CN106315603A - Preparation method of polymeric aluminum ferric silicate - Google Patents
Preparation method of polymeric aluminum ferric silicate Download PDFInfo
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- CN106315603A CN106315603A CN201610638758.7A CN201610638758A CN106315603A CN 106315603 A CN106315603 A CN 106315603A CN 201610638758 A CN201610638758 A CN 201610638758A CN 106315603 A CN106315603 A CN 106315603A
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 76
- 239000010881 fly ash Substances 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims description 130
- 238000006243 chemical reaction Methods 0.000 claims description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 35
- -1 ferrum aluminum salt Chemical class 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 13
- 239000007790 solid phase Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 13
- 239000004411 aluminium Substances 0.000 claims description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 12
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims 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 claims description 3
- 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 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000003513 alkali Substances 0.000 abstract description 5
- 238000005189 flocculation Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000016615 flocculation Effects 0.000 abstract description 3
- 239000002440 industrial waste Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- KRCAYUPYTQNRQM-UHFFFAOYSA-I aluminum;iron(2+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Fe+2] KRCAYUPYTQNRQM-UHFFFAOYSA-I 0.000 abstract 2
- 238000002791 soaking Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 42
- 239000002585 base Substances 0.000 description 25
- 239000007788 liquid Substances 0.000 description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000004115 Sodium Silicate Substances 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 10
- 229910052911 sodium silicate Inorganic materials 0.000 description 10
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 9
- 229920005591 polysilicon Polymers 0.000 description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000000717 retained effect Effects 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000003311 flocculating effect Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000202567 Fatsia japonica Species 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229920000592 inorganic polymer Polymers 0.000 description 2
- 150000002505 iron Chemical class 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000007818 Grignard reagent Substances 0.000 description 1
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000004795 grignard reagents Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- YNXURHRFIMQACJ-UHFFFAOYSA-N lithium;methanidylbenzene Chemical compound [Li+].[CH2-]C1=CC=CC=C1 YNXURHRFIMQACJ-UHFFFAOYSA-N 0.000 description 1
- OVEHNNQXLPJPPL-UHFFFAOYSA-N lithium;n-propan-2-ylpropan-2-amine Chemical compound [Li].CC(C)NC(C)C OVEHNNQXLPJPPL-UHFFFAOYSA-N 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- RPDAUEIUDPHABB-UHFFFAOYSA-N potassium ethoxide Chemical compound [K+].CC[O-] RPDAUEIUDPHABB-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
Abstract
The invention discloses a preparation method of polymeric aluminum ferric silicate. The preparation method of the polyaluminum ferric silicate comprises the steps of taking fly ash as a raw material, firstly soaking the fly ash in a strong acid solution, then reacting the fly ash with a strong alkali solution to obtain an iron aluminum hydroxide sol, meanwhile, acidifying unreacted fly ash and the strong alkali solution to obtain a polysilicic acid sol, and then reacting the iron aluminum hydroxide sol with the polysilicic acid sol to obtain the polyaluminum ferric silicate, so that the prepared polyaluminum ferric silicate has a good flocculation effect. In addition, the fly ash which is an industrial waste with wide sources is used as a raw material, so that waste can be changed into valuable, and the production cost is reduced.
Description
Technical field
The present invention relates to the technical field of flocculant, in particular to the preparation method of a kind of polymeric aluminium ferrum silicate.
Background technology
Flocculant mainly with just (bear) in electrical group and water with negative (just) electrical be difficult to some of separation
Particle or granule are close to each other, reduce its electromotive force so that it is play pendulum, and utilize its aggregation property to make these
Grain is concentrated, and is separated by physics or chemical method.Flocculant totally can be divided into inorganic flocculation according to its chemical composition
Agent and organic flocculant two class.Wherein inorganic flocculating agent includes again inorganic flocculant and inorganic polymer flocculant；Organic-flocculation
Agent includes again Syn-Organic flocculants, natural organic high-molecular flocculant and microbial flocculant.In recent years, for adapting to
The needs of different quality further treatment technique, inorganic polymer flocculant become hot research technology, this type of flocculant divides
Son amount is big, may replace part organic synthesis high polymer coagulant to avoid toxicity problem.Polysilicate is that a class novel inorganic is high
Molecular flocculant, is to grow up on the basis of the flocculant such as polysilicon acid (i.e. activated silicic acid) and traditional aluminium salt, iron salt
Polysilicon acid and the combination product of slaine.Such flocculant can combine the advantage of polysilicon acid and poly-aluminum, ferrum, fully sends out
Waving the strong point of the two, enhance charge neutrality and adsorption bridging effect, improve flocculating effect, and it is easily prepared, raw material sources are wide
General, low price.So, polysilicate New Inorganic High Polymer Coagulant has the hugest potential application foreground.
