CN115155518A - High-strength molecular sieve and preparation method thereof - Google Patents
High-strength molecular sieve and preparation method thereof Download PDFInfo
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- CN115155518A CN115155518A CN202210849724.8A CN202210849724A CN115155518A CN 115155518 A CN115155518 A CN 115155518A CN 202210849724 A CN202210849724 A CN 202210849724A CN 115155518 A CN115155518 A CN 115155518A
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract
The invention provides a high-strength molecular sieve and a preparation method thereof, wherein the preparation method comprises the steps of putting a formed molecular sieve into a glass fiber aqueous solution flowing slowly, driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid, enabling micron-sized glass fibers to be uniformly wrapped on the surface of the formed molecular sieve, and washing, drying and roasting to obtain the formed molecular sieve wrapped by the glass fibers; and (3) carrying out secondary crystallization on the formed molecular sieve wrapped by the glass fiber, and washing, drying and roasting the solid product to obtain the high-strength molecular sieve. The high-strength molecular sieve provided by the invention has higher mechanical strength and lower abrasion rate than a formed molecular sieve prepared by a conventional method, and has more smooth pore channels, so that the problems of activity reduction of the molecular sieve and the like caused by forming can be avoided.
Description
Technical Field
The invention belongs to the technical field of oil chemical industry, and particularly relates to a high-strength molecular sieve and a preparation method thereof, which are applied to aspects of gas/liquid adsorption separation and the like.
Background
Due to the special pore structure and chemical properties of the molecular sieve, the molecular sieve serving as a catalyst and an adsorbent is widely applied to petrochemical processes such as acid catalytic reaction and gas/liquid separation, dehydration, desulfurization and the like. During industrial applications, molecular sieves require frequent regeneration treatments, such as: the strong acidity of the molecular sieve is particularly easy to coke and generate carbon when catalyzing various alkane reactions, so that the catalyst is deactivated, and the catalyst needs to be regenerated by periodically burning the carbon. Pressure swing adsorption is a process of separating or purifying gases by pressure change by utilizing the difference of adsorption characteristics of different gases on an adsorbent and the characteristic that adsorption capacity changes along with pressure change, so that a molecular sieve serving as the adsorbent needs to face pressure alternation. In addition, the molecular sieve for gas dehydration or desulfurization also needs periodic dehydration or desulfurization regeneration after adsorption saturation. All of these regeneration or pressure swing processes can damage the structure of the molecular sieve, resulting in loss of molecular sieve fines, and catalytic or adsorptive properties decrease with increasing regeneration times. Therefore, the development of the high-strength molecular sieve is beneficial to prolonging the service life of the molecular sieve adsorbent/catalyst, and has important practical significance.
In order to improve the mechanical strength of the molecular sieve, a binder, a structural reinforcing agent, an organic solvent, or the like is generally added to the molecular sieve during the molecular sieve forming process to improve the strength of the formed molecular sieve. At present, many documents report methods for preparing high-strength molecular sieves, for example, patent CN2011103715680 introduces a structural reinforcing agent and a binder into a molecular sieve, and the obtained molecular sieve has significantly higher side pressure strength than a common molecular sieve, and at the same time, the abrasion rate is significantly reduced. Patent CN2006800294206 reports a preparation method for improving the abrasion resistance of methanol to olefin catalyst, which is to add a binder containing sodium silicate and acid alum to SAPO molecular sieve to increase the strength. Patent CN1044980C is to immerse a molecular sieve or a molecular sieve catalyst in an organic solution containing a silicon compound, an aluminum compound, a zirconium compound, etc. for a period of time, then recover the organic solvent, and dry and calcine the obtained molecular sieve to obtain a finished product, which has greatly improved mechanical strength. Patent US3354096 uses phosphate aqueous solution to treat the molecular sieve, and the mechanical strength of the finished molecular sieve is improved to a certain extent.
