CN105645431A - 4A-zeolite as well as preparation method and preparation equipment thereof - Google Patents
4A-zeolite as well as preparation method and preparation equipment thereof Download PDFInfo
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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
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Abstract
The invention discloses a 4A-zeolite as well as a preparation method and preparation equipment thereof and belongs to the technical field of 4A-zeolite. The method comprises the following steps of: roasting monohydrallite by use of a flash-smelting boiling furnace; putting the roasted monohydrallite into an alkaline solution so as to obtain a leachate; performing solid-liquid separation on alkaline-leaching silicon slurry, so as to obtain solid ore concentrate; performing solid-liquid separation on the alkaline-leaching silicon slurry, performing solid-liquid separation on leachate so as to obtain solid ore concentrate and liquid filtrate; preparing a sodium aluminate solution by use of the ore concentrate; preparing the 4A-zeolite by using the filtrate and sodium aluminate solution as ingredients. The equipment comprises a flash-smelting boiling furnace, a first reaction vessel, a second reaction vessel, a solid-liquid separation device, a sodium aluminate solution preparation device and an 4A-zeolite preparation device. The 4A-zeolite is prepared by use of the method and the equipment and is capable of improving the overall recovery of aluminum oxide and is high in yield and free from pollution.
Description
Technical field
The present invention relates to 4A zeolite technology field, particularly relate to preparation method and equipment, this 4A zeolite of a kind of 4A zeolite.
Background technology
Chemical formula is Na12Al12Si12O48��27H2O, the three-dimensional framework shape structural compounds being made up of silica and aluminum-oxygen tetrahedron, belong to cubic system, structure cell center is a diameter is 1.14A hole, it is formed by connecting by 8 rings and 6 similar holes, the free hole diameter that this 8 ring structures are formed is 4.12A, therefore is called 4A zeolite. The features such as the bauxite resource of China enriches, but the overwhelming majority is diaspore kaolinite type bauxite, and this Ore collection high alumina, high silicon, low alumina-silica ratio (A/S), low ferrum and crystallizable mineral carefully dissipate, composition is complicated. Owing to the alumina silica ratio of Ore is low, silicone content is high, the alumina producing energy consumption that makes China high, of poor benefits. Therefore take cost-effective pre-desiliconizing technique, improve the alumina silica ratio of alumina producing raw material, be realize the important channel that China's aluminium oxide efficient low-consume produces. At present, the method for desilication of bauxite mainly has biological desiliconization method and physics desiliconization method. Biological desiliconization method is the silicate and aluminium silicate mineral that utilize microorganism to come in decomposing ore, makes silicon be transformed into the silicon of solubility, and aluminium oxide exists with the form of insoluble matter, its shortcoming is that desiliconization speed is slow, cycle is long, and condition requires harshness, it is difficult to apply in the industrial production. Physics desiliconization method is the method for Applied Physics, such as floatation, realizes diaspore and the separation of silicate, aluminium silicate mineral, its shortcoming be due to aluminosilicate contain a number of aluminum, aluminum organic efficiency relatively low.
The method of alkali leaching desiliconization also had research in the past, but for the regeneration of alkali leaching desiliconization liquid, more traditional way is with lime treatment, generates hydration wollastonite (CaO SiO2��H2O). But the desilication efficiency of this method leachate is not high, is only 80��85%, affects the desilication efficiency of circulating leaching roasted ore; It addition, the recycling for wollastonite is furtherd investigate, if storing up process, losing value, and causing the secondary pollution of environment.
Summary of the invention
In view of this, the present invention provides preparation method and equipment, this 4A zeolite of a kind of 4A zeolite, and it can not only reclaim the aluminum in diaspore type bauxite, and can also reclaim the aluminum in aluminosilicate, and aluminium oxide overall recovery is more than 98%; Application the method and equipment prepare 4A zeolite, have not only stopped invalid outer row, and save the expense of waterglass, define high benefit, free of contamination environmental protection and economy flow process, thus more suitable for practicality.
In order to reach above-mentioned first purpose, the technical scheme of the preparation method of 4A zeolite provided by the invention is as follows:
The preparation method of 4A zeolite provided by the invention comprises the following steps:
Adopt flash boiling stove roasting bauxite;
Bauxite through roasting is placed in aqueous slkali, obtains leachate;
Described alkali being soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate;
Described alkali being soaked desiliconization serosity and carries out solid-liquid separation, described leachate is carried out solid-liquid separation, the solid obtained is ore concentrate, and the liquid obtained is filtrate;
Sodium aluminate solution is prepared with described ore concentrate;
Apply described filtrate and sodium aluminate solution as dispensing, prepare described 4A zeolite.
