X-mcm-41 mesoporous molecular sieve microsphere adsorbent and its forming method and application
By using a composite bonding system of attapulgite and guar gum and a precise temperature-controlled calcination process, the problem of forming X-MCM-41 mesoporous molecular sieve powder was solved, achieving a balance between high mechanical strength and adsorption performance, making it suitable for hygiene and care products.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-12
- Publication Date
- 2026-04-10
AI Technical Summary
Existing technologies make it difficult to efficiently shape X-MCM-41 mesoporous molecular sieve powder into fine particles of 40-60 mesh. Traditional methods lead to blockage of the mesoporous structure or biocompatibility risks, which cannot meet the safety and adsorption performance requirements of hygiene and care products.
Using attapulgite and guar gum as an all-natural composite binder, combined with atomization molding and precise temperature-controlled calcination processes, high-mechanical-strength X-MCM-41 mesoporous molecular sieve microspheres were prepared while maintaining the mesoporous structure and adsorption performance.
Microspheres with good sphericity, smooth surface and high mechanical strength were successfully prepared, which not only meet the safety requirements of hygiene care products but also maintain high adsorption performance, thus solving the technical bottleneck of traditional methods.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of advanced adsorbent material preparation and forming technology, in particular to X-MCM-41 mesoporous molecular sieve microsphere adsorbent and its forming method and application. BACKGROUND
[0002] The X-MCM-41 molecular sieve powder obtained by metal ion exchange modification has excellent adsorption performance on malodorous gases such as ammonia, trimethylamine and hydrogen sulfide produced by human metabolism, and has great potential for application in sanitary napkins, urine pads and other personal care products.
[0003] However, the powdery adsorbent material has obvious defects in actual product application: it is easy to leak out of the product, may cause discomfort when in contact with the skin, and is easy to migrate and aggregate in a liquid environment, resulting in a decrease in adsorption efficiency. Therefore, the powdery material must be formed into macroscopic particles. The particles obtained by the traditional tabletting and crushing method have sharp edges and corners, which is contrary to the requirements of skin comfort; and the extrusion and rounding method is difficult to efficiently prepare small particles of 40-60 mesh (0.25-0.42 mm).
[0004] Although atomization forming can directly prepare small spherical particles, the X-MCM-41 molecular sieve powder has low density and no self-bonding property, so that the green body with sufficient "green strength" cannot be obtained by direct atomization. If traditional inorganic binders such as silica sol and aluminum sol are introduced, the valuable mesoporous structure of X-MCM-41 will be seriously blocked, resulting in a sharp decrease in specific surface area and adsorption capacity. If synthetic polymer binders are used, there may be a risk of biocompatibility, and harmful gases will be generated during calcination.
[0005] Therefore, developing a forming method that can realize efficient atomization forming of X-MCM-41, maintain its mesoporous structure and adsorption performance, and meet the safety requirements of human contact, has become a key technical bottleneck for the application of this excellent adsorbent material in the field of sanitary care. SUMMARY
[0006] In view of the above technical bottleneck, the present application aims to provide a forming method for X-MCM-41 mesoporous molecular sieve microsphere adsorbent. The method uses safe and non-toxic natural raw materials as a composite binder system, prepares 40-60 mesh microspheres by atomization granulation, and accurately controls the process conditions, so that the obtained microspheres have high mechanical strength (high toughness, high hardness and low pulverization rate), while the high specific surface area and adsorption performance of X-MCM-41 are maintained to the greatest extent, finally meeting the requirements of direct application in sanitary care products.
[0007] The present application aims to provide a preparation of high-strength X-MCM-41 mesoporous molecular sieve microsphere adsorbent suitable for human hygiene care products and a forming method thereof. Although the X-MCM-41 adsorbent powder has excellent adsorption performance, the nano-powder morphology directly applied to sanitary napkins, urine pads and other personal care products has technical obstacles such as easy dusting, easy penetration of non-woven fabric and direct contact with the skin, easy migration and aggregation in a liquid environment leading to local failure, etc. Therefore, it is necessary to form it into macro-particles with certain size and mechanical strength.
[0008] Forming the X-MCM-41 molecular sieve powder into fine particles of 40-60 mesh faces significant technical challenges. The particles obtained by the traditional tablet crushing method are angular and have poor comfort when in contact with the skin; the extrusion and rounding method is difficult to efficiently prepare such fine and uniform spherical particles. Although atomization forming can directly prepare fine spherical particles, the X-MCM-41 molecular sieve powder has low density and no self-adhesion, and conventional binder systems such as silica sol, aluminum sol and other inorganic binders will seriously block the valuable mesoporous structure, resulting in a sharp decrease in specific surface area and adsorption capacity; while synthetic organic polymer binders have biological compatibility risks and may produce harmful by-products during high-temperature calcination, which are not suitable for the hygiene field directly contacted with the human body.
