CN115155519A - Preparation method of molecular sieve with strong adsorbability - Google Patents
Preparation method of molecular sieve with strong adsorbability Download PDFInfo
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- CN115155519A CN115155519A CN202210913534.8A CN202210913534A CN115155519A CN 115155519 A CN115155519 A CN 115155519A CN 202210913534 A CN202210913534 A CN 202210913534A CN 115155519 A CN115155519 A CN 115155519A
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 51
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000004927 clay Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 14
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000013067 intermediate product Substances 0.000 claims description 10
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical group O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000005995 Aluminium silicate Substances 0.000 claims description 6
- 235000012211 aluminium silicate Nutrition 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000000274 adsorptive effect Effects 0.000 claims 4
- 239000011344 liquid material Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- 239000007789 gas Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 244000275012 Sesbania cannabina Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a preparation method of a molecular sieve with strong adsorbability, which needs to provide the molecular sieve with strong adsorbability and comprises the following components in parts by weight: 70-80 parts of molecular sieve raw powder, 10-25 parts of clay, 5-10 parts of high clay, 15-60 parts of plant fiber powder and 15-20 parts of calcium oxalate; the invention can prepare the molecular sieve with high adsorption.
Description
Technical Field
The invention relates to the technical field of molecular sieve preparation, in particular to a preparation method of a molecular sieve with strong adsorbability.
Background
Carbon monoxide, nitrogen, methane, etc. are important industrial raw material gases, and the demand of the raw material gases is increasing with the development of the industry. Therefore, the separation and purification of these gases are of great industrial significance.
Pressure Swing Adsorption (PSA) technology, a gas separation technology that is industrially emerging in recent years, uses the difference of adsorption characteristics of gas components on solid materials and the characteristic that the adsorption amount changes with the change of pressure to realize the separation and purification of gas through a periodic pressure shift process. While the adsorbent is the basis of the PSA gas separation technology, the performance of the adsorbent directly influences the final separation effect, even the complexity of the process steps and the service life of PSA. Therefore, the adsorbent used in PSA has high adsorption capacity and separation selectivity for the target gas, and is of great significance for separation efficiency and energy saving.
One of the molecular sieve modification techniques is ion exchange, wherein 4A is subjected to ion exchange with salts such as calcium chloride and the like, and calcium ions replace sodium ions in 4A, so that the pore diameter is enlarged to prepare 5A, and the molecular sieve has a great effect on improving the adsorption performance of the adsorbent. The current more common methods are: the powder 4A and adhesive kaolin are mixed and formed, the kaolin is converted into metakaolin through high-temperature roasting, then the metakaolin is converted into the molecular sieve 4A through crystallization in 1-1.5mol/L sodium hydroxide solution, and the prepared adhesive-free molded molecular sieve 4A is subjected to liquid-phase calcium exchange to prepare the molded molecular sieve 5A, wherein the calcium exchange capacity of the method can reach 80%, and the improvement is difficult. CA2125314 discloses a method for improving ion exchange capacity, which is characterized in that a sodium carbonate solution with pH =8-9 is used for treating a sample for 3-4 times and then is exchanged with a calcium chloride solution, so that the calcium exchange capacity can be improved, but the method has multiple working procedures and good powder exchange effect.
Disclosure of Invention
In view of the above, the present invention aims to provide a method capable of preparing a high adsorption molecular sieve.
The invention is realized by adopting the following method: a preparation method of a molecular sieve with strong adsorbability needs to provide a molecular sieve with strong adsorbability, which is prepared from the following components in parts by weight: 70-80 parts of molecular sieve raw powder, 10-25 parts of clay, 5-10 parts of high clay, 15-60 parts of plant fiber powder and 15-20 parts of calcium oxalate; the preparation method comprises the following steps:
step S1, mixing the molecular sieve raw powder with clay and high clay, adding plant fiber powder, and stirring and granulating at high speed in a high-speed granulator;
s2, screening and drying the granulated intermediate product, and roasting at high temperature after drying;
s3, immersing the roasted intermediate product into a sodium hydroxide solution for alkali treatment, and performing Ca & lt 2+ & gt exchange by using a calcium oxalate solution after washing;
and S4, after washing and drying, carrying out secondary roasting on the granular product, drying after high-temperature steaming is finished, and increasing the porosity of the molecular sieve and the porosity of the molecular plug, thereby realizing the preparation of the molecular sieve with strong adsorbability.
