CN105984882A - High-adsorption-capacity oxygen generation molecular sieve and preparation method thereof - Google Patents
High-adsorption-capacity oxygen generation molecular sieve and preparation method thereof Download PDFInfo
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- CN105984882A CN105984882A CN201610031674.7A CN201610031674A CN105984882A CN 105984882 A CN105984882 A CN 105984882A CN 201610031674 A CN201610031674 A CN 201610031674A CN 105984882 A CN105984882 A CN 105984882A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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Abstract
The invention discloses a high-adsorption-capacity oxygen generation molecular sieve and a preparation method thereof. The molecular sieve is prepared from, by weight, 18-29 parts of halloysite, 13-21 parts of sepiolite, 28-36 parts of diatomite, 15-25 parts of wollastonite, 14-22 parts of potassium feldspar, 10-15 parts of spodumene, 8-14 parts of albite, 48-62 parts of sodium hydroxide, 32-44 parts of sodium metaaluminate, 24-36 parts of sodium metasilicate nonahydrate and 15-20 parts of seed crystal guide agent. The molecular sieve prepared by the method is high in nitrogen balance adsorption capacity which can reach higher than 30 ml/g, and has excellent mechanical strength and nitrogen-oxygen separation performance; a production process is simple, raw materials are extensive in source, and the molecular sieve is low in cost, renewable, reusable, environment-friendly and economical and can be popularized and applied in pressure-variable adsorption oxygen generators on a large scale.
Description
Technical field
The present invention relates to a kind of molecular sieve and preparation method thereof, be specifically related to a kind of high-adsorption-capacity oxygen molecular sieve and
Preparation method.
Background technology
In recent years, due to the exploitation of oxygen molecular sieve adsorbent processed and updating of technological process, pressure-variable adsorption is made
Oxygenerating technology is rapidly developed.Separating oxygen from air by means of pressure swing adsorption process has that the startup time is short, the construction period is short, operating cost
The feature such as low, automaticity is high, maintenance is simple, comprehensive energy consumption is low, is widely used in iron and steel, nonferrous metallurgy, chemical industry, stove joint
The fields such as energy, environmental protection, glass, papermaking, medical treatment.
Total well known, adsorbent of molecular sieve is the key core of omnibus control system technology, the performance of adsorbent of molecular sieve
Directly decide the investment of device, volume weight and unit produce the integrated performance index such as oxygen rate and gas consumption.It is used in the market
The molecular sieve of pressure swing adsorption oxygen making device is of a great variety, but mostly there is the low shortcoming of adsorption capacity, thus affects transformation
The final separation effect of adsorption oxygen-preparation device.
Content of the invention
Present invention aims to the deficiencies in the prior art, a kind of high-adsorption-capacity oxygen molecular sieve and system thereof are provided
Preparation Method.
For realizing your purpose above-mentioned, the present invention adopts the following technical scheme that:
A kind of high-adsorption-capacity oxygen molecular sieve, is made up of the raw material of following weight portion: galapectite 18-29, sepiolite 13-
21st, diatomite 28-36, wollastonite 15-25, potassium feldspar 14-22, spodumene 10-15, albite 8-14, NaOH 48-62,
Sodium metaaluminate 32-44, nine water sodium metasilicate 24-36, seeding director 15-20；
The preparation method of described seeding director is as follows: a, the raw material taking following weight portion: diatomite 19-27, galapectite
14-22, wollastonite 11-19, non-hydrate sodium metasilicate 26-34, NaOH 17-23, sodium metaaluminate 8-14；B, by diatomite, angstrom
Lip river stone, wollastonite mix, and 570-620 DEG C of calcining 0.5-1.5h, is 1:12-16 according to solid-to-liquid ratio after naturally cooling to normal temperature
Ratio mix with the sulfuric acid solution that molar concentration is 2mol/L, heating water bath to 75-85 DEG C, be incubated 25-40min, filter, wash
Wash, dry, 820-880 DEG C of calcining 1-2h, naturally cool to normal temperature, pulverize, grind, cross 150-250 mesh sieve；C, take NaOH
It is dissolved in the deionized water being equivalent to its 10-15 times amount, is subsequently adding the powder that step b prepares, in stirring after mixing
Under the conditions of add non-hydrate sodium metasilicate and sodium metaaluminate, at 70-80 DEG C, heat 1-2h after mixing, water-cooled to normal temperature, then
Still aging 18-24h and get final product.
