CN106145129B - A kind of coal ash for manufacturing for aluminium-magnesium silicate method - Google Patents
A kind of coal ash for manufacturing for aluminium-magnesium silicate method Download PDFInfo
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- CN106145129B CN106145129B CN201510149448.4A CN201510149448A CN106145129B CN 106145129 B CN106145129 B CN 106145129B CN 201510149448 A CN201510149448 A CN 201510149448A CN 106145129 B CN106145129 B CN 106145129B
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- aluminium
- magnesium silicate
- flyash
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- 238000000034 method Methods 0.000 title claims abstract description 45
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical compound [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000010883 coal ash Substances 0.000 title claims abstract description 9
- 239000010881 fly ash Substances 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims description 51
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 42
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 28
- 239000000047 product Substances 0.000 claims description 28
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 15
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000292 calcium oxide Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 235000011194 food seasoning agent Nutrition 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 229910020489 SiO3 Inorganic materials 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- QDMGKUOANLJICG-UHFFFAOYSA-N [Mg].[N+](=O)(O)[O-] Chemical compound [Mg].[N+](=O)(O)[O-] QDMGKUOANLJICG-UHFFFAOYSA-N 0.000 claims 1
- 239000011777 magnesium Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 abstract description 5
- 239000002689 soil Substances 0.000 abstract description 5
- 239000005995 Aluminium silicate Substances 0.000 abstract description 4
- 235000012211 aluminium silicate Nutrition 0.000 abstract description 4
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000001514 detection method Methods 0.000 description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 238000005245 sintering Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910001051 Magnalium Inorganic materials 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229940087511 calcium disodium versenate Drugs 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000006210 lotion Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- LLJZKKVYXXDWTB-UHFFFAOYSA-N acetic acid;sodium Chemical compound [Na].[Na].CC(O)=O LLJZKKVYXXDWTB-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940009868 aluminum magnesium silicate Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- ALSPKRWQCLSJLV-UHFFFAOYSA-N azanium;acetic acid;acetate Chemical compound [NH4+].CC(O)=O.CC([O-])=O ALSPKRWQCLSJLV-UHFFFAOYSA-N 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of coal ash for manufacturing for the method for aluminium-magnesium silicate, this method takes full advantage of that discharge amount is huge and the flyash of exhaust emission environment is as raw material, it overcomes and existing prepares yield and cost existing for the method for aluminium-magnesium silicate by the distribution of natural magnesium aluminium silicate mine soil and the limitation of reserves, economy can be developed a circular economy and be saved again simultaneously, and destruction of the discharge to natural ecological environment of flyash can be reduced；And the performance of aluminium-magnesium silicate product made from method provided by the invention meets professional standard, and the purity of product and whiteness etc. are even more outstanding than industry product index.
Description
Technical field
The present invention relates to a kind of preparation methods of aluminium-magnesium silicate, and in particular, to a kind of to use flyash as raw material system
The method of standby aluminium-magnesium silicate.
Background technique
Aluminium-magnesium silicate is a kind of white, nontoxic compound colloidal materials, in aqueous solution dispersibility with higher and stream
It is denaturalized, its chemical composition often indicates in the form of the oxide, predominantly silica, aluminium oxide and magnesia, is widely applied
In building, coating, daily-use chemical industry, and medicine and food service industry.
For example, the composite aluminium-magnesium-silicate thermal insulating material of synthesis, can be applied to the industries such as electric power, metallurgy, chemical industry.They
It is the excellent suspending agent of silty and the high-efficiency stabilizing agent of lotion in coating, emulsification paint, the anti-settling thixotroping of coating can be increased, hanged
Floating stablizing effect；In the production of metal and automotive polish, ceramic tile and glass cleaner, rubbing agent can also be made, play stabilization
The effect of emulsification；In addition, can be used as stabilizer, thickener and dispersing agent in cream hair care articles and toothpaste, make product it is fine and smooth,
It is smooth, there are dispersibility and uniform covering power well.Medically, since it has lasting deacidification, it can be used as system
Acid treating agent chylopoietic disease.
