CN107827122A - A kind of method for producing 4A zeolites using waste alumina and quartz sand - Google Patents
A kind of method for producing 4A zeolites using waste alumina and quartz sand Download PDFInfo
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- CN107827122A CN107827122A CN201711177438.7A CN201711177438A CN107827122A CN 107827122 A CN107827122 A CN 107827122A CN 201711177438 A CN201711177438 A CN 201711177438A CN 107827122 A CN107827122 A CN 107827122A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/14—Type A
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B39/14—Type A
- C01B39/145—Type A using at least one organic template directing agent
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Abstract
This hair is related to a kind of method for producing 4A zeolites using waste alumina and quartz sand, and this method can use wide material sources, cheap waste alumina, quartz sand and soda ash to reduce production cost as raw material.Meanwhile avoid the transport problem of dangerous liquid material, reduce the evaporation load of system, so as to reach stable high yield, cost efficiency purpose.
Description
Technical field
The present invention relates to a kind of method for producing 4A zeolites, and in particular to one kind utilizes waste alumina and quartz sand production 4A
The method of zeolite.
Background technology
Industrial conventional hydrothermal synthesis method production 4A zeolite molecular sieves at present, the silicon source of generally use be bauxite or
Aluminium hydroxide, the sodium aluminate solution obtained with liquid base dissolution under certain condition, silicon source are that sodium silicate solid passes through high temperature melting
Change obtained liquid soluble glass.Sodium aluminate solution and waterglass are carried out at low temperature after cooling, by certain proportioning
Pulp, after adding directed agents, aging for a period of time, then after heating up carries out crystallization, obtains qualified 4A zeolite molecular sieve products.This
The method of kind Hydrothermal Synthesiss 4A molecular sieves, 4A zeolite products per ton need to consume 0.5 ton of aluminium hydroxide, 0.6 ton of waterglass, caustic soda
0.4 ton, cost of material is big, and raw material is influenceed greatly, to be unfavorable for steady production by market fluctuation.Traditional method technological process in addition
Long, energy resource consumption is big, is unfavorable for energy-saving, therefore, invents a kind of low raw-material cost, the short 4A zeolites of technological process
Production method be always that professional endeavours the problem of to be solved.
The content of the invention
It is an object of the invention to solve, prior art offer is a kind of to produce 4A zeolites using waste alumina and quartz sand
Method, this method can use wide material sources, cheap waste alumina, quartz sand and soda ash to reduce production as raw material
Cost.Meanwhile the transport problem of dangerous liquid material is avoided, the evaporation load of system is reduced, so as to reach stable high yield, drop
The purpose of this synergy.
To achieve the above object, the present invention uses following technical scheme：
A kind of method for producing 4A zeolites using waste alumina and quartz sand, it specifically comprises the following steps：
(1) it is 1.0- according to Na2O/Al2O3 mol ratios using waste alumina of the alumina content not less than 60% as raw material
1.5 ratio mixes with soda ash, is calcined under conditions of 800~1000 DEG C, roasting time is 0.3~1h, is calcined
Material afterwards；
(2) material after the roasting that will be obtained in step (1) carries out dissolution with alkaline aqueous solution, is filtrated to get sodium aluminate solution
Liquid；
(3) concentration for preparing Na2O is 3-5mol/L alkaline solution, by modulus of water glass 2.5~3.5 to above-mentioned alkalescence
Quartz sand is added in solution to mix, and is reacted 1-3h at 160-200 DEG C, is obtained liquid soluble glass；
(4) liquid soluble glass that the sodium aluminate solution and step (3) obtained step (2) obtains mixes, and adds 4A zeolites
Directed agents, pulp, crystallization, it is filtrated to get 4A zeolite molecular sieve original powder.
Further, the Na2O concentration of step (2) the neutral and alkali aqueous solution is 50-100g/L.
