CN103787361A - Method for producing 4A zeolite by using waste aluminum oxide and quartz sand - Google Patents
Method for producing 4A zeolite by using waste aluminum oxide and quartz sand Download PDFInfo
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- CN103787361A CN103787361A CN201410024379.XA CN201410024379A CN103787361A CN 103787361 A CN103787361 A CN 103787361A CN 201410024379 A CN201410024379 A CN 201410024379A CN 103787361 A CN103787361 A CN 103787361A
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Abstract
The invention relates to a method for producing 4A zeolite by using waste aluminum oxide and quartz sand. In the method, waste aluminum oxide, quartz sand and sodium carbonate having the advantages of wide source and low cost can be taken as raw materials, so that the production cost is lowered. Meanwhile, the problem of difficulty in transporting liquid dangerous articles is solved, the evaporation load of a system is lowered, and the aims of increasing yield, enhancing stability, lowering cost and enhancing effect are fulfilled.
Description
Technical field
The present invention relates to a kind of method of the 4A of production zeolite, be specifically related to a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite.
Background technology
At present industrial conventional hydrothermal synthesis method is produced 4A zeolite molecular sieve, conventionally the aluminium source adopting is bauxite or aluminium hydroxide, with the sodium aluminate solution that liquid base stripping under certain condition obtains, silicon source is the liquid soluble glass that sodium silicate solid obtains through high temperature melting.Sodium aluminate solution and water glass, after cooling, carry out pulp at low temperatures by certain proportioning, adds after directed agents, and aging for some time, then carry out crystallization after heating up, obtain qualified 4A zeolite molecular sieve product.The method of this Hydrothermal Synthesis 4A molecular sieve, 4A zeolite product per ton need to consume 0.5 ton, aluminium hydroxide, 0.6 ton of water glass, 0.4 ton, caustic soda, raw materials cost is large, and raw material affects greatly by market fluctuation, is unfavorable for stably manufactured.Traditional method technical process is long in addition, and energy consumption is large, is unfavorable for saving energy and reduce the cost, and therefore, invents a kind of raw materials cost cheap, and the production method of the short 4A zeolite of technical process is that insider endeavours the problem that will solve always.
Summary of the invention
The object of the invention is to solve prior art provides a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite, and the method can adopt wide material sources, cheap waste alumina, quartz sand and soda ash as raw material, has reduced production cost.Meanwhile, avoid a transportation difficult problem for dangerous liquid material, reduced the evaporation load of system, thereby reached the object of stable high yield, cost efficiency.
For achieving the above object, the present invention is by the following technical solutions:
Utilize waste alumina and quartz sand to produce a method for 4A zeolite, it specifically comprises the steps:
(1) be not less than 60% waste alumina as raw material, according to Na take alumina content
2o/Al
2o
3mol ratio is that ratio and the soda ash of 1.0-1.5 mixes, and carries out roasting under the condition of 800 ~ 1000 ℃, and roasting time is 0.3 ~ 1h, obtains the material after roasting;
(2) the material alkaline aqueous solution after the roasting obtaining in step (1) is carried out to stripping, filter and obtain sodium aluminate solution;
(3) prepare Na
2the concentration of O is the basic solution of 3-5mol/L, adds quartz sand to mix by modulus of water glass 2.5 ~ 3.5 in above-mentioned basic solution, at 160-200 ℃, reacts 1-3h, obtains liquid soluble glass;
(4) liquid soluble glass that sodium aluminate solution step (2) being obtained and step (3) obtain mixes, and adds 4A guiding agent for zeolite, pulp, and crystallization, filters and obtains the former powder of 4A zeolite molecular sieve.
Further, the Na of described step (2) the neutral and alkali aqueous solution
2o concentration is 50-100g/L.
Further, described step (2) neutral and alkali aqueous solution add-on is for making Na in solution
2the mol ratio of O/Al2O3 is 1.5-2.0.
Further, the alkaline aqueous solution in described step (2) is that step (4) is filtered the 4A zeolite mother liquor after 4A zeolite molecular sieve.
