CN111841648A - Preparation method of niobium modified molecular sieve, product and application thereof - Google Patents
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Abstract
The invention discloses a preparation method of a niobium modified molecular sieve, a product and application thereof, wherein the niobium modified molecular sieve is obtained by modifying a molecular sieve by niobium oxalate and phosphoric acid solution step by step. The 5A or 13X molecular sieve is subjected to heat treatment at the temperature of 500 ℃, and is firstly soaked in a niobium oxalate solution, then modified by a phosphoric acid solution, dried and roasted to obtain the niobium manganese oxide. The material prepared by the preparation method disclosed by the invention not only improves the purification efficiency of formaldehyde, but also improves the adsorption strength of the formaldehyde, and avoids secondary pollution caused by temperature change.
Description
Technical Field
The invention belongs to the technical field of catalytic environmental protection, and particularly relates to a preparation method of a niobium modified molecular sieve, a product and an application thereof.
Background
Formaldehyde has high toxicity, and chronic respiratory diseases can be increased due to long-term contact or inhalation of low-concentration formaldehyde gas, and toxic symptoms comprise headache, neurasthenia, anxiety, vertigo, and nervous system function reduction; the high-concentration formaldehyde has certain toxic action on human nervous system, liver, skin and immune system. More seriously, formaldehyde is carcinogenic. The indoor formaldehyde is dispersed, the treatment amount is small, and the concentration is low, so that the adsorption method is more suitable for removing the indoor formaldehyde.
The adsorption method has the advantages of high removal efficiency, strong enrichment function, low energy consumption, mature process, easy popularization, good environmental benefit and the like, is suitable for deep treatment of low-concentration gaseous pollutants, is almost suitable for all volatile organic compounds, and becomes a common effective method for treating pollutants such as formaldehyde and the like. The adsorbent is critical. Compared with non-polar active carbon, molecular sieves have more regular pore channel structures and polar characteristics, so that the molecular sieves become the adsorption materials with the most development potential.
The molecular sieve has low formaldehyde adsorption capacity and needs to be modified, and the common method comprises the following steps: acid-base modification, metal modification, oxidation modification, and the like. The existing literature uses one method or needs multi-step treatment to achieve the aim of multiple modifications. Niobium salts have redox capabilities and are used as adjuvants or carriers in many reactions and exhibit greater oxidation under acidic conditions. However, few documents have reported using niobium modified molecular sieves.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a niobium modified molecular sieve.
Yet another object of the present invention is to: provides a niobium modified molecular sieve product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a niobium modified molecular sieve is obtained by modifying the molecular sieve by steps with niobium oxalate and phosphoric acid solution, and comprises the following steps:
(1) putting a molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4h, wherein the molecular sieve is a 5A or 13X molecular sieve;
(2) dissolving niobium oxalate in deionized water to prepare a niobium oxalate solution with the molar concentration not more than 0.003mol/L, namely the molar concentration of niobium oxalate is more than 0 and less than or equal to 0.003 mol/L;
(3) placing the molecular sieve obtained in the step (1) in the solution obtained in the step (2), stirring for 3-4h at room temperature, then placing in a water bath at 50 ℃, and continuously stirring until the molecular sieve is completely dried to obtain a sample of which the niobium oxalate accounts for 1% -3% of the mass fraction of the molecular sieve;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in a phosphoric acid solution with the same molar quantity as niobium oxalate at room temperature, namely, the molar ratio of phosphoric acid to niobium oxalate is 1:1, and stirring for 3-4h, wherein the concentration of the phosphoric acid solution is more than or equal to 0.005 mol/L and less than or equal to 0.01 mol/L;
(6) Performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4 h to obtain the niobium modified molecular sieve product.
The invention also provides a niobium modified molecular sieve which is prepared according to the method.
The invention also provides an application of the niobium modified molecular sieve material in room temperature purification of formaldehyde, which comprises the following steps: introducing mixed gas of formaldehyde and air into a continuous flow fixed bed device, wherein the reaction pressure is normal pressure to 1atm, the total flow of the gas is 500 mL/min, the initial concentration of the formaldehyde is 1.0-2.5ppm, and the mass of each obtained catalyst is 0.2 g.
The test shows that: at the temperature of 25 ℃ and 50 ℃, the formaldehyde purification efficiency of the niobium modified molecular sieve material provided by the method is superior to that of a sample obtained by heating the existing 5A molecular sieve and 13X molecular sieve in a muffle furnace at the speed of 2 ℃/min to 500 ℃ and preserving heat for 4 hours.
