CN111320194B - Preparation method of aluminum glue and polyaluminium chloride - Google Patents
Preparation method of aluminum glue and polyaluminium chloride Download PDFInfo
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- CN111320194B CN111320194B CN202010333301.1A CN202010333301A CN111320194B CN 111320194 B CN111320194 B CN 111320194B CN 202010333301 A CN202010333301 A CN 202010333301A CN 111320194 B CN111320194 B CN 111320194B
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Abstract
A preparation method of aluminum paste and polyaluminium chloride belongs to the technical field of preparation of aluminum paste and polyaluminium chloride. Mainly provides a high-activity aluminum adhesive and a preparation method of high-purity, low-energy-consumption and waste-residue-free polyaluminum chloride. Neutralizing the pH value of aluminum salt solution or dilute acid and sodium aluminate, potassium aluminate or dilute alkali solution to 4-8 within a certain time to prepare high-activity alumina gel, and then preserving the temperature of the alumina gel and the one-step solution for preparing the polyaluminium chloride at 65-95 ℃ for 0.5-2 h to prepare the polyaluminium chloride with the basicity of below 90%. The alumina gel prepared by the method is high-purity amorphous hydrated alumina, and when the polyaluminium chloride is further prepared, the solution is clear and transparent, no filter pressing or sedimentation is needed, no waste residue is generated, the preparation process does not need cooling, the production time is short, the energy consumption is low, and the purity of the finished product polyaluminium chloride is high.
Description
Technical Field
A preparation method of aluminum paste and polyaluminium chloride belongs to the technical field of preparation of aluminum paste and polyaluminium chloride.
Background
Polyaluminum chlorides of the PAC code, also commonly known as water-purifying agents or coagulants, are interposed between AlCl 3 And Al (OH) 3 A water-soluble inorganic high molecular polymer with a chemical general formula of Al n (OH) m Cl (3n-m) It is a high-efficiency and cheap inorganic polymer coagulant. It is widely applied to water treatment and other industries.
The production method of the polyaluminium chloride mainly comprises a one-step method and a two-step method:
one-step method: reacting aluminum hydroxide and hydrochloric acid in a reaction kettle at high temperature and under pressure, and filtering to obtain liquid polyaluminum chloride. In the one-step process, along with the hydrolysis, the acidity of the solution is increased, and the reaction reaches balance, so that the method can only synthesize polyaluminium chloride with low basicity (about 50 percent), and has poor coagulation performance; furthermore, the aluminum hydroxide must be kept in excess, and the excess aluminum hydroxide needs to be filtered off after the reaction is completed.
A two-step method: firstly, aluminium hydroxide or aluminium-containing raw material and hydrochloric acid are heated and reacted (normal pressure or pressure) to obtain a one-step solution with basicity of about 7-20%, then an alkalizer (basicity regulator) is added to make reaction to raise basicity, and after filtering, the liquid aluminium polychloride with basicity of 60-90% is obtained. The basifying agent currently used in large amounts in industry is calcium aluminate powder. The polyaluminium chloride produced by the method has high impurity content and even contains a considerable amount of heavy metal ions such as lead and the like. And the high-purity calcium aluminate powder is expensive. Meanwhile, the over-sintered inert calcium aluminate powder must be filtered and removed, the prepared polyaluminium chloride contains a large amount of unreacted calcium aluminate, the solution is turbid, and the solution needs to be further filtered, so that a large amount of industrial waste residues are generated and cannot be recycled, and the problem of waste residue treatment is always a great problem in industry. In addition, because the calcium aluminate powder reacts violently with the one-step liquid, the one-step liquid must be cooled to below 70-80 ℃ before the alkalizer is added. Thereby consuming time and heat.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a high-activity aluminum adhesive and a production method of polyaluminium chloride with high purity, short reaction time and low waste residue.
The technical scheme adopted by the invention for solving the technical problem is as follows: the preparation method of the aluminum paste is characterized by comprising the following steps: comprises the following steps:
1) quickly adding an aluminum salt or polyaluminium chloride solution with the alumina mass content of 3-6% into sodium metaaluminate or potassium metaaluminate with the alumina mass content of 3-7% or sodium hydroxide or potassium hydroxide solution with the mass fraction of 5-10%, quickly stirring, and neutralizing within 5-40 minutes until the pH value is 4-8;
2) and filtering the obtained filter residue to obtain the aluminum cement.