Currently, aluminium-magnesium silicate production method mainly with ore, bentonite, bentonite etc. for raw material, by crushing, slurrying, is divided
It is obtained from the methods of purification, pretreatment, modification, but its technique is longer, inferior separating effect, and yield and cost are by In Natural Silicate
The distribution of magnalium mine soil and the limitation of reserves, it is impossible to meet all trades and professions demands growing to aluminium-magnesium silicate product.
The research for preparing aluminium-magnesium silicate by the chemical reaction between grouping point is less, synthesizes in disclosed related chemical method
It prepares in the patent of aluminium-magnesium silicate, is mainly produced into sodium metasilicate, magnesium sulfate, aluminum sulfate etc. for Material synthesis aluminium-magnesium silicate
This is higher, is not suitable for large-scale production.
Therefore, there is an urgent need to develop a kind of new methods for preparing aluminium-magnesium silicate, are produced with meeting all trades and professions to aluminium-magnesium silicate
The growing demand of product.
Summary of the invention
It is an object of the invention to overcome it is existing to prepare raw material sources existing for the method for aluminium-magnesium silicate limited, lead to sulfuric acid
The yield and cost of magnalium product are unable to satisfy the defect of demand, provide a kind of coal ash for manufacturing for the method for aluminium-magnesium silicate.
Flyash is the solid waste that coal-burning power plant dumps, and China's flyash discharge capacity is very big, the discharge of flyash
Not only it occupies cultivated land but also pollutes environment, the chemical component of flyash is mainly silica (SiO2), aluminium oxide (Al2O3), three oxidation
Two iron (Fe2O3), calcium oxide (CaO) and uncombusted carbon etc., due in chemical composition of PCA containing there are many using element
(such as aluminium and silicon), if it is possible to efficiently use the utility in flyash to prepare aluminium-magnesium silicate, can both overcome silicic acid
To the distribution of natural magnesium aluminium silicate mine soil and the limitation of reserves in magnalium production, and economy can be developed a circular economy and save,
The destruction of natural ecological environment can be reduced again.
For this purpose, the present invention provides a new approach for the comprehensive utilization of flyash, product is greatly enhanced
Surcharge, while also providing a kind of coal ash for manufacturing for the new method of aluminium-magnesium silicate, this method comprises:
(1) under conditions of flyash alkaline process mentions silicon, flyash is placed in alkaline solution, obtain pre-desiliconizing solution and is mentioned
Silicon residue；
(2) the silicon residue that mentions for obtaining step (1) is uniformly mixed with sodium carbonate and/or calcium oxide, is roasted, is dissolved out,
Separation of solid and liquid obtains sodium aluminate filtrate；
(3) sodium aluminate filtrate obtained in pre-desiliconizing solution obtained in step (1) and step (2) is mixed, is then drawn
Enter magnesium nitrate solution to be reacted, filtering, drying obtain aluminium-magnesium silicate.
The present invention also provides the aluminium-magnesium silicate products that method as described above is prepared.
Method provided by the invention takes full advantage of that discharge amount is huge and the flyash of exhaust emission environment is as raw material, gram
The existing distribution for preparing yield and cost existing for the method for aluminium-magnesium silicate by natural magnesium aluminium silicate mine soil and reserves are taken
Limitation, while economy can be developed a circular economy and save again, and the discharge of flyash can be reduced to natural ecological environment
It destroys.The performance that parameter as shown in table 7 can be seen that aluminium-magnesium silicate product obtained in 1-2 of the embodiment of the present invention meets row
Industry standard, and the purity of product and whiteness etc. are even more outstanding than industry product index.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of coal ash for manufacturing for the method for aluminium-magnesium silicate, wherein this method comprises:
(1) under conditions of flyash alkaline process mentions silicon, flyash is placed in alkaline solution, obtain pre-desiliconizing solution and is mentioned
Silicon residue；
(2) the silicon residue that mentions for obtaining step (1) is uniformly mixed with sodium carbonate and/or calcium oxide, is roasted, is dissolved out,
Separation of solid and liquid obtains sodium aluminate filtrate；
(3) the sodium aluminate filtrate for obtaining pre-desiliconizing solution obtained in step (1) and step (2) mixes, and is subsequently introduced
Magnesium nitrate solution is reacted, and filtering, drying obtain aluminium-magnesium silicate.
