Method for adjusting bulk density of molecular sieve product
By increasing the temperature of sodium aluminosilicate gel slurry for crystallization at the set time and temperature, the problem of adjusting the specific gravity of the molecular sieve product is solved, the precise control of the specific gravity of the stack and the uniformity of particle distribution is achieved, and the process flow is simplified.
Patent Information
- Application Number
- CN202411297446.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-18
- Publication Date
- 2024-12-20
AI Technical Summary
The prior art is difficult to effectively adjust and control the stack ratio of molecular sieve products and cannot meet user needs.
By heating the sodium aluminosilicate gel slurry under set time and temperature conditions and crystallizing, the specific gravity of the molecular sieve product is regulated. The specific method includes setting different temperature enhancement times and temperatures, such as 90°C to 100°C. To form molecular sieve products with different stack specific gravity.
The precise adjustment of the specific gravity of the molecular sieve product stack is achieved, ensuring the uniformity of the particle distribution and performance of the product, simplifying the process flow, and maintaining the stability of the original process.
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Figure CN119160911A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of molecular sieves, and in particular to a method for adjusting the bulk density of a molecular sieve product. Background Art
[0002] Molecular sieves have uniform internal micropores, and their pore size is comparable to the size of general molecules. Substances with molecular diameters smaller than the diameter of the molecular sieve crystal pores can enter the molecular sieve crystals and be adsorbed, otherwise they are repelled, achieving the purpose of screening molecules. Molecular sieves can determine the order of priority adsorption according to the polarity of molecules of different substances. According to its effective pore size, it can be used to screen fluid molecules of different sizes. This effect is called molecular sieve effect. In order to accurately express the category of molecular sieves, the name of the substance should be added in front of the molecular sieve, such as zeolite molecular sieve, carbon molecular sieve, etc.
[0003] In the application process of molecular sieves, it is generally required to fill as many molecular sieve products as possible in a limited filling space to achieve the adsorption capacity required by the application. However, at present, the main research direction is often to improve the stable adsorption rate of molecular sieves, and there are few studies on how to adjust and control the bulk density of molecular sieves. The bulk density index of products cannot meet user needs. Summary of the invention
[0004] The present application provides a method for adjusting the bulk density of a molecular sieve product to solve the following technical problem: how to adjust the bulk density of a molecular sieve product.
[0005] In a first aspect, the present application provides a method for adjusting the bulk density of a molecular sieve product, the method comprising:
[0006] Under the condition of a set time, the sodium aluminosilicate gel slurry is heated to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product having a bulk density corresponding to the set time.
[0007] Optionally, the first temperature is 90°C to 100°C.
[0008] Optionally, the first temperature is 95°C to 100°C.
[0009] Optionally, the crystallization time is 6 h to 8 h.
[0010] Optionally, the set time is negatively correlated with the bulk density of the molecular sieve product.
[0011] Optionally, the set time t and the bulk density of the molecular sieve product satisfy the following relationship:
[0012] If the set time t satisfies 5min≤t≤20min, the bulk density of the molecular sieve product is greater than 0.7;
[0013] If the set time t satisfies 20 min < t ≤ 40 min, the bulk specific gravity of the molecular sieve product is 0.61 - 0.68;
[0014] If the set time t satisfies 40 min < t ≤ 60 min, the bulk specific gravity of the molecular sieve product is below 0.6.
[0015] Optionally, the initial temperature of the sodium aluminosilicate gel slurry is below 40°C.
[0016] Optionally, the molecular sieve product includes one of the following: 4A molecular sieve, 13X molecular sieve.
[0017] Optionally, the synthesis raw materials of the sodium aluminosilicate gel slurry include a silicon source solution and an aluminum source solution.
[0018] Optionally, the solid content of the sodium aluminosilicate gel slurry is 75 g / L - 230 g / L.
