CN101524639A - Prepartion method of high-intensity absorbent - Google Patents
Prepartion method of high-intensity absorbent Download PDFInfo
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Abstract
The invention relates to a preparation method of high-intensity absorbent, which is characterized in that components of the absorbent comprise a major active component LSX zeolite which accounts for 50-90% of weight, a caking agent selected from alumina gel, silicon gel and the like which accounts for 10-50% of weight, and a plasticiser/pore-expanding agent selected from methyl cellulose and the like which accounts for 1-3% of weight. The components are processed by treatments of pulping, drying, crushing and screening and then are moulded, dried, baked and activated, so as to obtain an absorbent product.
Description
Technical field
The present invention relates to the adsorption technology field, be a kind of high strength preparation of adsorbent method, this adsorbent is used for from gas except that anhydrating and carbon dioxide.The adsorbent that more particularly can be used for air, nitrogen, hydrogen and natural gas purification.
Technical background
Because carbon dioxide can freeze at low temperatures and generate hydrate with steam, so in gas application, it is a kind of undesirable impurity.For example, in fact the cryogenic system that is used for air separation production oxygen and nitrogen need remove carbon dioxide (1ppm or lower) and steam from air fully before separating.The carbon dioxide that exists in the air-flow of oil plant to hydrogen contamination and the quantity of moisture have similar requirement.In addition, petrochemical plant must be removed carbon dioxide and the water in monomer ethylene, the propylene, poisons and the polymer performance variation to prevent polymerization catalyst.
At present, two kinds of adsorption technologies are usually used in the gas separation: alternating temperature absorption (TSA) and transformation absorption (PSA).The efficient of two kinds of adsorption technologies is by the performance decision of adsorbent.The high adsorption capacity of carbon dioxide is the most important performance of this adsorbent.The fresh approach that is used for gas dewatering and carbon dioxide is to use molecular sieve, natural zeolite and synthetic zeolite.Known that synthetic A type zeolite and X type zeolite are the fertile absorbers of water and carbon dioxide.For example, US39811698,4711645,4986835,5156657 etc. proposes 5A, the 10A of use standard and the 13X molecular sieve adsorbent as carbon dioxide.With regard to the adsorption capacity of carbon dioxide, LSX is present optimal selection, but the adsorbent of making for the adsorption activity component with LSX, usually exist intensity low, shortcoming such as easy to wear makes the bed layer pressure of adsorbent increase, adsorbent is forced to change, and influences the production and the benefit of enterprise.
Because the bad mechanical strength of molecular sieve itself, in order to improve the mechanical strength of molecular sieve itself, people have adopted distinct methods, can be divided into four types:
One class is to add clay class adhesive in molecular sieve, after recrystallization and water treatment, improves the mechanical strength and the adsorption capacity of A type and X type molecular sieve.As JP03295802, DD299,635, JP295, patents such as 805.
One class is to add phosphate or inorganic oxide improving the mechanical strength of molecular sieve, handles with 5.0～43.0% ammonium phosphate solutions as benzene and ethylene alkylation zeolite catalyst and can improve mechanical strength, and US3,354,096 propose adding (NH in batching
4)
2HPO
4Make water polo, compression strength reaches 21.9 pounds, and Ger Offen 2,805,546 proposes to add oxide or its mixtures such as Cu, Ba, Mn, Fe, Co, Ni in molecular sieve, and the molecular sieve of making has better intensity.
One class is to add organic binding agent etc., JP59, and 269,22, JP59,26523, JP63,297,282 propose to add carbon fiber-containing element, plastics, coal, charcoal, paper pulp, plant, starch rubber polymer etc., compression strength＞17.3kg/cm
2
One class be under 550～700 ℃ with molecular sieve roasting under high-frequency electric field, can improve its mechanical strength, as USSR428,775.
Above-mentioned four class methods are being improved the molecular sieve mechanical strength in varying degrees, but said method does not all relate to the influence of granularity to mechanical strength.The intensity of the surface nature of powder after to its moulding plays an important role.Thin powder surface exists the chemical property of a large amount of unsaturated bonds and this fresh surface of lattice defect strong especially, and the chemical bond that the easiest with the most adjacent particle forms the interface combines and the atom diffusion.Particle is thin more, and external surface area is big more, and the duct is short more, and adsorption capacity is strong more, and absorption, desorb is fast more.Product strength with its moulding is higher, and high adsorption capacity.
The purpose of this invention is to provide a kind of high strength preparation of adsorbent method, this adsorbent is by the LSX molecular sieve pulp, and binding agent, plasticizer mix pulls an oar, and the slurries spray-drying is obtained thinner powder aftershaping make.The mechanical strength height is to the carbon dioxide high adsorption capacity.
Summary of the invention
The object of the present invention is to provide a kind of high strength preparation of adsorbent method, with the adsorbent mechanical strength height of its production, and to the carbon dioxide high adsorption capacity.