[0009] The present application successfully solves the above technical contradictions through an innovative binder system and precise process control.
[0010] The forming principle and mechanism of the present application are mainly based on the following aspects: first, the present application creatively uses attapulgite and sesbania gum to form a full-natural and non-toxic composite binder system. Attapulgite, as a natural one-dimensional nanofibrous silicate mineral, can form a stable three-dimensional network skeleton in the slurry, giving the slurry good thixotropy and suspension stability, preventing X-MCM-41 particles from settling, and providing the initial "skeleton strength" for the green microspheres. Sesbania gum, as an excellent natural plant gum, can form a high-viscosity pseudoplastic fluid after dissolving in water, which on the one hand ensures that the slurry reaches the required viscosity for atomization, and on the other hand wraps the X-MCM-41 and attapulgite particle surfaces as an excellent film-forming agent, greatly improving the plasticity of the material and the "green strength" and toughness of the green microspheres through the "bridging" action of its polymer chains, ensuring the smooth progress of the atomization process and the integrity of the green body.
[0011] Secondly, the application designs a unique post-processing technology of programmed temperature drying and precise temperature control calcination. The programmed drying strategy of "high humidity and low temperature first, then low humidity and high temperature" effectively controls the migration and evaporation rate of water from inside to outside, avoids the huge shrinkage stress caused by rapid surface water loss, thereby preventing the microsphere from cracking and deformation, significantly improving the yield and giving the shaped body good toughness. The subsequent calcination process can smoothly and completely decompose and remove the sesbania gum by controlling the heating rate (1-5 ℃ / min) and the final temperature (450-600 ℃), and at the same time, form a firm sintering neck between the attapulgite and X-MCM-41 particles, thereby giving the microsphere the final high hardness and low pulverization rate, and protecting the mesoporous structure of X-MCM-41 from being destroyed or blocked by high temperature to the maximum extent.
[0012] The application finds the best balance point between mechanical strength and adsorption performance by systemically regulating the proportion of ingredients (X-MCM-41 / attapulgite / sesbania powder). Although too high binder content can improve the strength, it will excessively occupy the pore space, resulting in the loss of specific surface area; too low binder content cannot realize effective molding. The preferred ratio determined by the application can ensure that the shaped body has high mechanical strength (abrasion rate ≤ 1.2 wt%) while the BET specific surface area is still maintained at a high level of more than 750 m 2 / g, thereby maximizing the retention of the excellent performance of the original powder adsorbent.
[0013] The application is not simply physical granulation of X-MCM-41 adsorbent powder, but creatively converts the high-performance X-MCM-41 adsorbent powder into a specific form (40-60 mesh microspheres) that can be directly applied to high-value-added health care products by selecting safe raw materials (attapulgite and sesbania gum) matched with human contact requirements and coupling atomization molding and precise heat treatment process. This realizes the key technical leap from "laboratory material" to "end product usable form".
[0014] The X-MCM-41 mesoporous molecular sieve microsphere adsorbent provided by the application has good sphericity, smooth surface and no sharp edges and corners, and will not leak from the product non-woven fabric, and can also provide comfortable skin touch. On the premise of retaining high adsorption capacity for target malodorous molecules such as ammonia, trimethylamine, hydrogen sulfide, isovaleric acid, methyl mercaptan and indole, the X-MCM-41 mesoporous molecular sieve microsphere adsorbent has excellent engineering application performance that traditional powder materials do not have, and perfectly meets the comprehensive requirements of health care products for adsorption materials in efficiency, safety and practicability.
[0015] The molding method of the X-MCM-41 mesoporous molecular sieve microsphere adsorbent comprises the following steps:
[0016] S1: slurry preparation: 50-85 parts of X-MCM-41 molecular sieve powder modified by metal ion exchange, 10-40 parts of attapulgite, 3-8 parts of sesbania powder, and 80-200 parts of water are mixed to form a uniform and flowable slurry by high-speed shearing at 2500 rpm;
[0017] S2: atomization and granulation: the slurry obtained in step S1 is atomized into droplets by an atomizing nozzle under the action of compressed gas flow, and the droplets are dried by hot air blowing at 100-250℃ in a granulation tower to form green microspheres of 40-60 mesh;
[0018] S3: drying: the green microspheres are dried by programmed temperature rising in a humidity environment of 70%-95%, the temperature is 30-60℃, and the time is 4-12 hours;
[0019] S4: calcination: the dried microspheres are heated to 450-600℃ at a rate of 1-5℃ / min in air or inert atmosphere, and calcined for 2-6 hours to obtain the X-MCM-41 mesoporous molecular sieve microsphere adsorbent.