However, the prior art method has difficulty in ensuring that the activity of the molecular sieve is not affected while improving the strength of the molecular sieve, and the addition of components such as a structure enhancer and a binder can block the microporous pore channels of the molecular sieve to some extent, thereby reducing the activity of the molecular sieve. Therefore, on the premise of not influencing the activity of the molecular sieve as a catalyst or an adsorbent, the stability and strength of the molecular sieve can be further improved, so that the requirement of industrial application is better met.
Disclosure of Invention
The invention aims to provide a high-strength molecular sieve with good mechanical strength and a preparation method thereof on the premise of not influencing the activity of the molecular sieve. The glass fiber is an inorganic non-metallic material with excellent performance, and has the advantages of strong heat resistance, good corrosion resistance, high mechanical strength and the like. The invention uses the slow flow of liquid to evenly wrap micron-sized glass fibers in the solution on the surface of a formed molecular sieve, and then the glass fibers and the formed molecular sieve material form strong interaction through secondary crystallization to strengthen the strength of the molecular sieve material; meanwhile, the silicon source or the aluminum source added as the binder in the forming process of the original formed molecular sieve is dissolved and participates in the secondary crystallization process, so that the pore channel is more smooth.
The technical scheme of the invention is as follows:
a preparation method of a high-strength molecular sieve comprises the following steps:
the first step is as follows: preparation of glass fiber wrapped molecular sieve
Placing the formed molecular sieve into a slow flowing glass fiber aqueous solution, driving the formed molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid, uniformly wrapping micron-sized glass fibers on the surface of the formed molecular sieve, and washing, drying and roasting to obtain the formed molecular sieve wrapped by the glass fibers; the flow rate of the glass fiber aqueous solution is 0.01-0.2m/s; the second step is that: secondary crystallization of molecular sieve
And (3) carrying out secondary crystallization on the formed molecular sieve wrapped by the glass fiber to ensure that the formed molecular sieve and the glass fiber form strong interaction, and washing, drying and roasting a solid product to obtain the high-strength molecular sieve.
The formed molecular sieve is a formed molecular sieve which can be prepared by engineers familiar with the field, and the shape of the formed molecular sieve comprises various shapes such as a sphere, a bar, a special shape, a microspheric shape and the like; the raw materials of the formed molecular sieve comprise an aluminosilicate molecular sieve and a binder; furthermore, the aluminosilicate molecular sieve is an A-type molecular sieve, an X-type molecular sieve, a Y-type molecular sieve, a Beta molecular sieve or a ZSM series molecular sieve.
The binder comprises silicon element and aluminum element.
The filament diameter of the glass fiber is less than 15 micrometers, and further, the filament diameter of the glass fiber is less than 6 micrometers.
The mass percent of the glass fiber aqueous solution is 0.1-10%; the time of the formed molecular sieve in the glass fiber aqueous solution is 1-50 hours.
The first step also comprises the recycling of the glass fiber aqueous solution.
In the first step, the drying temperature is 100-120 ℃, and the drying time is 12-24 hours; the roasting temperature is 500-600 ℃, and the roasting time is 5-12 hours.
Engineers familiar with the art can adopt the synthesis methods reported in the published documents and patents, select the synthesis formula and conditions of the corresponding molecular sieve, and perform the second hydrothermal crystallization on the molecular sieve coated by the glass fiber.
The washing process in the second step comprises washing the solid product with deionized water to a pH =8-9; the drying temperature is 100-120 ℃, and the drying time is 12-24 hours; the roasting temperature is 500-600 ℃, and the roasting time is 5-12 hours.
The invention also provides the high-strength molecular sieve obtained by the method.
