CN101148258B - Method for preparing hydrated aluminum silicate - Google Patents
Method for preparing hydrated aluminum silicate Download PDFInfo
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- CN101148258B CN101148258B CN2007101309258A CN200710130925A CN101148258B CN 101148258 B CN101148258 B CN 101148258B CN 2007101309258 A CN2007101309258 A CN 2007101309258A CN 200710130925 A CN200710130925 A CN 200710130925A CN 101148258 B CN101148258 B CN 101148258B
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- water
- water glass
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Abstract
The present invention is preparation process of aluminum silicate hydrate and belongs to the field of chemical technology. After granulated blast furnace slag as main material is added into water to form suspension, certain amount of sulfuric acid is added for aciddolysis reaction, the reaction resultant is filtered to obtain mixture solution with silicic acid and aluminum salt as main components, and the mixture solution is then reacted with proper amount of water glass to synthesize aluminum silicate hydrate. Through further ageing, polymerization, filtering, separating and drying, aluminum silicate hydrate product is produced ultimately. The preparation process is environment friendly, low in cost and simple, and has reasonable utilization of resource.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of preparation method who prepares hydrated aluminium silicate with blast furnace water quenching slag.
Background technology
At present, the preparation method of hydrated aluminium silicate can be summed up as following two kinds:
Traditional preparation process method: adopt Tai-Ace S 150 (industrial iron-free level) and water glass (the control modulus is 3.0～3.3) directly synthetic for raw material; Adopting the preparation method of this type of raw material now very ripe, is the technology that generally adopts both at home and abroad.
The in-situ modified method of chemical precipitation: concrete visible document " ultra-fine high-purity pure aluminium silicate new process of production research " (" chemical industry mineral and processing ", 2002, (4), pp:8～10), this method is a kind of comparatively novel preparation method, it is to have carried out modification simultaneously, made it to obtain the powder hydrated aluminium silicate product of polymolecularity adopting the traditional preparation process method to prepare in the process of hydrated aluminium silicate.
As fully visible, at present the preparation method of hydrated aluminium silicate is single, and prior art all is directly to adopt the industrial chemicals of particular requirement to make the hydrated aluminium silicate product, and production cost is higher.
Summary of the invention
Single in order to overcome the existing preparation method of hydrated aluminium silicate, the shortcoming that production cost is high, the present invention is useless admittedly according to a kind of industry---contain the characteristic of a large amount of aluminium and silicon constituent element in the blast furnace water quenching slag, provide a kind of abundant raw material to be easy to get, technical process is simple, the method for preparing hydrated aluminium silicate that product cost is low has also solved the problem that solid useless discharging is taken up an area of simultaneously.
Now the concrete preparation method with raw material involved in the present invention and hydrated aluminium silicate is described below:
1, the physicochemical property that mainly prepares raw material-blast furnace water quenching slag
Main preparation raw material involved in the present invention is a blast furnace water quenching slag.Aluminium in this slag, silicon are to be main existence form with the astable mineral of vitreous state, the generation of vitreous state is because during the water quenched slag chilling, have little time to form crystallizable mineral and wherein chemical energy is stored in wherein and forms, thereby have higher chemically reactive, easily form the solution system that contains aluminium salt and silicic acid equal blend after the acidolysis; The typical chemical ingredients of blast furnace slag is as shown in table 1:
The main chemical compositions of table 1 blast furnace water quenching slag
2, concrete preparation method
By the composition requirement of intended target product hydrated aluminium silicate, the powdery blast furnace water quenching slag added make aaerosol solution in the entry, add sulfuric acid solution in definite ratio, reaction finishes after-filtration and separates the mixing solutions that obtains based on silicic acid and aluminium salt.Mixing solutions and suitable quantity of water glass are carried out the building-up reactions of hydrated aluminium silicate, the suitable add-on of water glass is determined by the pH value, adds a small amount of aluminium flake in the process of building-up reactions and prevents ferrous oxidation in the solution again.After ageing, polymerization, filtration, separation, drying finally make the hydrated aluminium silicate product.
Preparation method's concrete steps are as follows:
(1) true quantitative powdery blast furnace water quenching slag and water (are pressed mass ratio W
Slag: W
Water≤ 1: 10) put into reactor and mix formation suspension.