The preparation method of 4A zeolite provided by the invention also can be applied to the following technical measures to achieve further.
As preferably, adopting flash boiling stove roasting bauxite to comprise the following steps:
Described bauxite is joined in the preheating furnace of described flash boiling stove and preheat, obtain the prebake ore deposit through preheating dehydration;
Described prebake ore deposit is joined in the fluidized bed furnace of flash boiling stove, carry out shower roasting, obtain shower roasting ore deposit;
Described shower roasting ore deposit is joined in the holding furnace of flash boiling stove and be incubated, obtain the bauxite through roasting.
As preferably,
Being joined by described bauxite when preheating in the preheating furnace of described fluidized bed furnace, the granularity span of described bauxite is :��0.15mm;
When carrying out shower roasting, the furnace temperature span of described flash boiling stove is 1000 DEG C��1100 DEG C;
When described shower roasting ore deposit joins insulation in holding furnace, the span of described insulation persistent period is 10min��30min.
As preferably, the preparation method of described 4A zeolite is further comprising the steps of:
Described filtrate is carried out the leaching desiliconization of n times circulation alkali and obtains n-th leachate;
Described n-th leachate is carried out solid-liquid separation, obtains n-th filtrate.
As preferably, the span of described cycle-index N is 2 or 3.
As preferably, the bauxite through roasting being placed in aqueous slkali, obtain in alkali leaching desiliconization slurry processes,
Alkali concn span in described aqueous slkali is 100g/L��150g/L;
The span of the temperature of described desiliconization is 90 DEG C��95 DEG C;
The span of the time of described desiliconization is 100min��120min;
The span of the liquid-solid ratio after described desiliconization is (3��5): 1.
As preferably, in described first time leachate, SiO2The span of concentration be 30g/L��40g/L.
As preferably, in described final leachate, SiO2The span of concentration be 90g/L��100g/L.
In order to reach above-mentioned second purpose, the technical scheme of the Preparation equipment of 4A zeolite provided by the invention is as follows:
The Preparation equipment of 4A zeolite provided by the invention includes flash boiling stove, the first reaction vessel, the second reaction vessel, equipment for separating liquid from solid, sodium aluminate solution preparation facilities, 4A zeolite preparation facilities,
Described flash boiling stove is for carrying out roasting to bauxite;
Described first reaction vessel is used for the accommodating bauxite through roasting and aqueous slkali, and, through the alkali leaching desiliconization serosity being obtained by reacting;
Alkali leaching desiliconization serosity is carried out the leachate that solid-liquid separation obtains for accommodating by described second reaction vessel;
Described equipment for separating liquid from solid is for carrying out solid-liquid separation to described leachate, and the solid obtained is ore concentrate, and the liquid obtained is filtrate;
Described sodium aluminate solution preparation facilities is for being prepared described sodium aluminate solution by described ore concentrate;
Described 4A zeolite preparation facilities applies described sodium aluminate solution and described filtrate as dispensing, prepares described 4A zeolite.
In order to reach above-mentioned 3rd purpose, the technical scheme of 4A zeolite provided by the invention is as follows:
4A zeolite provided by the invention applies preparation method provided by the invention and Preparation equipment provided by the invention prepares.
Apply 4A zeolite preparation method provided by the invention and 4A zeolite Preparation equipment is prepared in the process of 4A zeolite, by bauxite being carried out flash boiling stove calcination process, could alter that aluminum in bauxite, the form of silicon mineral and crystal form structure, particularly improve the crystal habit of silicon in aluminium silicate mineral, it is made to have the aluminium silicate mineral of crystalline state to be changed into amorphous amorphous silica, selective dissolution in aqueous slkali, thus reaching diaspore type bauxite desiliconization and improving the purpose of alumina silica ratio (A/S). It can not only reclaim the aluminum of diaspore, and can also reclaim the aluminum in aluminosilicate, and aluminium oxide overall recovery is more than 98%. Described alkali is soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate, the liquid obtained is filtrate, apply this ore concentrate and prepare sodium aluminate solution, the sodium aluminate solution that application obtains and this filtrate, prepare described 4A zeolite, not only stopped invalid outer row, and save the expense of waterglass, define high benefit, free of contamination environmental protection and economy flow process.