Compared with the prior art, the invention has the following beneficial effects:
the high-dispersion micron-sized glass fiber has high mechanical strength and is coated on the surface of the formed molecular sieve by utilizing the liquidity of liquid, and then the glass fiber and the formed molecular sieve form strong interaction through secondary hydrothermal crystallization. In addition, in the hydrothermal crystallization process, a silicon source or an aluminum source which is added as a binder in the forming process of the original formed molecular sieve can be dissolved and participate in the secondary crystallization process. Therefore, the high-strength molecular sieve provided by the invention has higher mechanical strength and lower abrasion rate than the formed molecular sieve prepared by the conventional method, and the pore channel is more smooth, so that the problems of activity reduction of the molecular sieve and the like caused by forming can be avoided.
Detailed Description
Example 1
Weighing 10g of industrial-grade spherical 13X molecular sieve (5-6 mm), putting the industrial-grade spherical 13X molecular sieve into 2% (mass percentage) of glass fiber aqueous solution flowing slowly at the flow rate of 0.1m/s, wherein the monofilament diameter of the glass fiber is 8 microns, soaking the glass fiber for 8 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-grade glass fibers are uniformly wrapped on the surface of the molecular sieve. Taking out the molecular sieve, drying for 10 hours at 110 ℃, and roasting for 5 hours at 540 ℃. 50g0.8M NaOH aqueous solution and 10g of spherical 13X molecular sieve coated with glass fiber are placed in a high-pressure hydrothermal crystallization kettle, crystallized at 90 ℃ for 24 hours, the obtained solid product is washed by deionized water until the pH is =8-9, dried at 110 ℃ for 10 hours, and roasted at 540 ℃ for 6 hours to obtain the high-strength spherical 13X molecular sieve (marked as A).
Example 2
Weighing 10g of industrial-grade spherical 13X molecular sieve (0.5-0.6 mm), putting the industrial-grade spherical 13X molecular sieve into a 0.12% glass fiber aqueous solution flowing slowly at the flow rate of 0.02m/s, wherein the diameter of a glass fiber monofilament is 4 microns, soaking for 2.5 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-grade glass fibers are uniformly coated on the surface of the molecular sieve. Taking out the molecular sieve, drying at 110 ℃ for 10 hours, and roasting at 540 ℃ for 5 hours. 50g of 0.3M NaOH aqueous solution and 10g of spherical 13X molecular sieve coated with glass fiber are placed in a high-pressure hydrothermal crystallization kettle, crystallization is carried out for 6 hours at 90 ℃, the obtained solid product is washed by deionized water until the pH value is =8-9, drying is carried out for 10 hours at 110 ℃, and roasting is carried out for 6 hours at 540 ℃, so as to obtain the high-strength spherical 13X molecular sieve (marked as B).
Example 3
Weighing 10g of industrial-grade strip-shaped ZSM-5 molecular sieve (phi 3 multiplied by 8 mm), putting the industrial-grade strip-shaped ZSM-5 molecular sieve into a 5% glass fiber aqueous solution flowing slowly at the flow rate of 0.15m/s, wherein the diameter of a single fiber of the glass fiber is 12 microns, infiltrating for 5 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-sized glass fibers are uniformly wrapped on the surface of the molecular sieve. Taking out the molecular sieve, drying at 110 ℃ for 10 hours, and roasting at 540 ℃ for 5 hours. 50g of 0.6% tetrapropylammonium hydroxide alkali solution, 0.06g of alumina and 10g of strip-shaped ZSM-5 molecular sieve coated with glass fibers are placed in a high-pressure hydrothermal crystallization kettle, crystallization is carried out for 24 hours at 170 ℃, the obtained solid product is washed by deionized water until the pH value is =8-9, drying is carried out for 10 hours at 110 ℃, and roasting is carried out for 6 hours at 540 ℃, so as to obtain the high-strength strip-shaped ZSM-5 molecular sieve (marked as C).