The invention also provides a preparation method of the aluminum adhesive, which is characterized by comprising the following steps: comprises the following steps:
1) quickly adding dilute hydrochloric acid or nitric acid or sulfuric acid with the mass fraction of 6-10% into sodium aluminate or potassium aluminate solution with the mass content of alumina of 3-7%, quickly stirring, and neutralizing within 5-40 minutes until the pH value is 4-8;
2) and filtering the obtained filter residue to obtain the aluminum cement.
In the two preparation methods of the alumina gel, if the reaction speed is too high, the amorphous hydrated alumina of the effective component in the alumina gel can be quickly separated out and agglomerated into blocks, if the reaction speed is too low, the crystallization state conversion occurs, and the aluminum hydroxide precipitation appears in the filter residue, so that a large amount of precipitation appears in the reaction liquid in the next step or the hydrated alumina which does not participate in the reaction causes the turbidity of the solution.
The reaction equation for preparing the aluminum paste is as follows: 3NaAlO 2 +AlCl 3 =2Al 2 O 3 (aq)+3NaCl。
The purity and activity of amorphous hydrated alumina in the finally prepared aluminum gel are extremely high, and free chloride ions and sodium ions or potassium ions can be obtainedThe active ingredients of the alumina gel prepared by the method are completely amorphous hydrated alumina, neither crystalline aluminum hydroxide or aggregated blocks nor partially crystalline hydrated alumina, nor completely free aluminum salt solution, so that the active ingredients of the alumina gel can be separated from free H in the process of preparing polyaluminium chloride + The reaction is rapid and sufficient, the acidity of the solution is reduced, and the high-basicity polyaluminium chloride is obtained.
Preferably, the time for the neutralization reaction of the two preparation methods is 7.5-28.5 minutes.
Preferably, the neutralization reaction end point in the step 1) in the two preparation methods is that the pH value of the solution is 5-7.
The application also relates to a preparation method of the polyaluminium chloride, which comprises the following steps:
1) mixing hydrochloric acid with the mass fraction of 15% -30% with aluminum hydroxide or aluminum-containing raw materials to obtain H + With Al 3+ Heating and reacting at the molar ratio of 2.8-3.1: 1 under normal pressure or pressurization, and filtering to obtain one-step liquid with the basicity of 7-20%;
2) adding the aluminum glue prepared by the preparation method into the one-step liquid according to the basicity of the required polyaluminium chloride and the weight ratio of the aluminum glue to the one-step liquid of 0.25-1.6: 1, wherein the aluminum glue is positively correlated according to the target basicity, and the heat is preserved for 0.5-2 hours at 65-95 ℃ to prepare the polyaluminium chloride with the basicity of 60-90%; the polyaluminium chloride with any basicity less than 90 percent can be synthesized by adjusting the adding amount of the alumina gel. As the addition amount of the aluminum paste is increased, the basicity of the obtained polyaluminum chloride is increased.
Preferably, the heat preservation temperature is 80-90 ℃.
Compared with the prior art, the invention has the following beneficial effects: in the process, the alumina gel has high purity and activity, and can quickly and fully react with free H in reaction liquid + The reaction is carried out, the acidity of the solution is reduced, and the reaction is continued, therefore, the processThe method can synthesize any basicity polyaluminium chloride with the basicity of less than 90 percent, and the alumina gel can completely participate in the reaction, does not generate industrial waste residue like a calcium aluminate two-step method, can realize the slagging-free production of the polyaluminium chloride, and simultaneously does not influence the purity of the polyaluminium chloride when the polyaluminium chloride synthesized by the one-step liquid reaction is carried out because the alumina gel does not contain other metal ions except aluminum and crystalline hydrated alumina.
On the other hand, in order to ensure the reactivity of the calcium aluminate powder in the traditional process, the calcium aluminate powder contains free calcium oxide, when the basicity is adjusted by using the calcium aluminate powder, the temperature of one-step liquid must be reduced to below 70-80 ℃, otherwise, the reaction is violent, the slurry can boil, and the production is safe in crisis.