According to the present invention, in step (1), the concentration of the alkaline solution can be 10-50 weight %；Flyash with it is described
The weight ratio of alkaline solution can be 1:4-6.The alkaline process mention silicon reaction condition include: reaction temperature be 80-120 DEG C, instead
It is 30-120 minutes between seasonable；Preferably, reaction temperature is 90-100 DEG C, and the reaction time is 30-60 minutes.Under the above conditions
It carries out alkaline process and mentions silicon, can make to be present in flyash with activity SiO existing for glass phase2It is dissolved the better effect come out.
Under preferable case, it can be washed and dried to silicon residue is mentioned described in obtaining, the condition of the drying may include: drying
Temperature is 80-120 DEG C, and drying time is 4-12 hours.
In step (2) of the present invention, sodium carbonate and calcium oxide are used to therefore can both use with mentioning silicon residue and form sodium aluminate
Calcium oxide also can be used in sodium carbonate, naturally it is also possible to while sodium carbonate and calcium oxide are used, their specific dosage can root
Be adjusted in very large range according to actual needs, under preferable case, relative to 100 parts by weight steps (1) obtain to mention silicon residual
The dosage of slag, sodium carbonate can be 100-150 parts by weight, and the dosage of calcium oxide can be 40-70 parts by weight；Preferably, relatively
Silicon residue is mentioned in what 100 parts by weight steps (1) obtained, the dosage of sodium carbonate can be 120-130 parts by weight, the dosage of calcium oxide
It can be 45-55 parts by weight.The contained aluminium mentioned in silicon residue can be made more thoroughly to form sodium aluminate within the above range, from
It and is that can efficiently prepare aluminum magnesium silicate.
The condition of the roasting includes: that maturing temperature is 950-1250 DEG C, and calcining time is 30-90 minutes；Preferably, it roasts
Burning temperature is 950-1250 DEG C, and calcining time is 30-60 minutes.
According to the present invention, in step (2), the dissolution includes: that the product after roasting is added in seasoning liquid to carry out instead
It answers, the seasoning liquid is the aqueous solution containing sodium aluminate, sodium hydroxide and sodium carbonate, and the concentration of sodium aluminate is 30-50 grams per liter,
The concentration of sodium hydroxide is 5-10 grams per liter, and the concentration of sodium carbonate is 15-20 grams per liter；The product of roasting and the aqueous solution
Weight ratio is 1:3-10, preferably 1:4-6.In step (2) of the present invention, the temperature of the dissolution reaction is 50-100 DEG C, reaction
Time be 10-30 minutes.
In process in accordance with the present invention (3), pre-desiliconizing liquid, sodium aluminate filtrate, molar ratio in magnesium nitrate solution are as follows: AlO2 -:
SiO3 2-=1.5-3.5；Mg2+:AlO2 -=0.4-0.8.The concentration of the magnesium nitrate solution can change in very large range, excellent
Selection of land, the concentration of the magnesium nitrate solution are 1-5mol/L, pH 4-6.In step (3) of the present invention, the condition of the reaction can
To include: reaction temperature for 60-90 DEG C, the reaction time is 1-5 hours, pH value 7-9.
The present invention also provides the aluminium-magnesium silicate products that method as described above is prepared.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
The following examples will be further described this method, but and be not so limited.
The chemical component of flyash used in embodiment is as shown in table 1.