Further, the preparation Na in described step (3)
2the concentration of O is that the concrete operations of the basic solution of 3-5mol/L are that the 4A zeolite mother liquor obtaining after filtration 4A zeolite molecular sieve in step (4) is concentrated and obtained.
Further, in described step (4), the synthetic ratio of sodium aluminate solution, liquid soluble glass is: Na
2o:Al
2o
3: SiO
2: H
2o=2-4:1:1.9-2.1:50-200.
Further, described pulp temperature is 50 ~ 70 ℃, and slurry time is 10 ~ 20min.
Further, in described step (4), crystallization temperature is 80 ~ 100 ℃, and crystallization time is 60 ~ 180min.
Further, the directed agents in described step (4) meets lower ratio: Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300.
Further, the addition of described directed agents is 0.1-0.5%.
Compared with prior art, the beneficial effect that the present invention obtains is:
Method of the present invention is on the technique basis of Synthesis of 4 A-type Zeolite by Hydrothermal molecular sieve, and original raw materials for production have been carried out improving thoroughly.Utilize the aluminum oxide waste material of domestic each Alumina Enterprise as aluminium source, wide material sources, price is suitable; Utilize the high white quartz sand of Area, Fengyang County, Anhui as silicon source.First by aluminum oxide waste material and soda ash according to certain alkali than mixing, carry out at a certain temperature roasting with rotary kiln, the material after roasting can obtain qualified sodium aluminate solution with the alkali lye stripping of lower concentration.Secondly, 4A zeolite mother liquor, through being evaporated to after finite concentration, reacts at a certain temperature with quartz sand, obtains liquid soluble glass.According to suitable proportioning, two kinds of solution are fully mixed under violent stirring condition, after certain hour, can obtain qualified 4A zeolite molecular sieve product.The present invention has changed the raw materials for production of the former powder of 4A zeolite molecular sieve, adopts wide material sources, cheap waste alumina, quartz sand and soda ash, has reduced production cost.Meanwhile, by rational proportioning, adopt new technique, make the Na in system
2o obtains rational balance, need not supplement liquid caustic soda, has avoided a transportation difficult problem for dangerous liquid material, has reduced the evaporation load of system, thereby reaches the object of stable high yield, cost efficiency.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing 1 and specific embodiment, the present invention is described in more detail.
What the middle waste alumina in the present embodiment was alumina industry land material or the material etc. that scabs, wherein alumina content is greater than 60% all the other composition silicon-dioxide and is less than 6%, calcium oxide 5% left and right, iron 2-3%.
embodiment 1
The preparation of Part1 sodium aluminate solution
Get the waste alumina in alumina industry, it is mainly containing following composition: 82%Al after testing
2o
3, 5% silicon-dioxide, 5% calcium oxide and iron 2%, according to Al in aluminum oxide waste material
2o
3content, according to Na
2o, Al
2o
3mol ratio 1.15 add soda ash, and mix, by rotary kiln roasting under 950 ℃ of conditions.Roasting time, by revolution and the discharge quantity of rotary kiln, is controlled at 0.5h, and roasting material is with containing Na
2o concentration is the stripping of 75g/L alkaline aqueous solution, makes Na in whole solution
2o/Al
2o
3mol ratio be 2, obtain sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The rare mother liquor of 4A zeolite, by evaporation, makes Na
2o concentration reaches 3.5mol/l, according to the Na of mother liquid evaporation
2o concentration, the modulus of water glass 2.9 that the add-on of quartz sand is keeping system at reaction kettle for reaction 2h, obtains liquid soluble glass under 180 ℃ of conditions.
The preparation of the former powder of Part3 4A zeolite molecular sieve
Liquid soluble glass prepared by sodium aluminate prepared by part1 and part2, the proportioning Na producing according to 4A zeolite
2o:Al
2o
3: SiO
2: H
2o=4:1; 2.1:200, adds 0.1% directed agents (Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300), through pulp 15min under 60 ℃ of conditions, then crystallization 60min under 80 ℃ of conditions, then through filtering, wash, dry, packing, can obtain the qualified former powder of 4A zeolite molecular sieve.
