CN115672264B - Preparation method of pressure swing adsorbent - Google Patents
Preparation method of pressure swing adsorbent Download PDFInfo
- Publication number
- CN115672264B CN115672264B CN202110867859.2A CN202110867859A CN115672264B CN 115672264 B CN115672264 B CN 115672264B CN 202110867859 A CN202110867859 A CN 202110867859A CN 115672264 B CN115672264 B CN 115672264B
- Authority
- CN
- China
- Prior art keywords
- temperature
- adsorbent
- molecular sieve
- hours
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003463 adsorbent Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002808 molecular sieve Substances 0.000 claims abstract description 39
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 39
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000004202 carbamide Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 22
- 239000003112 inhibitor Substances 0.000 claims description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 230000007062 hydrolysis Effects 0.000 claims description 19
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000005995 Aluminium silicate Substances 0.000 claims description 7
- 235000012211 aluminium silicate Nutrition 0.000 claims description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 229960000892 attapulgite Drugs 0.000 claims description 5
- 229910052625 palygorskite Inorganic materials 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000005909 Kieselgur Substances 0.000 claims 1
- 244000275012 Sesbania cannabina Species 0.000 claims 1
- 150000003863 ammonium salts Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 25
- 239000004927 clay Substances 0.000 abstract description 14
- 239000011148 porous material Substances 0.000 abstract description 12
- 239000003513 alkali Substances 0.000 abstract description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 description 8
- 238000000926 separation method Methods 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000012467 final product Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 241000219782 Sesbania Species 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- -1 polysiloxane Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052665 sodalite Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000009495 sugar coating Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a preparation method of a pressure swing adsorbent. Firstly, uniformly mixing 5A molecular sieve raw powder, clay and an auxiliary agent, then forming and roasting, then placing the formed body adsorbent into urea aqueous solution, hydrolyzing urea to form alkali solution by increasing the temperature, dissolving the clay blocked between the molecular sieve adsorbents, and realizing the smoothness of pore channels of the adsorbent. In the method, urea is used as an alkali source, so that the 5A molecular sieve can be effectively prevented from being exchanged for the 4A molecular sieve, the original structure of the molecular sieve adsorbent is protected, and the adsorption efficiency is effectively improved.
Description
Technical Field
The invention belongs to the field of adsorbent synthesis, and particularly relates to a preparation method of a pressure swing adsorbent.
Background
The 5A molecular sieve has a good adsorption separation effect and is widely applied to adsorption separation devices. The 5A molecular sieve adsorbents can generally be synthesized by several routes: (1) Performing calcium ion exchange on the 4A molecular sieve raw powder to obtain a 5A molecular sieve, and then forming; (2) The 5A molecular sieve is obtained by calcium ion exchange after the 4A molecular sieve is molded; and (3) directly molding the 5A molecular sieve raw powder. The 5A raw powder is directly molded, clay such as kaolin and attapulgite is generally selected as a binder, and the molded adsorbent synthesized by the method has higher strength, but the adsorption efficiency of the molecular sieve is greatly reduced because the clay is easy to block the pore channels of the molecular sieve.
Patent CN 106475049a describes a method for preparing 5A molecular sieve without alkali treatment and in-situ crystallization, mixing NaA molecular sieve raw powder with CaO with particle size smaller than 50 microns in proportion, shaping, drying and roasting the obtained powder, washing with water to pH smaller than 10, and activating to obtain the binder-free 5A molecular sieve adsorbent. Patent CN 109534356a describes a method for preparing a 5A molecular sieve composite material by compression molding, which takes 5A molecular sieve raw powder, polysiloxane and carbon material as raw materials to form a composite material with high thermal conductivity. Patent CN 1248488A describes a molecular sieve molding method, which directly adopts 5A molecular sieve raw powder, clay and water glass liquid to be molded by a sugar coating machine in a rolling ball way, thus obtaining the molded body adsorbent. The patent CN 105749859A mixes the 5A molecular sieve raw powder with natural clay, adds calcium nitrate solution, and then carries out rolling ball forming to obtain the formed molecular sieve adsorbent. In many methods, clay such as kaolin, attapulgite and the like is generally selected as a binder for direct molding of the 5A raw powder, and the clay is easy to block pore channels of the molecular sieve, so that the effective structure of the molecular sieve is greatly reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an adsorbent. Firstly, uniformly mixing 5A molecular sieve raw powder, clay and an auxiliary agent, then forming and roasting, then placing the formed body adsorbent into urea aqueous solution, hydrolyzing urea to form alkali solution by increasing the temperature, dissolving the clay blocked between the molecular sieve adsorbents, and realizing the smoothness of pore channels of the adsorbent. Meanwhile, urea is used as an alkali source, so that the urea can be effectively prevented from being exchanged into a 4A molecular sieve, the original structure of the molecular sieve adsorbent is protected, and the adsorption efficiency is effectively improved.