Further, the high-temperature roasting temperature in the step S2 ranges from 300 ℃ to 1200 ℃.
Further, the weight percentage of the sodium hydroxide solution in the step S3 is between 6 and 30 percent.
Further, the high clay is kaolin.
Further, the liquid-to-material weight ratio of the sodium hydroxide solution to the intermediate product is 4-15: 3, and the weight ratio of pure calcium oxalate contained in the calcium oxalate solution to the intermediate product is 0.3-1: 0.5.
The invention has the beneficial effects that: the invention adds calcium oxalate, which can improve the adsorption capacity of each adsorbate, the adsorption capacity of nitrogen can reach 11.5ml/g, the adsorption capacity of carbon monoxide can reach more than 34ml/g, and the adsorption capacity of normal hexane can reach more than 16% (weight); the method is mainly applied to an adsorption process, so that the method has great significance for industrial use, cost saving and energy source saving; the invention reduces the consumption of clay in the preparation of the molecular sieve and improves the adsorption capacity of the product; the plant fiber powder is added, so that the porous structure of the product is improved, and the diffusion rate of the product is increased.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
Fig. 2 is a test report of the present invention applied to drinking water.
Fig. 3 is a test result of the molecular sieve of the present invention placed in drinking water for treatment.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a method for preparing a molecular sieve with strong adsorption property, wherein the method for preparing the molecular sieve with strong adsorption property is to provide a molecular sieve with strong adsorption property, and the molecular sieve comprises the following components by weight: 70-80 parts of molecular sieve raw powder, 10-25 parts of clay, 5-10 parts of high clay, 15-60 parts of plant fiber powder and 15-20 parts of calcium oxalate; the preparation method comprises the following steps:
step S1, mixing the molecular sieve raw powder with clay and high clay, adding plant fiber powder, and stirring at high speed in a high-speed granulator for granulation;
s2, screening and drying the granulated intermediate product, and roasting at high temperature after drying;
s3, immersing the roasted intermediate product into a sodium hydroxide solution for alkali treatment, and performing Ca & lt 2+ & gt exchange by using a calcium oxalate solution after washing;
and S4, after washing and drying, carrying out secondary roasting on the granular product, drying after high-temperature steaming is finished, and increasing the porosity of the molecular sieve and the porosity of the molecular plug, thereby realizing the preparation of the molecular sieve with strong adsorbability.
The invention is further illustrated by the following specific examples:
example 1
70 parts of molecular sieve raw material, 5 parts of kaolin, 10 parts of clay, 15 parts of sesbania powder and 15 parts of calcium oxalate are added into a turntable of a granulator for granulation, the diameter of the granulator is 2.0m, the horizontal inclination angle of the granulator is 50 degrees, and the rotation speed of the granulator is 60r/min; in the granulation process, after the particle size of the molecular sieve reaches 1mm, the added calcium oxalate is adjusted to 16 parts, and the amount of other materials is unchanged, and the granulation is continued; after the particle size of the molecular sieve is 2mm, adjusting the added calcium oxalate to 17 parts, keeping the amount of other materials unchanged, and continuing to granulate; finally obtaining the spherical adsorbent with the particle size of 3 mm. The calcium oxalate added in the whole granulation process accounts for 2 percent of the total weight. Drying the finally obtained spherical molecular sieve at 120 ℃ for 4h, wherein the heating rate is 6 ℃/min. And then roasting the molecular sieve, wherein the roasting temperature rise rate is 5 ℃/min, the final temperature is 550 ℃, and the constant temperature is kept for 3.5 hours.