The obtained former powder of 4A zeolite molecular sieve is carried out to Performance Detection, and recording water absorption index is 28.
embodiment 2
The preparation of Part1 sodium aluminate solution
Get the waste alumina in alumina industry, it is mainly containing following composition: 82%Al after testing
2o
3, 5% silicon-dioxide, 5% calcium oxide and iron 2%, according to Al in aluminum oxide waste material
2o
3content, according to Na
2o, Al
2o
3mol ratio 1.0 add soda ash, and mix, by rotary kiln roasting under 1000 ℃ of conditions.Roasting time, by revolution and the discharge quantity of rotary kiln, is controlled at 0.3h, and roasting material is with containing Na
2o concentration is the stripping of 50g/L alkaline aqueous solution, makes Na in whole solution
2o/Al
2o
3mol ratio be 1.5, obtain sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The rare mother liquor of 4A zeolite, by evaporation, makes Na
2o concentration reaches 3mol/l, according to the Na of mother liquid evaporation
2o concentration, the modulus of water glass 2.5 that the add-on of quartz sand is keeping system at reaction kettle for reaction 1h, obtains liquid soluble glass under 160 ℃ of conditions.
The preparation of the former powder of Part3 4A zeolite molecular sieve
Liquid soluble glass prepared by sodium aluminate prepared by part1 and part2, the proportioning Na producing according to 4A zeolite
2o:Al
2o
3: SiO
2: H
2o=2:1:1.9:100, adds 0.5% directed agents (Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300), through pulp 10min under 50 ℃ of conditions, then crystallization 120min under 100 ℃ of conditions, then through filtering, wash, dry, packing, can obtain the qualified former powder of 4A zeolite molecular sieve.
The obtained former powder of 4A zeolite molecular sieve is carried out to Performance Detection, and recording water absorption index is 28.
embodiment 3
The preparation of Part1 sodium aluminate solution
Get the waste alumina in alumina industry, it is mainly containing following composition: 82%Al after testing
2o
3, 5% silicon-dioxide, 5% calcium oxide and iron 2%, according to Al in aluminum oxide waste material
2o
3content, according to Na
2o, Al
2o
3mol ratio 1.5 add soda ash, and mix, by rotary kiln roasting under 800 ℃ of conditions.Roasting time, by revolution and the discharge quantity of rotary kiln, is controlled at 1h, and roasting material is with containing Na
2o concentration is the stripping of 100g/L alkaline aqueous solution, makes Na in whole solution
2o/Al
2o
3mol ratio be 2, obtain sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The rare mother liquor of 4A zeolite, by evaporation, makes Na
2o concentration reaches 5mol/l, according to the Na of mother liquid evaporation
2o concentration, the modulus of water glass 3 that the add-on of quartz sand is keeping system at reaction kettle for reaction 2h, obtains liquid soluble glass under 200 ℃ of conditions.
The preparation of the former powder of Part3 4A zeolite molecular sieve
Liquid soluble glass prepared by sodium aluminate prepared by part1 and part2, the proportioning Na producing according to 4A zeolite
2o:Al
2o
3: SiO
2: H
2o=3:1:2:150, adds 0.3% directed agents (Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300), through pulp 20min under 70 ℃ of conditions, then crystallization 180min under 90 ℃ of conditions, then through filtering, wash, dry, packing, can obtain the qualified former powder of 4A zeolite molecular sieve.
The obtained former powder of 4A zeolite molecular sieve is carried out to Performance Detection, and recording water absorption index is 28.
embodiment 4
The preparation of Part1 sodium aluminate solution
Get the waste alumina in alumina industry, it is mainly containing following composition: 82%Al after testing
2o
3, 5% silicon-dioxide, 5% calcium oxide and iron 2%, according to Al in aluminum oxide waste material
2o
3content, according to Na
2o, Al
2o
3mol ratio 1.25 add soda ash, and mix, by rotary kiln roasting under 900 ℃ of conditions.Roasting time, by revolution and the discharge quantity of rotary kiln, is controlled at 0.7h, and roasting material is with containing Na
2o concentration is the stripping of 80g/L alkaline aqueous solution, makes Na in whole solution
2o/Al
2o
3mol ratio be 1.7, obtain sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The rare mother liquor of 4A zeolite, by evaporation, makes Na
2o concentration reaches 4mol/l, according to the Na of mother liquid evaporation
2o concentration, the modulus of water glass 3.5 that the add-on of quartz sand is keeping system at reaction kettle for reaction 3h, obtains liquid soluble glass under 190 ℃ of conditions.