In prior art, the flocculating effect of polymeric aluminium ferrum silicate is poor.
Summary of the invention
In view of this, the invention reside in the preparation method that a kind of polymeric aluminium ferrum silicate is provided, this preparation method prepare
Polymeric aluminium ferrum silicate effect is preferable.
The preparation method of a kind of polymeric aluminium ferrum silicate, comprises the following steps:
(1) flyash and strong acid solution are reacted, and separate formation solid phase and ferrum aluminum salt solution；
(2) described ferrum aluminum salt solution and strong base solution are reacted, obtain ferrum aluminium hydroxide colloidal sol；
(3) described solid phase and strong base solution are reacted, obtain silicate solutions；
(4) described silicate solutions and strong acid solution are reacted, obtain polysilicic acid sol；
(5) described polysilicic acid sol and described ferrum aluminium hydroxide colloidal sol are reacted, obtain polyferric silicate sulfate aluminum.
Further, in step (1):
The consumption of described strong acid solution is 0.02～0.06, is in terms of 1 by the quality of flyash；
Preferably, the temperature of described reaction is 60～70 DEG C, and the time of described reaction is 1～3h；
Preferably, the mass fraction of described strong acid solution is 10～30%；
Preferably, described strong acid solution is hydrochloric acid；
Preferably, described reaction is under agitation carried out, and the rotating speed of described stirring is 50～300rpm.
Further, in step (2):
The consumption of described strong base solution is the consumption that pH is 2～4 making reactant liquor；
Preferably, the mass fraction of described strong base solution is 20～40%；
Preferably, described strong base solution is Strong oxdiative sodium solution；
Preferably, the time of described reaction is 2～4h.
Further, in step (3):
The consumption of described strong base solution is 0.05～0.2, is in terms of 1 by the quality of solid phase；
Preferably, the temperature of described reaction is 130～170 DEG C, and the time of described reaction is 3～5h, the pressure of described reaction
Power is 0.2～0.6MPa；
Preferably, the mass fraction of described strong base solution is 20～40%；
Preferably, described strong base solution is Strong oxdiative sodium solution.
Further, in step (4):
The mass fraction of described silicate solutions is 2～5%；
Preferably, the mass fraction of described strong acid solution is 10～30%；
Preferably, described strong acid solution is sulfuric acid solution；
Preferably, the process of described reaction includes, first makes silicate solutions and part strong acid solution be 3 at pH～enter for 5 times
The row first stage reacts, then makes described first stage product be 1 with part strong acid solution at pH～carry out second-order 3 times
Duan Fanying；
Preferably, the time of reaction of described first stage is 1～3h；
Preferably, the time of described second stage reaction is 1～3h.
Further, in step (5):
The ratio of described polysilicic acid sol and described ferrum aluminium hydroxide collosol substance amount is 1～1.5:1；
Preferably, the time of described reaction is 1～3h, and the temperature of described reaction is 20～30 DEG C；
Preferably, described reaction is under agitation carried out, and the rotating speed of described stirring is 50～300rpm.
Further, the standing that its product is carried out 20～28h is also included after step (5) described reaction.
Further, the step of activation is also included before described step (1).
Further, described activation uses the mode of roasting.
Further, the temperature of described roasting is 650～750 DEG C, and the time of described roasting is 3～5h.