The preparation method of the pressure swing adsorbent comprises the following steps:
(1) Taking 75-90 parts by weight of 5A molecular sieve, 10-25 parts by weight of binder and 2-10 parts by weight of bonding auxiliary agent, uniformly mixing, and then forming, drying and roasting to obtain an intermediate adsorbent;
(2) Adding 10-30 parts by weight of an intermediate adsorbent into urea solution with a certain concentration, uniformly stirring, reacting for 1-8 hours at 90-150 ℃, and dissolving out a binder blocked in an adsorbent pore canal by alkali generated by urea hydrolysis to realize the smoothness of the adsorbent pore canal;
(3) And (3) separating the product obtained in the step (2), and washing, drying and roasting the obtained solid to obtain the final adsorbent product.
Further, the binder in the step (1) is generally one or more selected from kaolin, attapulgite, diatomite and bentonite, and the binding aid can be one or more selected from sesbania powder, carboxymethyl cellulose and sodium carboxymethyl cellulose. The molding method adopts the conventional method in the field, such as extrusion, rolling, extrusion and rolling.
Further, the conditions of drying and baking in step (1) are conventional conditions in the art. If the drying temperature is generally 80-120 ℃, the drying time is generally 6-24 hours; the roasting temperature is generally 350-550 ℃, and the roasting time is generally 1-6 h.
Further, the concentration of the urea aqueous solution in the step (2) is generally 0.2 to 1.0 mol/L. The liquid-solid ratio of the urea aqueous solution to the intermediate adsorbent is generally 3 to 10mL/g. Preferably, a certain amount of hydrolysis inhibitor is added into the urea aqueous solution in the heating reaction process, so that the urea hydrolysis reaction is stably carried out, and the side effect caused by the instant over-high pH value of the system is avoided.
Further, the inhibitor added in the step (2) is selected from more than one of ammonium chloride, ammonium sulfide, ammonium bicarbonate or ammonium carbonate.
Further, the hydrolysis inhibitor is preferably added in two steps to maintain a relatively stable alkalinity in the system. When the temperature of the system reaches 80-95 ℃, adding a hydrolysis inhibitor into the solution at a speed of 0.001-0.008 mol/L per ten minutes, and when the temperature is raised to 95-120 ℃, adding the hydrolysis inhibitor into the system at a speed of 0.01-0.02 mol/L per ten minutes until the concentration of the inhibitor in the urea aqueous solution reaches 0.1-0.5 mol/L.
Further, the reaction temperature in the step (2) is preferably 95-120 ℃, and the reaction time is preferably 4-6 hours.
Further, the temperature raising process in the step (2) is performed in two steps: the initial reaction speed is 5-10 ℃/min; and after the inhibition is started to be added into the system, the temperature rising rate is adjusted to be 0.5-2 ℃/min.
Further, the separation, washing, drying and calcination in step (4) are conventional operations in the art. If separation can be achieved by filtration, washing refers to washing with deionized water several times; the drying temperature is generally 80-150 ℃, and the drying time is generally 12-48 h; the roasting temperature is generally 300-550 ℃, and the roasting time is generally 2-10 h.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a preparation method of a pressure swing adsorbent, which adopts urea as an alkali source, utilizes the characteristic that urea solution is neutral at low temperature, and the pH value of the solution is gradually increased by urea decomposition after the solution reaches a certain temperature, replaces the traditional strong alkali sodium hydroxide, and hydroxyl ions generated by urea hydrolysis can react with clay blocked in pore channels and dissolve the clay so as to realize the smoothness of the pore channels of the adsorbent, solve the problem that the formed body adsorbent is influenced by the blocking of the clay, and further improve the mass transfer rate of the formed body adsorbent.
