CN102344157B - Method for preparing aluminium polychlorid with high content of Al13 - Google Patents
Method for preparing aluminium polychlorid with high content of Al13 Download PDFInfo
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- CN102344157B CN102344157B CN2010102412169A CN201010241216A CN102344157B CN 102344157 B CN102344157 B CN 102344157B CN 2010102412169 A CN2010102412169 A CN 2010102412169A CN 201010241216 A CN201010241216 A CN 201010241216A CN 102344157 B CN102344157 B CN 102344157B
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- 238000000034 method Methods 0.000 title claims abstract description 54
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 44
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000004411 aluminium Substances 0.000 title claims abstract description 42
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 129
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 120
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 239000000539 dimer Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 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 abstract description 3
- 239000011734 sodium Substances 0.000 claims abstract description 3
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 4
- 230000001419 dependent effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 67
- 239000000047 product Substances 0.000 description 35
- 238000002360 preparation method Methods 0.000 description 18
- 238000006116 polymerization reaction Methods 0.000 description 7
- 238000011481 absorbance measurement Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- -1 aluminium chlorohydroxide Chemical compound 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229920000592 inorganic polymer Polymers 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a method for preparing aluminium polychlorid with high content of Al13, which belongs to the technical field of environmental protection. The method is completed in the following way: the aluminium polychlorid with high content of Al13 is prepared by taking crystallized aluminium chloride, sodium hydroxide and sodium metaaluminate as raw materials. The method for preparing aluminium polychlorid with high content of Al13 comprises the following steps of: (1) taking and adding a certain amount of AlCl3 solution into a three-neck flask which is assembled with a stirring plug, a stirring rod and a condensation pipe, and heating in water bath at constant temperature; (2) taking a certain amount of NaOH solution to be preheated; (3) adding the preheated NaOH solution into the AlCl3 solution, heating, stirring, reacting, and generating dimer Al2 and polymer Al6 after the reaction of NaOH and AlCl3; (4) adding NaAlO2 solution into the mixing solution of dimer Al2 and polymer Al6, heating, stirring and reacting; and (5) after a certain reacting time, obtaining the aluminium polychlorid finished product. The invention has the advantages of simple technology, low cost, high production efficiency, no secondary pollution, excellent aluminium polychlorid performance and long stabilization time.
Description
Technical field
The present invention relates to environmental technology field, particularly a kind of high Al for the preparation of sewage flocculation treatment
13The method of content polymerize aluminum chloride.
Technical background
In inorganic polymer flocculant, aluminium based flocculating agent kind is more, and process of preparing is comparatively ripe.Polymerize aluminum chloride (Polyaluminium Chloride) wherein, be called for short PAC, the kind that, usually also referred to as aluminium chlorohydroxide, poly-oxyaluminum etc., be that the current industrial production technology is the most ripe, usefulness is the highest, is most widely used.The polymerize aluminum chloride representative be not a certain specific mineral compound, but the general name of a series of inorganic polymers.Polymerize aluminum chloride is actually the intermediate product of hydrolysis-polymerization of controlling aluminium under certain condition-precipitation process, and its chemical form belongs to multinuclear hydroxo complex and inorganic macromolecule compound, and particulate matter in water is played the efficient flocculating effect.
The development of polymerize aluminum chloride and exploitation start from the Japan in the later stage sixties, after this, many research workers of the states such as Europe, the U.S. and USSR (Union of Soviet Socialist Republics) have carried out a large amount of research and developments to its synthesis and preparation process, both at home and abroad existing a large amount of patents and bibliographical information preparation technology and the method for tens of kinds of polymerize aluminum chlorides.
Usually the method for preparing polymerize aluminum chloride has following several:
1, the production method take aluminium or active aluminium sesquioxide as raw material
Chemical process take aluminium or active aluminium sesquioxide (comprising aluminium bits, aluminium slag, aluminium ash and the active aluminium sesquioxide that is made by clay pit or calcined coal gangue) as raw material.A certain amount of aluminium or active aluminium sesquioxide are dissolved in hydrochloric acid, and along with the carrying out of reaction, the pH value of system raises gradually, and impels at a certain temperature Al (H
2O)
6 3+Hydrolysis and polyreaction occur.Can make the polymeric aluminum chlorides solution of finite concentration aluminium, certain basicity, certain polymerization degree.