Further, step (2) the neutral and alkali aqueous solution addition is that the mol ratio for making Na2O/Al2O3 in solution is
1.5-2.0。
Further, the alkaline aqueous solution in the step (2) is that step (4) filters the 4A zeolites after 4A zeolite molecular sieves
Mother liquor.
Further, the concentration of the preparation Na2O in the step (3) is the concrete operations of 3-5mol/L alkaline solution
It is to be concentrated to give the 4A zeolite mother liquors obtained after filtering 4A zeolite molecular sieves in step (4).
Further, sodium aluminate solution, the synthesis ratio of liquid soluble glass are in the step (4)：Na2O：Al2O3：
SiO2：H2O=2-4：1：1.9-2.1：50-200.
Further, the slurrying temperature is 50~70 DEG C, and slurry time is 10~20min.
Further, crystallization temperature is 80~100 DEG C in the step (4), and crystallization time is 60~180min.
Further, the directed agents in the step (4) meet lower ratio：Na2O：Al2O3：SiO2：H2O=15：1：
10：300.
Further, the addition of the directed agents is 0.1-0.5%.
Compared with prior art, what the present invention obtained has the beneficial effect that：
The method of the present invention is on the Process ba- sis of Synthesis of 4 A-type Zeolite by Hydrothermal molecular sieve, and original raw materials for production are carried out
Thoroughly improve.Oxidation aluminium waste by the use of domestic each Alumina Enterprise is used as silicon source, wide material sources, affordable；Utilize
The high crystobalite sand of Area, Fengyang County, Anhui is as silicon source.Aluminium waste and soda ash will be aoxidized first to mix according to certain alkali ratio, with revolution
Kiln is calcined at a certain temperature, and the alkali lye dissolution of the material low concentration after roasting can obtain qualified sodium aluminate solution
Liquid.Secondly, 4A zeolite mother liquors react at a certain temperature after being evaporated to finite concentration, with quartz sand, obtain liquid water glass
Glass.According to appropriate proportioning, two kinds of solution are sufficiently mixed under the conditions of strong agitation, after certain time, you can it is qualified to obtain
4A zeolite molecular sieve products.The present invention changes the raw materials for production of 4A zeolite molecular sieve original powder, low using wide material sources, price
Honest and clean waste alumina, quartz sand and soda ash, reduces production cost.Meanwhile by reasonably matching, using new technique, make
Na2O in system is reasonably balanced, and without supplement liquid caustic soda, is avoided the transport problem of dangerous liquid material, is reduced system
Evaporation load, so as to reach stable high yield, cost efficiency purpose.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
The present invention is described in more detail below in conjunction with accompanying drawing 1 and specific embodiment.
Landing material or scab material etc. of the middle waste alumina for alumina industry in the present embodiment, wherein alumina content is big
In 60% remaining composition silica less than 6%, calcium oxide 5% or so, iron 2-3%.
Embodiment 1
The preparation of Part1 sodium aluminate solutions
The waste alumina in alumina industry is taken, it mainly contains following component after testing：82%Al2O3,5% titanium dioxide
Silicon, 5% calcium oxide and iron 2%, according to the content of Al2O3 in oxidation aluminium waste, add according to Na2O, Al2O3 mol ratio 1.15
Enter soda ash, and be well mixed, be calcined by rotary kiln under the conditions of 950 DEG C.Revolution and blanking of the roasting time by rotary kiln
Amount, is controlled in 0.5h, and roasting material is made in whole solution with the dissolution that concentration containing Na2O is 75g/L alkaline aqueous solutions
Na2O/Al2O3 mol ratio is 2, obtains sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The dilute mother liquor of 4A zeolites makes Na2O concentration reach 3.5mol/l, according to the Na2O concentration of evaporation mother liquor, stone by evaporation
The addition of sand is the modulus of water glass 2.9 of holding system, reacts 2h in a kettle under the conditions of 180 DEG C, obtains liquid
Waterglass.