The preparation method of a kind of high-adsorption-capacity oxygen molecular sieve, comprises the following steps:
(1) galapectite, wollastonite, potassium feldspar are mixed, pulverize, cross 150 mesh sieves, then according to solid-to-liquid ratio is 1:
Powder after the ratio of 15-20 will be sieved joins in the sulfuric acid solution that molar concentration is 1.5mol/L, heating water bath to 70-80
DEG C, ultrasonic disperse 20-40min, filter, washing, dry, stand-by；
(2) sepiolite, diatomite, spodumene, albite are mixed, 780-820 DEG C of calcining 2-3h, naturally cool to
Normal temperature, pulverizes, and crosses 150-250 mesh sieve, stand-by；
(3) powder preparing step (1) mixes with the powder that step (2) prepares, and adds appropriate deionized water
Making the suspension that concentration is 50-55%, microwave treatment 30-50min, microwave power is 300-500W, then magnetic agitation 25-
35min, rotating speed is 1500-2500r/min, is then spray dried to powder, stand-by；
(4) NaOH, sodium metaaluminate, nine water sodium metasilicate are mixed, be subsequently adding and be equivalent to 14-18 times of mixture
The deionized water of amount, adds the powder that step (3) prepares after stirring, stir 2-4h, then stand old at 75-85 DEG C
Changing 12-24h, adding seeding director, heating water bath is to 90-100 DEG C, and 6-8h is reacted in stirring, then is warming up to 100-110 DEG C,
Thermostatic crystallization 15-20h, after reaction terminates, filters, and being washed to filter residue pH value is 7-8, then dries, and grinds, sieves, must become
Product.
Beneficial effects of the present invention:
The molecular sieve nitrogen balance adsorption capacity that the present invention prepares is high, up to more than 30ml/g, has excellent machinery simultaneously
Intensity and nitrogen oxygen separating system can, and production technology is simple, and raw material sources are extensive, with low cost, can regenerate and can be used for multiple times, ring
Protect economy, can in pressure swing adsorption oxygen making device large-scale promotion application.
Detailed description of the invention
A kind of high-adsorption-capacity oxygen molecular sieve, is made up of the raw material of following weight (kg): galapectite the 23rd, sepiolite is the 18th,
Diatomite the 33rd, wollastonite the 20th, potassium feldspar the 18th, spodumene the 12nd, albite the 10th, NaOH the 54th, sodium metaaluminate the 39th, nine water sodium metasilicate
32nd, seeding director 17；
The preparation method of described seeding director is as follows: a, the raw material taking following weight (kg): diatomite the 24th, galapectite
18th, wollastonite the 16th, non-hydrate sodium metasilicate the 30th, NaOH the 19th, sodium metaaluminate 11；B, by diatomite, galapectite, wollastonite mixing
Uniformly, 590 DEG C of calcining 1h, according to the sulphur that the ratio that solid-to-liquid ratio is 1:14 and molar concentration are 2mol/L after naturally cooling to normal temperature
Acid solution mixes, and heating water bath, to 80 DEG C, is incubated 30min, filters, and washing is dried, 840 DEG C of calcining 1.5h, often naturally cools to
Temperature, pulverizes, and grinds, and crosses 200 mesh sieves；C, take NaOH and be dissolved in the deionized water being equivalent to its 12 times amount, be subsequently adding step
The powder that rapid b prepares, adds non-hydrate sodium metasilicate and sodium metaaluminate after mixing under conditions of stirring, after mixing
Heating 1.5h at 75 DEG C, water-cooled is to normal temperature, more still aging 22h and get final product.
The preparation method of a kind of high-adsorption-capacity oxygen molecular sieve, comprises the following steps:
(1) galapectite, wollastonite, potassium feldspar are mixed, pulverize, cross 150 mesh sieves, then according to solid-to-liquid ratio is 1:17
Ratio will sieve after powder join in the sulfuric acid solution that molar concentration is 1.5mol/L, heating water bath is to 75 DEG C, ultrasonic
Dispersion 30min, filters, and washing is dried, stand-by；
(2) sepiolite, diatomite, spodumene, albite are mixed, 810 DEG C of calcining 2.5h, often naturally cool to
Temperature, pulverizes, and crosses 200 mesh sieves, stand-by；
(3) powder preparing step (1) mixes with the powder that step (2) prepares, and adds appropriate deionized water
Making the suspension that concentration is 52%, microwave treatment 40min, microwave power is 400W, then magnetic agitation 30min, and rotating speed is
2000r/min, is then spray dried to powder, stand-by；
(4) NaOH, sodium metaaluminate, nine water sodium metasilicate are mixed, be subsequently adding and be equivalent to mixture 16 times amount
Deionized water, add after stirring step (3) prepare powder, at 80 DEG C stir 2-4h, then still aging
18h, adds seeding director, and heating water bath is to 95 DEG C, and 7h is reacted in stirring, then is warming up to 105 DEG C, thermostatic crystallization 18h, reaction
After end, filtering, being washed to filter residue pH value is 8, then dries, and grinds, sieves, get product.
The service check of the oxygen molecular sieve processed that above-described embodiment prepares the results are shown in Table 1.
