CN100577565C - Method for producing 4A zeolite - Google Patents
Method for producing 4A zeolite Download PDFInfo
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- CN100577565C CN100577565C CN200710119905A CN200710119905A CN100577565C CN 100577565 C CN100577565 C CN 100577565C CN 200710119905 A CN200710119905 A CN 200710119905A CN 200710119905 A CN200710119905 A CN 200710119905A CN 100577565 C CN100577565 C CN 100577565C
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- CN
- China
- Prior art keywords
- zeolite
- sodium aluminate
- aluminate solution
- production
- bayer process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 47
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000010457 zeolite Substances 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 51
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 31
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004131 Bayer process Methods 0.000 claims abstract description 26
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 4
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 235000019795 sodium metasilicate Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 230000007423 decrease Effects 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 238000005406 washing Methods 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 11
- 230000008025 crystallization Effects 0.000 description 11
- 239000003599 detergent Substances 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 235000019353 potassium silicate Nutrition 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000024287 Areas Species 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a method to produce 4A zeolite, in particular to a method to produce the 4A zeolite from a sodium aluminate solution produced in the production process of aluminum oxide. The invention is characterized by producing 4A zeolite from the sodium aluminate solution produced in the production process of aluminium oxide by Bayer process; the producing process is that: an industrial dense sodium metasilicate with a SiO2 weight proportional concentration ranging from 26 percent to 28 percent and Rho density ranging from 1.38 to 1.40 g/cm3 is added into the sodium aluminate solution by Bayer process and well mixed, and stirred for 1 to 3 hours, and the molar proportion of SiO2 / Al2O3 is 1.8 to 2. The method of the invention directly adopts the sodium aluminate solution produced in the production process of aluminum oxide by Bayer process and normal temperature industrial dense sodium metasilicate, 'low temperature and one-step' to produce the 4A zeolite, and good quality cleaning additive 4A zeolite products are obtained after being filtered, cleaned and dried. The invention effectively cuts down the production cost of aluminum oxide by Bayer process, and decreases the ineffective circulation of aluminum in the solution in the production process.
Description
Technical field
A kind of method of producing the 4A zeolite relates to a kind of method that adopts the sodium aluminate solution in the aluminum oxide production process to produce the 4A zeolite.
Background technology
The 4A zeolite is a kind of multiduty product, be widely used in building, chemistry, chemical industry and the daily life, but 4A zeolite consumption maximum is as washing auxiliary detergent.Different Application Areass also has nothing in common with each other to the performance requriements of 4A zeolite, such as, the 4A zeolite adsorption capacity that is used for chemical industry is most important performance index, and most important two performance index of 4A zeolite that are used as washing auxiliary detergent are whiteness and calcium exchange capacity.
At present, 4A zeolite production method is synthetic with hydrothermal synthesis method under the alkali environment mostly, and hydro-thermal is synthesized the process that pulp, crystallization (one section crystallization or two sections crystallization are arranged) are all arranged usually, and the process of temperature raising is promptly all arranged, and crystallization temperature eventually is general all about 90～100 ℃.
Relevant both at home and abroad production washing auxiliary detergent has many with the patent of 4A zeolite, its production technique mostly is to be raw material with technical pure aluminium hydroxide, as United States Patent (USP) 4339418,4339419 is described, its technology is that technical pure aluminium hydroxide is become sodium aluminate solution with the liquid sodium hydroxide prepared in reaction, produces the 4A zeolite with the water glass raw material reaction with this then as the aluminium source.The 4A zeolite quality height of producing, but corresponding cost is also very high.Directly adopt the sodium aluminate solution in the aluminum oxide production process to produce the effective way that the 4A zeolite is its production cost of reduction.
The patent of the production method of domestic relevant 4A zeolite, related to the sodium aluminate solution in the alumina producing is the processing method in aluminium source, as patent documentation CN86106033A, ZL200410155444.9, ZL200410155443.4 discloses the production method that adopts the sodium aluminate solution in the sintering process for alumina production in 200410155445.3 grades.