In conclusion, the aluminum glue prepared by the preparation method has the characteristic of high activity, and the prepared polyaluminium chloride has the advantages of high purity, high synthesis speed, low energy consumption and no slag.
Detailed Description
Examples 1 and 9 are preferred embodiments of the present invention, and the present invention will be further described with reference to the following examples.
All of the following 10% alumina content aluminum salt solutions or low basicity polyaluminium chlorides were obtained from polyaluminium chloride one-step liquids produced by Tianze water purification materials, Inc.
Example 1
A preparation method of aluminum glue.
A sodium metaaluminate solution having an alumina content of 6.4% was prepared by adding 1548g of water to 260g of aluminum hydroxide solids and 600g of 30% sodium hydroxide solution.
1500g of 10% aluminum salt solution with an alumina content was diluted to 6% aluminum salt solution with 1000g of water.
And (3) inserting a real-time pH meter into the sodium metaaluminate solution, adding the aluminum salt solution, rapidly stirring, finally adding 1275g of the aluminum salt solution to the pH value of 7 within 15 minutes, filtering, and collecting filter residues to obtain the alumina gel.
Example 2
A preparation method of aluminum glue.
A potassium metaaluminate solution having an alumina content of 3% was prepared by adding 4300g of water to 260g of aluminum hydroxide solid and 600g of 30% potassium hydroxide solution.
4000g of 10% alumina salt solution was diluted with 2667g of water to give 6% alumina salt solution.
And (3) inserting a real-time pH meter into the potassium metaaluminate solution, adding the aluminum salt solution, rapidly stirring, finally adding 1380g of the aluminum salt solution to the pH value of 6 within 5 minutes, filtering, and collecting filter residues to obtain the aluminum adhesive.
Example 3
A preparation method of aluminum glue.
A sodium metaaluminate solution of 3% alumina content was prepared by adding 4300g of water to 260g of aluminum hydroxide solids and 600g of 30% potassium hydroxide solution.
To 4000g of 10% alumina content aluminum salt solution was added 2667g of water to dilute the solution to 6% alumina content aluminum salt solution.
And inserting a real-time pH meter into the sodium metaaluminate solution, adding the aluminum salt solution, stirring quickly, finally adding 1620g of the aluminum salt solution to the pH value of 4 within 30 minutes, filtering, and collecting filter residues to obtain the aluminum glue.
Example 4
A preparation method of aluminum glue.
A sodium metaaluminate solution having an alumina content of 6.4% was prepared by adding 1548g of water to 260g of aluminum hydroxide solids and 600g of 30% sodium hydroxide solution.
And (3) inserting a real-time pH meter into the sodium metaaluminate solution, adding 10% dilute hydrochloric acid solution, rapidly stirring, adding 1645g of dilute hydrochloric acid solution until the pH value is 5 after 15 minutes, filtering, and collecting filter residues to obtain the alumina gel.
Example 5
Other conditions of this example were the same as in example 4, and only the dilute hydrochloric acid solution was changed to a dilute nitric acid solution.
Example 6
Other conditions of this example were the same as in example 4 except that the 10% diluted hydrochloric acid solution was changed to a 5% diluted sulfuric acid solution.
Comparative example 1
The other conditions of this comparative example were the same as in example 1, and the time taken to add only the aluminum salt solution was set to 3 minutes.
Comparative example 2
The other conditions of this comparative example were the same as in example 1, and only the time taken to add the aluminum salt solution was set to 40 minutes.
Comparative example 3
The conditions for preparing the sodium metaaluminate solution in the comparative example are the same as those of the example 1, 800g of the prepared sodium metaaluminate solution with the alumina content of 6.4 percent is taken, the aluminum salt solution prepared under the conditions the same as those of the example 1 is added, 2400g of the aluminum salt solution is finally added within 15 minutes until the pH value is 3, and the aluminum colloid is obtained by filtering and collecting filter residues.
Comparative example 4
Other conditions of this comparative example were the same as in example 1, except that the aluminum salt solution having an alumina content of 6% was added in a total amount of 1400g and the final pH was 9.
Comparative example 5
A sodium metaaluminate solution of 8% alumina content was prepared by adding 1075g of water to 260g of aluminum hydroxide solids and 600g of 30% sodium hydroxide solution.