The preparation method of the polymeric aluminium ferrum silicate of the present invention, with flyash as raw material, first with strong acid solution impregnate, then with
Strong base solution reaction obtains ferrum aluminium hydroxide colloidal sol, is gathered with strong base solution, again acidifying by unreacted flyash meanwhile
Silica sol, then ferrum aluminium hydroxide colloidal sol is reacted with polysilicic acid sol obtain polymeric aluminium ferrum silicate, thus prepare polymerization silicon
Acid ferro-aluminum has preferable flocculating effect.Additionally, the trade waste flyash relatively broad with source is as raw material, can become useless
For treasured, reduce production cost.
Detailed description of the invention
For the ease of understanding the present invention, close embodiment below and further illustrate technical scheme.
As used herein, term:
" one ", " a kind of " and " described " are used interchangeably and refer to one or more.
"and/or" for represent the one or both of illustrated situation all it may happen that, such as, A and/or B includes (A
And B) and (A or B)；
It addition, all numerical value that the scope stated by end points herein is comprised in the range of including this (such as, 1 to 10 bag
Include 1.4,1.9,2.33,5.75,9.98 etc.).
It addition, the statement of " at least one " herein include one and above all numbers (such as, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
The preparation method of the polymeric aluminium ferrum silicate of the present invention, comprises the following steps:
(1) flyash and strong acid solution are reacted, and separate formation solid phase and ferrum aluminum salt solution；
(2) described ferrum aluminum salt solution and strong base solution are reacted, obtain ferrum aluminium hydroxide colloidal sol；
(3) described solid phase and strong base solution are reacted, obtain silicate solutions；
(4) described silicate solutions and strong acid solution are reacted, obtain polysilicic acid sol；
(5) described polysilicic acid sol and described ferrum aluminium hydroxide colloidal sol are reacted, obtain polyferric silicate sulfate aluminum.
Above-mentioned flyash refers to receive the flue gas after coal combustion catch the fine ash got off, and flyash is that coal-burning power plant discharges
Primary solids refuse, its major oxide constituents is SiO2、Al2O3、Fe2O3.The present invention with industrial waste gas thing flyash as raw material,
Avoid and prior art uses iron salt, aluminium salt in a large number, reduce production cost cost；Owing to flyash source is relatively broad,
It has expanded the commercial production application of polymeric aluminium ferrum silicate.
In above-mentioned steps (1), solid phase may be appreciated and refers to that flyash is not dissolved by strong acid solution and the residue that reacts away
Part.This solid phase main active is SiO2.Flyash and strong acid solution react generated ferrum aluminum salt solution for being mixed with
Ferric ion, the water soluble salt of trivalent aluminium ion, its principle is, hydrion and Al in strong acid2O3、Fe2O3Reaction.
In above-mentioned steps (1), strong acid solution is strong aqueous acid, and strong acid refers to ionization constant in aqueous herein,
Acidity coefficient pKa (the negative logarithm of ionization constant) less than 1 for strong acid (pKa=1～4 is middle strong acid, is weak acid more than 4).By force
Acid solution can be mineral acid, such as hydrochloric acid, sulphuric acid, nitric acid etc., it is possible to for mineral acid, such as benzenesulfonic acid, trifluoroacetic acid etc., this
Bright preferably hydrochloric acid.
In above-mentioned steps (1), strong acid solution consumption be advisable with 0.02～0.06, such as 0.02,0.025,0.03,
0.04,0.05,0.055,0.057,0.058,0.059 or 0.60 etc., preferably 0.04, it is in terms of 1 by the quality of coal ash.As for by force
The concentration of acid solution, does not make the most harsh restriction, but is preferably 10～30% for its mass fraction, such as its mass fraction
It is 10%, 11%, 12%, 15%, 20%, 25%, 26%, 28%, 29% or 30% etc., preferably 20%.
In above-mentioned steps (1), the temperature of reaction is preferred with 60～70 DEG C, such as 60 DEG C, 62 DEG C, 65 DEG C, 67 DEG C, 68 DEG C,
69 DEG C or 70 DEG C, preferably 65 DEG C.Under this reaction temperature, the time of reaction can be 1～3h, such as 1h, 1.2h, 1.5h,
2h, 2.5h or 3h, preferably 2h.It is understood that for the condition maintaining constant temperature equilibrium temperature, reaction can be at the bar of water-bath
Implement under part.Herein, also can arrange agitating device, such as machine mixer in the reaction, the rotating speed of stirring can be set in 50～
300rpm, such as 50rpm, 55rpm, 60rpm, 80rpm, 100rpm, 150rpm, 180rpm, 200rpm, 250rpm or 300rpm
Deng, preferably 100rpm.
As for aforesaid separation, its means can use filtration, such as sucking filtration etc..
In above-mentioned steps (2), strong base solution refers to the aqueous solution of highly basic, and highly basic refers to ionize out completely hydroxyl herein
The electrolyte of ion.Highly basic can list organic alkali, as the strongest, if organometallic lithium compounds is (such as fourth in metallization alkaloids
Base lithium, diisopropyl ammonia lithium, benzyl lithium etc.), Grignard reagent, alkyl copper lithium etc..Followed by sodium alkoxide or potassium alcoholate are (such as Feldalat NM, second
Sodium alkoxide, potassium ethoxide, sodium tert-butoxide etc.), can be the most also inorganic strong alkali, such as alkali metal highly basic, such as sodium hydroxide, hydroxide
Lithium, potassium hydroxide etc..Strong base solution with the reaction principle of ferrum aluminum salt solution is, water-soluble iron ion and aluminium ion and hydroxyl from
Son combines the colloidal sol producing hydroxide (being mixed with aluminium hydroxide, hydrated ferric oxide .).In order to ensure the form that product is colloidal sol, by force
The consumption of aqueous slkali is that the consumption that pH is 2～4 making reactant liquor, the i.e. consumption of strong base solution are to maintain the pH of reaction system for 2
～4.Such as, pH can be 2,2.2,2.5,2.8,3,3.5,3.8 or 4 etc..As for the concentration of strong base solution, do not make the most harsh
Limit, but be preferably 20～40% for its mass fraction, such as its mass fraction is 20%, 21%, 22%, 25%, 30%,
35%, 36%, 38%, 39% or 40% etc., preferably 30%.The temperature of reaction can be room temperature, such as 20～30 DEG C.
Under this reaction temperature, the time of reaction can be 2～4h, such as 2h, 2.2h, 2.5h, 3h, 3.5h or 4h, preferably 3h.
In above-mentioned steps (3), the principle of solid phase and strong base solution reaction is, the active component silicon dioxide in solid phase is with strong
Alkali reaction generates silicate.Here, the as defined above of strong base solution is stated, and highly basic is preferably sodium hydroxide solution.Strong base solution
Consumption be 0.05～0.2, such as 0.05,0.055,0.06,0.07,0.1,0.12,0.125,0.13,0.15,0.18,
0.19,0.20 etc., preferably 0.1, it is in terms of 1 by the quality of solid phase.As for the concentration of highly basic, its mass fraction can be 20～
40%, such as 20%, 21%, 22%, 25%, 30%, 35%, 36%, 38%, 39% or 40% etc., preferably 30%.Reaction
Temperature be preferred with 130～170 DEG C, such as 130 DEG C, 132 DEG C, 135 DEG C, 140 DEG C, 142 DEG C, 145 DEG C, 150 DEG C, 160 DEG C,
165 DEG C, 167 DEG C, 169 DEG C or 170 DEG C etc., preferably 150 DEG C；The pressure of reaction is 0.2～0.6MPa, such as 0.2MPa,
0.22MPa、0.25MPa、0.30MPa、0.40MPa、0.45MPa、0.50MPa、0.55MPa、0.56MPa、0.57MPa、
0.58MPa, 0.59MPa, 0.60MPa etc., preferably 0.4MPa；Under this temperature and this pressure, time of its reaction be 3～
5h, such as 3h, 3.2h, 3.5h, 4h, 4.5h, 4.8h or 5h, preferably 4h.