Will pass through stripping again behind the high temperature sintering (1000～1250 ℃) because " sintering process " sintering process is produced aluminum oxide, complex process, energy consumption high product cost height cause the production cost of 4A zeolite also still higher; And by contrast, alumina producing Bayer process is without the direct stripping of sintering (180～240 ℃ of stripping temperature), have the advantages that than sintering process production technique is easy, energy consumption is low, product cost is low, it is the cost of sodium aluminate solution that the cost of the sodium aluminate solution in the Bayer process aluminum oxide production process will be lower than in the alumina by sintering production process; But in Bayer process alumina producing process in leaching, because organism is planted matter with corruption in bauxite and the pitch state exists, pitch is not dissolved in alkaline solution, all discharges in company with red mud.Corruption is planted matter and is then entered solution with alkaline solution effect generation Sodium salts humic acids.Organism in the solution under the effect of air, is in the process of continuous oxidation, decomposes a class simple organic and resinous substancess such as changing sodium oxalate into gradually.Make Bayer process sodium aluminate solution present pitch black red-purple.The whiteness value of the Bayer process aluminium hydroxide product that this solution branch parses is generally about 91%～92%.And sintering process is produced in the alumina process, and ore volatilizees organism through high temperature sintering fully, almost is water white through stripping gained sodium aluminate solution, and the whiteness value of the aluminium hydroxide product that alumina producing goes out is generally about 97%～98%.For example middle aluminium Shandong branch office is that sintering process is produced alumina technology, and the white aluminum hydroxide of being produced becomes the symbol of high-quality artificial onyx filler.
Although the sodium aluminate solution cost during the sodium aluminate solution liquor ratio alumina by sintering in the Bayer process alumina producing is produced is low, but normally not will consider and do raw material with it and produce washing auxiliary detergent that the dialogue degree has a high requirement (washing with whiteness 〉=96% of 4A zeolite, the whiteness of premium grads＞98%) with 4A zeolite product (being to dissolve again with aluminium hydroxide to make sodium aluminate solution in the foreign patent).
Summary of the invention
The objective of the invention is deficiency, provide a kind of and can effectively reduce production costs, simplify production technique, improve the method for the employing Bayer process sodium aluminate solution of output capacity as aluminium source production 4A zeolite at above-mentioned prior art existence.
The objective of the invention is by realizing with technical scheme.
A kind of method of producing the 4A zeolite is characterized in that be adopting the sodium aluminate solution in the alumina producing Bayer process process to produce the 4A zeolite for the aluminium source.
A kind of method of producing the 4A zeolite of invention is characterized in that containing Al in the Bayer process sodium aluminate solution as the aluminium source
2O
3Concentration is 60～100g/l; Contain Na
2O concentration is 130～180g/l; Temperature is 50～70 ℃.
A kind of method of producing the 4A zeolite of invention is characterized in that its production process is with SiO
2Weight ratio concentration is 26%～28%, ρ is 1.38～1.40g/cm
3Industrial concentrated sodium silicate join Bayer process sodium aluminate solution and mix; Stirred 1～3 hour; Its mole ratio of components is SiO
2/ Al
2O
3: 1.8～2.
The method of production 4A zeolite of the present invention, be to generate the 4A zeolite in low temperature (50～70 a ℃) step: the 4A zeolite production method of reporting in document and the patent is synthetic with hydrothermal synthesis method under the alkali environment mostly, the synthetic process that pulp, crystallization (one section crystallization or two sections crystallization are arranged) are all arranged usually of hydro-thermal, the process that temperature raising is promptly all arranged, crystallization temperature eventually are general all about 90～100 ℃.And method of the present invention directly adopts sodium aluminate solution and normal temperature service water glass in the alumina producing Bayer process process to do raw material, need not temperature raising, step generation 4A zeolite (pulp, the crystallization operation of routine are reduced to a step).
The maximum benefit of method of the present invention: improved the output capacity of 4A zeolite greatly, reduced production costs; In production practice, the output capacity of A zeolite is generally 73～110g/l, (this is because the reaction radix of A type zeolite---in 1 premium on currency, participate in the mole number of the aluminum oxide of reaction, routine is 0.2～0.3M, improve the output that the reactive group digital display so helps increasing zeolite, but radix is too high, is unfavorable for into glue and crystallization, the difficult quality guarantee of product.) adopt method of the present invention, the output capacity＞220g/l of 4A zeolite.(by the reaction radix that calculates the system that can get is 0.63～0.71.)
