CN1631779A - Method for preparing A type zeolite by gangue - Google Patents
Method for preparing A type zeolite by gangue Download PDFInfo
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- CN1631779A CN1631779A CN 200410064592 CN200410064592A CN1631779A CN 1631779 A CN1631779 A CN 1631779A CN 200410064592 CN200410064592 CN 200410064592 CN 200410064592 A CN200410064592 A CN 200410064592A CN 1631779 A CN1631779 A CN 1631779A
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- gangue
- coal gangue
- zeolite
- sio
- alkali fusion
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention is a method of prepare A zeolite with coal gangue which is by burning the coal gangue and mixing it with alkaline fusion solution to react at high temperature, then extracting the alkaline fusion in the water to remove the Fe, adding aluminum salt and heating to crystallize, finally filtering, washing and drying the crystallization to obtain the high quality A zeolite. The invention has got advantages such as easy and simple techniques in the process, small reacting devices, low cost, exact repeatability. The obtained A zeolite is of narrower particle distribution, quite perfect crystal shape and high crystalline.
Description
Technical field
The present invention is a kind of method of the A of preparation type zeolite, relates in particular to a kind of method for preparing A type zeolite with the coal gangue for the raw material two step method.
Background technology
China has coal gangue burden 30～4,000,000,000 tons now.The accumulation of coal gangue, land occupation, contaminated soil and water quality are destroyed the eubiosis, cause serious environmental problem, are various countries, the world today one of stubborn problems for it.Along with further implementing and the further in-depth of Chinese industrial process of the global strategy of sustainable development, the Chinese government is continuing to increase the dynamics of environmental protection work.Carry out comprehensive utilization development research, from coal gangue, extract various Chemicals, not only improve environment, solve, more can turn waste into wealth, create economic benefit by idle resource and the soil that takies to coal gangue.
In recent years, Feng Fangxia etc. are at " petroleum journal " 1997,13 (4): described in 104 pages of " is the synthetic ZSM-35 zeolite of raw material with the coal gangue " literary compositions and utilized the activation of coal gangue strong acid, the method of alkaline water heat condition synthesizing high-silicon zeolite, but the condition that this method requires is relatively harsher, must be purer kaolin as raw material.Ni Zheng etc. are in " petrochemical complex " 2000,29 (4): described in 336 pages of " producing NaX type zeolite by coal gangue " literary compositions and utilized activation of coal gangue alkali fusion and the synthetic NaX of acquisition of hydro-thermal type zeolite, but not removal of impurities in its process, products obtained therefrom certainty purity is not high.
Summary of the invention
The invention provides a kind of is the method for feedstock production purity, the high A type of degree of crystallinity zeolite with the coal gangue.
The present invention is achieved in that calcined coal gangue handles back and alkali fusion agent by mixing pyroreaction, and the alkali fusion thing is mended and added the aluminium salt crystallization that heats up again after water-soluble deironing, then crystallization product after filtration, wash, final drying gets high-quality A zeolite.
Synthetic method of the present invention comprises the steps:
1, coal gangue is pulverized below 60 orders, calcined 0.5-15 hour down at 400-1100 ℃;
2, SiO is pressed in coal gangue and the alkali fusion agent after will calcining
2: Na
2The O mol ratio is 1: 1.0-4.0 mixes, and reacts 0.5-10 hour down at 200-1200 ℃, obtains the alkali fusion thing, and wherein coal gangue is pressed contained SiO in the coal gangue
2Metering;
3, be H by water sodium mol ratio
2O: Na
2O=15-200 gives in the alkali fusion thing to add entry, after the deironing of physics method, gets the initial action thing.
4, in the initial action thing, add aluminium salt, make silica alumina ratio SiO
2: Al
2O
3Be 1.0-3.0: 1; Reacted crystallization 0.5-240 hour down at 25-180 ℃;
5, crystallization product gets throw out after filtration, and to the throw out deionized water wash, making sedimentary PH is 8-10, and dry under 80-180 ℃, gets high-quality 4A zeolite.