Table 1
Embodiment 1
(1) in the sodium hydroxide for being 20 weight % by 600ml concentration, it is added to 200g main component powder as shown in Table 1
In coal ash (weight ratio of flyash and the alkaline solution is 1:4.2), stirs evenly, be placed in mechanic whirl-nett reaction kettle, twist
Heating and stirring button (stirring rate 150rpm) are opened after good reaction kettle sealing cover.Temperature is set as 110 DEG C, the reaction time
It is 1 hour.After reaction, while being passed through cooling water makes autoclave body cool down rapidly.It is reduced to room temperature to unscrew kettle to temperature in the kettle
Lid, is poured out reacting slurry.It is filtered by vacuum, obtains pre-desiliconizing solution (as shown in table 2 below at being grouped as) and mentions silicon residue；
(2) the silicon residue that mentions for obtaining step (1) mixes mixing, ratio with calcium oxide and sodium carbonate are as follows: relative to 100 weights
The desciccate that amount part step (1) obtains, the dosage of sodium carbonate are 120 parts by weight, and the dosage of calcium oxide is 45 parts by weight.It is put into
Muffle kiln roasting, sintering temperature are set as 950 DEG C, and sintering time is 60 minutes, after sintering time reaches, is taken out, cooling, obtain
To sintered clinker；
(3) aqueous solution containing sodium aluminate, sodium hydroxide and sodium carbonate is prepared, the concentration of sodium aluminate is 30 grams per liters, hydrogen-oxygen
The concentration for changing sodium is 5 grams per liters, and the concentration of sodium carbonate is 15 grams per liters；Product of roasting that step (2) obtains (roasting clinker) with it is upper
The weight ratio for stating aqueous solution is 1:4.It is reacted, is filtered after reaction, filtrate under conditions of being 75 DEG C, 15 minutes in temperature
As sodium aluminate solution (as shown in table 2 below at being grouped as)；
(4) it measures the pre-desiliconizing solution that 100ml step (1) obtains to be added in 1000ml beaker, in magnetic agitation heater
On be heated to 85 DEG C, adjust pH value of solution to 8；
(5) sodium aluminate solution that 200ml step (3) obtain is added, continues stirring to temperature and is increased to 85 DEG C, adjust solution
PH to 8；
(6) configuration concentration is 1mol/l magnesium nitrate solution 100ml, addition dilute hydrochloric acid adjusting solution ph to 6, and and step
Pre-desiliconizing solution (4) and the mixing of the sodium aluminate solution of step (5) (relative to 100 moles of sodium aluminate, silicon in pre-desiliconizing solution
The dosage of sour sodium is 45 moles；The dosage of magnesium nitrate is 45 moles in magnesium nitrate solution), continue to be heated to 85 DEG C, react 2 hours
Afterwards, it filters, dry, obtain aluminium-magnesium silicate product A1 (main component is as shown in table 3 below).
Table 2
| Al2O3g/l | Na2O g/l | SiO2g/l | |
| Desiliconization liquid | 3.2 | 110.8 | 60 |
| Sodium aluminate solution | 56.10 | 96.7 | 7.05 |
Table 3
| Ingredient | Al2O3 | MgO | SiO | Fe2O3 |
| Weight % | 50.4 | 17.2 | 31.7 | 0.04 |
Embodiment 2
(1) in the sodium hydroxide for being 15 weight % by 680ml concentration, it is added to 200g main component powder as shown in Table 1
In coal ash (weight ratio of flyash and the alkaline solution is 1:5.5), stirs evenly, be placed in mechanic whirl-nett reaction kettle, twist
Heating and stirring button (stirring rate 150rpm) are opened after good reaction kettle sealing cover.Temperature is set as 95 DEG C, the reaction time
It is 30 minutes.After reaction, while being passed through cooling water makes autoclave body cool down rapidly.It is reduced to room temperature to unscrew kettle to temperature in the kettle
Lid, is poured out reacting slurry.It is filtered by vacuum, obtains pre-desiliconizing solution (as shown in table 2 below at being grouped as) and mentions silicon residue, mentioned
Silicon residue is dried 8 hours at a temperature of being placed in 120 in electric drying oven with forced convection through hot water wash 4 times；
(2) product after drying that step (1) obtains is mixed into mixing, ratio with calcium oxide and sodium carbonate are as follows: relative to
The desciccate that 100 parts by weight steps (1) obtain, the dosage of sodium carbonate are 125 parts by weight, and the dosage of calcium oxide is 50 weight
Part.It is put into Muffle kiln roasting, sintering temperature is set as 1150 DEG C, and sintering time is 45 minutes, after sintering time reaches, is taken
Out, cooling, obtain sintered clinker；
(3) aqueous solution containing sodium aluminate, sodium hydroxide and sodium carbonate is prepared, the concentration of sodium aluminate is 40 grams per liters, hydrogen-oxygen
The concentration for changing sodium is 10 grams per liters, and the concentration of sodium carbonate is 20 grams per liters；Product of roasting that step (2) obtains (roasting clinker) with it is upper
The weight ratio for stating aqueous solution is 1:4.It is reacted, is filtered after reaction, filtrate under conditions of being 80 DEG C, 15 minutes in temperature
As sodium aluminate solution (as shown in table 4 below at being grouped as)；
(4) it measures the pre-desiliconizing solution that 200ml step (1) obtains to be added in 1000ml beaker, in magnetic agitation heater
On be heated to 65 DEG C, adjust pH value of solution to 9；
(5) sodium aluminate solution that 300ml step (3) obtain is added, continues stirring to temperature and is increased to 65 DEG C, adjust solution
PH to 9；
(6) configuration concentration is 1mol/l magnesium nitrate solution 200ml, addition dilute hydrochloric acid adjusting solution ph to 4, and and step
Pre-desiliconizing solution (4) and the mixing of the sodium aluminate solution of step (5) (relative to 100 moles of sodium aluminate, silicon in pre-desiliconizing solution
The dosage of sour sodium is 47 moles；The dosage of magnesium nitrate is 47 moles in magnesium nitrate solution), after reaction 4 hours, filtering, drying are obtained
To aluminium-magnesium silicate product A2 (main component is as shown in table 5 below).