[0019] The above technical solution provided by the embodiments of the present application has the following advantages compared with the prior art:
[0020] The method for adjusting the bulk specific gravity of the molecular sieve product provided by the present application includes: under the condition of a set time, heating the sodium aluminosilicate gel slurry to a first temperature for crystallization of the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk specific gravity corresponding to the set time. The gel particles in the sodium aluminosilicate gel slurry are aggregated from loose gel small particles. Heating the sodium aluminosilicate gel slurry to the first temperature for crystallization, when the heating rate is increased, the sodium aluminosilicate gel instantly obtains a large amount of kinetic energy and the aggregation is intensified, and it is easy to form particles of different sizes; while when heating slowly, the original sodium aluminosilicate gel formed by the aggregation of small particles has a certain dispersion time to form a basically uniform particle distribution; therefore, there is a one-to-one correspondence between the particle distribution of the product and the particle distribution of the gel. Therefore, by controlling the set time, the bulk specific gravity of the molecular sieve product can be adjusted. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The drawings here are incorporated into the specification and form a part of this specification, showing the embodiments consistent with the present application, and are used together with the specification to explain the principles of the present application.
[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.
[0023] Figure 1A schematic flow chart of a method for adjusting the bulk density of a molecular sieve product provided in an embodiment of the present application;
[0024] Figure 2 A microscopic morphology of a molecular sieve product provided in Example 1 of the present application;
[0025] Figure 3 A microscopic morphology of a molecular sieve product provided in Example 2 of the present application;
[0026] Figure 4 This is a microscopic morphology of a molecular sieve product provided in Example 3 of the present application. DETAILED DESCRIPTION
[0027] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.
[0028] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present application; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values within the range. For example, the range description from 1 to 6 should be considered to have specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.
[0029] In addition, in the description of the present application, the terms "include", "comprise", etc. mean "including but not limited to". In this document, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations.
[0030] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this application can be purchased from the market or prepared by existing methods.
[0031] In a first aspect, the present application provides a method for adjusting the bulk density of a molecular sieve product. Figure 1A schematic diagram of a method for adjusting the bulk density of a molecular sieve product provided in an embodiment of the present application is shown in FIG. Figure 1 , the method comprising:
[0032] In a first aspect, the present application provides a method for adjusting the bulk density of a molecular sieve product, the method comprising:
[0033] S1. Under the condition of a set time, the sodium aluminosilicate gel slurry is heated to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product having a bulk density corresponding to the set time.
[0034] In the embodiment of the present application, the gel particles in the sodium aluminosilicate gel slurry are formed by the agglomeration of loose small gel particles. The sodium aluminosilicate gel slurry is heated to a first temperature for crystallization. When the heating speed is accelerated, the sodium aluminosilicate gel instantly obtains a large amount of kinetic energy and intensifies the agglomeration, and it is easy to form particles of different sizes; when the temperature is slowly increased, the original sodium aluminosilicate gel formed by the agglomeration of small particles has a certain dispersion time to form a basically uniform particle distribution; therefore, the particle distribution of the product has a one-to-one correspondence with the particle distribution of the gel, so by adjusting the set time, the bulk density of the molecular sieve product can be adjusted.
[0035] In some embodiments, the first temperature is 90°C to 100°C.
[0036] In some embodiments, the first temperature is 95°C to 100°C.
[0037] In the embodiment of the present application, the first temperature represents the crystallization temperature, and crystallization is the process of converting the gel into crystals. This process requires power, and the crystallization temperature is to provide the required power for the crystallization process. The crystallization temperature can be 90°C to 100°C, which provides sufficient power for the crystallization of the sodium aluminosilicate gel slurry, thereby ensuring the performance of the molecular sieve product. Exemplarily, the crystallization temperature can be 90°C, 91°C, 92°C, 93°C, 94°C, 95°C, 96°C, 97°C, 98°C, 99°C, 100°C, etc., and further, the crystallization temperature can be 95°C, 96°C, 97°C, 98°C, 99°C, 100°C, etc.
[0038] In some embodiments, the crystallization time is 6 h to 8 h.
[0039] In the embodiment of the present application, the crystallization time can be 6h to 8h, which provides sufficient time for the sodium aluminosilicate gel slurry to fully crystallize, thereby ensuring the performance of the molecular sieve product. Exemplarily, the crystallization time can be 6h, 6.5h, 7h, 7.5h, 8h, etc.
[0040] In some embodiments, the set time is negatively correlated with the bulk specific gravity of the molecular sieve product.