Described coal gangue is: all kinds, place of production difference, the coal gangue that composition differs.
Described alkali fusion agent is: sodium hydroxide, and yellow soda ash, or sodium bicarbonate etc.
Described aluminium salt is: aluminium hydroxide, aluminum oxide, metallic aluminium or Tai-Ace S 150 etc.
The present invention compared with prior art has following advantage:
The inventive method has fully activated and has comprised all quartzy sial effective constituents in the coal gangue, obtains high-crystallinity and highly purified A type zeolite by hydrothermal crystallizing.Method is simple for technology synthetic zeolite of the present invention, installs for a short time, and cost is low, repeats, and synthetic A zeolite has narrower size-grade distribution, quite perfectly crystalline form and high degree of crystallinity.
Embodiment
Embodiment 1
Getting 5g is crushed to 60 purpose Shanxi kalimeris coal gangues and (consists of: 49.85%SiO
2, 37.25%Al
2O
3) calcined 2 hours down at 800 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 1.5, mixes, and reacts 6 hours down at 400 ℃.By water sodium mol ratio is H
2O/Na
2O=34 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminium hydroxide, and making silica alumina ratio is 2.Reacted crystallization 0.5 hour down at 80 ℃.Crystallization product filters, and uses deionized water wash, and making sedimentary PH is 8, and at 110 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 2
Getting 5g is crushed to the bent coal gangue in 100 purpose Shanxi east and (consists of: 55.05%SiO
2, 35.83%Al
2O
3) calcined 8 hours down at 500 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 1.5, mixes, and reacts 4 hours down at 650 ℃.By water sodium mol ratio is H
2O/Na
2O=60 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminum oxide, and making silica alumina ratio is 1.5.Reacted crystallization 3 hours down at 80 ℃.Crystallization product filters, and uses deionized water wash, and making sedimentary PH is 9, and at 100 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 3
Getting 5g is crushed to 80 purpose Shanxi and collects blue coal gangue and (consist of: 58.20%SiO
2, 26.84%Al
2O
3) calcined 4 hours down at 700 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 1.9, mixes, and reacts 8 hours down at 400 ℃.By water sodium mol ratio is H
2O/Na
2O=15 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds Tai-Ace S 150, and making silica alumina ratio is 2.0.Reacted crystallization 240 hours down at 25 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 10, and at 80 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 4
Getting 5g is crushed to 60 purpose Shanxi town pit coal spoil and (consists of: 55.45%SiO
2, 25.71%Al
2O
3) calcined 2 hours down at 800 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 4.0, mixes, and reacts 3 hours down at 750 ℃.By water sodium mol ratio is H
2O/Na
2O=50 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminium hydroxide, and making silica alumina ratio is 1.0.Reacted crystallization 1 hour down at 90 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 8, and at 110 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 5
Getting 5g is crushed to the bent coal gangue in 100 purpose Shanxi west and (consists of: 56.50%SiO
2, 23.41%Al
2O
3) calcined 0.5 hour down at 1100 ℃.Add yellow soda ash then by Na
2O and SiO
2Mol ratio is 2.5, mixes, and reacts 15 hours down at 200 ℃.By water sodium mol ratio is H
2O/Na
2O=100 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminium hydroxide, and making silica alumina ratio is 1.4.Reacted crystallization 5 hours down at 150 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 8, and at 110 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 6
Getting 5g is crushed to 80 purpose Shanxi Xishan coal spoils and (consists of: 58.21%SiO
2, 28.25%Al
2O
3) calcined 1 hour down at 1000 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 1.0, mixes, and reacts 2 hours down at 800 ℃.By water sodium mol ratio is H
2O/Na
2O=80 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds metallic aluminium, and making silica alumina ratio is 1.9.Reacted crystallization 5 hours down at 60 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 8, and at 80 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 7
Getting 5g is crushed to 120 purpose Shan Xizhang village coal gangues and (consists of: 53.25%SiO
2, 33.15%Al
2O
3) calcined 0.5 hour down at 1100 ℃.Press Na with sodium hydroxide then
2O and SiO
2Mol ratio is 2.0, mixes, and reacts 7 hours down at 500 ℃.By water sodium mol ratio is H
2O/Na
2O=200 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminium hydroxide, and making silica alumina ratio is 2.5.Reacted crystallization 8 hours down at 180 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 8, and at 180 ℃ of dry down products that get, detecting through the X-diffraction is the A zeolite.