1500g of 10% aluminum salt solution with an alumina content was diluted with 1000g of water to give an aluminum salt solution with an alumina content of 6%.
Inserting a real-time pH meter into the sodium metaaluminate solution, slowly adding the aluminum salt solution while stirring quickly, finally adding 1727g of the aluminum salt solution within 15 minutes until the pH value is 7, filtering, and collecting filter residues to obtain the aluminum glue.
Comparative example 6
6880g of water was added to 260g of the aluminum hydroxide solid and 600g of 30% sodium hydroxide solution to make a sodium metaaluminate solution with 2% alumina content.
1500g of 10% aluminum salt solution with an alumina content was diluted with 1000g of water to give an aluminum salt solution with an alumina content of 6%.
Inserting a real-time pH meter into the sodium metaaluminate solution, slowly adding the aluminum salt solution while stirring quickly, finally adding 1727g of aluminum salt solution within 15 minutes until the pH value is 7, filtering, and collecting filter residues to obtain the aluminum gel.
Comparative example 7
A preparation method of aluminum glue.
A sodium metaaluminate solution having an alumina content of 6.4% was prepared by adding 1548g of water to 260g of aluminum hydroxide solids and 600g of 30% sodium hydroxide solution.
1500g of 10% aluminum salt solution with an alumina content was diluted with 643g of water to give a 7% aluminum salt solution with an alumina content.
Inserting a real-time pH meter into the sodium metaaluminate solution, slowly adding the aluminum salt solution while rapidly stirring, finally adding 2130g of the aluminum salt solution within 15 minutes until the pH value is 8, filtering, and collecting filter residues to obtain the aluminum glue.
Comparative example 8
A preparation method of aluminum glue.
A sodium metaaluminate solution having an alumina content of 6.4% was prepared by adding 1548g of water to 260g of aluminum hydroxide solids and 600g of 30% sodium hydroxide solution.
1500g of 10% aluminum salt solution with an alumina content was diluted with 6000g of water to give an aluminum salt solution with an alumina content of 2%.
Inserting a real-time pH meter into the sodium metaaluminate solution, slowly adding the aluminum salt solution while rapidly stirring, finally adding 7100g of the aluminum salt solution within 28 minutes until the pH value is 8, filtering, and collecting filter residues to obtain the aluminum glue.
Examples 7 to 10 and comparative example 9
The preparation method of the polyaluminum chloride comprises the following steps:
1) using 15% -30% hydrochloric acid and aluminium hydroxide or aluminium-containing raw material to make H in the solution + With Al 3+ Heating and reacting at the molar ratio of 2.8-3.1: 1 under normal pressure or pressurization, and filtering to obtain one-step liquid with the basicity B of 7-20%;
2) the alumina cement prepared by the preparation method of the embodiment 1-4 is added into the one-step solution, the heat preservation time t is 0.5-2 hours, the heat preservation temperature is 65-95 ℃, and the proportion is in direct proportion correlation according to the target basicity.
The one-step liquid salt basicity, reaction conditions and final polyaluminium chloride basicity used in each example are shown in table 1 below.
Product detection:
and (3) detecting the activity of the aluminum paste: and (3) observing the turbidity and transparency degree of the finally prepared polyaluminum chloride by naked eyes, wherein the higher the activity is, the more uniform, clear and transparent the polyaluminum chloride prepared in the next step is.
And (3) detecting the components of the aluminum paste: the purity is determined by X-ray diffraction patterns, in which diffraction peaks appear if crystalline transformation occurs.
And the mass fractions of impurities such as the salinity of the polyaluminium chloride, alumina, ferric oxide, lead and the like are measured by adopting a GB15892-2009 detection method.
The calcium chloride content was determined by EDTA titration.
And (3) detection results:
the final polyaluminum chloride solution of the aluminum cement obtained in the embodiments 1-6 is clear and transparent and has no suspended matters in the activity detection of the aluminum cement, and the aggregation phenomenon of small blocks in filter residues is more obvious along with the higher neutralization speed.