Al in its product
13Content is lower, and owing to containing more detrimental impurity in raw material, the PAC foreign matter content of its production is higher.
2, the method take sodium aluminate or aluminium hydroxide as raw material.。
Sodium aluminate or aluminium hydroxide and hydrochloric acid are reacted by a certain percentage and generates polymerize aluminum chloride in reactor.The working condition that this method is produced polymerize aluminum chloride requires High Temperature High Pressure, and cost is higher, and the Al in product quality indicator
13Content can only reach 40～50%.
3, the production method take aluminum chloride as raw material.Common method mainly contains following four kinds:
1. electrolytic process
Chinese Academy of Sciences's ecological center is more to the research of this respect.Usually take aluminium sheet as anode, take stainless steel as negative electrode, aluminum chloride is electrolytic solution, passes to direct current, under the condition of low pressure, high electric current, makes polymerize aluminum chloride.Developed a kind of technology of preparing of high-quality polymerize aluminum chloride as Chinese Academy of Sciences's ecological center, this technology is take aluminum chloride as electrolytic solution, and aluminium sheet is anode, and iron plate is negative electrode, lead to the low voltage of certain hour, the direct current of large electric current, can make the liquid product of polymerize aluminum chloride.Although its basicity is higher, its composition Al that effectively flocculates
13Massfraction is 70% left and right.But the method is take aluminium sheet as anode, in the polymerize aluminum chloride of preparation, most of aluminium is from the dissolving of anode aluminium sheet, cause the production cost of this method relatively high, can't meet the needs of scale operation, and wherein still have 20%～40% aluminium to exist with aluminum ion and aluminium hydroxide form.
The teachers such as the Qu Jiuhui of Ecological Envionment Research Centre, Chinese Academy of Sciences go out polymerization 13 aluminium with the dimensional stable anode electrolytic preparation and account for the polymerize aluminum chloride of total aluminium 60～90%.But electrolysis time is longer, and generally more than 10 hours, the polymerization 13 easy deposition cathode of aluminium surfaces cause electrode passivation, and electrolytic efficiency reduces, and polymerization 13 aluminium content remain further to be improved.
2. electroosmose process.
The method is take aluminum chloride as electrolytic solution, with two anion-exchange membranes (out-phase), forms reaction chamber, and graphite cake is anode, and monolithic porous is negative electrode, and logical certain hour direct current, namely make the PAC liquid product.Though this technique is advanced, the place one's entire reliance upon quality of ion-exchange membrane of this method complex process, the quality product of manufacturing, exists easy generation film and pollute this thorny difficult problem, and the more expensive cost of PAC that causes of the price of film is higher.
3. thermal decomposition method
Take crystal aluminum chloride as raw material, also can adopt the boiling pyrolysis method to make solid PAC, crystal aluminum chloride is pyrolysis at a certain temperature, decomposite hydrogenchloride and water, polymerization becomes powdered product, and namely PAC (grog), add certain water gaging with grog and stir, be solidified into the resinousness product within a short period of time, drying, pulverizing get final product to obtain solid PAC product.
This method investment of production equipment is large, and decomposition efficiency is lower, and easily produces aluminium sesquioxide, and the polymerization degree of product is generally below 50%.
4. neutralisation.
Add the alkaline matters such as sodium hydroxide, lime, Wingdale, sodium carbonate in aluminum trichloride solution, improve the concentration of hydroxide ion,, to promote the hydrolysis of aluminum chloride, different add alkali number and can obtain different basicity products.The actual production of this method is wayward, can not realize the stoichiometric(al) of suitable basicity and aluminium active constituent, and quality product is stable not, Al
13Content is lower.The result of laboratory study is also not the same.It has been generally acknowledged that the Al of micro-alkali adding method (extremely slow add alkali speed) products obtained therefrom
13Massfraction can reach more than 80%, to have made total aluminium concentration be 0.59mol/L to Zhao Huazhang etc. by improving the means such as temperature, Al
13Massfraction reach 80.7% product.But there is report to point out slowly to add alkali and can not get Al in the situation that aluminum concentration is very low abroad
13, can obtain Al by adding fast alkali on the contrary under 90 ℃
13Massfraction be 100% PAC solution, in the use such as moonlight dropwise alkali adding method make polymerize aluminum chloride, the product that makes it is said Al
13Content is not high yet.
To sum up, the existing polymerize aluminum chloride method for preparing exists that cost is higher, product effective constituents A l
13The weak points such as not high, the easy generation pollution of lower, the total Al concentration of content.
Summary of the invention
The objective of the invention is to prepare in the polymerize aluminum chloride method for existing that existing cost is higher, product effective constituents A l
13The weak points such as not high, the easy generation pollution of lower, the total Al concentration of content, provide to have that cost is low, product effective constituents A l
13A kind of method for preparing high Al13 content polymerize aluminum chloride of the advantages such as high, the total Al concentration of content is higher, pollution is few.
The present invention is a kind of prepares high Al
13The technical scheme that the method for content polymerize aluminum chloride adopts is completed in the following way: prepare high Al
13It is raw material that the content polymerize aluminum chloride adopts crystal aluminum chloride, sodium hydroxide, sodium metaaluminate, prepares high Al
13The method of content polymerize aluminum chloride comprises the following steps:
(1) get a certain amount of AlCl
3Solution adds in the there-necked flask that stirring plug, stirring rod, prolong are housed, the water bath with thermostatic control heating;
(2) getting a certain amount of NaOH solution preheats;
(3) the NaOH solution after preheating adds AlCl
3In solution, the heated and stirred reaction, make NaOH and AlCl
3Reaction generates dimer Al
2With polymer Al
6
(4) to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2Solution, carry out the heated and stirred reaction;
(5) after the reaction certain hour, obtain the polymerize aluminum chloride finished product.
Wherein the part principle of step (3), step (4) is seen following reaction:
Dimer Al
2, polymer Al
6Building-up reactions: AlCl
3+ NaOH → Al
2+ Al
6
Al
13Form reaction: Al
2+ Al
6+ Al (OH)
4 -→ Al
13
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, AlCl
3Solution is that employing concentration is the AlCl of 0.4～0.6mol/L
3Solution, the temperature of water bath with thermostatic control heating is 80～90 ℃.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, NaOH solution is that employing concentration is the NaOH solution of 0.6～0.8mol/L, and pre-warmed temperature is 80～90 ℃.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, the NaOH solution after preheating adds AlCl
3Amount in solution is according to mole ratio n (AlCl
3): n (NaOH) is 1: 1.5～1.6 ratio-dependent.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, the NaOH solution after preheating adds AlCl
3In solution, the bath temperature of the heated and stirred reaction of carrying out is 80～90 ℃, and stirring velocity is 100～120r/min, and the time of heated and stirred reaction is 25～35min.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2Solution is that employing concentration is the NaAlO of 0.2～0.4mol/L
2Solution, to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2The amount of solution is according to mole ratio n (AlCl
3): n (NaAlO
2) be 1: 0.4～0.5 ratio-dependent.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2The method of solution is to adopt the method that slowly drips to carry out, and the bath temperature of the heated and stirred reaction of carrying out is 80～90 ℃, and stirring velocity is 130～150r/min, and time for adding is 20～30min.
At the high Al of above-mentioned preparation
13In the method for content polymerize aluminum chloride, to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2After the dropwise reaction that solution carries out is complete, after continuing reaction 5～10min, obtain Al
13Content 〉=97%, the liquid aluminium polychloride of steady time 〉=24 month.
The present invention is from Al
13Form this angle of principle and set out, first by certain ratio, NaOH is added AlCl
3In solution, the pH value of regulator solution is with the Al of synthesizing octahedral structure
2And Al
6Add a certain amount of NaAlO again in solution
2Solution, due to NaAlO
2In Al be Al (OH) with positive tetrahedron
4 -Form exists, can be as core, with the Al of the octahedral structure that generates in solution
2And Al
6Reaction generates Al
13.So not only passablely obtain high Al
13The liquid aluminium polychloride of content, high Al total concn, and realized the efficient and rational utilization of resource, reduced and produced the environmental pollution that causes in polymerize aluminum chloride, meet the continuable development principle of " energy-saving and environmental protection ".
The present invention compares with the existing method for preparing polymerize aluminum chloride, has following outstanding feature:
1, simple, the low production cost of technical process, production efficiency are high, non-secondary pollution.
2, prepared polymerize aluminum chloride superior performance, wherein Al
13Content 〉=97%, basicity 〉=85%.Steady time 〉=24 of product month in addition.
Embodiment
Below by embodiment, the present invention is made further instructions.
Embodiment 1
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.4mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 90 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.5, gets a certain amount of 0.6mol/L NaOH solution and preheats, and bath temperature is 90 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 90 ℃, stirring velocity is 100r/min;
(4) after question response 35min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.5, get a certain amount of 0.2mol/LNaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 90 ℃, and stirring velocity is 130r/min, and time for adding is 30min;
(5) after dropwise reaction is complete, continue reaction 5min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 94.20%, and basicity is 85.3%.
Embodiment 2
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.5mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 85 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.6, gets a certain amount of 0.8mol/L NaOH solution and preheats, and bath temperature is 85 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 85 ℃, stirring velocity is 120r/min;
(4) after question response 30min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.4, get a certain amount of 0.4mol/LNaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 85 ℃, and stirring velocity is 150r/min, and time for adding is 20min;
(5) after dropwise reaction is complete, continue reaction 10min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 97.40%, and basicity is 86.7%.
Embodiment 3
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.6mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 80 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.55, gets a certain amount of 0.7mol/L NaOH solution and preheats, and bath temperature is 80 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 80～90 ℃, stirring velocity is 110r/min;
(4) after question response 25min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.45, get a certain amount of 0.3mol/LNaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 80 ℃, and stirring velocity is 140r/min, and time for adding is 25min;
(5) after dropwise reaction is complete, continue reaction 8min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 95.10%, and basicity is 85.8%.
Embodiment 4
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.45mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 90 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.6, gets a certain amount of 0.7mol/L NaOH solution and preheats, and bath temperature is 90 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 90 ℃, stirring velocity is 120r/min;
(4) after question response 35min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.5, get a certain amount of 0.4mol/LNaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 90 ℃, and stirring velocity is 150r/min, and time for adding is 30min;
(5) after dropwise reaction is complete, continue reaction 10min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 96.10%, and basicity is 86.4%.
Embodiment 5
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.55mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 80 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.5, gets a certain amount of 0.6mol/L NaOH solution and preheats, and bath temperature is 80 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 80～90 ℃, stirring velocity is 100r/min;
(4) after question response 30min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.4, get a certain amount of 0.2NaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 80 ℃, and stirring velocity is 140r/min, and time for adding is 25min;
(5) after dropwise reaction is complete, continue reaction 5min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 94.50%, and basicity is 85.9%.
Embodiment 6
A kind ofly prepare high Al
13The method of content polymerize aluminum chloride, its preparation process is:
(1) get a certain amount of 0.6mol/LAlCl
3Solution is in being equipped with the there-necked flask that stirs plug, stirring rod, prolong, and water bath with thermostatic control is heated to 85 ℃;
(2) according to mole ratio n (AlCl
3): n (NaOH) is the ratio of 1: 1.57, gets a certain amount of 0.65mol/L NaOH solution and preheats, and bath temperature is 85 ℃;
(3) the NaOH solution after preheating adds AlCl
3In solution, heated and stirred, bath temperature is 85 ℃, stirring velocity is 110r/min;
(4) after question response 25min, according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio of 1: 0.45, get a certain amount of 0.25mol/LNaAlO
2Solution slowly is added drop-wise in mixing solutions, heated and stirred, and bath temperature is 85 ℃, and stirring velocity is 150r/min, and time for adding is 25min;
(5) after dropwise reaction is complete, continue reaction 10min, obtain the liquid aluminium polychloride finished product.