This preparation method provided by the invention, (the sodium ion mass fraction accounts for 90% of whole exchangeable cations gross mass marks at least with self-designed L SX molecular sieve, preferred 95%) is the adsorption activity component, the plasticizer that before the LSX molecular sieve does not filter, adds the binding agent of 10～50%wt and the 1～3%wt (vigorous stirring 0.5～5 hour of pulling an oar, preferred 1 hour), filter, washing, by the drying equipment drying, pulverize, sieve, the batch mixing extrusion molding or the rolling balling that obtain, drying, roasting, activation.Obtain the adsorbent of high strength, high carbon dioxide adsorption capacity.
A kind of high strength preparation of adsorbent method is characterized in that:
This adsorbent is formed and is comprised main active component and binding agent, and plasticizer/expanding agent;
Main active component accounts for 50～90% weight, is that silica/alumina mole ratio is 2.0～2.3 LSX zeolite; Binding agent accounts for 10～50% weight, for being selected from one or more of aluminium glue, silica gel, amorphous aluminum silicide, bentonite, kaolin, clinoptilolite, attapulgite or montmorillonite; Plasticizer/expanding agent accounts for 1～3% weight, for being selected from one or more of methylcellulose, sodium carboxymethylcellulose, sesbania powder;
This preparation of adsorbent technical process comprises:
(1) the LSX slurries that sodium ion exchange back sodium ion mass fraction in the LSX molecular sieve accounted at least whole exchangeable cations gross mass mark 90-98% mix making beating with binding agent, plasticizer/expanding agent, and the processing time is 0.5～5 hour;
(2) with the slurries drying in the step (1), the processing of pulverizing, sieve; Gained powder size≤50 μ m, gained powder solid content is 40～80%;
(3) batch mixing extrusion modling or the rolling moulding that step (2) is obtained, select a kind of mode of spray-drying, pneumatic conveying drying, rotary flashing drying or drum dried to carry out drying, then in 450～600 ℃ of following roastings 1～4 hour, activation processing, obtain the adsorbent product.
According to preparation method of the present invention, it is characterized in that sodium ion mass fraction in the described LSX molecular sieve of preparation process (1) step accounts for the 90-98% of whole exchangeable cations gross mass marks, preferred 95% at least.
According to preparation method of the present invention, it is characterized in that in the LSX molecular sieve pulp after binding agent and plasticizer/expanding agent in preparation process (1) step directly add the sodium ion exchange, vigorous stirring, the processing time is 0.5～5 hour, preferred 1 hour.
According to preparation method of the present invention, it is characterized in that optional drying mode of preparation process (2) step is spray-drying, pneumatic conveying drying, rotary flashing drying or drum dried, preferably spray drying.
According to preparation method of the present invention, it is characterized in that preparation process (2) step gained powder size≤50 μ m, preferred≤25 μ m.
According to preparation method of the present invention, it is characterized in that preparation process (2) step gained powder solid content is 40～80%, preferred 65%.
Vigorous stirring can make the granular size of LSX molecular sieve drop to 2～4 μ m from 3～5 μ m during the preparation process making beating.
The spray-drying that is adopted in said method is to adopt atomizer that raw slurry is dispersed into droplet, and uses the heated-air drying droplet, and obtains a kind of method of product.Spray-drying can be by the control hot blast temperature, flow, and the aperture is waited and is obtained varigrained powder and powder solid content, so that product conforms to quality requirements.
The adsorbent that the present invention is prepared has the following advantages:
1) high strength, high-wearing feature;
2) high absorption property is especially to CO
2Absorption.
This adsorbent is applicable to the cryogenic system of air separation production oxygen and nitrogen, is used for removing carbon dioxide (1ppm or lower) and steam fully from air before separating.
The specific embodiment
Example 1,
With 15%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose, LSX molecular sieve powder (surplus).Appropriate amount of deionized water was mediated 0.5 hour, product was extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 1 in 5 hours.
Example 2,
15%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 40～140 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 90 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 2 in 5 hours.
Example 3,
15%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 20～70 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 45 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 3 in 5 hours.
Example 4
15%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 5～40 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 20 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 4 in 5 hours.
Example 5,
With 20%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose, LSX molecular sieve powder (surplus).Appropriate amount of deionized water was mediated 0.5 hour, product was extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 5 in 5 hours.
Example 6,
20%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose are joined the powder that vigorous stirring in the LSX molecular sieve pulp, spray-drying particle diameter are distributed in 40～140 μ m, and the most probable particle diameter is 90 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 6 in 5 hours.
Example 7,
20%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 20～70 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 45 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 7 in 5 hours.
Example 8,
20%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 5～40 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 20 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 8 in 5 hours.
Example 9
With 25%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose, LSX molecular sieve powder (surplus).Appropriate amount of deionized water was mediated 0.5 hour, product was extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 9 in 5 hours.