When the temperature is increased from 25 ℃ to 50 ℃, the purification efficiency of the niobium modified molecular sieve material for formaldehyde does not change obviously, and the purification efficiency of 5A molecular sieve and 13X molecular sieve samples for formaldehyde is greatly reduced. Therefore, the material prepared by the preparation method disclosed by the invention not only improves the purification efficiency of formaldehyde, but also improves the adsorption strength of formaldehyde, and avoids secondary pollution caused by temperature change.
The invention has the advantages that: provides a simple method for modifying the molecular sieve, not only improves the purification efficiency of formaldehyde, but also improves the adsorption strength of the formaldehyde, and avoids secondary pollution caused by temperature change.
Detailed Description
Example 1
A niobium modified molecular sieve is obtained by modifying a molecular sieve with niobium oxalate and phosphoric acid solution step by step and is prepared according to the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 5.4 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 30 mL of 0.01mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) suction filtering, and drying in 50 deg.C oven.
(7) Roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 3% niobium oxalate-13X molecular sieve.
Formaldehyde purification efficiency: 92.1% at 25 ℃; at 50 ℃ and 92.7%, see Table 1 for details.
Example 2
A niobium modified molecular sieve, similar to example 1, prepared by the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 16.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in 60 mL of 0.005mol/L phosphoric acid solution at the room temperature, and stirring for 4 h;
(6) suction filtering, and drying in 50 deg.C oven.
(7) Roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 1% niobium oxalate-13X molecular sieve.
Formaldehyde purification efficiency: 25 ℃, 85.4%; 50 ℃, 85.8%, see table 1 for details.
Example 3
A niobium modified molecular sieve, similar to example 1, prepared by the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 200 mL of deionized water to prepare a niobium oxalate solution;
(3) Weighing 16.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in 60 mL of 0.005mol/L phosphoric acid solution at the room temperature, and stirring for 4 h;
(6) performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 1% niobium oxalate-13X molecular sieve.
Formaldehyde purification efficiency: 90.6 percent at 25 ℃; 50 ℃ and 90.9% in Table 1.
Example 4
A niobium modified molecular sieve, similar to example 1, prepared by the following steps:
(1) placing the 5A molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 150 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 8.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 37.5 mL of 0.008 mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) Performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 2% niobium oxalate-5A molecular sieve.
Formaldehyde purification efficiency: 78.7% at 25 ℃; at 50 ℃ and 78.5%, see Table 1 for details.
Example 5
A niobium modified molecular sieve, similar to example 1, prepared by the following steps:
(1) placing the 5A molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 8.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 37.5 mL of 0.008 mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 2% niobium oxalate-5A molecular sieve.
Formaldehyde purification efficiency: 86.9% at 25 ℃; at 50 ℃ and 86.8%, see Table 1 for details.
Comparative example
And (3) placing the 13X molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving the temperature for 4 h to obtain the sample of the comparative example 1.
Formaldehyde purification efficiency: 45.2% at 25 ℃; at 50 ℃ and 41.0%, see Table 1 for details.
And (3) placing the 5A molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving the temperature for 4 h to obtain a sample of the comparative example 2.
Formaldehyde purification efficiency: 38.6 percent at 25 ℃; 50 ℃ and 34.8%, see Table 1 for details.
The obtained materials were tested for formaldehyde purification performance:
the materials obtained in examples 1 to 5 and comparative example were examined for their room temperature purification performance for formaldehyde. Introducing mixed gas of formaldehyde and air into a continuous flowing fixed bed device, wherein the reaction pressure is normal pressure to 1atm, the total flow of the gas is 500 mL/min, and the initial concentration of the formaldehyde is 1.0-2.5 ppm; weighing 0.2 g of each catalyst; the purifying effect of the material on formaldehyde is respectively considered at 25 ℃ and 50 ℃, and the maximum purifying efficiency of the formaldehyde purification is listed in table 1:
from the data in table 1, it can be seen that the materials obtained in examples 1-5 have better formaldehyde purification efficiency at 25 ℃ and 50 ℃ than comparative examples 1 and 2. When the temperature is increased from 25 ℃ to 50 ℃, the purifying efficiency of the materials of the examples 1-5 to formaldehyde does not change obviously, while the purifying efficiency of the materials of the comparative example 1 and the comparative example 2 to formaldehyde is greatly reduced. Therefore, the material prepared by the preparation method disclosed by the invention not only improves the purification efficiency of formaldehyde, but also improves the adsorption strength of formaldehyde, and avoids secondary pollution caused by temperature change.