(2), measure the vitriol oil of 98% (mass percentage concentration) and be mixed with the dilution heat of sulfuric acid of 15%～20% (mass percentage concentration) by 1.2～1.5 times of the required stoichiometry [seeing following reaction formula (1) and (2)] of acid and slag reaction.
(3) dilute acid soln for preparing is slowly poured in the reactor, slag is carried out acidolysis, and constantly stir, treat that the acidolysis system pH arrives between 1.8～2.2, and reaction system do not have bubble and produce, think that reaction reaches home.Control acidolysis temperature 60 ℃～90 ℃ scopes by water bath with thermostatic control therebetween.
(4) above-mentioned acidolysis reaction product is filtered removal throw out (being mainly gypsum and acid non-soluble substance), get filtrate (being mainly aluminium salt and monomer silicic acid is main mixing solutions), standby.
(5) with industrial goods water glass solution (Na
2OnSiO
2, n is a modulus of water glass) be diluted with water to and contain the solution that water glass is 15%～20% (mass percentage concentration), standby.
(6) water glass solution that will dilute for w=15%～20% is heated to 80 ℃ of constant temperature, to extract again in the water glass solution after filtrate that the blast furnace slag acid hydrolysis solution obtains slowly adds dilution, and constantly stir, make it reaction, reach about 4.0 up to the pH of system value, stop to add filtrate.Add a small amount of aluminium flake in the process and prevent ferrous oxidation in the system, and hierarchy of control temperature is not less than 65 ℃, about 70 ℃, system is carried out the about 30min of ageing then, make it abundant reaction, polymerization.
(7) filter cake that above-mentioned reacted system is filtered, separation is obtained, water stirs evenly cleaning, suction filtration repeatedly, to remove foreign ion, gets solid matter, with getting white solid after this solid matter drying, the pulverizing, be target product of the present invention: hydrated aluminium silicate.
3, the main chemical reactions of preparation process
Reaction formula (1):
(n
1SiO
2，n
2Al
2O
3，n
3CaO，n
4MgO，n
5Fe
2O
3，n
6FeO)+(3n
2+n
3+n
4+3n
5+n
6)H
2SO
4＝n
1H
2SiO
3+2n
2Al
3++n
3CaSO
4↓+n
4Mg
2++2n
5Fe
3++n
6Fe
2++(3n
2+n
4+3n
5+n
6)SO
4 2-+(-n
1+3n
2+n
3+n
4+3n
5+n
6)H
2O
Reaction formula (2):
2Al
3++(a-n)H
2SiO
3+Na
2O·nSiO
2+(b+n+3-a)H
2O
=Na
2OAl
2O
3ASiO
2BH
2O+6H
+(a is 9～11, and b is 4～6)
The present invention be with blast furnace water quenching slag as main material production high value added product hydrated aluminium silicate, prepared hydrated aluminium silicate is a kind of fine auxiliary chemicals, applicable to fields such as coating, printing ink, papermaking.Because the used main raw material of preparation is the blast furnace waste residue, has reduced the wasting of resources, also alleviated simultaneously the pollution that it directly drains in the environment to be caused.This preparation method is with low cost, and process is simple, has rationally utilized resource, has the remarkable economical social benefit.
Embodiment
Embodiment 1: configure mass percentage concentration earlier and be 15% dilution heat of sulfuric acid, and standby.The 50g blast furnace slag powder that takes by weighing the pre-treatment powdering adds in the 500mL water, mix, stir, make aaerosol solution, add the about 430mL of 15% sulphuric acid soln again, the order of adding is that pre-assigned dilution heat of sulfuric acid is slowly added in the blast furnace slag aaerosol solution, and constantly stirs, treat that the acidolysis system pH reaches about 2.0, and when reaction system did not have the bubble generation, the blast furnace slag acidolysis was complete, and control acidolysis reaction system temperature is at 60 ℃ in the process.It is carried out suction filtration, then filtrate taking-up is placed beaker, standby.The industrial goods water glass solution is diluted with water to contains the solution that water glass is 15% (mass percentage concentration), standby.Measure the pre-assigned water glass solution of 120mL and be heated to 80 ℃ of constant temperature, will separate the filtrate that acid hydrolysate obtains again and join in the water glass solution, constantly stir; When reaching 4.0 left and right sides, system pH stops to drip filtrate, add a small amount of aluminium flake (about 5g) in the process, and hierarchy of control temperature is 70 ℃, then system is carried out the about 30min of ageing under this temperature, refilter separation, the anticaustic water of the filter cake that obtains is stirred evenly cleaning, suction filtration (triplicate, each about 400mL of water), to remove foreign ion, get solid matter.Place 250 ℃ baking oven to dry solid matter, promptly get hydrated aluminium silicate product (Na after the pulverizing
2OAl
2O
3ASiO
2BH
2O, a are 9～11, and b is 4～6).
Embodiment 2: configure mass percentage concentration earlier and be 20% dilution heat of sulfuric acid, and standby.The 50g blast furnace slag powder that takes by weighing the pre-treatment powdering adds in the 500mL water, mix, stir, make aaerosol solution, add the about 370mL of 20% sulphuric acid soln again, the order of adding is that pre-assigned dilution heat of sulfuric acid is slowly added in the blast furnace slag aaerosol solution, and constantly stirs, treat that the acidolysis system pH reaches about 2.0, and when reaction system did not have the bubble generation, the blast furnace slag acidolysis was complete, and control acidolysis reaction system temperature is at 70 ℃ in the process.It is carried out suction filtration, then filtrate taking-up is placed beaker, standby.The industrial goods water glass solution is diluted with water to contains the solution that water glass is 15% (mass percentage concentration), standby.Measure the pre-assigned water glass solution of 120mL and be heated to 80 ℃ of constant temperature, to separate the filtrate that acid hydrolysate obtains again joins in the water glass solution, constantly stir, when reaching 4.0 left and right sides, system pH stops to drip filtrate, add a small amount of aluminium flake (about 5g) in the process, hierarchy of control temperature is 70 ℃, and system carried out ageing (about 30min) under this temperature, refilter separation, the anticaustic water of the filter cake that obtains is stirred evenly cleaning, suction filtration (triplicate, each about 400mL of water), to remove foreign ion, get solid matter.Place 250 ℃ baking oven to dry solid matter, promptly get hydrated aluminium silicate product (Na after the pulverizing
2OAl
2O
3ASiO
2BH
2O, a are 9～11, and b is 4～6).
Embodiment 3: configure concentration earlier and be 20% dilution heat of sulfuric acid, and standby.The 50g blast furnace slag powder that takes by weighing the pre-treatment powdering adds in the 500mL water, mix, stir, make aaerosol solution, add the about 370mL of 20% sulphuric acid soln again, the order of adding is that pre-assigned dilution heat of sulfuric acid is slowly added in the blast furnace slag aaerosol solution, and constantly stirs, treat that the acidolysis system pH reaches about 2.0, and when reaction system did not have the bubble generation, the blast furnace slag acidolysis was complete, and control acidolysis reaction system temperature is at 90 ℃ in the process.It is carried out suction filtration, then filtrate taking-up is placed beaker, standby.The industrial goods water glass solution is diluted with water to contains the solution that water glass is 15% (mass percentage concentration), standby.Measure the pre-assigned water glass solution of 120mL and be heated to 80 ℃ of constant temperature, will separate the filtrate that acid hydrolysate obtains again and join in the water glass solution, constantly stir; When reaching 4.0 left and right sides, system pH stops to drip filtrate, add a small amount of aluminium flake (about 5g) in the process, and hierarchy of control temperature is 70 ℃, then system is carried out the about 30min of ageing under this temperature, refilter separation, the anticaustic water of the filter cake that obtains is stirred evenly cleaning, suction filtration (triplicate, each about 400mL of water), to remove foreign ion, get solid matter.Place 250 ℃ baking oven to dry solid matter, promptly get hydrated aluminium silicate product (Na after the pulverizing
2OAl
2O
3ASiO
2BH
2O, a are 9～11, and b is 4～6).
Claims (1)
1. the preparation method of a hydrated aluminium silicate is characterized in that with the blast furnace water quenching slag being raw material, and the preparation method is made up of the following step:
(1) with the blast furnace water quenching slag and the water of true quantitative pre-treatment powdering, put into reactor smaller or equal to 1: 10, mix forming suspension by slag and quality ratio;
(2),, measure the vitriol oil of mass percentage concentration 98% and be configured to the dilution heat of sulfuric acid of mass percentage concentration 15%～20% by required stoichiometric 1.2～1.5 times of acid and slag reaction according to the chemical constitution of blast furnace water quenching slag;
(3) acid solution is slowly poured in the reactor, and constantly stirred, the question response system does not have bubble and produces, and system pH is between 1.8～2.2, and acidolysis reaction finishes, and therebetween, acidolysis temperature is controlled at 60 ℃～90 ℃ scopes;
(4) above-mentioned acidolysis reaction product is filtered the removal throw out, get filtrate, standby;
(5) with industrial goods water glass solution: Na
2OnSiO
2, n is a modulus of water glass, is diluted with water to that to contain the water glass mass percentage concentration be 15%～20% solution, and is standby;
(6) be that 15%～20% water glass solution is heated to 80 ℃ of constant temperature with above-mentioned mass percentage concentration, again step (4) acidolysis reaction product is filtered in the water glass solution after the filtrate that obtains slowly adds dilution, and constantly stir, make it reaction, reach 4.0, stop to add filtrate up to the pH of system value, add a small amount of aluminium flake in the process and prevent ferrous oxidation in the system, and hierarchy of control temperature is not less than 65 ℃, at 70 ℃ system carried out ageing 30min then, makes it abundant reaction, polymerization;
(7) the reacted system of step (6) is filtered, with the filter cake that separation obtains, water stirs evenly cleaning, suction filtration repeatedly, gets solid matter, with obtaining white solid after this solid matter drying, the pulverizing, is the hydrated aluminium silicate product.
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|---|---|---|---|
| CN2007101309258A CN101148258B (en) | 2007-08-31 | 2007-08-31 | Method for preparing hydrated aluminum silicate |
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|---|---|---|---|
| CN2007101309258A CN101148258B (en) | 2007-08-31 | 2007-08-31 | Method for preparing hydrated aluminum silicate |
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| CN101148258B true CN101148258B (en) | 2010-09-15 |
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| CN108033699A (en) * | 2017-12-19 | 2018-05-15 | 安徽工业大学 | A kind of method that building materials gelling agent is prepared using blast furnace slag as raw material |
| CN109336122B (en) * | 2018-12-06 | 2023-02-28 | 中国矿业大学(北京) | Preparation method of aluminum silicate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1077899B1 (en) * | 1998-05-04 | 2003-08-06 | J.M. Huber Corporation | High surface area silicate pigment and method for its production |
| CN1817793A (en) * | 2005-09-22 | 2006-08-16 | 中国石油化工股份有限公司 | Production of superfine aluminium silicate from waste clay |
| CN1915813A (en) * | 2006-08-23 | 2007-02-21 | 山东铝业股份有限公司 | Method for preparing superfine alumina silicate |
-
2007
- 2007-08-31 CN CN2007101309258A patent/CN101148258B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1077899B1 (en) * | 1998-05-04 | 2003-08-06 | J.M. Huber Corporation | High surface area silicate pigment and method for its production |
| CN1817793A (en) * | 2005-09-22 | 2006-08-16 | 中国石油化工股份有限公司 | Production of superfine aluminium silicate from waste clay |
| CN1915813A (en) * | 2006-08-23 | 2007-02-21 | 山东铝业股份有限公司 | Method for preparing superfine alumina silicate |
Non-Patent Citations (6)
| Title |
|---|
| 徐旺生等，.超细高纯硅酸铝生产新工艺研究.化工矿物与加工31 (4).2002,31((4)),8-10. |
| 徐旺生等.超细高纯硅酸铝生产新工艺研究.化工矿物与加工31 (4).2002,31((4)),8-10. * |
| 戴志成等，.硅化合物的生产与应用 第1版.成都科技大学出版社,1994,143-146. |
| 戴志成等.硅化合物的生产与应用 第1版.成都科技大学出版社,1994,143-146. * |
| 李辽沙等，.含铝废液制备超细硅酸铝中除杂机理探讨.硅酸盐通报26 (3).2007,26((3)),436-440. |
| 李辽沙等.含铝废液制备超细硅酸铝中除杂机理探讨.硅酸盐通报26 (3).2007,26((3)),436-440. * |
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