Accompanying drawing explanation
By reading hereafter detailed description of the preferred embodiment, various other advantage and benefit those of ordinary skill in the art be will be clear from understanding. Accompanying drawing is only for illustrating the purpose of preferred implementation, and is not considered as limitation of the present invention. And in whole accompanying drawing, it is denoted by the same reference numerals identical parts. In the accompanying drawings:
Fig. 1 is the flow chart of steps of the preparation method of 4A zeolite provided by the invention;
Fig. 2 is the material modified flow figure in the preparation method process of 4A zeolite provided by the invention;
Fig. 3 is the schematic diagram of the detailed description of the invention of the Preparation equipment of 4A zeolite provided by the invention.
Detailed description of the invention
The present invention solves prior art Problems existing, preparation method and equipment, this 4A zeolite of a kind of 4A zeolite are provided, it can not only reclaim the aluminum in diaspore type bauxite, and can also reclaim the aluminum in aluminosilicate, and aluminium oxide overall recovery is more than 98%; Application the method and equipment prepare 4A zeolite, have not only stopped invalid outer row, and save the expense of waterglass, define high benefit, free of contamination environmental protection and economy flow process, thus more suitable for practicality.
For further setting forth that the present invention reaches technological means and effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, preparation method and equipment, this 4A zeolite to the 4A zeolite proposed according to the present invention, its detailed description of the invention, structure, feature and effect thereof, describe in detail as after.In the following description, what different " embodiments " or " embodiment " referred to is not necessarily same embodiment. Additionally, special characteristic in one or more embodiment, structure or feature can be combined by any suitable form.
The terms "and/or", is only a kind of incidence relation describing affiliated partner, and expression can exist three kinds of relations, such as, A and/or B, concrete is interpreted as: can include A and B simultaneously, can individualism A, it is also possible to individualism B, it is possible to possess above-mentioned three kinds of any one situations.
Referring to accompanying drawing 1 and accompanying drawing 2, the preparation method of 4A zeolite provided by the invention comprises the following steps:
Step S1: adopt flash boiling stove roasting bauxite;
Step S2: after roasting,
There is following chemical reaction in the diaspore in bauxite:
Wherein, �� '-Al2O3It is an intermediate product, ��-Al2O3It is corundum type aluminium oxide,
The raw following chemical reaction of siliceous mineral trichite in bauxite:
Wherein, the SiO of generation2For can with the unformed product of alkali reaction;
Step S3: the bauxite through roasting is placed in aqueous slkali, obtains leachate;
Step S4: alkali being soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate;
Step S5: alkali being soaked desiliconization serosity and carries out solid-liquid separation, leachate is carried out solid-liquid separation, the solid obtained is ore concentrate, and the liquid obtained is filtrate;
Step S6: prepare sodium aluminate solution with ore concentrate;
Step S7: application filtrate and sodium aluminate solution, as dispensing, prepare 4A zeolite.
Apply 4A zeolite preparation method provided by the invention and 4A zeolite Preparation equipment is prepared in the process of 4A zeolite, by bauxite being carried out flash boiling stove calcination process, could alter that aluminum in bauxite, the form of silicon mineral and crystal form structure, particularly improve the crystal habit of silicon in aluminium silicate mineral, it is made to have the aluminium silicate mineral of crystalline state to be changed into amorphous amorphous silica, selective dissolution in aqueous slkali, thus reaching diaspore type bauxite desiliconization and improving the purpose of alumina silica ratio (A/S). It can not only reclaim the aluminum of diaspore, and can also reclaim the aluminum in aluminosilicate, and aluminium oxide overall recovery is more than 98%. Described alkali is soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate, the liquid obtained is filtrate, apply this ore concentrate and prepare sodium aluminate solution, the sodium aluminate solution that application obtains and this filtrate, prepare described 4A zeolite, not only stopped invalid outer row, and save the expense of waterglass, define high benefit, free of contamination environmental protection and economy flow process.
In the present embodiment, filtrate can Substitute For Partial waterglass, as the production dispensing of 4A zeolite.
Wherein, flash boiling stove roasting bauxite is adopted to comprise the following steps:
Step S11: joined by bauxite in the preheating furnace of flash boiling stove and preheat, obtains the prebake ore deposit through preheating dehydration;
Step S12: prebake ore deposit is joined in the fluidized bed furnace of flash boiling stove, carry out shower roasting, obtain shower roasting ore deposit;
Step S13: shower roasting ore deposit is joined in the holding furnace of flash boiling stove and be incubated, obtain the bauxite through roasting.