[0020] Optionally, the X-MCM-41 molecular sieve powder in the present application is a functionalized powder after metal ion exchange, and the metal ion is at least one selected from Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ , Ag + . The preparation process of the X-MCM-41 molecular sieve powder after metal ion exchange: ion exchange of MCM-41 raw powder with a solution containing Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ or Ag + at a suitable concentration to obtain different ion-exchanged mesoporous molecular sieve powders, denoted as X-MCM-41.
[0021] Optionally, in step S1, the weight ratio of the X-MCM-41 molecular sieve powder, attapulgite and sesbania powder is (65-75):(20-30):(4-6).
[0022] Optionally, in step S1, the solid content of the slurry is 30%-40%, and the viscosity is 800-2500 mPa·s.
[0023] Optionally, in step S3, the specific steps of the programmed temperature drying are as follows: first, constant temperature and humidity at 30-40 DEG C and humidity of 90-95% for 2-4 hours, then slowly heating to 50-60 DEG C and humidity of 70-80% for 2-8 hours.
[0024] Optionally, in step S4, the preferred conditions of the calcination are as follows: heating to 500-550 DEG C at a rate of 2 DEG C / min and calcining for 3-5 hours.
[0025] The X-MCM-41 molecular sieve powder is obtained by exchanging MCM-41 raw powder with Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ , Ag + metal ions respectively, and then washing, drying and calcining.
[0026] Preparation of MCM-41 raw powder: a proper amount of dodecyltrimethylammonium bromide (DTAB) is added into 4.8 L distilled water to form a homogeneous solution under stirring. 35 mL of sodium hydroxide (2 M) solution is added into the solution, and stirring is continued at 80 DEG C for 5 minutes. Then a proper amount of tetraethyl orthosilicate (TEOS) is added, and stirring is continued at 80 DEG C for 10 hours. After the reaction, the product is collected, washed with distilled water, and dried at 60 DEG C for 24 hours. Finally, the obtained MCM-41 material is calcined at 550 DEG C for 5 hours to completely remove the surfactant, and dry MCM-41 raw powder is obtained.
[0027] The silicon-aluminum ratio of the MCM-41 raw powder is 40-80, in terms of molar ratio of SiO2 and Al2O3.
[0028] Compared with the existing molding technology, the present application has the following beneficial effects:
[0029] The present application successfully solves the molding technology bottleneck of high-performance X-MCM-41 mesoporous molecular sieve microsphere adsorbent in the field of health care, and prepares mesoporous microspheres with uniform particle size (40-60 mesh), good sphericity, high mechanical strength (good toughness, high hardness and low pulverization rate) through atomization molding.
[0030] The present application innovatively uses attapulgite and sesbania gum as a full-natural composite bonding system, which is safe, non-toxic and has high biocompatibility, and perfectly meets the stringent safety requirements of human health care products on materials.
[0031] The application realizes excellent balance between strength and adsorption performance by optimizing the proportion of ingredients and precisely controlling the drying and calcination process, while significantly improving the mechanical strength of the material and minimizing the loss of high specific surface area and mesoporous structure of X-MCM-41, so that the saturated adsorption capacity is extremely small.
[0032] The X-MCM-41 mesoporous molecular sieve microsphere adsorbent provided by the application can be directly used as a functional filler in the absorption layer of sanitary napkins, urine pads and the like, realizes efficient and continuous adsorption of various irritating odor molecules, and fundamentally improves the comfort and functionality of the products, thereby providing core material support for upgrading of the products. BRIEF DESCRIPTION OF DRAWINGS
[0033] Figure 1 The physical adsorption isotherm of ammonia gas for multiple examples and comparative examples of the application is compared.
[0034] Figure 2 The X-MCM-41 molecular sieve powder exchanged by zinc ions (Zn 2+ ) in Example 1 of the application is shown in the actual product picture.