Example 10,
25%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 40～140 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 90 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 10 in 5 hours.
Example 11,
25%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 20～70 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 45 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 11 in 5 hours.
Example 12,
25%wt attapulgite, 1%wt methylcellulose, 0.2%wt sodium carboxymethylcellulose joined vigorous stirring, spray-drying obtain the powder that particle diameter is distributed in 5～40 μ m in the LSX molecular sieve pulp, the most probable particle diameter is 20 μ m, formed absorbent.Product is extruded the form of φ 1.6mm extruded stock.Then extruded stock was descended dry 4 hours at 110 ℃, 550 ℃ of following roastings promptly got sample 12 in 5 hours.
Adsorbent intensity, absorption property the results are shown in table 1,2.The dynamic carbon dioxide adsorption capacity of molecular sieve is measured and is all adopted the 13X of the Ministry of Chemical Industry molecular sieve industry standard method to measure.Compression strength, rate of wear are measured and are all adopted the Ministry of Chemical Industry's standard method.
Table one, contain 15% binding agent performance of the adsorbent result
| Sample number | Compression strength N/cm | Rate of wear (%) | Dynamic CO absorption 2 mg/g(20℃) | Dynamic CO absorption 2 mg/g(10℃) |
| Sample 1 | 28 | 0.17 | 14.2 | 17.5 |
| Sample 2 | 34 | 0.15 | 14.3 | 17.2 |
| Sample 3 | 65 | 0.07 | 14.1 | 17.5 |
| Sample 4 | 82 | 0.06 | 14.2 | 17.4 |
Table two, contain 20% binding agent performance of the adsorbent result
| Sample number | Compression strength N/cm | Rate of wear (%) | Dynamic CO absorption 2 mg/g(20℃) | Dynamic CO absorption 2 mg/g(10℃) |
| Sample 5 | 34 | 0.16 | 13.1 | 16.1 |
| Sample 6 | 39 | 0.14 | 13.2 | 16.2 |
| Sample 7 | 75 | 0.06 | 13.1 | 16.2 |
| Sample 8 | 92 | 0.05 | 13.2 | 16.1 |
| Reference 1 (spherical) | 32N/ | 0.15 | 8.6 | 11.5 |
| Reference 2 (strip) | 50 | 0.18 | 9.8 | 12.5 |
| Reference 3 (strip) | 60 | 0.16 | 7.5 | 10.1 |
Table three, contain 25% binding agent performance of the adsorbent result
| Sample number | Compression strength N/cm | Rate of wear (%) | Dynamic CO absorption 2 mg/g(20℃) | Dynamic CO absorption 2 mg/g(10℃) |
| Sample 5 | 40 | 0.16 | 12.1 | 14.9 |
| Sample 6 | 42 | 0.14 | 12.2 | 14.7 |
| Sample 7 | 86 | 0.05 | 12.0 | 15.1 |
| Sample 8 | 102 | 0.05 | 12.2 | 15.2 |
Claims (2)
1, a kind of high strength preparation of adsorbent method is characterized in that:
Adsorbent is formed and is comprised main active component and binding agent, and plasticizer/expanding agent;
Main active component accounts for 50～90% weight, is that silica/alumina mole ratio is 2.0～2.3 LSX zeolite; Binding agent accounts for 10～50% weight, for being selected from one or more of aluminium glue, silica gel, amorphous aluminum silicide, bentonite, kaolin, clinoptilolite, attapulgite or montmorillonite; Plasticizer/expanding agent accounts for 1～3% weight, for being selected from one or more of methylcellulose, sodium carboxymethylcellulose, sesbania powder;
The preparation of adsorbent technical process comprises:
(1) the LSX slurries that sodium ion exchange back sodium ion mass fraction in the LSX molecular sieve accounted at least whole exchangeable cations gross mass mark 90-98% mix making beating with binding agent, plasticizer/expanding agent, and the processing time is 0.5～5 hour;
(2) with the slurries drying in the step (1), the processing of pulverizing, sieve; Gained powder size≤50 μ m, gained powder solid content is 40～80%;
(3) batch mixing extrusion modling or the rolling moulding that step (2) is obtained, select a kind of mode of spray-drying, pneumatic conveying drying, rotary flashing drying or drum dried to carry out drying, then in 450～600 ℃ of following roastings 1～4 hour, activation processing, obtain the adsorbent product.
2, according to the described preparation method of claim 1, it is characterized in that:
Sodium ion exchange back sodium ion mass fraction accounts for whole exchangeable cations gross mass marks at least and is chosen as 95% LSX slurries in the described LSX molecular sieve of preparation process (1) step; Mixing the making beating processing time is 1 hour; It is spray-drying that preparation process (2) step is selected drying mode, gained powder size≤25 μ m; The powder solid content is 65%.
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