2. The hydrolysis rate of urea is greatly affected by temperature, and at low temperature, the hydrolysis rate of urea is slower, and after reaching a certain temperature, the hydrolysis reaction is more severe, but the 5A formed body needs a relatively stable environment, so that the temperature rising rate and the reaction time need to be controlled very accurately, and the operation severity is increased. In the invention, in order to slow down or inhibit the severe hydrolysis reaction of urea after the temperature of the system is raised, a proper amount of inhibitor is added into the system so as to create a relatively stable alkaline environment. The addition of the inhibitor can effectively control the excessive ionization speed of the ammonia water and maintain the stable alkalinity environment of the system, so that on one hand, the controllable dissolution reaction of the binder in the adsorbent pore canal can be realized, and on the other hand, the operation severity can be greatly reduced.
3. According to the invention, the urea aqueous solution without sodium ions is used as an alkali source, so that the 5A molecular sieve is prevented from being exchanged into the 4A molecular sieve or the sodalite as much as possible on the premise of effectively solving the problem that clay blocks the pore canal of the adsorbent, the original structure of the 5A molecular sieve is maintained, and the adsorption efficiency is further improved.
Detailed Description
The technical contents and effects of the present invention are further described below with reference to the examples, but the present invention is not limited to the examples. The specific surface area of the 5A molecular sieve is 672m 2 Per g, pore volume of 0.2746cm 3 Kaolin/g was taken from Suzhou.
Example 1
Taking 90 parts by weight of 5A molecular sieve, 10 parts by weight of kaolin and 6 parts by weight of sesbania powder, mechanically mixing uniformly, molding, drying at 100 ℃ for 12 hours, and roasting at 400 ℃ for 3 hours to obtain an intermediate molded body. 15 parts by weight of the intermediate molded body was added to a urea solution (liquid-solid ratio: 6 mL/g) of 0.8mol/L and stirred uniformly. First, after raising the temperature to 80℃at a rate of 6℃per minute, the addition of ammonium chloride to the solution was started at a rate of 0.006mol/L per ten minutes while continuing to raise the temperature to 105℃at a rate of 1℃per minute, ammonium chloride was added to the solution at a rate of 0.015 mol/L per ten minutes until the concentration of the hydrolysis inhibitor in the solution reached 0.3mol/L, and reaction 4h was continued. After separation and washing, the mixture was dried at 100℃for 24 hours and calcined at 400℃for 2 hours to obtain a final product, and the results of the performance evaluation are shown in Table 1.
Example 2
Taking 85 parts by weight of 5A molecular sieve, 15 parts by weight of bentonite and 2 parts by weight of carboxymethyl cellulose, mechanically mixing uniformly, molding, drying at 120 ℃ for 6 hours, and roasting at 550 ℃ for 1 hour to obtain an intermediate molded body. 15 parts by weight of the intermediate molded body was added to a urea solution (3 mL/g in terms of liquid-solid ratio) of 0.2mol/L and stirred well. First, after raising the temperature to 95℃at a rate of 10℃per minute, the addition of ammonium chloride to the solution was started at a rate of 0.008mol/L per ten minutes while continuing to raise the temperature to 110℃at a rate of 2℃per minute, ammonium chloride was added to the solution at a rate of 0.01mol/L per ten minutes until the concentration of the hydrolysis inhibitor in the solution reached 0.2mol/L, and reaction 4h was carried out. After separation and washing, the mixture was dried at 150℃for 12 hours and calcined at 350℃for 10 hours to obtain a final product, and the results of the performance evaluation are shown in Table 1.
Example 3
Taking 80 parts by weight of 5A molecular sieve, 20 parts by weight of kaolin and 10 parts by weight of sesbania powder, mechanically mixing uniformly, molding, drying at 80 ℃ for 20h, and roasting at 350 ℃ for 2h to obtain an intermediate molded body. 15 parts by weight of the intermediate molded body was added to a 1.0mol/L urea solution (liquid-solid ratio: 10 mL/g) and stirred well. First, after raising the temperature to 90℃at a rate of 5℃per minute, the addition of ammonium chloride to the solution was started at a rate of 0.006mol/L per ten minutes while continuing to raise the temperature to 120℃at a rate of 1.5℃per minute, and ammonium chloride was added to the solution at a rate of 0.02mol/L per ten minutes until the concentration of the hydrolysis inhibitor in the solution reached 0.5mol/L, and reaction 4h was carried out. After separation and washing, the mixture was dried at 120℃for 20 hours and calcined at 500℃for 10 hours to obtain a final product, and the results of the performance evaluation are shown in Table 1.