[0035] Figure 3 The X-MCM-41 mesoporous molecular sieve microsphere adsorbent formed in Example 1 of the application is shown in the actual product picture. DETAILED DESCRIPTION
[0036] The application will be further described in detail below in combination with examples, but the implementation manner of the application is not limited thereto. The experimental method not specified in the following examples is usually carried out according to the conventional conditions.
[0037] Unless otherwise specified, the X-MCM-41 molecular sieve powder used in the examples of the application is prepared by the following steps:
[0038] (1) Preparation of MCM-41 raw powder: a proper amount of cetyltrimethylammonium bromide (DTAB) is added to 4.8 L of distilled water to form a homogeneous solution under stirring. 35 mL of sodium hydroxide (2 M) solution is added to the solution, and stirring is continued at 80℃ for 5 minutes. Then, a proper amount of tetraethyl orthosilicate (TEOS) is added, and the stirring reaction is continued at 80℃ for 10 hours. After the reaction is completed, the product is collected, washed with distilled water, and dried at 60℃ for 24 hours. Finally, the obtained MCM-41 material is calcined at 550℃ for 5 hours to completely remove the surfactant, and the dried MCM-41 raw powder is obtained;
[0039] (2) Preparation of X-MCM-41 molecular sieve powder: the X-MCM-41 molecular sieve powder is prepared by ion exchange with Li + , K + , Mg 2+ , Ca2+ Fe 2+ Zn 2+ Ag + The MCM-41 raw powder obtained in (1) is ion exchanged with a solution of one of Fe, Zn, Ag, and Cu to obtain a mesoporous molecular sieve powder with different ion exchange, denoted as X-MCM-41 (X represents the type of metal); attapulgite, sesbania powder, etc. are all purchased through commercial channels, and the specifications are conventional specifications in the technical field.
[0040] The performance test method of the X-MCM-41 mesoporous molecular sieve microsphere adsorbent is as follows:
[0041] Wear rate: using a shock wear tester, a certain mass (m0) of microsphere sample is shaken and rubbed under specific conditions, the un-powdered particles are screened and weighed (m1), and the wear rate = (m - m1) / m0 x 100%.
[0042] BET specific surface area: obtained by BET (Brunauer-Emmett-Teller) model calculation using nitrogen adsorption-desorption isotherm.
[0043] Single particle compressive strength: randomly select 30 intact microspheres for testing using a micro-force testing machine, and take the average value.
[0044] Adsorption capacity: at a specific temperature (such as human body temperature 309K) and pressure, the saturated adsorption amount of the target gas (such as ammonia) is determined.
[0045] Example 1
[0046] 50g of cetyltrimethylammonium bromide (DTAB) was added to 4.8L of distilled water to form a homogeneous solution under stirring. 35 mL of sodium hydroxide (2 M) solution was added to the solution, and stirring was continued at 80℃ for 5 minutes. Then 250 mL of tetraethyl orthosilicate (TEOS) was added, and the stirring reaction was continued at 80℃ for 10h. After the reaction was completed, the product was collected, washed with distilled water, and dried at 60℃ for 24h. Finally, the obtained MCM-41 mesoporous molecular sieve was calcined at 550℃ for 5 hours to completely remove the surfactant, and dry MCM-41 raw powder was obtained. The silicon aluminum ratio of the MCM-41 raw powder was determined by XRF, and the silicon aluminum ratio was selected to be 40-80.
[0047] Example 2
[0048] The obtained MCM-41 raw powder (selecting the silicon aluminum ratio SiO2 / Al2O3=60) was ion exchanged with zinc ions (Zn 2+ ) (zinc ion exchange degree of 75%), and then activated by calcination at 350℃ under vacuum atmosphere for 10 hours to obtain Zn-MCM-41 powder.
[0049] The obtained MCM-41 raw powder is respectively subjected to Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ , Ag + metal ion exchange to obtain Li-MCM-41, K-MCM-41, Mg-MCM-41, Ca-MCM-41, Fe-MCM-41, Zn-MCM-41, Ag-MCM-41 powder, and the above are collectively referred to as X-MCM-41 powder.
[0050] Example 3
[0051] 70 g of Zn-MCM-41 powder (silicon aluminum ratio of 60, ion exchange degree of 75%) exchanged with zinc ions (Zn 2+ ) is weighed, 25 g of attapulgite, and 5 g of sesbania powder are weighed. In a high-speed blender, the sesbania powder is first added to 120 g of 50°C warm water, and stirred at 1000 rpm until completely dissolved into a transparent viscous liquid. Then, the Zn-MCM-41 powder and the attapulgite are added, and the stirring speed is increased to 2500 rpm, and the shearing stirring is continued for 40 minutes to obtain a uniform and flowable slurry with a solid content of about 38% and a viscosity of about 1500 mPa·s;
[0052] The prepared slurry is transferred to the feed tank of the pressure type spray granulation tower; a gas flow type atomizing nozzle with a pore size of 0.5 mm is used, and the atomization is carried out under a compressed air pressure of 0.5 MPa; the hot air inlet temperature of the tower is set to 180°C, and the outlet temperature is about 80°C; the green microspheres of 40-60 mesh are collected at the cyclone separator at the bottom of the tower;
[0053] The green microspheres are placed in a constant temperature and humidity box, and first aged and dried at 35°C and a humidity of 93% for 3 hours; then the temperature is programmed to increase to 55°C at a rate of 10°C / hour, while the humidity is reduced to 75%, and the drying is continued under this condition for 5 hours;
[0054] The dried microspheres are transferred to a muffle furnace, and are programmed to increase in temperature from room temperature to 520°C at a rate of 2°C / minute under an air atmosphere, and are calcined at 520°C for 4 hours; then the furnace is naturally cooled to room temperature, and the Zn-MCM-41 mesoporous molecular sieve microsphere adsorbent of the application is obtained, which is recorded as sample M1.
[0055] Example 4
[0056] 80 g of Ca-MCM-41 powder (silicon aluminum ratio of 60, ion exchange degree of 75%) exchanged with calcium ions (Ca 2+) exchanged Ca-MCM-41 powder (Si / Al ratio of 50, ion exchange degree of 70%), 15 g attapulgite, 5 g sesbania powder, 130 g deionized water were weighed; the slurry was prepared and the subsequent atomization, drying and calcination steps were the same as in Example 3. The obtained Ca-MCM-41 mesoporous molecular sieve microsphere adsorbent was recorded as sample M2.
[0057] Example 5
[0058] 65 g Ag + ) exchanged Ag-MCM-41 powder (Si / Al ratio of 70, ion exchange degree of 65%), 30 g attapulgite, 5 g sesbania powder, 150 g deionized water were weighed; the slurry was prepared and the subsequent atomization, drying and calcination steps were the same as in Example 3. The obtained Ag-MCM-41 mesoporous molecular sieve microsphere adsorbent was recorded as sample M3.
[0059] Comparative Example 1 (no sesbania powder)
[0060] 70 g molecular sieve Zn-MCM-41 powder, 25 g attapulgite, 0 g sesbania powder were weighed, and 120 g deionized water was added. After mixing according to the method of Example 3, the slurry could not obtain sufficient viscosity and was in a suspension state, which quickly separated into layers after standing. When atomization was attempted, the droplets could not maintain a spherical shape, and after drying, a large amount of irregular fragments and powder was obtained, and complete 40-60 mesh particles could not be collected. This was recorded as sample D1.
[0061] Comparative Example 2 (high temperature rapid drying)
[0062] The ingredients were exactly the same as in Example 3. After obtaining the green microspheres by atomization, instead of using programmed temperature drying, the microspheres were directly placed in a 105°C air drying oven for rapid drying for 2 hours. Obvious cracks were observed on the surface of the dried microspheres, and the strength was poor. The subsequent calcination step was the same as in Example 1. The obtained microspheres were recorded as sample D2.
[0063] Comparative Example 3 (too high calcination temperature)
[0064] The ingredients were exactly the same as in Example 3. The atomization and drying steps were the same as in Example 3. In the calcination stage, the final calcination temperature was increased to 650°C, and the other conditions remained unchanged. The obtained microspheres were recorded as sample D3.
[0065] Table 1 Performance comparison table
[0066]
[0067] Result analysis
[0068] As can be seen from the comparison between Example 3 and Comparative Example 1, the use of rice bean powder as a thickening agent and a binder is essential for forming a stable slurry and obtaining green microspheres with sufficient "green strength", and the absence of rice bean powder directly leads to the failure of spray forming.
[0069] As can be seen from the comparison between Example 3 and Comparative Example 2, the use of the temperature-programmed drying process according to the present application is essential for preventing microspheres from cracking and obtaining low powdering rate and high toughness. Rapid high-temperature drying leads to the concentration of internal stress, a significant increase in the powdering rate of the product, and a serious decrease in the mechanical strength.