The preparation of the former powder of Part3 4A zeolite molecular sieve
Liquid soluble glass prepared by sodium aluminate prepared by part1 and part2, the proportioning Na producing according to 4A zeolite
2o:Al
2o
3: SiO
2: H
2o=3.5:1:2:50, adds 0.5% directed agents (Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300), through pulp 15min under 65 ℃ of conditions, then crystallization 100min under 90 ℃ of conditions, then through filtering, wash, dry, packing, can obtain the qualified former powder of 4A zeolite molecular sieve.
The obtained former powder of 4A zeolite molecular sieve is carried out to Performance Detection, and recording water absorption index is 28.
embodiment 5
Get the waste alumina in alumina industry, it is mainly containing following composition: 90%Al after testing
2o
3, 2% silicon-dioxide, 5% calcium oxide and iron 1%, according to Al in aluminum oxide waste material
2o
3content, according to Na
2o, Al
2o
3mol ratio 1.25 add soda ash, and mix, by rotary kiln roasting under 900 ℃ of conditions.Roasting time, by revolution and the discharge quantity of rotary kiln, is controlled at 0.7h, and roasting material is with containing Na
2o concentration is the stripping of 80g/L alkaline aqueous solution, makes Na in whole solution
2o/Al
2o
3mol ratio be 1.7, obtain sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The rare mother liquor of 4A zeolite, by evaporation, makes Na
2o concentration reaches 4mol/l, according to the Na of mother liquid evaporation
2o concentration, the modulus of water glass 3.5 that the add-on of quartz sand is keeping system at reaction kettle for reaction 3h, obtains liquid soluble glass under 190 ℃ of conditions.
The preparation of the former powder of Part3 4A zeolite molecular sieve
Liquid soluble glass prepared by sodium aluminate prepared by part1 and part2, the proportioning Na producing according to 4A zeolite
2o:Al
2o
3: SiO
2: H
2o=3.5:1:2:50, adds 0.2% directed agents (Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300), through pulp 15min under 65 ℃ of conditions, then crystallization 100min under 90 ℃ of conditions, then through filtering, wash, dry, packing, can obtain the qualified former powder of 4A zeolite molecular sieve.
The obtained former powder of 4A zeolite molecular sieve is carried out to Performance Detection, and recording water absorption index is 28.
comparative example 1
Difference from Example 5 is to substitute waste alumina with domestic bauxite, and other parameters and condition are with embodiment 5.
comparative example 2
Difference from Example 5 is to substitute waste alumina with import bauxite, and other parameters and condition are with embodiment 5.
effect example 1
The water absorption index of solubility rate, utilization ratio and the final former powder of 4A zeolite molecular sieve obtaining to aluminum oxide in embodiment 5 and comparative example 1 and 2 technical schemes compares, in table 1.
| Project | Embodiment 5 | Comparative example 1 | Comparative example 2 |
| Digesting efficiency of alumina % | 85% | 65% | 60% |
| Aluminum oxide utilization ratio | 88% | 70% | 65% |
| Water adsorptive value | 28 | 26.5 | 27 |
Conclusion, method of the present invention, has searched out the 4A zeolite synthesis raw material of price cheapness, and has found out suitable stripping and reaction conditions for the singularity of raw material, has significantly improved the utilization ratio of aluminum oxide, obtains the former powder of 4A zeolite molecular sieve of better performances.
The above embodiment is only the preferred embodiments of the present invention, and is not the exhaustive of the feasible enforcement of the present invention.For persons skilled in the art, any apparent change of under the prerequisite that does not deviate from the principle of the invention and spirit, it having been done, within all should being contemplated as falling with claim protection domain of the present invention.