The performance test results of table 1 oxygen molecular sieve processed
| Project | Unit | Test result |
| Bulk density | g/ml | 0.71 |
| Compression strength | N | 35 |
| Nitrogen balance adsorbance | ml/g | 34 |
| N2/O2Select coefficient | - | 6.5 |
Claims (2)
1. a high-adsorption-capacity oxygen molecular sieve, it is characterised in that be made up of the raw material of following weight portion: galapectite 18-
29th, sepiolite 13-21, diatomite 28-36, wollastonite 15-25, potassium feldspar 14-22, spodumene 10-15, albite 8-
14th, NaOH 48-62, sodium metaaluminate 32-44, nine water sodium metasilicate 24-36, seeding director 15-20；
The preparation method of described seeding director is as follows: a, the raw material taking following weight portion: diatomite 19-27, galapectite 14-
22nd, wollastonite 11-19, non-hydrate sodium metasilicate 26-34, NaOH 17-23, sodium metaaluminate 8-14；B, by diatomite, Ai Luo
Stone, wollastonite mix, and 570-620 DEG C of calcining 0.5-1.5h, is 1:12-16's according to solid-to-liquid ratio after naturally cooling to normal temperature
Ratio mixes with the sulfuric acid solution that molar concentration is 2mol/L, and heating water bath, to 75-85 DEG C, is incubated 25-40min, filters, washes
Wash, dry, 820-880 DEG C of calcining 1-2h, naturally cool to normal temperature, pulverize, grind, cross 150-250 mesh sieve；C, take NaOH
It is dissolved in the deionized water being equivalent to its 10-15 times amount, is subsequently adding the powder that step b prepares, in stirring after mixing
Under the conditions of add non-hydrate sodium metasilicate and sodium metaaluminate, at 70-80 DEG C, heat 1-2h after mixing, water-cooled to normal temperature, then
Still aging 18-24h and get final product.
2. the preparation method of a high-adsorption-capacity oxygen molecular sieve as claimed in claim 1, it is characterised in that include following
Step:
(1) galapectite, wollastonite, potassium feldspar are mixed, pulverize, cross 100-200 mesh sieve, then according to solid-to-liquid ratio is 1:
Powder after the ratio of 15-20 will be sieved joins in the sulfuric acid solution that molar concentration is 1.5mol/L, heating water bath to 70-80
DEG C, ultrasonic disperse 20-40min, filter, washing, dry, stand-by；
(2) sepiolite, diatomite, spodumene, albite are mixed, 780-820 DEG C of calcining 2-3h, often naturally cool to
Temperature, pulverizes, and crosses 150-250 mesh sieve, stand-by；
(3) powder preparing step (1) mixes with the powder that step (2) prepares, and adds appropriate deionized water to make
Concentration is the suspension of 50-55%, microwave treatment 30-50min, and microwave power is 300-500W, then magnetic agitation 25-35min,
Rotating speed is 1500-2500r/min, is then spray dried to powder, stand-by；
(4) NaOH, sodium metaaluminate, nine water sodium metasilicate are mixed, be subsequently adding and be equivalent to mixture 14-18 times amount
Deionized water, adds the powder that step (3) prepares after stirring, stir 2-4h at 75-85 DEG C, then still aging
12-24h, adds seeding director, and heating water bath is to 90-100 DEG C, and 6-8h is reacted in stirring, then is warming up to 100-110 DEG C, permanent
Temperature crystallization 15-20h, after reaction terminates, filters, and being washed to filter residue pH value is 7-8, then dries, and grinds, sieves, get product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984767A (en) * | 2017-05-27 | 2017-07-28 | 苏州兴业材料科技股份有限公司 | Casting silicate binder |
| CN108190914A (en) * | 2018-02-08 | 2018-06-22 | 西安建筑科技大学 | A kind of synthetic method of solid waste multi-stage porous block ECR-1 zeolites |
| CN113264538A (en) * | 2021-05-29 | 2021-08-17 | 山西腾茂科技股份有限公司 | Preparation method and application of molecular sieve adsorbent based on LiNaKLSX |
| CN114797810A (en) * | 2022-04-13 | 2022-07-29 | 华南理工大学 | Sodium metasilicate modified halloysite powder and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789127A (en) * | 2004-12-15 | 2006-06-21 | 中国石油化工股份有限公司 | Preparation method of Y type molecular sieve enriched with mesopore |
-
2016
- 2016-01-18 CN CN201610031674.7A patent/CN105984882A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1789127A (en) * | 2004-12-15 | 2006-06-21 | 中国石油化工股份有限公司 | Preparation method of Y type molecular sieve enriched with mesopore |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984767A (en) * | 2017-05-27 | 2017-07-28 | 苏州兴业材料科技股份有限公司 | Casting silicate binder |
| CN106984767B (en) * | 2017-05-27 | 2018-12-07 | 苏州兴业材料科技股份有限公司 | Silicate binder is used in casting |
| CN108190914A (en) * | 2018-02-08 | 2018-06-22 | 西安建筑科技大学 | A kind of synthetic method of solid waste multi-stage porous block ECR-1 zeolites |
| CN108190914B (en) * | 2018-02-08 | 2021-06-15 | 西安建筑科技大学 | Method for synthesizing solid waste hierarchical porous block ECR-1 zeolite |
| CN113264538A (en) * | 2021-05-29 | 2021-08-17 | 山西腾茂科技股份有限公司 | Preparation method and application of molecular sieve adsorbent based on LiNaKLSX |
| CN114797810A (en) * | 2022-04-13 | 2022-07-29 | 华南理工大学 | Sodium metasilicate modified halloysite powder and preparation method and application thereof |
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