In above-mentioned steps (4), the principle of silicate solutions and strong acid solution reaction is, strong acid and the silicate in silicate
Ions binding becomes silicic acid, shortens generation polysilicon acid between silicic acid molecule into.In order to ensure that silicic acid does not occur colloidal sol, participate in the silicon of reaction
The concentration of acid salt solution is preferably 2～5% for its mass fraction, such as 2%, 2.1%, 2.2% .25%, 3%, 3.5%,
4%, 4.5%, 4.6%, 4.7%, 4.8%, 4.9% or 5% etc., preferably 3.5% etc..Strong acid solution can be same as aforementioned,
But preferably sulfuric acid solution.As for its concentration, its mass fraction is 10%, 11%, 12%, 15%, 20%, 25%, 26%,
28%, 29% or 30% etc., preferably 20%.
In above-mentioned steps (4), the process of reaction can be implemented according to two stages, the first stage for make silicate solutions and
Part strong acid solution is 3 at pH～carries out for 5 times, and such as pH is 3,3.2,3.5,4,4.5 or 5, preferably 4；This stage completes silicon
Acid salt solution and strong acid solution are combined into silicic acid；Second stage is that first stage product is being at pH with part strong acid solution
1～carry out for 3 times, such as 1,1.2,1.5,2,2.5 or 3, preferably 2, this stage completes the shrink of silicic acid.Herein, the first stage
Time be preferred with 1～3h, such as 1h, 1.2h, 2h, 2.5h or 3h, preferably 2h；The time of second stage is preferred with 1～3h,
Such as 1h, 1.2h, 2h, 2.5h or 3h, preferably 2h.
In above-mentioned steps (5), the ratio of polysilicic acid sol and described ferrum aluminium hydroxide collosol substance amount with 1～1.5:1 is
Good, such as 1:1,1.02:1,1.05:1,1.08:1,1.1:1,1.2:1,1.25:1,1.30:1,1.40:1,1.45:1,1.48:
1,1.50:1, preferably 1:1.The temperature of reaction is 20～30 DEG C, such as 20 DEG C, 22 DEG C, 25 DEG C, 27 DEG C, 28 DEG C, 29 DEG C or 30
℃.Under this reaction temperature, the time of reaction is preferred with 1～3h, such as 1h, 1.2h, 2h, 2.5h or 3h, preferably 2h.Also may be used
Arranging agitating device, such as machine mixer in the reaction, the rotating speed of stirring can be set in 50～300rpm, such as 50rpm,
55rpm, 60rpm, 80rpm, 100rpm, 150rpm, 180rpm, 200rpm, 250rpm or 300rpm etc., preferably 100rpm.
In above-mentioned steps (5), the standing that its product is carried out 20～28h can also be included after reaction, such as
20h, 22h, 23h, 24h, 25h, 26h, 27h or 28h etc., preferably 24h.
In order to improve flyash and the reactivity of strong acid solution reaction, activation can be used before step (1).Activation is adopted
By the mode of roasting, other known mode the most also can be used.The temperature of roasting can be 680～720 DEG C, such as 680
℃、682℃、685℃、690℃、690℃、700℃、710℃、715℃、718℃、720℃、；At a temperature of this roasting, roasting
The time burnt is 3～5h, such as 3h, 3.2h, 4h, 4.5h or 5h, preferably 4h.
Embodiment 1
(1), by flyash put into roaster and carry out roasting, control sintering temperature at 680 DEG C, roasting 5h.
(2), being added in flyash by the hydrochloric acid that mass fraction is 10%, the consumption of strong acid solution is 0.02, with flyash
Quality be 1 meter, in the water bath with thermostatic control of 60 DEG C, stir 3h with the speed of 50rpm.Filter is utilized to be filtered by reactant liquor,
Obtaining liquid and filtering residue after filter, filtrate is ferrum aluminum salt solution, and filtering residue is standby.
(3), after filter, liquid adds 20% sodium hydroxide regulation pH is 2, stands 2h and is allowed to polymerization to obtain polyferric silicate sulfate molten
Liquid.Filtering residue is standby.
(4), the filtering residue of above-mentioned gained is retained, and filtering residue is dried, grinds, by filtering residue and the sodium hydroxide solution of 20%
Being mixed into slurry input autoclave, the consumption of strong base solution is 0.05, is in terms of 1 by the quality of filtering residue.At 0.2MPa pressure
React 3h under conditions of being 140 DEG C with temperature, reacting liquid filtering is obtained sodium silicate solution.
(5), by the sodium silicate solution of gained it is diluted with water to the solution that mass fraction is 2%, and adjusts with the sulphuric acid of 10%
Joint pH value of solution is standing 1h after 3, then is 3 polymerization 1h with sulfur acid for adjusting pH, can obtain sodium polysilicate solution.
(6), be 0.9:1 mixing by polysilicon acid and Polyaluminium iron solution in the amount ratio of optimisation substance, at ambient temperature, with
The speed stirring of 50rpm, is allowed to react 1h, then stands 20hr, i.e. can get poly aluminium iron silicate solution.
Embodiment 2
(1), by flyash put into roaster and carry out roasting, control sintering temperature at 720 DEG C, roasting 3h.
(2), being added in flyash by the hydrochloric acid that mass fraction is 30%, the consumption of strong acid solution is 0.06, with flyash
Quality be 1 meter, in the water bath with thermostatic control of 70 DEG C, stir 1h with the speed of 300rpm.Filter is utilized to be carried out by reactant liquor
Filter, it is thus achieved that liquid and filtering residue after filter, filtrate is ferrum aluminum salt solution, and filtering residue is standby.
(3), after filter, liquid adds 40% sodium hydroxide regulation pH is 4, stands 2h and is allowed to polymerization to obtain polyferric silicate sulfate molten
Liquid.Filtering residue is standby.
(4), the filtering residue of above-mentioned gained is retained, and filtering residue is dried, grinds, by filtering residue and the sodium hydroxide solution of 40%
Being mixed into slurry input autoclave, the consumption of strong base solution is 0.2, is in terms of 1 by the quality of filtering residue.At 0.6MPa pressure and
Temperature reacts 3h under conditions of being 160 DEG C, and reacting liquid filtering obtains sodium silicate solution.
(5), by the sodium silicate solution of gained it is diluted with water to the solution that mass fraction is 5%, and adjusts with the sulphuric acid of 30%
Joint pH value of solution is standing 3h after 5, then is 5 polymerization 1h with sulfur acid for adjusting pH, can obtain sodium polysilicate solution.
(6), be 1.1:1 mixing by polysilicon acid and Polyaluminium iron solution in the amount ratio of optimisation substance, at ambient temperature, with
The speed stirring of 300rpm, is allowed to react 3h, then stands 28hr, i.e. can get poly aluminium iron silicate solution.
Embodiment 3
(1), by flyash put into roaster and carry out roasting, control sintering temperature at 680 DEG C, roasting 5h.
(2), being added in flyash by the hydrochloric acid that mass fraction is 30%, the consumption of strong acid solution is 0.06, with flyash
Quality be 1 meter, in the water bath with thermostatic control of 70 DEG C, stir 3h with the speed of 300rpm.Filter is utilized to be carried out by reactant liquor
Filter, it is thus achieved that liquid and filtering residue after filter, filtrate is ferrum aluminum salt solution, and filtering residue is standby.
(3), after filter, liquid adds 40% sodium hydroxide regulation pH is 2, stands 4h and is allowed to polymerization to obtain polyferric silicate sulfate molten
Liquid.Filtering residue is standby.
(4), the filtering residue of above-mentioned gained is retained, and filtering residue is dried, grinds, by filtering residue and the sodium hydroxide solution of 40%
Being mixed into slurry input autoclave, the consumption of strong base solution is 0.2, is in terms of 1 by the quality of filtering residue.At 0.6MPa pressure and
Temperature reacts 5h under conditions of being 160 DEG C, and reacting liquid filtering obtains sodium silicate solution.
(5), by the sodium silicate solution of gained it is diluted with water to the solution that mass fraction is 5%, and adjusts with the sulphuric acid of 30%
Joint pH value of solution is standing 1～3h after 5, then is 5 polyase 13 h with sulfur acid for adjusting pH, can obtain sodium polysilicate solution.
(6), be 1.1:1 mixing by polysilicon acid and Polyaluminium iron solution in the amount ratio of optimisation substance, at ambient temperature, with
The speed stirring of 300rpm, is allowed to react 3h, then stands 28hr, i.e. can get poly aluminium iron silicate solution.