Claims (8)
1. The preparation method of the niobium modified molecular sieve is characterized in that the molecular sieve is obtained by modifying niobium oxalate and phosphoric acid solution step by step, and comprises the following steps:
(1) putting a molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4h, wherein the molecular sieve is a 5A or 13X molecular sieve;
(2) dissolving niobium oxalate in deionized water to prepare a niobium oxalate solution with the molar concentration not more than 0.003mol/L, namely the molar concentration of niobium oxalate is more than 0 and less than or equal to 0.003 mol/L;
(3) placing the molecular sieve obtained in the step (1) in the solution obtained in the step (2), stirring for 3-4h at room temperature, then placing in a water bath at 50 ℃, and continuously stirring until the molecular sieve is completely dried to obtain a sample of which the niobium oxalate accounts for 1% -3% of the mass fraction of the molecular sieve;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in a phosphoric acid solution with the same molar quantity as niobium oxalate at room temperature, namely, the molar ratio of phosphoric acid to niobium oxalate is 1:1, and stirring for 3-4h, wherein the concentration of the phosphoric acid solution is more than or equal to 0.005 mol/L and less than or equal to 0.01 mol/L;
(6) performing suction filtration, and drying in a 50 ℃ oven;
(7) and roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve.
2. The method for preparing the niobium modified molecular sieve of claim 1, comprising the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 5.4 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 30 mL of 0.01mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) suction filtering, and drying in 50 deg.C oven.
(7) Roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 3% niobium oxalate-13X molecular sieve.
3. The method for preparing the niobium modified molecular sieve of claim 1, comprising the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) Weighing 16.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in 60 mL of 0.005mol/L phosphoric acid solution at the room temperature, and stirring for 4 h;
(6) suction filtering, and drying in 50 deg.C oven.
(7) Roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 1% niobium oxalate-13X molecular sieve.
4. The method for preparing the niobium modified molecular sieve of claim 1, comprising the following steps:
(1) putting a 13X molecular sieve into a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 200 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 16.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the obtained product in the step (4) in 60 mL of 0.005mol/L phosphoric acid solution at the room temperature, and stirring for 4 h;
(6) Performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 1% niobium oxalate-13X molecular sieve.
5. The method for preparing the niobium modified molecular sieve of claim 1, comprising the following steps:
(1) placing the 5A molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) dissolving 0.16 g of niobium oxalate in 150 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 8.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 37.5 mL of 0.008 mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 2% niobium oxalate-5A molecular sieve.
6. The method for preparing the niobium modified molecular sieve of claim 1, comprising the following steps:
(1) placing the 5A molecular sieve in a muffle furnace, heating to 500 ℃ at the speed of 2 ℃/min, and preserving heat for 4 h;
(2) Dissolving 0.16 g of niobium oxalate in 100 mL of deionized water to prepare a niobium oxalate solution;
(3) weighing 8.1 g of the molecular sieve obtained in the step (1), placing the molecular sieve in the solution in the step (2), stirring the molecular sieve for 4 hours at room temperature, and then placing the molecular sieve in a water bath at 50 ℃ to continuously stir until the molecular sieve is completely dried;
(4) continuing to dry the sample obtained in the step (3) in an oven at 50 ℃ overnight;
(5) dispersing the sample obtained in the step (4) in 37.5 mL of 0.008 mol/L phosphoric acid solution at room temperature, and stirring for 4 h;
(6) performing suction filtration, and drying in a 50 ℃ oven;
(7) roasting at 400 ℃ for 4h to obtain the niobium modified molecular sieve 2% niobium oxalate-5A molecular sieve.
7. A niobium modified molecular sieve, characterized in that it is prepared by a process according to any one of claims 1 to 6.
8. The application of the niobium modified molecular sieve material in the claim 7 to the room temperature purification of formaldehyde, wherein a mixed gas of formaldehyde and air is introduced into a continuous flow fixed bed device, the reaction pressure is normal pressure to 1atm, the total gas flow is 500 mL/min, the initial concentration of formaldehyde is 1.0-2.5 ppm, and the weight of the niobium modified molecular sieve catalyst is 0.2 g.
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