Embodiment 8
Getting 5g is crushed to 120 purpose Shanxi Lu Cun coal gangues and (consists of: 59.05%SiO
2, 35.23%Al
2O
3) calcined 2 hours down at 900 ℃.Hydro-oxidation sodium is pressed Na then
2O and SiO
2Mol ratio is 3.0, mixes, and reacts 3 hours down at 750 ℃.By water sodium mol ratio is H
2O/Na
2O=80 gives in the alkali fusion thing to add entry, after the deironing of physics method, adds aluminium hydroxide, and making silica alumina ratio is 3.Reacted crystallization 5 hours down at 70 ℃.Crystallization product filters, uses deionized water wash, and making sedimentary PH is 8, and at 110 ℃ of dry down products that get, detecting through the X-diffraction is high-quality A zeolite.
Claims (3)
1, a kind of method of preparing A type zeolite by gangue is characterized in that comprising the steps:
(1), coal gangue is pulverized below 60 orders, 400-1100 ℃ of following calcining 0.5-15 hour;
(2), SiO is pressed in coal gangue and the alkali fusion agent after will calcining
2: Na
2The O mol ratio is 1: 1.0-4.0 mixes, and reacts 0.5-10 hour down at 200-1200 ℃, obtains the alkali fusion thing, and wherein coal gangue is pressed contained SiO in the coal gangue
2Metering;
(3), be H by water sodium mol ratio
2O: Na
2O=15-200 gives in the alkali fusion thing to add entry, after the deironing of physics method, gets the initial action thing.
(4), in the initial action thing, add aluminium salt, make silica alumina ratio SiO
2: Al
2O
3Be 1.0-3.0: 1; Reacted crystallization 0.5-240 hour down at 25-180 ℃;
(5), crystallization product after filtration throw out, to the throw out deionized water wash, making sedimentary PH is 8-10, and 80-180 ℃ down dry, high-quality 4A zeolite.
2, the method for a kind of preparing A type zeolite by gangue as claimed in claim 1 is characterized in that described alkali fusion agent is sodium hydroxide, yellow soda ash or sodium bicarbonate.