Method of the present invention, saved the raw material allotment operation in the conventional production, temperature raising process and high temperature crystallization process in the conventional production have been saved, the output capacity of 4A zeolite is from 73～110g/l of routine, bring up to greater than 220g/l, but the washing auxiliary detergent of output excellent performance 4A zeolite reduces cost about 100～200 yuan/ton; Reduce the Bayer process alumina production cost simultaneously, reduce the invalid circulation of aluminium in Production Flow Chart in the solution.
Embodiment
A kind of method of producing the 4A zeolite is with ratio of components (mol ratio) SiO
2/ Al
2O
3: 1.8～2 ratio directly adds service water glass in the sodium aluminate solution (50～70 ℃) in the alumina producing Bayer process process; After stirring, be incubated 1～3 hour, filter, wash, dry washing auxiliary detergent 4A zeolite product.
Embodiment 1
At Al
2O
3Concentration is 65g/l, and α k is 2.90, and temperature is 55 ℃ of sodium aluminate solutions in the alumina producing Bayer process process, adds SiO
2Concentration is the water glass of 26.5% (weight ratio), the back insulation 3 hours that stirs, filter, wash, dry washing auxiliary detergent 4A zeolite product.Index is as follows:
Calcium exchange granularity＜4um (%) whiteness (%) pH
310mgCaCO
3/g 96.3 97.8 10.97
Embodiment 2
At Al
2O
3Concentration is 70g/l, and α k is about 2.95, and temperature is 60 ℃ of sodium aluminate solutions in the alumina producing Bayer process process, adds SiO
2Concentration is the water glass of 26.0% (weight ratio), the back insulation 2.5 hours that stirs, filter, wash, dry washing auxiliary detergent 4A zeolite product.Index is as follows:
Calcium exchange granularity＜4um (%) whiteness (%) pH
312mgCaCO
3/g 96.1 97.6 10.95
Embodiment 3
At Al
2O
3Concentration is 75g/l, and α k is about 2.98, and temperature is 65 ℃ of sodium aluminate solutions in the alumina producing Bayer process process, adds SiO
2Concentration is the water glass of 27.1% (weight ratio), the back insulation 2 hours that stirs, filter, wash, dry washing auxiliary detergent 4A zeolite product.Index is as follows:
Calcium exchange granularity＜4um (%) whiteness (%) pH
317mgCaCO
3/g 96.7 98.0 10.94
Embodiment 4
At Al
2O
3Concentration is 85g/l, and α k is 3.0, and temperature is 68 ℃ of sodium aluminate solutions in the alumina producing Bayer process process, adds SiO
2Concentration is the water glass of 27.5% (weight ratio), the back insulation 1.5 hours that stirs, filter, wash, dry washing auxiliary detergent 4A zeolite product.Index is as follows:
Calcium exchange granularity＜4um (%) whiteness (%) pH
312mgCaCO
3/g 95.2 97.9 10.99
Embodiment 5
At Al
2O
3Concentration is 90g/l, and α k is about 3.05, and temperature is 64 ℃ of sodium aluminate solutions in the alumina producing Bayer process process, adds SiO
2Concentration is the water glass of 26.8% (weight ratio), the back insulation 2.0 hours that stirs, filter, wash, dry washing auxiliary detergent 4A zeolite product.Index is as follows:
Calcium exchange granularity＜4um (%) whiteness (%) pH
319mgCaCO
3/g 95.9 97.6 10.90
Claims (1)
1. method of producing the 4A zeolite is characterized in that it being that to adopt the sodium aluminate solution in the alumina producing Bayer process process be the aluminium source, and next step produces the 4A zeolite 50～70 ℃ of temperature; As containing Al in the sodium aluminate solution in the alumina producing Bayer process process in aluminium source
2O
3Concentration is 60～100g/l, contains Na
2O concentration is 130～180g/l, and temperature is 50～70 ℃; In its production process with SiO
2Weight ratio concentration is 26%～28%, ρ is 1.38～1.40g/cm
3Industrial concentrated sodium silicate join in the sodium aluminate solution in the alumina producing Bayer process process and mix, stirred 1～3 hour, the mole ratio of components that industrial concentrated sodium silicate joins the sodium aluminate solution in the alumina producing Bayer process process is SiO
2/ Al
2O
3: 1.8～2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710119905A CN100577565C (en) | 2007-08-03 | 2007-08-03 | Method for producing 4A zeolite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710119905A CN100577565C (en) | 2007-08-03 | 2007-08-03 | Method for producing 4A zeolite |
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| Publication Number | Publication Date |
|---|---|
| CN101125661A CN101125661A (en) | 2008-02-20 |
| CN100577565C true CN100577565C (en) | 2010-01-06 |
Family
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|---|---|---|---|
| CN200710119905A Active CN100577565C (en) | 2007-08-03 | 2007-08-03 | Method for producing 4A zeolite |
Country Status (1)
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| CN (1) | CN100577565C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101264899B (en) * | 2008-04-18 | 2011-01-26 | 中国铝业股份有限公司 | Technique for synthesizing 4A zeolite for detergent by using economic aluminum source |
| CN102320620B (en) * | 2011-06-20 | 2013-04-17 | 太原理工大学 | Method for preparing 4A zeolite by using alumina red mud |
| CN104845757B (en) * | 2015-03-30 | 2018-07-06 | 石家庄健达高科化工有限公司 | A kind of method of 4A zeolites slurry production washing powder |
| CN104845760B (en) * | 2015-03-30 | 2018-07-06 | 石家庄健达高科化工有限公司 | A kind of method of the 4A zeolites slurry production washing powder of high-efficiency environment friendly |
| CN108275695B (en) * | 2018-01-15 | 2020-06-02 | 内蒙古日盛可再生资源有限公司 | Method for preparing 4A zeolite for washing aid from high-aluminum coal gangue |
| CN117843011B (en) * | 2024-03-06 | 2024-05-14 | 南京农业大学 | NaP1 zeolite synthesized by red mud hydrothermal method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86106033A (en) * | 1986-09-11 | 1988-03-23 | 山东铝厂 | Produce the method for detergent use molecular sieve-4A zeolite with industrial sodium aluminate solution |
| EP0392400A2 (en) * | 1989-04-10 | 1990-10-17 | Lonza Ag | Process for the preparation of a finely divided cristalline type A zeolithe powder with predetermined gram size distribution |
| CN1453213A (en) * | 2003-04-30 | 2003-11-05 | 中国日用化学工业研究院 | Technological process and special apparatus for preparing 4A zeolite |
| RU2003122223A (en) * | 2000-12-19 | 2005-01-10 | Нэшнл Алюминиум Компани Лимитед (In) | METHOD FOR PRODUCING ZEOLITE-A SUITABLE AS A DETERGENT MODIFIING ADDITIVE |
| CN1623899A (en) * | 2004-11-12 | 2005-06-08 | 山东铝业股份有限公司 | Guiding agent for preparing 4A zeolite |
-
2007
- 2007-08-03 CN CN200710119905A patent/CN100577565C/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86106033A (en) * | 1986-09-11 | 1988-03-23 | 山东铝厂 | Produce the method for detergent use molecular sieve-4A zeolite with industrial sodium aluminate solution |
| EP0392400A2 (en) * | 1989-04-10 | 1990-10-17 | Lonza Ag | Process for the preparation of a finely divided cristalline type A zeolithe powder with predetermined gram size distribution |
| RU2003122223A (en) * | 2000-12-19 | 2005-01-10 | Нэшнл Алюминиум Компани Лимитед (In) | METHOD FOR PRODUCING ZEOLITE-A SUITABLE AS A DETERGENT MODIFIING ADDITIVE |
| CN1453213A (en) * | 2003-04-30 | 2003-11-05 | 中国日用化学工业研究院 | Technological process and special apparatus for preparing 4A zeolite |
| CN1623899A (en) * | 2004-11-12 | 2005-06-08 | 山东铝业股份有限公司 | Guiding agent for preparing 4A zeolite |
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|---|---|
| CN101125661A (en) | 2008-02-20 |
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