Example 2
Adding 75 parts of molecular sieve raw material, 10 parts of kaolin, 25 parts of clay, 30 parts of cellulose and 18 parts of calcium oxalate into a rotary table of a granulator for granulation, wherein the diameter of the granulator is 1.5mm, the horizontal inclination angle of the granulator is 45 degrees, and the rotating speed of the granulator is 45r/min; in the granulation process, after the particle size of the molecular sieve reaches 0.8mm, the amount of the added calcium oxalate is adjusted to 19 parts, and the amount of other materials is unchanged, and the granulation is continued; after the particle size of the molecular sieve is 1.9mm, adjusting the amount of the added calcium oxalate to 20 parts, keeping the amount of other materials unchanged, and continuing to granulate; finally obtaining the spherical adsorbent with the particle size of 2.8 mm. The amount of starch added during the whole granulation process was 7% of the total amount. Drying the finally obtained spherical molecular sieve at 100 ℃ for 6h, wherein the heating rate is 8 ℃/min. And then roasting the molecular sieve, wherein the roasting temperature rise rate is 8 ℃/min, the final temperature is 6000 ℃, and the constant temperature is kept for 5 hours.
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (5)
1. The preparation method of the molecular sieve with strong adsorbability is characterized in that the preparation method needs to provide the molecular sieve with strong adsorbability, and the molecular sieve is prepared from the following components in parts by weight: 70-80 parts of molecular sieve raw powder, 10-25 parts of clay, 5-10 parts of high clay, 15-60 parts of plant fiber powder and 15-20 parts of calcium oxalate; the preparation method comprises the following steps:
step S1, mixing the molecular sieve raw powder with clay and high clay, adding plant fiber powder, and stirring at high speed in a high-speed granulator for granulation;
s2, screening and drying the granulated intermediate product, and roasting at high temperature after drying;
s3, immersing the roasted intermediate product into a sodium hydroxide solution for alkali treatment, and performing Ca & lt 2+ & gt exchange by using a calcium oxalate solution after washing;
and S4, after washing and drying, carrying out secondary roasting on the granular product, drying after high-temperature steaming is finished, and increasing the porosity of the molecular sieve and the porosity of the molecular plug, thereby realizing the preparation of the molecular sieve with strong adsorbability.
2. A method for preparing a strongly adsorptive molecular sieve according to claim 1, wherein: the high-temperature roasting temperature range in the step S2 is between 300 and 1200 ℃.
3. A method for preparing a strongly adsorptive molecular sieve according to claim 1, wherein: the weight percentage of the sodium hydroxide solution in the step S3 is between 6 and 30 percent.
4. A method for preparing a strongly adsorptive molecular sieve according to claim 1, wherein: the high clay is kaolin.
5. A method for preparing a strongly adsorptive molecular sieve according to claim 1, wherein: wherein the liquid-material weight ratio of the sodium hydroxide solution to the intermediate product is 4-15: 3, and the weight ratio of pure calcium oxalate contained in the calcium oxalate solution to the intermediate product is 0.3-1: 0.5.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087030A (en) * | 1992-11-17 | 1994-05-25 | 中国科学院大连化学物理研究所 | The preparation of binder free 5A wax molecular sieve adsorbent |
| 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 |
| CN1962047A (en) * | 2006-10-17 | 2007-05-16 | 太原理工大学 | Method for preparing molecular sieve absorbent with high adsorption capacity |
| CN111362276A (en) * | 2020-03-24 | 2020-07-03 | 南京永成分子筛有限公司 | 3A molecular sieve with high adsorption and low dust 0 pollution, and forming process and application thereof |
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- 2022-08-01 CN CN202210913534.8A patent/CN115155519A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087030A (en) * | 1992-11-17 | 1994-05-25 | 中国科学院大连化学物理研究所 | The preparation of binder free 5A wax molecular sieve adsorbent |
| 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 |
| CN1962047A (en) * | 2006-10-17 | 2007-05-16 | 太原理工大学 | Method for preparing molecular sieve absorbent with high adsorption capacity |
| CN111362276A (en) * | 2020-03-24 | 2020-07-03 | 南京永成分子筛有限公司 | 3A molecular sieve with high adsorption and low dust 0 pollution, and forming process and application thereof |
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