Table 4
| Al2O3g/l | Na2O g/l | SiO2g/l | |
| Desiliconization liquid | 23.2 | 140.8 | 120.5 |
| Sodium aluminate solution | 145.10 | 100.7 | 12.05 |
Table 5
| Ingredient | Al2O3 | MgO | SiO2 | Fe2O3 |
| Weight % | 45.80 | 21.7 | 31.3 | 0.06 |
Detect embodiment 1-2
It is examined by performance of the professional standard detection method to aluminium-magnesium silicate product A1-A2 obtained in embodiment 1-2
It surveys, the sector standard detecting method includes:
Moisture content detection: taking this product 100g, and dry to constant weight at 105 DEG C, less loss weight must not exceed 8.0%.
Loss on ignition detection: this product 1.0g is taken, is set in 800 DEG C of high temperature furnaces, ignition to constant weight, less loss weight must not mistake
17.0%.
Aluminium content detection: taking this product 1.0g, add hydrochloric acid 2ml, add water 50ml, and boiling makes molten, lets cool, and filters, filter residue and appearance
Device is washed by several times with water 25ml, merging filtrate and washing lotion, ammonia solution is added dropwise to lucky, precipitating is precipitated, then dilute hydrochloric acid is added dropwise to make to precipitate
Just after dissolution, add acetic acid-ammonium acetate buffer (pH6.0) 10ml, precision measures Calcium Disodium Versenate titrating solution
(0.05mol/L) 25ml is boiled 10 minutes, is let cool, and adds xylenol orange indicator solution 1ml, is dripped with zinc titrating solution (0.05mol/L)
It is fixed, until solution becomes red from yellow, and the result of titration is corrected with blank test.Every 1ml Calcium Disodium Versenate drop
Determine the Al that liquid (0.05mol/L) is equivalent to 1.349mg.
Content of magnesium detection: taking this product 1.0g, add hydrochloric acid 5ml, add water 50ml, and boiling makes molten, lets cool, the red indicator solution of methylate
1 drop, ammonia solution, which is added dropwise, makes solution become yellow from red, then boils 5 minutes, filters while hot, filter residue and container are molten with 2% ammonium chloride
Liquid 30ml is washed by several times, and merging filtrate and washing lotion are let cool, ammonification test solution 10ml and triethanolamine solution (1 → 2) 5ml, then plus chromium
Black indicator is a small amount of, is titrated with Calcium Disodium Versenate titrating solution (0.05mol/L), until solution shows pure blue.Every 1ml second two
Four acetic acid disodium titrating solution (0.05mol/L) of amine is equivalent to the Mg of 1.215mg.
PH detection: taking this product 5g, and the cold water 100ml newly boiled is added, and mixes, and with several measurements of pH, pH value is 9.0~11.0
For normal range (NR).
Whiteness detection: taking a small amount of sample, after the sample box sample preparation provided according to whiteness instrument, measures the whiteness of sample.
Apparent viscosity detection: a small amount of sample is taken, is measured by room temperature type NDJ-79 type viscosimeter.
As a result as shown in table 7 below.
Detect comparative example 1
(Guangzhou is commercially available to market product as shown in table 6 is mainly formed by method identical with detection embodiment 1-2
The top grade aluminium-magnesium silicate of Bo Feng Chemical Industry Science Co., Ltd) performance detected, the results are shown in Table 7.
