CN1792794A - Process for preparing nano grade 4A zeolite using flyash as raw material - Google Patents
Process for preparing nano grade 4A zeolite using flyash as raw material Download PDFInfo
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- CN1792794A CN1792794A CN 200610000624 CN200610000624A CN1792794A CN 1792794 A CN1792794 A CN 1792794A CN 200610000624 CN200610000624 CN 200610000624 CN 200610000624 A CN200610000624 A CN 200610000624A CN 1792794 A CN1792794 A CN 1792794A
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Abstract
A process for preparing nano-class 4A zeolite from powdered coal ash includes such steps as breaking, efficient magentic separation for removing Fe, high-temp calcining to become active argil, efficient magnetic separation for removing Fe, gelatinizing in alkali solution, regulating Si/Al ratio, breaking by shearing, collision and hydrating, crystallizing, washing and drying.
Description
Technical field
The present invention relates to flyash is the method for raw material synthesizing washing adjuvant nano-scale 4 A zeolite
Background technology
There is the abundant in coal resource in China, in the present generating set of China, have 80% be fired power generating unit.Be subjected to the restriction of each side condition, Chinese future very long one period will be based on coal fired power generation.The construction of thermal power station is the major portion of power house construction in 2005.Estimate that the generating set that state approval is invested to build will be a fired power generating unit during " 11th Five-Year ".Waste coal ash, cinder after fuel-burning power plant, city heat supply, boiler for domestic and the civil boiler burning have generally all been lost as rubbish in vain, fail to be fully used, and have caused the waste of resource.For this reason, we respond national policy, at the non-renewable and environmental pollution of the wasting of resources, resource anxiety, resource, and the environmental protection project of utilizing again of exploit natural resources emphatically saving, resource.Because the iron-holder in the flyash is higher, the product whiteness that adopts usual way to obtain is relatively poor, does not have actual utility value, and the present invention addresses this problem emphatically, and makes the product of production reach nano level.
Summary of the invention
The present invention is to be raw material with power plant, boiler and domestic refuse flyash, after crushed, adopt efficient iron removal by magnetic separation, through high-temperature calcination, make it be converted into atlapulgite fully after the drying, carry out the efficient iron removal by magnetic separation of secondary then, silica alumina ratio is adjusted in then gel in alkali lye, passes through shearing hypervelocity impact again, last crystallization, washing, drying, and obtain high-activity nano level washing auxiliary detergent 4A zeolite.Its suspension is good, and specific surface area is big, and is active high.Because the novel process of twice deferrization before and after having adopted, its product whiteness can reach more than 95.
Process explanation and condition
1, adopting power plant, boiler and domestic refuse flyash is raw material, through pulverizer it is crushed to below 325 orders.
2, use several times row deironing for the first time of highly-effective magnetic separator.
3, will be through the flyash after the deironing by pressure-filteration drying, in entering 900-1000 ℃ calcining furnace, calcine the loss on ignition after the calcining≤0.5%.
4, the active white powder after will calcining carries out the efficient magnetic separation second time, and this moment, the iron-holder of raw material was reduced to below 0.5%.
5, dropping into concentration is the NaOH solution gelatinizing pond of 18%-24%, adjusts its sial ratio and required chemical ingredients, heats to 30-70 ℃ and carries out gel.Be converted into colloidal aluminum silicate after gel 3-72 hour.According to colloidal gel degree, through 10-45 minute shearing hypervelocity impact hydrated bruising.Shearing hypervelocity impact rotating speed 360-3000r/min.
6, the aluminosilicate glue after the gel is added deionized water and be diluted to Na
2O content 6%-8% carries out crystallization at 70-130 ℃ then, crystallization time 20-90 minute, reaches 100% and suspends.
7, water-containing product is squeezed into pressure filter through underflow pump and is carried out mother liquor and reclaim after the crystallization, reclaims the back and washs (temperature of deionized water is 15-30 ℃) with deionized water, is washed till the ph value below 10.5.Washing water concentrate 8%-18% through vaporizer, sneak into mother liquor, and mother liquor is added the NaOH solution that NaOH is modulated into 18%-24%, reuse.
8, the water-containing product after the washing carries out drying in moisture eliminator.Drying temperature 125-135 ℃.Dry back product loss on ignition reaches below 21%, nano-scale 4 A zeolite.
Embodiment
Example one
With Shanxi Province's Houma City coal ash of power plant 1000 grams, be crushed to median size 325 orders through pulverizer, the powder after pulverizing is passed through highly-effective magnetic separator, through in 950 ℃ calcining furnace, calcining the loss on ignition after the calcining≤0.5% behind the pressure-filteration drying.Active white powder after the calcining is carried out efficient magnetic separation second time, drop into concentration and be 18% NaOH solution gelatinizing pond, the adjustment silica alumina ratio is heated to 30-70 ℃ and is carried out gel.Gel is converted into colloidal aluminum silicate after 48 hours.Shearing hypervelocity impact hydrated bruising through 20 minutes.Shearing hypervelocity impact rotating speed 1000r/min.Aluminosilicate glue after the gel is added deionized water be diluted to Na
2O content 8% carries out crystallization at 80 ℃ then, and crystallization time 60 minutes reaches 100% and suspends.Water-containing product after the washing carries out drying in moisture eliminator, 125 ℃ of drying temperatures.Dry back product loss on ignition≤21%, nano-scale 4 A zeolite.