Example 4
Taking 70 parts by weight of 5A molecular sieve, 30 parts by weight of attapulgite and 8 parts by weight of carboxymethyl cellulose, mechanically mixing uniformly, molding, drying at 110 ℃ for 24 hours, and roasting at 400 ℃ for 6 hours to obtain an intermediate molded body. 15 parts by weight of the intermediate molded body was added to a urea solution (liquid-solid ratio: 8 mL/g) of 0.6mol/L and stirred uniformly. First, after raising the temperature to 85℃at a rate of 8℃per minute, the addition of ammonium chloride to the solution was started at a rate of 0.005mol/L per ten minutes while continuing to raise the temperature to 95℃at a rate of 0.5℃per minute, ammonium chloride was added to the solution at a rate of 0.012mol/L per ten minutes until the concentration of the hydrolysis inhibitor in the solution reached 0.1mol/L, and reaction 6h was carried out. After separation and washing, the mixture was dried at 110℃for 18 hours and calcined at 300℃for 2 hours to obtain a final product, and the results of the performance evaluation are shown in Table 1.
Example 5
The adsorbent was prepared and evaluated essentially as in example 1. The difference is that: during the addition of the aqueous urea solution, no inhibitor was added. The results of evaluating the properties of the final product are shown in Table 1.
Comparative example 1
The adsorbent was prepared and evaluated as in example 1, except that: the molded product was directly used as a product without alkali treatment to prepare a reference agent B1, and the performance evaluation results are shown in Table 1.
Comparative example 2
The adsorbent was prepared and evaluated as in example 1, except that: the sodium hydroxide was used as an alkali source to prepare a reference agent B2, and the results of performance evaluation thereof are shown in Table 1.
In the examples and comparative examples of the present invention, the specific surface area was calculated by using nitrogen as the adsorbent and the BET method, the pore volume was calculated by using the t-plot method, and N 2 The adsorption quantity is measured by a volumetric adsorption instrument, and the intensity is measured by a GB/T13550-2515 method.
TABLE 1 evaluation results of adsorbent Performance
Claims (8)
1. A method for preparing a pressure swing adsorbent, comprising the steps of:
(1) Taking 75-90 parts by weight of 5A molecular sieve, 10-25 parts by weight of binder and 2-10 parts by weight of bonding auxiliary agent, uniformly mixing, and then forming, drying and roasting to obtain an intermediate adsorbent;
(2) Adding 10-30 parts by weight of an intermediate adsorbent into a urea aqueous solution with a certain concentration, uniformly stirring, and reacting for 1-8 hours at 90-150 ℃;
(3) Separating the product obtained in the step (2), and washing, drying and roasting the obtained solid to obtain a final adsorbent product;
wherein, in the step (2), adding a certain amount of hydrolysis inhibitor into the urea aqueous solution, wherein the hydrolysis inhibitor is soluble ammonium salt;
the hydrolysis inhibitor is added in two steps: when the temperature of the system reaches 80-95 ℃, adding a hydrolysis inhibitor into the system at a speed of increasing 0.001-0.008 mol/L per ten minutes; when the temperature of the system reaches 95-120 ℃, adding a hydrolysis inhibitor into the system at a speed of 0.01-0.02 mol/L per ten minutes until the concentration of the inhibitor in the urea aqueous solution reaches 0.1-0.5 mol/L;
the temperature rising process in the step (2) is as follows: the initial temperature rising rate of the reaction is 5-10 ℃/min; and after the hydrolysis inhibitor is added into the system, the temperature rising rate is adjusted to be 0.5-2 ℃/min.
2. The preparation method according to claim 1, wherein the binder is one or more selected from kaolin, attapulgite, diatomaceous earth and bentonite, and the binding aid is one or more selected from sesbania powder, carboxymethyl cellulose and sodium carboxymethyl cellulose.
3. The method according to claim 1, wherein the concentration of the urea aqueous solution is 0.2 to 1.0 mol/L.
4. The method according to claim 1, wherein the hydrolysis inhibitor is one or more selected from the group consisting of ammonium chloride, ammonium sulfide, ammonium bicarbonate and ammonium carbonate.