[0041] In some embodiments, the set time t and the bulk specific gravity of the molecular sieve product satisfy the following relationship:
[0042] If the set time t satisfies 5 min ≤ t ≤ 20 min, the bulk specific gravity of the molecular sieve product is 0.7 or more;
[0043] If the set time t satisfies 20 min < t ≤ 40 min, the bulk specific gravity of the molecular sieve product is 0.61 - 0.68;
[0044] If the set time t satisfies 40 min < t ≤ 60 min, the bulk specific gravity of the molecular sieve product is below 0.6.
[0045] In the embodiments of the present application, the gel particles in the sodium aluminosilicate gel slurry are agglomerated from loose gel small particles. When the sodium aluminosilicate gel slurry is heated to the first temperature for crystallization, the heating rate is fast, and the sodium aluminosilicate gel instantaneously obtains a large amount of kinetic energy and agglomerates more severely, easily forming particles of different sizes; while when heating slowly, the original sodium aluminosilicate gel formed by the agglomeration of small particles has a certain dispersion time to form a basically uniform particle distribution; therefore, there is a one-to-one correspondence between the particle distribution of the product and the particle distribution of the gel. Therefore, by regulating the set time, the bulk specific gravity of the molecular sieve product can be adjusted. As the set time (heating time) prolongs, the bulk specific gravity of the molecular sieve product decreases, gradually providing the driving force for gel crystallization, so that a molecular sieve with a basically uniform particle distribution can be obtained. If the set time t satisfies 5 min ≤ t ≤ 20 min, the bulk specific gravity of the molecular sieve product can reach 0.7 or more. If the set time t satisfies 20 min < t ≤ 40 min, the bulk specific gravity of the molecular sieve product can reach 0.61 - 0.68. If the set time t satisfies 40 min < t ≤ 60 min, the bulk specific gravity of the molecular sieve product can reach below 0.6. Exemplarily, if the set time t satisfies 5 min ≤ t ≤ 20 min, the bulk specific gravity of the molecular sieve can be 0.7, 0.72, 0.74, 0.76, etc.; if the set time t satisfies 20 min < t ≤ 40 min, the bulk specific gravity of the molecular sieve can be 0.61, 0.63, 0.65, 0.67, 0.68, etc.; if the set time t satisfies 40 min < t ≤ 60 min, the bulk specific gravity of the molecular sieve can be 0.6, 0.58, 0.59, 0.57, etc. In addition, when the steam pressure and temperature are constant, the set time can be accurately controlled by controlling the valve opening of the steam control valve, so as to meet the process requirements for controlling the bulk specific gravity.
[0046] In some embodiments, the initial temperature of the sodium aluminosilicate gel slurry is below 40°C.
[0047] In the embodiment of the present application, the initial temperature of the sodium aluminosilicate gel slurry may be below 40° C. For example, the initial temperature of the sodium aluminosilicate gel slurry may be 40° C., 39° C., 38° C., 37° C., etc.
[0048] In some embodiments, the molecular sieve product includes one of the following: 4A molecular sieve, 13X molecular sieve.
[0049] In the embodiments of the present application, the molecular sieve product can be one of 4A molecular sieve and 13X molecular sieve. Type A zeolite has a tetragonal structure similar to sodium chloride, and its chemical formula is Na2O·Al2O3·2SiO2·4.5H2O. Its internal pore size is 4.2 angstroms, so it is referred to as 4A zeolite. When more than 60% of the sodium ions in the 4A zeolite molecular sieve are replaced by potassium ions, it is called 3A zeolite molecular sieve; when more than 70% of the sodium ions in the 4A zeolite molecular sieve are replaced by calcium ions, it is called 5A zeolite molecular sieve. Therefore, 4A molecular sieve is the basic raw material for preparing 3A and 5A molecular sieves. 4A molecular sieve can be used for refrigerator refrigerant drying, hollow glass, dehydration, etc. 3A molecular sieve is used for drying ethylene and natural gas, separation of petroleum cracking gas and hollow glass, etc. 5A molecular sieve is used for pressure swing adsorption device to produce O2, N2, H2. 13X molecular sieve chemical formula: Na2O·Al2O3·(2.8±0.2)·SiO2·(6-7)H2O, with FAU topology. 13X molecular sieve is a special molecular sieve for air separation oxygen production, and can also be used for desulfurization of petroleum gas and natural gas.
[0050] In some embodiments, the raw materials for synthesizing the sodium aluminosilicate gel slurry include a silicon source solution and an aluminum source solution.
[0051] In the embodiment of the present application, the sodium aluminosilicate gel slurry is obtained by chemically reacting a silicon source solution and an aluminum source solution. Exemplarily, water glass (silicon source solution) and sodium aluminate solution (aluminum source solution) are chemically reacted to obtain the sodium aluminosilicate gel slurry.
[0052] In some embodiments, the solid content of the sodium aluminosilicate gel slurry is 75 g / L to 230 g / L.
[0053] In the embodiment of the present application, the solid content of the sodium aluminosilicate gel slurry can be 75g / L to 230g / L to ensure that the sodium aluminosilicate gel slurry has sufficient sodium ions, and the desired molecular sieve product is obtained under the condition of adjusting the set time. If the solid content of the sodium aluminosilicate gel slurry is too low and lower than 75g / L, the concentration of sodium ions in the sodium aluminosilicate gel slurry is low, the gel crystallization rate is slow, and even if the temperature is quickly raised, it is difficult to form agglomerated particles of sodium aluminosilicate (zeolite); if the solid content of the sodium aluminosilicate gel slurry is too high and higher than 230g / L, the sodium aluminosilicate gel slurry is not suitable for rapid heating. Since the crystallization rate is too fast at this time, the sodium aluminosilicate gel slurry is prone to crystallization, thereby generating a mixed phase. Exemplarily, the solid content of the sodium aluminosilicate gel slurry can be 75 g / L, 80 g / L, 85 g / L, 90 g / L, 100 g / L, 110 g / L, 120 g / L, 130 g / L, 150 g / L, 180 g / L, 200 g / L, 210 g / L, 220 g / L, 230 g / L, etc.
[0054] The present application will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are intended only to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods for which specific conditions are not specified in the following examples are usually measured according to industry standards. If there is no corresponding industry standard, then the conditions recommended by the manufacturer are followed.
[0055] Example 1
[0056] A method for adjusting the bulk density of a molecular sieve product, comprising: S11, under the condition of a set time, raising the temperature of sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk density corresponding to the set time; wherein the sodium aluminosilicate gel slurry is synthesized according to 2.84Na2O·Al2O3·1.98SiO2·152H2O, and the solid content of the sodium aluminate gel slurry is 137g / L; the initial temperature of the sodium aluminosilicate gel slurry is 39°C; the set time is 15min, the first temperature is 98°C, the crystallization time is 6 hours, the product bulk density is 0.7342, and the molecular sieve product is 4A molecular sieve.
[0057] Example 2
[0058] A method for adjusting the bulk density of a molecular sieve product, comprising: S12, under the condition of a set time, raising the temperature of sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk density corresponding to the set time; wherein the sodium aluminosilicate gel slurry is synthesized according to 2.92Na2O·Al2O3·2.65SiO2·167H2O, and the solid content of the sodium aluminates gel slurry is 152g / L; the initial temperature of the sodium aluminosilicate gel slurry is 40°C; the set time is 18min, the first temperature is 95°C, the crystallization time is 8 hours, the product bulk density is 0.7581, and the molecular sieve product is a 13X molecular sieve.
[0059] Example 3
[0060] A method for adjusting the bulk density of a molecular sieve product, comprising: S13, under the condition of a set time, raising the temperature of sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk density corresponding to the set time; wherein the sodium aluminosilicate gel slurry is synthesized according to 2.86Na2O·Al2O3·1.98SiO2·107H2O, and the solid content of the sodium aluminates gel slurry is 173g / L; the initial temperature of the sodium aluminosilicate gel slurry is 37°C; the set time is 32min, the first temperature is 96°C, the crystallization time is 6 hours, the product bulk density is 0.6258, and the molecular sieve product is 4A molecular sieve.