Wherein,
In step s 11, being joined by bauxite when preheating in the preheating furnace of fluidized bed furnace, the granularity span of bauxite is :��0.15mm;
In step s 13, when carrying out shower roasting, the furnace temperature span of flash boiling stove is 1000 DEG C��1100 DEG C;
In step s 13, when shower roasting ore deposit joins insulation in holding furnace, the span of insulation persistent period is 10min��30min.
Wherein, 4A zeolite preparation method is further comprising the steps of:
Filtrate is carried out the leaching desiliconization of n times circulation alkali and obtains n-th leachate;
N-th leachate is carried out solid-liquid separation, obtains n-th filtrate.
SiO in first time filtrate2Concentration is between 30g/L��40g/L, increases cycle-index, it is possible to improve SiO2Concentration in leachate.
Wherein, the span of cycle-index is 2 or 3. In this way, it is possible to make SiO2Concentration in filtrate brings up between 90g/L��100g/L. Now, this filtrate can substitute waterglass completely, as the dispensing that 4A zeolite produces.
Wherein, the bauxite through roasting is placed in aqueous slkali, obtains in alkali leaching desiliconization slurry processes,
Alkali concn span in aqueous slkali is 100g/L��150g/L;
The span of the temperature of desiliconization is 90 DEG C��95 DEG C;
The span of the time of desiliconization is 100min��120min;
The span of the liquid-solid ratio after desiliconization is (3��5): 1.
Wherein, in first time leachate, SiO2The span of concentration be 30g/L��40g/L.
Wherein, in final leachate, SiO2The span of concentration be 90g/L��100g/L.
Referring to accompanying drawing 3, the Preparation equipment of 4A zeolite provided by the invention includes flash boiling stove, the first reaction vessel, the second reaction vessel, equipment for separating liquid from solid, sodium aluminate solution preparation facilities, 4A zeolite preparation facilities, and flash boiling stove is for carrying out roasting to bauxite; First reaction vessel is used for the accommodating bauxite through roasting and aqueous slkali, and, through the alkali leaching desiliconization serosity being obtained by reacting; Alkali leaching desiliconization serosity is carried out the leachate that solid-liquid separation obtains for accommodating by the second reaction vessel; Equipment for separating liquid from solid is for carrying out solid-liquid separation to leachate, and the solid obtained is ore concentrate, and the liquid obtained is filtrate; Sodium aluminate solution preparation facilities is for being prepared sodium aluminate solution by ore concentrate; 4A zeolite preparation facilities application sodium aluminate solution and filtrate, as dispensing, prepare 4A zeolite.
Apply in the preparation method process of 4A zeolite provided by the invention, bauxite is carried out flash boiling stove calcination process by application flash boiling stove, could alter that aluminum in bauxite, the form of silicon mineral and crystal form structure, particularly improve the crystal habit of silicon in aluminium silicate mineral, it is made to have the aluminium silicate mineral of crystalline state to be changed into amorphous amorphous silica, in the first reaction vessel, selective dissolution in aqueous slkali, thus reaching diaspore type bauxite desiliconization and improving the purpose of alumina silica ratio (A/S). It can not only reclaim the aluminum in diaspore type bauxite, and can also reclaim the aluminum in aluminosilicate, and aluminium oxide overall recovery is more than 98%. Pass through equipment for separating liquid from solid, alkali is soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate and filtrate, application sodium aluminate solution preparation facilities is for being prepared sodium aluminate solution by ore concentrate, application sodium aluminate solution and this filtrate, as dispensing, prepare 4A zeolite, have not only stopped invalid outer row, and save the expense of waterglass, define high benefit, free of contamination environmental protection and economy flow process.
4A zeolite provided by the invention applies preparation method provided by the invention and Preparation equipment provided by the invention prepares.
Embodiment 1��21
Although preferred embodiments of the present invention have been described, but those skilled in the art are once know basic creative concept, then these embodiments can be made other change and amendment.So, claims are intended to be construed to include preferred embodiment and fall into all changes and the amendment of the scope of the invention.
Obviously, the present invention can be carried out various change and modification without deviating from the spirit and scope of the present invention by those skilled in the art. So, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. the preparation method of a 4A zeolite, it is characterised in that comprise the following steps:
Adopt flash boiling stove roasting bauxite;
Bauxite through roasting is placed in aqueous slkali, obtains leachate;
Described alkali being soaked desiliconization serosity and carries out solid-liquid separation, the solid obtained is ore concentrate;
Described alkali being soaked desiliconization serosity and carries out solid-liquid separation, described leachate is carried out solid-liquid separation, the solid obtained is ore concentrate, and the liquid obtained is filtrate;
Sodium aluminate solution is prepared with described ore concentrate;
Apply described filtrate and sodium aluminate solution as dispensing, prepare described 4A zeolite.