The preparation of Part34A zeolite molecular sieve original powder
Liquid soluble glass prepared by the part1 sodium aluminates prepared and part2, the proportioning Na2O produced according to 4A zeolites：
Al2O3：SiO2：H2O=4：1；2.1：200, add 0.1% directed agents (Na2O：Al2O3：SiO2：H2O=15：1：10：
300), by pulp 15min under the conditions of 60 DEG C, the then crystallization 60min under the conditions of 80 DEG C, then by filtering, washing, drying,
Packaging, you can obtain qualified 4A zeolite molecular sieve original powder.
Performance detection is carried out to resulting 4A zeolite molecular sieve originals powder, measures water absorption index as 28.
Embodiment 2
The preparation of Part1 sodium aluminate solutions
The waste alumina in alumina industry is taken, it mainly contains following component after testing：82%Al2O3,5% titanium dioxide
Silicon, 5% calcium oxide and iron 2%, according to the content of Al2O3 in oxidation aluminium waste, added according to Na2O, Al2O3 mol ratio 1.0
Soda ash, and be well mixed, it is calcined by rotary kiln under the conditions of 1000 DEG C.Revolution and blanking of the roasting time by rotary kiln
Amount, is controlled in 0.3h, and roasting material is made in whole solution with the dissolution that concentration containing Na2O is 50g/L alkaline aqueous solutions
Na2O/Al2O3 mol ratio is 1.5, obtains sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The dilute mother liquor of 4A zeolites makes Na2O concentration reach 3mol/l, according to the Na2O concentration of evaporation mother liquor, quartz by evaporation
The addition of sand is the modulus of water glass 2.5 of holding system, reacts 1h in a kettle under the conditions of 160 DEG C, obtains liquid water
Glass.
The preparation of Part3 4A zeolite molecular sieve original powder
Liquid soluble glass prepared by the part1 sodium aluminates prepared and part2, the proportioning Na2O produced according to 4A zeolites：
Al2O3：SiO2：H2O=2：1：1.9：100, add 0.5% directed agents (Na2O：Al2O3：SiO2：H2O=15：1：10：
300), by pulp 10min under the conditions of 50 DEG C, then the crystallization 120min under the conditions of 100 DEG C, then by filtering, washing, baking
Dry, packaging, you can obtain qualified 4A zeolite molecular sieve original powder.
Performance detection is carried out to resulting 4A zeolite molecular sieve originals powder, measures water absorption index as 28.
Embodiment 3
The preparation of Part1 sodium aluminate solutions
The waste alumina in alumina industry is taken, it mainly contains following component after testing：82%Al2O3,5% titanium dioxide
Silicon, 5% calcium oxide and iron 2%, according to the content of Al2O3 in oxidation aluminium waste, added according to Na2O, Al2O3 mol ratio 1.5
Soda ash, and be well mixed, it is calcined by rotary kiln under the conditions of 800 DEG C.Roasting time by the revolution and discharge quantity of rotary kiln,
In 1h, roasting material makes Na2O/ in whole solution with the dissolution that concentration containing Na2O is 100g/L alkaline aqueous solutions for control
Al2O3 mol ratio is 2, obtains sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The dilute mother liquor of 4A zeolites makes Na2O concentration reach 5mol/l, according to the Na2O concentration of evaporation mother liquor, quartz by evaporation
The addition of sand is the modulus of water glass 3 of holding system, reacts 2h in a kettle under the conditions of 200 DEG C, obtains liquid water glass
Glass.
The preparation of Part3 4A zeolite molecular sieve original powder
Liquid soluble glass prepared by the part1 sodium aluminates prepared and part2, the proportioning Na2O produced according to 4A zeolites：
Al2O3：SiO2：H2O=3：1：2：150, add 0.3% directed agents (Na2O：Al2O3：SiO2：H2O=15：1：10：300),
By pulp 20min under the conditions of 70 DEG C, the then crystallization 180min under the conditions of 90 DEG C, then by filtering, washing, drying, packaging,
It can obtain qualified 4A zeolite molecular sieve original powder.