5. The process according to claim 1, wherein the liquid-solid ratio of the urea aqueous solution to the intermediate adsorbent in the step (2) is 3 to 10mL/g.
6. The preparation method according to claim 1, wherein the reaction temperature in the step (2) is 95-120 ℃ and the reaction time is 4-6 hours.
7. The preparation method of claim 1, wherein the temperature of the drying in the step (3) is 80-150 ℃ and the drying time is 12-48 h; and (3) roasting at the temperature of 300-550 ℃ for 2-10 hours.
8. The preparation method of claim 1, wherein the temperature of the drying in the step (1) is 80-120 ℃ and the drying time is 6-24 hours; and (3) roasting at the temperature of 350-550 ℃ for 1-6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110867859.2A CN115672264B (en) | 2021-07-30 | 2021-07-30 | Preparation method of pressure swing adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110867859.2A CN115672264B (en) | 2021-07-30 | 2021-07-30 | Preparation method of pressure swing adsorbent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115672264A CN115672264A (en) | 2023-02-03 |
| CN115672264B true CN115672264B (en) | 2024-02-02 |
Family
ID=85058695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110867859.2A Active CN115672264B (en) | 2021-07-30 | 2021-07-30 | Preparation method of pressure swing adsorbent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115672264B (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1530167A (en) * | 2003-03-11 | 2004-09-22 | 中美合资上海锦中分子筛有限公司 | High-performance variable-pressure adsorption 5A molecular sieve and preparing method thereof |
| CN101524637A (en) * | 2009-04-23 | 2009-09-09 | 中国海洋石油总公司 | Preparation method of LSX-molecular-sieve-rich cementing-agent-free absorbent |
| CN105236444A (en) * | 2015-09-11 | 2016-01-13 | 大连理工大学 | Multi-level pore channel molecular sieve preparation method |
| CN105749859A (en) * | 2014-12-17 | 2016-07-13 | 中国石油天然气股份有限公司 | Method for preparing adsorbent for deacidification of methyl methacrylate |
| CN105800637A (en) * | 2016-03-18 | 2016-07-27 | 大连理工大学 | Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve |
| CN106475048A (en) * | 2015-08-28 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of 5A molecular sieve spherical adsorbent of binder free and preparation method |
| CN107089669A (en) * | 2017-05-26 | 2017-08-25 | 中国矿业大学 | A kind of synthetic method of the molecular sieves of c axle orientating type Zn ZSM 5 under externally-applied magnetic field effect |
| CN109692658A (en) * | 2017-10-24 | 2019-04-30 | 中国石油化工股份有限公司 | A kind of binder free spherical shape 5A adsorbent of molecular sieve and preparation method thereof |
| CN111097367A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Adsorbent for adsorbing normal alkane and preparation method and application thereof |
| CN111701623A (en) * | 2020-06-23 | 2020-09-25 | 南开大学 | Hydrocracking isomerization catalyst, preparation method and application thereof |
| CN112871188A (en) * | 2021-02-07 | 2021-06-01 | 浙江工业大学 | Preparation method of copper-based catalyst and application of copper-based catalyst in acetylene hydration reaction |
-
2021
- 2021-07-30 CN CN202110867859.2A patent/CN115672264B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1530167A (en) * | 2003-03-11 | 2004-09-22 | 中美合资上海锦中分子筛有限公司 | High-performance variable-pressure adsorption 5A molecular sieve and preparing method thereof |
| CN101524637A (en) * | 2009-04-23 | 2009-09-09 | 中国海洋石油总公司 | Preparation method of LSX-molecular-sieve-rich cementing-agent-free absorbent |
| CN105749859A (en) * | 2014-12-17 | 2016-07-13 | 中国石油天然气股份有限公司 | Method for preparing adsorbent for deacidification of methyl methacrylate |
| CN106475048A (en) * | 2015-08-28 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of 5A molecular sieve spherical adsorbent of binder free and preparation method |
| CN105236444A (en) * | 2015-09-11 | 2016-01-13 | 大连理工大学 | Multi-level pore channel molecular sieve preparation method |
| CN105800637A (en) * | 2016-03-18 | 2016-07-27 | 大连理工大学 | Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve |
| CN107089669A (en) * | 2017-05-26 | 2017-08-25 | 中国矿业大学 | A kind of synthetic method of the molecular sieves of c axle orientating type Zn ZSM 5 under externally-applied magnetic field effect |
| CN109692658A (en) * | 2017-10-24 | 2019-04-30 | 中国石油化工股份有限公司 | A kind of binder free spherical shape 5A adsorbent of molecular sieve and preparation method thereof |
| CN111097367A (en) * | 2018-10-29 | 2020-05-05 | 中国石油化工股份有限公司 | Adsorbent for adsorbing normal alkane and preparation method and application thereof |
| CN111701623A (en) * | 2020-06-23 | 2020-09-25 | 南开大学 | Hydrocracking isomerization catalyst, preparation method and application thereof |
| CN112871188A (en) * | 2021-02-07 | 2021-06-01 | 浙江工业大学 | Preparation method of copper-based catalyst and application of copper-based catalyst in acetylene hydration reaction |
Non-Patent Citations (4)
| Title |
|---|
| An improved and rapid 5A molecular sieve method for gas chromatography isotope ratio mass spectrometry of n-alkanes (C8–C30+);Kliti Grice et al.;Organic Geochemistry;第39卷;第284-288页 * |
| ZSM-5分子筛骨架铝落位对甲醇转化制芳烃催化性能影响;张立伟等;燃料化学学报;第47卷(第第12期期);第1468-1475页 * |
| 复合改性5A 分子筛对水中Cr3 +的吸附研究;张莹等;应用化工;第49卷(第11期);第2737-2747页 * |
| 结构化5A分子筛吸附床结构及工艺参数对N2/H2吸附性能的影响;王鹏等;化工学报;第71卷(第第7期期);第3114-3122页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115672264A (en) | 2023-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9517941B2 (en) | Introduction of mesoporosity in low Si/Al zeolites | |
| CA2427992C (en) | Sodium zirconium carbonate and zirconium basic carbonate and methods of making the same | |
| US20190314784A1 (en) | Method for producing an adsorbent material and method for extracting lithium from saline solutions using the material | |
| CA2521388A1 (en) | Aluminosilicates of zeolite n structure | |
| CN113731371B (en) | Preparation method of lithium ion adsorption material | |
| US20220033269A1 (en) | Zeolite and preparation method therefor | |
| EP1819720A1 (en) | A cost-effective process for preparation of manufacture of iron sucrose | |
| CN111804270B (en) | Aluminum-based lithium adsorbent and preparation method thereof | |
| CN109665536B (en) | Method for purifying attapulgite | |
| KR102316889B1 (en) | Manufaturing method of zeolite using lithium residue | |
| CN115672264B (en) | Preparation method of pressure swing adsorbent | |
| CN113603110B (en) | Template-free preparation method of porous LSX zeolite molecular sieve | |
| CN113264538B (en) | Preparation method and application of molecular sieve adsorbent based on LiNaKLSX | |
| JP3332817B2 (en) | Mesoporous silica and method for producing the same | |
| CN114433014B (en) | Preparation method of 5A molecular sieve adsorbent | |
| CN110965122B (en) | Preparation method of layered octahedral aragonite crystal and obtained product | |
| CN114433017B (en) | High-strength molecular sieve adsorbent and preparation method thereof | |
| KR102474955B1 (en) | Method for synthesizing high-crystalline CHA zeolite by addition of organic acid | |
| CN114873598A (en) | Novel silicon dioxide and preparation method thereof | |
| CN112047353A (en) | Production process for preparing sodium silicate by using sodium sulfate | |
| CN117482908A (en) | Adsorption material for selectively adsorbing calcium and magnesium ions in hard water and preparation method thereof | |
| RU2082493C1 (en) | Method of preparing sorbent | |
| CN116809011A (en) | Synthesis method of aluminum lithium ion sieve and application of aluminum lithium ion sieve in field of lithium extraction in salt lake | |
| CN114149011A (en) | Pharmaceutic adjuvant magnesium aluminum silicate and synthesis method thereof | |
| CN111187230A (en) | Preparation method of 2,4, 6-trimercapto-1, 3,5 triazine trisodium salt (TMT) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20240130 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Country or region after: China Applicant after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Country or region before: China Applicant before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |