其特征在于采用如权利要求1-3任一所述的合成方法制备得到。4. An alkali metal-doped macroporous SiO2 catalyst, characterized in that it is prepared by the synthesis method according to any one of claims 1-3. 5.如权利要求4所述的一种碱金属掺杂大孔SiO2催化剂，其特征在于载体为具有大孔结构的SiO2，平均孔径在70nm以上；铝离子由于价态与Si接近，可直接掺杂进入SiO2的骨架结构，最后再通过高温焙烧的方式以氧化物形式高度分散；硅酸盐中碱金属离子、铝酸钠中Na+通过高温焙烧的方式以氧化物形式高度分散在大孔SiO2的孔道内。5 . The alkali metal-doped macroporous SiO 2 catalyst according to claim 4 , wherein the carrier is SiO 2 with a macroporous structure, and the average pore diameter is above 70 nm; the aluminum ion is close to Si due to its valence state, and can It is directly doped into the skeleton structure of SiO 2 , and finally highly dispersed in the form of oxides by high-temperature roasting; alkali metal ions in silicate and Na + in sodium aluminate are highly dispersed in the form of oxides by high-temperature roasting. within the pores of macroporous SiO2 .
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