Performance detection is carried out to resulting 4A zeolite molecular sieve originals powder, measures water absorption index as 28.
Embodiment 4
The preparation of Part1 sodium aluminate solutions
The waste alumina in alumina industry is taken, it mainly contains following component after testing：82%Al2O3,5% titanium dioxide
Silicon, 5% calcium oxide and iron 2%, according to the content of Al2O3 in oxidation aluminium waste, add according to Na2O, Al2O3 mol ratio 1.25
Enter soda ash, and be well mixed, be calcined by rotary kiln under the conditions of 900 DEG C.Revolution and blanking of the roasting time by rotary kiln
Amount, is controlled in 0.7h, and roasting material is made in whole solution with the dissolution that concentration containing Na2O is 80g/L alkaline aqueous solutions
Na2O/Al2O3 mol ratio is 1.7, obtains sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The dilute mother liquor of 4A zeolites makes Na2O concentration reach 4mol/l, according to the Na2O concentration of evaporation mother liquor, quartz by evaporation
The addition of sand is the modulus of water glass 3.5 of holding system, reacts 3h in a kettle under the conditions of 190 DEG C, obtains liquid water
Glass.
The preparation of Part3 4A zeolite molecular sieve original powder
Liquid soluble glass prepared by the part1 sodium aluminates prepared and part2, the proportioning Na2O produced according to 4A zeolites：
Al2O3：SiO2：H2O=3.5：1：2：50, add 0.5% directed agents (Na2O：Al2O3：SiO2：H2O=15：1：10：300),
By pulp 15min under the conditions of 65 DEG C, the then crystallization 100min under the conditions of 90 DEG C, then by filtering, washing, drying, packaging,
It can obtain qualified 4A zeolite molecular sieve original powder.
Performance detection is carried out to resulting 4A zeolite molecular sieve originals powder, measures water absorption index as 28.
Embodiment 5
The waste alumina in alumina industry is taken, it mainly contains following component after testing：90%Al2O3,2% titanium dioxide
Silicon, 5% calcium oxide and iron 1%, according to the content of Al2O3 in oxidation aluminium waste, add according to Na2O, Al2O3 mol ratio 1.25
Enter soda ash, and be well mixed, be calcined by rotary kiln under the conditions of 900 DEG C.Revolution and blanking of the roasting time by rotary kiln
Amount, is controlled in 0.7h, and roasting material is made in whole solution with the dissolution that concentration containing Na2O is 80g/L alkaline aqueous solutions
Na2O/Al2O3 mol ratio is 1.7, obtains sodium aluminate solution.
The preparation of Part2 liquid soluble glass
The dilute mother liquor of 4A zeolites makes Na2O concentration reach 4mol/l, according to the Na2O concentration of evaporation mother liquor, quartz by evaporation
The addition of sand is the modulus of water glass 3.5 of holding system, reacts 3h in a kettle under the conditions of 190 DEG C, obtains liquid water
Glass.
The preparation of Part3 4A zeolite molecular sieve original powder
Liquid soluble glass prepared by the part1 sodium aluminates prepared and part2, the proportioning Na2O produced according to 4A zeolites：
Al2O3：SiO2：H2O=3.5：1：2：50, add 0.2% directed agents (Na2O：Al2O3：SiO2：H2O=15：1：10：300),
By pulp 15min under the conditions of 65 DEG C, the then crystallization 100min under the conditions of 90 DEG C, then by filtering, washing, drying, packaging,
It can obtain qualified 4A zeolite molecular sieve original powder.
Performance detection is carried out to resulting 4A zeolite molecular sieve originals powder, measures water absorption index as 28.