[0070] As can be seen from the comparison between Example 3 and Comparative Example 3, the calcination temperature has a decisive influence on the balance between the mechanical strength and the adsorption performance of the microspheres. A too high calcination temperature (650°C) can further improve the hardness and the compressive strength of the microspheres, but will lead to the partial collapse or sintering of the mesoporous structure, resulting in a significant decrease in the specific surface area and the adsorption capacity, and the loss of the core function of the microspheres as an adsorbent.
[0071] As can be seen from the comparison between Examples 3-5, within the range of the ingredients described in the present application, microspheres with excellent comprehensive performance can be successfully prepared. Example 3 (M1) achieves the best balance between the mechanical strength (abrasion rate 0.8%, compressive strength 6.5N) and the adsorption performance (specific surface area 820m 2 / g, adsorption capacity 3.5 mmol / g), and has the best comprehensive performance. Example 4 (M2) has the highest MCM-41 content, the largest specific surface area and adsorption capacity, but the mechanical strength is slightly inferior. Example 5 (M3) has the highest mechanical strength due to the high content of the binder skeleton (attapulgite), but the specific surface area and the adsorption capacity are sacrificed. In practical applications, different proportions can be selected according to specific needs.
[0072] The above is only a few specific embodiments of the present application, and does not limit the present application in any form. Any simple modification, equivalent change and modification made according to the technical essence of the present application to the above embodiments still falls within the scope of the technical solutions of the present application.
Claims
1. A method for molding X-MCM-41 mesoporous molecular sieve microsphere adsorbent, characterized in that, Preparation by the following steps: S1: slurry preparation: 50-85 parts of X-MCM-41 molecular sieve powder modified by metal ion exchange, 10-40 parts of attapulgite, 3-8 parts of sesbania powder and 80-200 parts of water are mixed to prepare a uniform and flowable slurry by high-speed shearing at 2500 rpm; the solid content of the slurry is controlled at 30%-40%, and the viscosity is 800-2500 mPa·s; the X-MCM-41 molecular sieve powder modified by metal ion exchange is at least one of Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ , Ag + ; the selected weight ratio of the X-MCM-41 molecular sieve powder modified by metal ion exchange, attapulgite and sesbania powder is (65-75):(20-30):(4-6); S2: atomization granulation: the slurry obtained in step S1 is atomized into droplets by an atomizing nozzle under the action of compressed air, and the droplets are dried by hot air blowing at 100-250℃ in a granulation tower to form 40-60 mesh green microspheres; S3: drying: the green microspheres are subjected to programmed temperature drying in a humidity environment of 70%-95% at a temperature of 30-60℃ for 4-12 hours; the specific steps of the programmed temperature drying are: first constant temperature and humidity at 30-40℃ and 90%-95% humidity for 2-4 hours, then slowly heated to 50-60℃ and constant temperature and humidity at 70%-80% humidity for 2-8 hours; S4: calcination: the dried microspheres are heated to 450-600℃ at a rate of 1-5℃ / min in air or inert atmosphere, and calcined for 2-6 hours to obtain the X-MCM-41 mesoporous molecular sieve microsphere adsorbent.
2. The method for forming the X-MCM-41 mesoporous molecular sieve microsphere adsorbent according to claim 1, characterized in that, The preparation process of the metal ion exchanged X-MCM-41 molecular sieve powder: ion exchange MCM-41 raw powder with a solution containing Li + , K + , Mg 2+ , Ca 2+ , Fe 2+ , Zn 2+ or Ag + , to obtain different ion exchanged mesoporous molecular sieve powder, denoted as X-MCM-41.
3. The method for forming the X-MCM-41 mesoporous molecular sieve microsphere adsorbent according to claim 1, characterized in that, The selected conditions for calcination are: heating to 500-550℃ at a rate of 2℃ / min, and calcining for 3-5 hours.
4. The X-MCM-41 mesoporous molecular sieve microsphere adsorbent obtained from the shaping method according to any one of claims 1 to 3, characterized in that, The particle size range is 40-60 mesh.
5. The X-MCM-41 mesoporous molecular sieve microsphere adsorbent according to claim 4, characterized in that, The performance index meets: wear rate ≤ 1.2 wt%, BET specific surface area ≥ 750 m 2 / g.
6. Use of the X-MCM-41 mesoporous molecular sieve microsphere adsorbent according to claim 5, characterized in that, In the preparation of sanitary napkins, urine pads, or other sanitary care products that directly contact human skin, it is used for adsorbing one or more irritating odor gas of ammonia, trimethylamine, hydrogen sulfide, isovaleric acid, methyl mercaptan, indole, nonanal, decanal.
Citation Information
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