2. the preparation method of 4A zeolite according to claim 1, it is characterised in that adopt flash boiling stove roasting bauxite to comprise the following steps:
Described bauxite is joined in the preheating furnace of described flash boiling stove and preheat, obtain the prebake ore deposit through preheating dehydration;
Described prebake ore deposit is joined in the fluidized bed furnace of flash boiling stove, carry out shower roasting, obtain shower roasting ore deposit;
Described shower roasting ore deposit is joined in the holding furnace of flash boiling stove and be incubated, obtain the bauxite through roasting.
3. the preparation method of 4A zeolite according to claim 4, it is characterised in that
Being joined by described bauxite when preheating in the preheating furnace of described fluidized bed furnace, the granularity span of described bauxite is :��0.15mm;
When carrying out shower roasting, the furnace temperature span of described flash boiling stove is 1000 DEG C��1100 DEG C;
When described shower roasting ore deposit joins insulation in holding furnace, the span of described insulation persistent period is 10min��30min.
4. the preparation method of 4A zeolite according to claim 1, it is characterised in that
Further comprising the steps of:
Described filtrate is carried out the leaching desiliconization of n times circulation alkali and obtains n-th leachate;
Described n-th leachate is carried out solid-liquid separation, obtains n-th filtrate.
5. the preparation method of 4A zeolite according to claim 4, it is characterised in that
The span of described cycle-index N is 2 or 3.
6. the preparation method of 4A zeolite according to claim 1, it is characterised in that be placed in aqueous slkali by the bauxite through roasting, obtains in alkali leaching desiliconization slurry processes,
Alkali concn span in described aqueous slkali is 100g/L��150g/L;
The span of the temperature of described desiliconization is 90 DEG C��95 DEG C;
The span of the time of described desiliconization is 100min��120min;
The span of the liquid-solid ratio after described desiliconization is (3��5): 1.
7. the preparation method of 4A zeolite according to claim 1, it is characterised in that in described first time leachate, SiO2The span of concentration be 30g/L��40g/L.
8. the preparation method of 4A zeolite according to claim 4, it is characterised in that in described final leachate, SiO2The span of concentration be 90g/L��100g/L.
9. the Preparation equipment of a 4A zeolite, it is characterised in that include flash boiling stove, the first reaction vessel, the second reaction vessel, equipment for separating liquid from solid, sodium aluminate solution preparation facilities, 4A zeolite preparation facilities,
Described flash boiling stove is for carrying out roasting to bauxite;
Described first reaction vessel is used for the accommodating bauxite through roasting and aqueous slkali, and, through the alkali leaching desiliconization serosity being obtained by reacting;
Alkali leaching desiliconization serosity is carried out the leachate that solid-liquid separation obtains for accommodating by described second reaction vessel;
Described equipment for separating liquid from solid is for carrying out solid-liquid separation to described leachate, and the solid obtained is ore concentrate, and the liquid obtained is filtrate;
Described sodium aluminate solution preparation facilities is for being prepared described sodium aluminate solution by described ore concentrate;
Described 4A zeolite preparation facilities applies described sodium aluminate solution and described filtrate as dispensing, prepares described 4A zeolite.
10. a 4A zeolite, it is characterised in that the preparation method described in arbitrary in application claim 1��8 and the Preparation equipment described in claim 9 prepare.
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| CN108025920A (en) * | 2016-06-23 | 2018-05-11 | 旭化成株式会社 | MWF type zeolites |
| CN110451523A (en) * | 2019-09-18 | 2019-11-15 | 中国铝业股份有限公司 | A method of 4A zeolite is prepared using red mud wash liquor and bauxite chemistry desiliconization solution |
| CN113924272A (en) * | 2019-06-05 | 2022-01-11 | 雷奥技术公司 | Synthesis of adsorbent Material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108025920A (en) * | 2016-06-23 | 2018-05-11 | 旭化成株式会社 | MWF type zeolites |
| CN108025920B (en) * | 2016-06-23 | 2021-04-13 | 旭化成株式会社 | MWF type zeolite |
| CN113924272A (en) * | 2019-06-05 | 2022-01-11 | 雷奥技术公司 | Synthesis of adsorbent Material |
| CN110451523A (en) * | 2019-09-18 | 2019-11-15 | 中国铝业股份有限公司 | A method of 4A zeolite is prepared using red mud wash liquor and bauxite chemistry desiliconization solution |
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| CN105645431B (en) | 2018-03-02 |
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