Example two
With Xi'an interpretative science institute boiler coal ash 1000 grams, be crushed to median size 325 orders through pulverizer.Powder after pulverizing is passed through highly-effective magnetic separator, through in 950 ℃ calcining furnace, calcining behind the pressure-filteration drying.Loss on ignition after the calcining≤0.5%.Active white powder after the roasting calcining is carried out efficient magnetic separation second time, drop into concentration and be 20% NaOH solution gelatinizing pond, the adjustment silica alumina ratio is heated to 30-70 ℃ and is carried out gel.Gel is converted into colloidal aluminum silicate after 24 hours.Shearing hypervelocity impact hydrated bruising through 20 minutes.Shearing hypervelocity impact rotating speed 1000r/min.Aluminosilicate glue after the gel is added deionized water be diluted to Na
2O content 8% carries out crystallization at 80 ℃ then, and crystallization time 50 minutes reaches 100% and suspends.Water-containing product after the washing carries out drying in moisture eliminator, 125 ℃ of drying temperatures.Dry back product loss on ignition≤21%, nano-scale 4 A zeolite.
Example three
With Yuncheng residential quarter flyash 1000 grams, be crushed to median size 325 orders through pulverizer.Powder after pulverizing is passed through highly-effective magnetic separator, through in 950 ℃ calcining furnace, calcining behind the pressure-filteration drying.Loss on ignition after the calcining≤0.5%.Active white powder after the calcining is carried out efficient magnetic separation second time, and input concentration is 22% NaOH solution gelatinizing pond, heats to 30-70 ℃ and carries out gel.Gel is converted into colloidal aluminum silicate after 24 hours.Shearing hypervelocity impact hydrated bruising through 30 minutes.Shearing hypervelocity impact rotating speed 2600r/min.Aluminosilicate glue after the gel is added deionized water be diluted to Na
2O content 8% carries out crystallization at 80 ℃ then, and crystallization time 30 minutes reaches 100% and suspends.Water-containing product after the washing carries out drying in moisture eliminator, 135 ℃ of drying temperatures.Dry back product loss on ignition≤20%, nano-scale 4 A zeolite.
Claims (10)
1. a method of utilizing flyash for the feedstock production nano-scale 4 A zeolite is characterized in that, is raw material with power plant, boiler, domestic refuse flyash, utilizes twice efficient iron removal by magnetic separation in front and back and shearing hypervelocity impact technology.
2. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that the grinding particle size of flyash is between the 325-1250 order, calcining temperature is 900 ℃-1000 ℃.
3. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that, flyash will carry out the efficient iron removal by magnetic separation of secondary respectively after the pulverizing and after the calcining, and this moment, the iron-holder of raw material was reduced to below 0.5%.
4. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that, be raw material with flyash, in the gel process, gelatinization temperature 30-70 ℃, mixed gel time 3-72 hour.
5. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that raw material need be adjusted the when required chemical ingredients of its sial in the gel pond.
6. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that, carry out aquation according to the gel degree, high 10-45 minute shearing-crushing time of collision, aquation shearing hypervelocity impact speed 360-3000r/min.
7. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that, in crystallization process, crystallization temperature 70-130 ℃, crystallization time 20-90 minute.
8. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that in washing process, the temperature of deionized water is 15-30 ℃.
9. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that, in drying process, 125 ℃-135 ℃ of drying temperatures, loss on ignition reaches below 21%.
10. according to claim 1 a kind of be the novel method that prepared using shearing hypervelocity impact technology prepares nano-scale 4 A zeolite with flyash, it is characterized in that prepared 4A zeolite particle size is minimum, reaches nano level.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610000624 CN1792794A (en) | 2006-01-10 | 2006-01-10 | Process for preparing nano grade 4A zeolite using flyash as raw material |
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| CN 200610000624 CN1792794A (en) | 2006-01-10 | 2006-01-10 | Process for preparing nano grade 4A zeolite using flyash as raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450805B (en) * | 2007-12-09 | 2010-09-01 | 张勤善 | Novel process for synthesizing molecular sieve by calcining fly ash through wet alkalization |
| CN106745042A (en) * | 2016-12-01 | 2017-05-31 | 神华集团有限责任公司 | Flyash acid system residue of aluminum-extracted prepares the method and the Application way of flyash of 4A types molecular sieve and the type molecular sieves of ZSM 5 |
-
2006
- 2006-01-10 CN CN 200610000624 patent/CN1792794A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450805B (en) * | 2007-12-09 | 2010-09-01 | 张勤善 | Novel process for synthesizing molecular sieve by calcining fly ash through wet alkalization |
| CN106745042A (en) * | 2016-12-01 | 2017-05-31 | 神华集团有限责任公司 | Flyash acid system residue of aluminum-extracted prepares the method and the Application way of flyash of 4A types molecular sieve and the type molecular sieves of ZSM 5 |
| CN106745042B (en) * | 2016-12-01 | 2018-11-20 | 神华集团有限责任公司 | Flyash acid system residue of aluminum-extracted prepares the method for 4A type molecular sieve and type ZSM 5 molecular sieve and the utilization method of flyash |
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Open date: 20060628 |