Embodiment 4
(1), by flyash put into roaster and carry out roasting, control sintering temperature at 700 DEG C, roasting 4h.
(2), being added in flyash by the hydrochloric acid that mass fraction is 20%, the consumption of strong acid solution is 0.04, with flyash
Quality be 1 meter, in the water bath with thermostatic control of 65 DEG C, stir 3h with the speed of 100rpm.Filter is utilized to be carried out by reactant liquor
Filter, it is thus achieved that liquid and filtering residue after filter, filtrate is ferrum aluminum salt solution, and filtering residue is standby.
(3), after filter, liquid adds 20% sodium hydroxide regulation pH is 2, stands 4h and is allowed to polymerization to obtain polyferric silicate sulfate molten
Liquid.Filtering residue is standby.
(4), the filtering residue of above-mentioned gained is retained, and filtering residue is dried, grinds, by filtering residue and the sodium hydroxide solution of 20%
Being mixed into slurry input autoclave, the consumption of strong base solution is 0.2, is in terms of 1 by the quality of filtering residue.At 0.6MPa pressure and
Temperature reacts 5h under conditions of being 160 DEG C, and reacting liquid filtering obtains sodium silicate solution.
(5) solution that mass fraction is 3.5%, by the sodium silicate solution of gained it is diluted with water to, and with the sulphuric acid of 20%
Regulation pH value of solution is standing 2h after 4, then is 4 polymerization 2h with sulfur acid for adjusting pH, can obtain sodium polysilicate solution.
(6), be 1:1 mixing by polysilicon acid and Polyaluminium iron solution in the amount ratio of optimisation substance, at ambient temperature, with
The speed stirring of 100rpm, is allowed to react 3h, then stands 24hr, i.e. can get poly aluminium iron silicate solution.
Embodiment 5
(1), by flyash put into roaster and carry out roasting, control sintering temperature at 700 DEG C, roasting 4h.
(2), being added in flyash by the hydrochloric acid that mass fraction is 20%, the consumption of strong acid solution is 0.04, with flyash
Quality be 1 meter, in the water bath with thermostatic control of 65 DEG C, stir 2h with the speed of 100rpm.Filter is utilized to be carried out by reactant liquor
Filter, it is thus achieved that liquid and filtering residue after filter, filtrate is ferrum aluminum salt solution, and filtering residue is standby.
(3), after filter, liquid adds 30% sodium hydroxide regulation pH is 3, stands 3h and is allowed to polymerization to obtain polyferric silicate sulfate molten
Liquid.Filtering residue is standby.
(4), the filtering residue of above-mentioned gained is retained, and filtering residue is dried, grinds, by filtering residue and the sodium hydroxide solution of 30%
Being mixed into slurry input autoclave, the consumption of strong base solution is 0.1, is in terms of 1 by the quality of filtering residue.At 0.4MPa pressure and
Temperature reacts 4h under conditions of being 150 DEG C, and reacting liquid filtering obtains sodium silicate solution.
(5) solution that mass fraction is 3.5%, by the sodium silicate solution of gained it is diluted with water to, and with 10～30%
Sulfuric acid regulation solution pH is standing 2h after 4, then is 4 polymerization 2h with sulfur acid for adjusting pH, can obtain sodium polysilicate solution.
(6), be 1:1 mixing by polysilicon acid and Polyaluminium iron solution in the amount ratio of optimisation substance, at ambient temperature, with
The speed stirring of 100rpm, is allowed to react 2h, then stands 24hr, i.e. can get poly aluminium iron silicate solution.
Slurry paper plant bio-chemical effluent is made according to known test mode by the polymeric aluminium ferrum silicate prepared by embodiment 1～5
Testing COD, turbidity and colourity, each flocculant is tested with the chemical feeding quantity of 250mg/L, and experimental result is as shown in table 1 below:.
Table 1 test result
Flocculant prepared by preparation method of the present invention, its COD removal efficiency is the highest is 79.1%, and color removal efficiency is
Height can be 96.5%, and turbidity removal efficiency is the highest is 72.1.0%, and slurry paper plant bio-chemical effluent can reach after its flocculation treatment
The requirement of GB3544-2008 pulp and paper industry pollution discharge standard.