3, the method for a kind of preparing A type zeolite by gangue as claimed in claim 1 is characterized in that described aluminium salt is aluminium hydroxide, aluminum oxide, metallic aluminium or Tai-Ace S 150.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410064592XA CN1298628C (en) | 2004-12-07 | 2004-12-07 | Method for preparing A type zeolite by gangue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410064592XA CN1298628C (en) | 2004-12-07 | 2004-12-07 | Method for preparing A type zeolite by gangue |
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| Publication Number | Publication Date |
|---|---|
| CN1631779A true CN1631779A (en) | 2005-06-29 |
| CN1298628C CN1298628C (en) | 2007-02-07 |
Family
ID=34846415
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410064592XA Expired - Fee Related CN1298628C (en) | 2004-12-07 | 2004-12-07 | Method for preparing A type zeolite by gangue |
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|---|---|
| CN (1) | CN1298628C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530978A (en) * | 2011-08-09 | 2012-07-04 | 中国环境科学研究院 | Method for preparing sodium type zeolite molecular sieves by utilizing red mud |
| CN108483460A (en) * | 2018-06-04 | 2018-09-04 | 陕西师范大学 | A method of using gangue be raw material two-step method Synthesis of 4 A-type Zeolite by Hydrothermal |
| CN108975348A (en) * | 2018-09-05 | 2018-12-11 | 中国神华能源股份有限公司 | A kind of method of production of 4 A molecular sifter |
| CN109305688A (en) * | 2017-11-16 | 2019-02-05 | 中国石油化工股份有限公司 | A kind of method of catalytic cracking spent catalyst synthesis NaA type molecular screen material |
| CN110395745A (en) * | 2019-09-04 | 2019-11-01 | 沈阳建筑大学 | A kind of P-A type molecular sieve and preparation method thereof prepared with self-igniting coal gangue |
| CN111017951A (en) * | 2019-12-26 | 2020-04-17 | 河北欣芮再生资源利用有限公司 | A-type zeolite molecular sieve and preparation method and application thereof |
| CN112209399A (en) * | 2020-09-11 | 2021-01-12 | 内蒙古师范大学 | Method for preparing X-type zeolite from coal gangue |
| CN114477213A (en) * | 2022-01-14 | 2022-05-13 | 上海大学 | Submicron 4A type molecular sieve and preparation method thereof |
| CN114751425A (en) * | 2022-04-02 | 2022-07-15 | 四川大学 | Preparation method and application of zeolite soil passivator with high iron content |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226081C (en) * | 2001-09-24 | 2005-11-09 | 复旦大学 | High-temp alkali fusing-hydrothermal crystallizing process for preparing A-type zeolite from coal gangue |
-
2004
- 2004-12-07 CN CNB200410064592XA patent/CN1298628C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530978A (en) * | 2011-08-09 | 2012-07-04 | 中国环境科学研究院 | Method for preparing sodium type zeolite molecular sieves by utilizing red mud |
| CN102530978B (en) * | 2011-08-09 | 2014-04-30 | 中国环境科学研究院 | Method for preparing sodium type zeolite molecular sieves by utilizing red mud |
| CN109305688A (en) * | 2017-11-16 | 2019-02-05 | 中国石油化工股份有限公司 | A kind of method of catalytic cracking spent catalyst synthesis NaA type molecular screen material |
| CN109305688B (en) * | 2017-11-16 | 2021-11-05 | 中国石油化工股份有限公司 | Method for synthesizing NaA type molecular sieve material by catalytic cracking waste catalyst |
| CN108483460A (en) * | 2018-06-04 | 2018-09-04 | 陕西师范大学 | A method of using gangue be raw material two-step method Synthesis of 4 A-type Zeolite by Hydrothermal |
| CN108975348A (en) * | 2018-09-05 | 2018-12-11 | 中国神华能源股份有限公司 | A kind of method of production of 4 A molecular sifter |
| CN110395745A (en) * | 2019-09-04 | 2019-11-01 | 沈阳建筑大学 | A kind of P-A type molecular sieve and preparation method thereof prepared with self-igniting coal gangue |
| CN111017951A (en) * | 2019-12-26 | 2020-04-17 | 河北欣芮再生资源利用有限公司 | A-type zeolite molecular sieve and preparation method and application thereof |
| CN111017951B (en) * | 2019-12-26 | 2021-07-27 | 河北欣芮再生资源利用有限公司 | A-type zeolite molecular sieve and preparation method and application thereof |
| CN112209399A (en) * | 2020-09-11 | 2021-01-12 | 内蒙古师范大学 | Method for preparing X-type zeolite from coal gangue |
| CN114477213A (en) * | 2022-01-14 | 2022-05-13 | 上海大学 | Submicron 4A type molecular sieve and preparation method thereof |
| CN114751425A (en) * | 2022-04-02 | 2022-07-15 | 四川大学 | Preparation method and application of zeolite soil passivator with high iron content |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1298628C (en) | 2007-02-07 |
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Granted publication date: 20070207 Termination date: 20121207 |