Table 6
| Ingredient | Al2O3 | MgO | SiO2 | Fe2O3 | K2O | CaO |
| Weight % | 29.1-35.5 | 11-14 | 29.2-35 | 1-1.5 | 0.2-0.3 | 2-3 |
Table 7
| Moisture content | Loss on ignition | Al:Mg | pH | Whiteness | Apparent viscosity (mpa.s) | |
| Rower | " 8% | " 17% | 0.5-1.2 | 9-11 | 》85 | 》2500 |
| A1 | 7% | 15% | 1.2 | 9 | 90 | 3000 |
| A2 | 7% | 14% | 1 | 10 | 90 | 3000 |
| It is commercially available | 8% | 16% | 1 | 9-11 | 85 | 3000 |
It can be seen that aluminium-magnesium silicate product obtained in 1-2 of the embodiment of the present invention from the data of upper table 3, table 5 and table 7
Performance meets professional standard, and the purity of product and whiteness etc. are even more outstanding than industry product index, while the present invention
The method of offer takes full advantage of that discharge amount is huge and the flyash of exhaust emission environment is as raw material, overcomes and existing prepares silicon
The distribution and reserves of yield existing for the method for sour magnalium and cost by natural magnesium aluminium silicate mine soil are limited, while again can
Economy is developed a circular economy and saved, and destruction of the discharge to natural ecological environment of flyash can be reduced.
Claims (10)
1. a kind of coal ash for manufacturing is for the method for aluminium-magnesium silicate, wherein this method comprises:
(1) under conditions of flyash alkaline process mentions silicon, flyash is placed in alkaline solution, pre-desiliconizing solution is obtained and to mention silicon residual
Slag；
(2) the silicon residue that mentions for obtaining step (1) is uniformly mixed with sodium carbonate and/or calcium oxide, is roasted, is dissolved out, solid-liquid
Isolated sodium aluminate filtrate；
(3) sodium aluminate filtrate obtained in pre-desiliconizing solution obtained in step (1) and step (2) is mixed, and introduces nitric acid
Magnesium solution is reacted, and filtering, drying obtain aluminium-magnesium silicate.
2. according to the method described in claim 1, wherein, in step (1), the concentration of the alkaline solution is 10-50 weight %；
The weight ratio of flyash and the alkaline solution is 1:4-6.
3. according to the method described in claim 1, wherein, in step (1), the condition that the alkaline process mentions silicon includes: reaction temperature
It is 80-120 DEG C, the reaction time is 30-120 minutes.
4. according to the method described in claim 1, wherein, in step (2), mentioning silicon relative to what 100 parts by weight steps (1) obtained
Residue, the dosage of sodium carbonate are 100-150 parts by weight, and the dosage of calcium oxide is 40-70 parts by weight.
5. according to the method described in claim 1, wherein, in step (2), the condition of the roasting includes: that maturing temperature is
950-1250 DEG C, calcining time is 30-90 minutes.
6. according to the method described in claim 1, wherein, in step (2), the dissolution includes: that the product after roasting is added
Reacted into seasoning liquid, the seasoning liquid be the aqueous solution containing sodium aluminate, sodium hydroxide and sodium carbonate, sodium aluminate it is dense
Degree is 30-50 grams per liter, and the concentration of sodium hydroxide is 5-10 grams per liter, and the concentration of sodium carbonate is 15-20 grams per liter；The roasting produces
The weight ratio of object and the aqueous solution is 1:3-10.
7. according to the method described in claim 6, wherein, in step (2), the temperature of the dissolution reaction is 50-100 DEG C, instead
The time answered is 10-30 minutes.
8. according to the method described in claim 1, wherein, in step (3), pre-desiliconizing liquid, sodium aluminate filtrate, in magnesium nitrate solution
Molar ratio are as follows:
AlO2 -:SiO3 2-=1.5-3.5
Mg2+:AlO2-=0.4-0.8.
9. method according to claim 1 or 8, wherein the concentration of the magnesium nitrate solution is 1-5mol/L, pH 4-6.
10. method according to claim 1 to 8, wherein in step (3), the condition of the reaction includes: anti-
Answering temperature is 60-90 DEG C, and the reaction time is 1-5 hours, pH value 7-9.
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