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments,
As long as but the most envisioned any numerical value fallen in this numerical range above-mentioned of those skilled in the art all can implement this
Invention, the most also includes the combination in any of occurrence in the range of some numerical value.Herein, for the consideration of length, eliminate to
Going out the embodiment of occurrence in certain one or more numerical range, this disclosure being not to be construed as technical scheme is not filled
Point.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention have to rely on above-mentioned in detail
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete mode selection etc., falls in the protection of the present invention
In the range of.
Claims (10)
1. the preparation method of a polymeric aluminium ferrum silicate, it is characterised in that comprise the following steps:
(1) flyash and strong acid solution are reacted, and separate formation solid phase and ferrum aluminum salt solution；
(2) described ferrum aluminum salt solution and strong base solution are reacted, obtain ferrum aluminium hydroxide colloidal sol；
(3) described solid phase and strong base solution are reacted, obtain silicate solutions；
(4) described silicate solutions and strong acid solution are reacted, obtain polysilicic acid sol；
(5) described polysilicic acid sol and described ferrum aluminium hydroxide colloidal sol are reacted, obtain polyferric silicate sulfate aluminum.
Preparation method the most according to claim 1, it is characterised in that in step (1):
The consumption of described strong acid solution is 0.02～0.06, is in terms of 1 by the quality of flyash；
Preferably, the temperature of described reaction is 60～70 DEG C, and the time of described reaction is 1～3h；
Preferably, the mass fraction of described strong acid solution is 10～30%；
Preferably, described strong acid solution is hydrochloric acid；
Preferably, described reaction is under agitation carried out, and the rotating speed of described stirring is 50～300rpm.
Preparation method the most according to claim 1 and 2, it is characterised in that in step (2):
The consumption of described strong base solution is the consumption that pH is 2～4 making reactant liquor；
Preferably, the mass fraction of described strong base solution is 20～40%；
Preferably, described strong base solution is Strong oxdiative sodium solution；
Preferably, the time of described reaction is 2～4h.
4. according to the preparation method described in claims 1 to 3 any one, it is characterised in that in step (3):
The consumption of described strong base solution is 0.05～0.2, is in terms of 1 by the quality of solid phase；
Preferably, the temperature of described reaction is 130～170 DEG C, and the time of described reaction is 3～5h, and the pressure of described reaction is
0.2～0.6MPa；
Preferably, the mass fraction of described strong base solution is 20～40%；
Preferably, described strong base solution is sodium hydroxide solution.
5. according to the preparation method described in Claims 1-4 any one, it is characterised in that in step (4):
The mass fraction of described silicate solutions is 2～5%；
Preferably, the mass fraction of described strong acid solution is 10～30%；
Preferably, described strong acid solution is sulfuric acid solution；
Preferably, the process of described reaction includes, first makes silicate solutions and part strong acid solution be 3 at pH～carry out for 5 times
One elementary reaction, then to make described first stage product be 1～to carry out second stage 3 times anti-with part strong acid solution at pH
Should；
Preferably, the time of reaction of described first stage is 1～3h；
Preferably, the time of described second stage reaction is 1～3h.
6. according to the preparation method described in claim 1 to 5 any one, it is characterised in that in step (5):
The ratio of described polysilicic acid sol and described ferrum aluminium hydroxide collosol substance amount is 1～1.5:1；
Preferably, the time of described reaction is 1～3h, and the temperature of described reaction is 20～30 DEG C；
Preferably, described reaction is under agitation carried out, and the rotating speed of described stirring is 50～300rpm.
7. according to the preparation method described in claim 1 to 6 any one, it is characterised in that after step (5) described reaction also
Including the standing that its product is carried out 20～28h.
8. according to the preparation method described in claim 1 to 7 any one, it is characterised in that also include before described step (1)
The step of activation.
Preparation method the most according to claim 8, it is characterised in that described activation uses the mode of roasting.
Preparation method the most according to claim 9, it is characterised in that the temperature of described roasting is 650～750 DEG C, described
The time of roasting is 3～5h.
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