Example 4
Weighing 10g of industrial-grade strip Beta molecular sieve (phi 3 multiplied by 10 mm) and putting the industrial-grade strip Beta molecular sieve into 4% glass fiber aqueous solution flowing slowly at the flow rate of 0.15m/s, wherein the diameter of a single fiber of the glass fiber is 10 microns, soaking the glass fiber for 5 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-grade glass fibers are uniformly wrapped on the surface of the molecular sieve. Taking out the molecular sieve, drying at 110 ℃ for 10 hours, and roasting at 540 ℃ for 5 hours. 50g of 0.6 percent tetraethylammonium hydroxide alkali solution, 0.06g of alumina and 10g of strip Beta molecular sieve coated with glass fiber are placed in a high-pressure hydrothermal crystallization kettle, crystallized at 150 ℃ for 24 hours, the obtained solid product is washed by deionized water until the pH is =8-9, dried at 110 ℃ for 10 hours and roasted at 540 ℃ for 6 hours, and the high-strength strip Beta molecular sieve (marked as D) is obtained.
Example 5
Weighing 10g of industrial-grade spherical 3A molecular sieve (3-5 mm), putting the molecular sieve into a 2% glass fiber aqueous solution flowing slowly at the flow rate of 0.08m/s, soaking the glass fiber aqueous solution for 6 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-grade glass fibers are uniformly wrapped on the surface of the molecular sieve. Taking out the molecular sieve, drying for 10 hours at 110 ℃, and roasting for 5 hours at 540 ℃. 50g of 0.5M NaOH aqueous solution, 0.01g of sodium metaaluminate and 10g of spherical 3A molecular sieve coated with glass fiber are placed in a high-pressure hydrothermal crystallization kettle, crystallized at 100 ℃ for 4 hours, the obtained solid product is washed by deionized water until the pH value is =8-9, dried at 110 ℃ for 10 hours, and roasted at 540 ℃ for 6 hours, and the high-strength spherical 3A molecular sieve (marked as E) is obtained.
Example 6
Weighing 10g of industrial-grade strip NaY molecular sieve (phi 3 multiplied by 10 mm) and putting the industrial-grade strip NaY molecular sieve into a 2% glass fiber aqueous solution flowing slowly at the flow rate of 0.1m/s, wherein the diameter of a single fiber of the glass fiber is 10 microns, soaking the glass fiber for 10 hours, and driving the molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid so that micron-grade glass fibers are uniformly wrapped on the surface of the molecular sieve. Taking out the molecular sieve, drying for 10 hours at 110 ℃, and roasting for 5 hours at 540 ℃. 50g of 0.8M NaOH aqueous solution and 10g of strip NaY molecular sieve coated with glass fiber are placed in a high-pressure hydrothermal crystallization kettle, crystallization is carried out for 8 hours at 90 ℃, the obtained solid product is washed by deionized water until the pH is =8-9, drying is carried out for 10 hours at 110 ℃, and roasting is carried out for 6 hours at 540 ℃, thus obtaining the high-strength strip NaY molecular sieve (recorded as F).
Test example 1
The side compressive strength and the abrasion ratio of the above samples were measured, respectively, and as shown in Table 1, the side compressive strength and the abrasion ratio of the original industrial sample and each of the samples (A to F) after the preparation of the present invention are shown, it can be seen that the molecular sieve prepared by the present invention has higher mechanical strength and lower abrasion ratio than the industrially shaped molecular sieve prepared by the conventional method.
TABLE 1 side compressive Strength and abrasion Rate of the samples
Test example 2
Material texture measurements were performed on technical grade spheres 13X (5-6 mm and 0.5-0.6 mm) and examples 1-2 (A and B) by nitrogen physisorption with the results shown in Table 2. As shown in the data in the table, the specific surface area, pore volume and other data of the formed molecular sieve prepared by the method and the original formed molecular sieve are increased to a certain extent, so that the pore channel is smoother than the original formed material.