Comparative example 1
Difference from Example 5 is to substitute waste alumina, other specification and the same embodiment of condition with domestic bauxite
5。
Comparative example 2
Difference from Example 5 is to substitute waste alumina, other specification and the same embodiment of condition with import bauxite
5。
Effect example 1
To the dissolution rate of aluminum oxide, utilization rate and the 4A boilings finally obtained in embodiment 5 and the technical scheme of comparative example 1 and 2
The water absorption index of stone molecular screen primary powder is compared, and is shown in Table 1.
Claims (10)
- A kind of 1. method for producing 4A zeolites using waste alumina and quartz sand, it is characterised in that：It specifically comprises the following steps：(1) it is 1.0~1.5 according to Na2O/Al2O3 mol ratios using waste alumina of the alumina content not less than 60% as raw material Ratio and soda ash mix, be calcined under conditions of 800~1000 DEG C, roasting time is 0.3~1h, after being calcined Material；(2) material after the roasting that will be obtained in step (1) carries out dissolution with alkaline aqueous solution, is filtrated to get sodium aluminate solution；(3) concentration for preparing Na2O is 3~5mol/L alkaline solution, by modulus of water glass 2.5~3.5 to above-mentioned alkaline solution Middle addition quartz sand mixes, and reacts 1-3h at 160~200 DEG C, obtains liquid soluble glass；(4) liquid soluble glass that the sodium aluminate solution and step (3) obtained step (2) obtains mixes, and adds 4A zeolites and is oriented to Agent, pulp, crystallization, it is filtrated to get 4A zeolite molecular sieve original powder.
- A kind of 2. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： The Na2O concentration of step (2) the neutral and alkali aqueous solution is 50~100g/L.
- A kind of 3. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： Step (2) the neutral and alkali aqueous solution addition is to make the mol ratio of Na2O/Al2O3 in solution be 1.5-2.0.
- A kind of 4. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： Alkaline aqueous solution in the step (2) filters the 4A zeolite mother liquors after 4A zeolite molecular sieves for step (4).
- A kind of 5. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： The concentration of preparation Na2O in the step (3) is that the concrete operations of 3-5mol/L alkaline solution are will to be filtered in step (4) The 4A zeolite mother liquors obtained after 4A zeolite molecular sieves are concentrated to give.
- A kind of 6. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： Sodium aluminate solution, the synthesis ratio of liquid soluble glass are in the step (4)：Na2O：Al2O3：SiO2：H2O=2-4：1： 1.9-2.1：50-200.
- A kind of 7. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： The slurrying temperature is 50~70 DEG C, and slurry time is 10~20min.
- A kind of 8. method for producing 4A zeolites using waste alumina and quartz sand according to claim 1, it is characterised in that： Crystallization temperature is 80~100 DEG C in the step (4), and crystallization time is 60~180min.
- 9. a kind of method for producing 4A zeolites using waste alumina and quartz sand according to claim any one of 1-8, its It is characterised by：Directed agents in the step (4) meet lower ratio：Na2O：Al2O3：SiO2：H2O=15：1：10：300.
- 10. a kind of method for producing 4A zeolites using waste alumina and quartz sand according to claim 9, its feature exist In：The addition of the directed agents is 0.1-0.5%.Reach stable high yield, the purpose of cost efficiency.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2787819C1 (en) * | 2022-05-19 | 2023-01-12 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing synthetic zeolite |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787361A (en) * | 2014-01-20 | 2014-05-14 | 石家庄健达高科化工有限公司 | Method for producing 4A zeolite by using waste aluminum oxide and quartz sand |
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2017
- 2017-11-23 CN CN201711177438.7A patent/CN107827122A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103787361A (en) * | 2014-01-20 | 2014-05-14 | 石家庄健达高科化工有限公司 | Method for producing 4A zeolite by using waste aluminum oxide and quartz sand |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2787819C1 (en) * | 2022-05-19 | 2023-01-12 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method for producing synthetic zeolite |
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