The liquid aluminium polychloride finished product is carried out absorbance measurement, and the form of calculating Al distributes.Result is: Al in the polymerize aluminum chloride finished product
13Content is 96.80%, and basicity is 87.3%.
Claims (3)
1. one kind prepares high Al
13The method of content polymerize aluminum chloride is characterized in that: prepare high Al
13The raw material of content polymerize aluminum chloride adopts crystal aluminum chloride, sodium hydroxide, sodium metaaluminate, prepares high Al
13The step of content polymerize aluminum chloride is as follows:
⑴ get the AlCl that a certain amount of concentration is 0.4～0.6mol/L
3Solution adds in the there-necked flask that stirring plug, stirring rod, prolong are housed, the water bath with thermostatic control heating, and the temperature of water bath with thermostatic control heating is 80～90 ℃;
⑵ get a certain amount of concentration is that the NaOH solution of 0.6～0.8mol/L preheats, and pre-warmed temperature is 80～90 ℃;
⑶ the NaOH solution after will preheat adds AlCl
3In solution, the heated and stirred reaction, make NaOH and AlCl
3Reaction generates dimer Al
2With polymer Al
6, wherein, the NaOH solution after preheating adds AlCl
3Amount in solution is according to mole ratio n (AlCl
3): n (NaOH) is the ratio-dependent of 1:1.5～1.6, and the bath temperature of the heated and stirred reaction of carrying out is 80～90 ℃, and stirring velocity is 100～120r/min, and the time of heated and stirred reaction is 25～35min;
⑷ to dimer Al
2With polymer Al
6Mixing solutions in to add concentration be the NaAlO of 0.2～0.4mol/L
2Solution, carry out the heated and stirred reaction, wherein, adds NaAlO
2The amount of solution is according to mole ratio n (AlCl
3): n (NaAlO
2) be the ratio-dependent of 1:0.4～0.5, the bath temperature of the heated and stirred reaction of carrying out is 80～90 ℃, stirring velocity is 130～150r/min;
⑸ after reaction certain hour, obtain the polymerize aluminum chloride finished product.
2. a kind of high Al for preparing according to claim 1
13The method of content polymerize aluminum chloride is characterized in that: to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2The method of solution is to adopt the method that slowly drips to carry out, and time for adding is 20～30min.
3. a kind of high Al for preparing according to claim 1
13The method of content polymerize aluminum chloride is characterized in that: to dimer Al
2With polymer Al
6Mixing solutions in add NaAlO
2After the dropwise reaction that solution carries out is complete, after continuing reaction 5～10min, obtain Al
13Content 〉=97%, the liquid aluminium polychloride of steady time 〉=24 month.
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| US5997838A (en) * | 1995-09-18 | 1999-12-07 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
| CN101264964A (en) * | 2007-04-26 | 2008-09-17 | 北京科技大学 | Method for preparing high-A113 content high-concentration polymerized aluminum water solution and device thereof |
| CN101279756A (en) * | 2007-04-05 | 2008-10-08 | 江苏宜净环保有限公司 | Preparation of polyaluminium sulfate |
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| US5997838A (en) * | 1995-09-18 | 1999-12-07 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
| CN101279756A (en) * | 2007-04-05 | 2008-10-08 | 江苏宜净环保有限公司 | Preparation of polyaluminium sulfate |
| CN101264964A (en) * | 2007-04-26 | 2008-09-17 | 北京科技大学 | Method for preparing high-A113 content high-concentration polymerized aluminum water solution and device thereof |
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