[0061] Example 4
[0062] A method for adjusting the bulk density of a molecular sieve product, comprising: S14, under the condition of a set time, raising the temperature of sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk density corresponding to the set time, wherein the sodium aluminosilicate gel slurry is synthesized according to 2.86Na2O·Al2O3·1.98SiO2·107H2O, and the solid content of the sodium aluminate gel slurry is 173g / L; the initial temperature of the sodium aluminosilicate gel slurry is 37°C; the set time is 53min, the first temperature is 98°C, the crystallization time is 6 hours, the product bulk density is 0.5547, and the molecular sieve product is 4A molecular sieve.
[0063] Example 5
[0064] A method for adjusting the bulk density of a molecular sieve product, comprising: S15, under the condition of a set time, raising the temperature of sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry to obtain a molecular sieve product with a bulk density corresponding to the set time; wherein the sodium aluminosilicate gel slurry is synthesized according to 2.87Na2O·Al2O3·2.65SiO2·160H2O, and the solid content of the sodium aluminates gel slurry is 156 g / L; the initial temperature of the sodium aluminosilicate gel slurry is 40°C; the set time is 36 min, the first temperature is 95°C, the crystallization time is 8 hours, the product bulk density is 0.6323, and the molecular sieve product is a 13X molecular sieve.
[0065] In Examples 1 to 5 of the present application, molecular sieve products with different bulk densities can be obtained by adjusting the set time. For example, Figure 2 This is a microscopic morphology of a molecular sieve product provided in Example 1 of the present application; see Figure 2 , indicating that the crystal morphology is regular and the distribution of large and small particles is reasonable; Figure 3 This is a microscopic morphology of a molecular sieve product provided in Example 2 of the present application; see Figure 3 , indicating that the particles are obviously agglomerated and the distribution of large and small particles is reasonable; Figure 4 This is a microscopic morphology of a molecular sieve product provided in Example 3 of the present application; see Figure 4 , indicating that the crystal morphology is regular and there are significantly fewer small particles.
[0066] In addition, one or more technical solutions in the embodiments of the present application have at least the following technical effects or advantages:
[0067] (1) A method for adjusting the bulk density of the molecular sieve raw powder product by changing the crystallization temperature raising time while keeping the original process unchanged;
[0068] (2) This adjustment method does not require changing the original process and is therefore simple and feasible.
[0069] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest range consistent with the principles and novel features applied for herein.
Claims
1. A method for adjusting the bulk density of a molecular sieve product, characterized in that: The method includes: Under the condition of a set time, heating the sodium aluminosilicate gel slurry to a first temperature to crystallize the sodium aluminosilicate gel slurry, thereby obtaining a molecular sieve product having a bulk specific gravity corresponding to the set time.
2. The method according to claim 1, characterized in that The first temperature is 90°C to 100°C.
3. The method according to claim 2, characterized in that The first temperature is 95°C to 100°C.
4. The method according to claim 1, characterized in that The crystallization time is 6h to 8h.
5. The method according to claim 1, characterized in that The set time is negatively correlated with the bulk specific gravity of the molecular sieve product.
6. The method according to claim 1 or 5, characterized in that: The set time t and the bulk specific gravity of the molecular sieve product satisfy the following relationship: If the set time t satisfies 5 min ≤ t ≤ 20 min, the bulk specific gravity of the molecular sieve product is 0.7 or more; If the set time t satisfies 20 min < t ≤ 40 min, the bulk specific gravity of the molecular sieve product is 0.61 to 0.68; If the set time t satisfies 40 min < t ≤ 60 min, the bulk specific gravity of the molecular sieve product is below 0.
6.
7. The method according to claim 1, characterized in that The initial temperature of the sodium aluminosilicate gel slurry is 40°C or below.
8. The method according to claim 1, characterized in that The molecular sieve product includes one of the following: 4A molecular sieve, 13X molecular sieve.
9. The method according to claim 1, characterized in that: The synthesis raw materials of the sodium aluminosilicate gel slurry include a silicon source solution and an aluminum source solution.
10. The method according to claim 1 or 9, characterized in that: The solid content of the sodium aluminosilicate gel slurry is 75 g / L to 230 g / L.