Claims (10)
1. utilize waste alumina and quartz sand to produce a method for 4A zeolite, it is characterized in that: it specifically comprises the steps:
(1) be not less than 60% waste alumina as raw material, according to Na take alumina content
2o/Al
2o
3mol ratio is that 1.0 ~ 1.5 ratio and soda ash mix, and carries out roasting under the condition of 800 ~ 1000 ℃, and roasting time is 0.3 ~ 1h, obtains the material after roasting;
(2) the material alkaline aqueous solution after the roasting obtaining in step (1) is carried out to stripping, filter and obtain sodium aluminate solution;
(3) prepare Na
2the concentration of O is the basic solution of 3 ~ 5mol/L, adds quartz sand to mix by modulus of water glass 2.5 ~ 3.5 in above-mentioned basic solution, at 160 ~ 200 ℃, reacts 1-3h, obtains liquid soluble glass;
(4) liquid soluble glass that sodium aluminate solution step (2) being obtained and step (3) obtain mixes, and adds 4A guiding agent for zeolite, pulp, and crystallization, filters and obtains the former powder of 4A zeolite molecular sieve.
2. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: the Na of described step (2) the neutral and alkali aqueous solution
2o concentration is 50 ~ 100g/L.
3. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: described step (2) neutral and alkali aqueous solution add-on is for making Na in solution
2o/Al
2o
3mol ratio be 1.5-2.0.
4. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: the alkaline aqueous solution in described step (2) is that step (4) is filtered the 4A zeolite mother liquor after 4A zeolite molecular sieve.
5. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: the preparation Na in described step (3)
2the concentration of O is that the concrete operations of the basic solution of 3-5mol/L are that the 4A zeolite mother liquor obtaining after filtration 4A zeolite molecular sieve in step (4) is concentrated and obtained.
6. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: in described step (4), the synthetic ratio of sodium aluminate solution, liquid soluble glass is: Na
2o:Al
2o
3: SiO
2: H
2o=2-4:1:1.9-2.1:50-200.
7. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: described pulp temperature is 50 ~ 70 ℃, and slurry time is 10 ~ 20min.
8. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 1, is characterized in that: in described step (4), crystallization temperature is 80 ~ 100 ℃, and crystallization time is 60 ~ 180min.
9. according to a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite described in claim 1-8 any one, it is characterized in that: the directed agents in described step (4) meets lower ratio: Na
2o:Al
2o
3: SiO
2: H
2o=15:1:10:300.
10. a kind of method of utilizing waste alumina and quartz sand to produce 4A zeolite according to claim 9, is characterized in that: the addition of described directed agents is 0.1-0.5%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105236443A (en) * | 2015-09-16 | 2016-01-13 | 山东磊宝锆业科技股份有限公司 | Technology for preparing 4A zeolite from AZS solid waste material |
| CN107827122A (en) * | 2017-11-23 | 2018-03-23 | 达州励志环保科技有限公司 | A kind of method for producing 4A zeolites using waste alumina and quartz sand |
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| CN1749163A (en) * | 2005-10-25 | 2006-03-22 | 东营市海星化工有限公司 | Process for producing 4A zeolite |
| CN101913637A (en) * | 2010-08-13 | 2010-12-15 | 刘德华 | Process method for producing fluorine compounds and silicon compounds by cleanly utilizing fluosilicic acid |
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2014
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| CN1749163A (en) * | 2005-10-25 | 2006-03-22 | 东营市海星化工有限公司 | Process for producing 4A zeolite |
| CN101913637A (en) * | 2010-08-13 | 2010-12-15 | 刘德华 | Process method for producing fluorine compounds and silicon compounds by cleanly utilizing fluosilicic acid |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236443A (en) * | 2015-09-16 | 2016-01-13 | 山东磊宝锆业科技股份有限公司 | Technology for preparing 4A zeolite from AZS solid waste material |
| CN105236443B (en) * | 2015-09-16 | 2017-10-13 | 山东磊宝锆业科技股份有限公司 | The technique that AZS solid wastes prepare 4A zeolites |
| CN107827122A (en) * | 2017-11-23 | 2018-03-23 | 达州励志环保科技有限公司 | A kind of method for producing 4A zeolites using waste alumina and quartz sand |
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