TABLE 2 texture Structure of materials for technical grade spherical 13X (5-6 mm and 0.5-0.6 mm) and molecular sieve products of examples 1-2 (A and B)
Claims (7)
1. A preparation method of a high-strength molecular sieve is characterized by comprising the following steps: the method comprises the following steps:
the first step is as follows: preparation of glass fiber wrapped molecular sieve
Placing the formed molecular sieve into a slow flowing glass fiber aqueous solution, driving the formed molecular sieve to suspend and rotate by utilizing the circulating fluidity of liquid, uniformly wrapping micron-sized glass fibers on the surface of the formed molecular sieve, and washing, drying and roasting to obtain the formed molecular sieve wrapped by the glass fibers; the flow rate of the glass fiber aqueous solution is 0.01-0.2m/s;
the second step is that: secondary crystallization of molecular sieve
And (3) carrying out secondary crystallization on the formed molecular sieve wrapped by the glass fiber, and washing, drying and roasting the solid product to obtain the high-strength molecular sieve.
2. The method of claim 1, wherein the step of preparing a high strength molecular sieve comprises: the raw materials of the formed molecular sieve comprise an aluminosilicate molecular sieve and a binder.
3. The method of claim 2, wherein the step of preparing a high strength molecular sieve comprises: the aluminosilicate molecular sieve is an A-type molecular sieve, an X-type molecular sieve, a Y-type molecular sieve, a Beta molecular sieve or a ZSM series molecular sieve.
4. The method of claim 1, wherein the step of preparing a high strength molecular sieve comprises: the monofilament diameter of the glass fiber is less than 15 microns.
5. The method of claim 1, wherein the step of preparing a high strength molecular sieve comprises: the mass percent of the glass fiber aqueous solution is 0.1-10%; the time of the formed molecular sieve in the glass fiber aqueous solution is 1-50 hours.
6. The method of claim 1, wherein the step of preparing a high strength molecular sieve comprises: the first step also comprises the recycling of the glass fiber aqueous solution.
7. A high strength molecular sieve obtainable by the process of claim 1.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05146676A (en) * | 1991-11-27 | 1993-06-15 | Kawata Mfg Co Ltd | Honeycomb-like ceramic body containing adsorptive zeolite and production thereof |
| JP2000042366A (en) * | 1998-08-03 | 2000-02-15 | Nisshin Steel Co Ltd | Nox and sox decomposing and removing material, and its production |
| US20130225397A1 (en) * | 2010-08-23 | 2013-08-29 | Shanghai Research Institute Of Petrochemical Technology, Sinopec | Binderless Molecular Sieve Catalyst and a Preparation Method Thereof |
| CN108905970A (en) * | 2018-07-23 | 2018-11-30 | 山东建筑大学 | The preparation method and application of cadmium adsorbent is removed based on the modified water body of clinoptilolite |
| CN111760589A (en) * | 2020-07-10 | 2020-10-13 | 大唐国际化工技术研究院有限公司 | Molecular sieve catalyst, preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05146676A (en) * | 1991-11-27 | 1993-06-15 | Kawata Mfg Co Ltd | Honeycomb-like ceramic body containing adsorptive zeolite and production thereof |
| JP2000042366A (en) * | 1998-08-03 | 2000-02-15 | Nisshin Steel Co Ltd | Nox and sox decomposing and removing material, and its production |
| US20130225397A1 (en) * | 2010-08-23 | 2013-08-29 | Shanghai Research Institute Of Petrochemical Technology, Sinopec | Binderless Molecular Sieve Catalyst and a Preparation Method Thereof |
| CN108905970A (en) * | 2018-07-23 | 2018-11-30 | 山东建筑大学 | The preparation method and application of cadmium adsorbent is removed based on the modified water body of clinoptilolite |
| CN111760589A (en) * | 2020-07-10 | 2020-10-13 | 大唐国际化工技术研究院有限公司 | Molecular sieve catalyst, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘咏;魏巍;赵仕林;张爱平;张宇;: "稀土/Y分子筛多相催化电解氧化深度去除渗滤液中难降解有机物", 环境科学学报, no. 04, pages 806 - 813 * |
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