Comparative example 1 during the preparation of the aluminum paste, the aluminum paste is rapidly precipitated, the stirring speed is passively reduced, and the aluminum paste is coagulated into lumps; after the aluminum glue prepared in the comparative example 3 is filtered, aluminum ions appear in the filtrate, which proves that the aluminum ions do not participate in the reaction and the waste is serious; comparative example 4 polyaluminum chloride prepared after standing for 22 hours was jellified.
Compared with the comparative examples 6 and 8, the alumina gel has good activity, but the consumed water amount is increased, so that waste is caused; comparative examples 5 and 7, the slurry coagulated into lumps during the preparation of the aluminum paste. The alumina sol prepared in comparative example 2 became less active, namely: the liquid polyaluminum chloride slurry prepared further was cloudy.
The alumina contents in the alumina gels obtained in examples 1 to 6 are respectively as follows:
example 1 (Al) 2 O 3 %）：49.3%；
Example 2 (Al) 2 O 3 %）：44.5%；
Example 3 (Al) 2 O 3 %）：50.1%；
Example 4 (Al) 2 O 3 %）：48.9%；
Example 5 (Al) 2 O 3 %）：49.7%；
Example 6 (Al) 2 O 3 %）：50.3%。
Table 2 shows the performance test results of the examples 7-10 and the comparative example 9 on the conventional polyaluminum chloride prepared by a one-step method and a two-step method.
It can be seen that the polyaluminium chloride prepared by the alumina gel prepared by the method of the invention has no white turbidity or precipitation visible to the naked eye.
Comparative example 9 is a conventional method for preparing an aluminum paste using calcium aluminate powder, which produces about 10% of non-reusable slag, whereas the present application has substantially no non-reusable slag in the preferred range.
The insoluble alumina gel in the solution is most uniform in macroscopic view of the alumina gel solution obtained in the embodiment 1, the filter residue particles are fine and uniform, the polyaluminum chloride solution obtained in the next preparation process of the polyaluminum chloride is clear and transparent, no small solid particles are precipitated on the wall of the container, and the activity of the alumina gel is good and the reaction with the low-basicity polyaluminum chloride is most sufficient. The higher the adding speed in the preparation process of the aluminum adhesive, the higher the viscosity of the slurry, the lower the adding speed, the conversion to a crystalline form is carried out, even small sand-shaped particles are generated, the prepared polyaluminium chloride is possibly turbid, and when the neutralization time is within the range of 7.5-28.5 minutes, the properties of the aluminum adhesive and the reaction effect of preparing the high-basicity polyaluminium chloride in the second step are most consistent with the expected effect.
The polyaluminium chloride prepared by the method can reach the high basicity of a two-step method, and can also obtain the characteristic of no other impurities in the one-step method. Meanwhile, the whole process does not need cooling. Waste residue which can not be recycled is hardly generated in the preparation process, and the preparation method is applied to industrial production, can greatly improve the product quality, saves the production energy consumption, improves the production efficiency and has outstanding significance on environmental protection.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (4)
1. The preparation method of the aluminum paste is characterized by comprising the following steps: comprises the following steps:
1) adding an aluminum salt or polyaluminum chloride solution with the alumina mass content of 3-6% into a sodium metaaluminate or potassium metaaluminate solution with the alumina mass content of 3-7% or a sodium hydroxide or potassium hydroxide solution with the alumina mass content of 5-10%, rapidly stirring, and neutralizing within 7.5-28.5 minutes until the pH value is 5-7;
2) and filtering the obtained filter residue to obtain the alumina gel.
2. The preparation method of the aluminum paste is characterized by comprising the following steps: comprises the following steps:
1) quickly adding dilute hydrochloric acid, nitric acid or sulfuric acid with the mass fraction of 6-12% into sodium aluminate or potassium aluminate solution with the mass content of alumina of 3-7%, quickly stirring, and neutralizing until the pH value is 5-7 within 7.5-28.5 minutes;
2) and filtering the obtained filter residue to obtain the aluminum cement.
3. A preparation method of polyaluminum chloride is characterized in that: comprises the following steps:
1) mixing 15-30% hydrochloric acid with aluminum-containing raw material to obtain H + With Al 3+ Heating and reacting at the molar ratio of 2.8-3.1: 1 under normal pressure or pressurization, and filtering to obtain one-step liquid with the basicity of 7-20%;
2) adding the aluminum adhesive prepared by the preparation method of any one of claims 1 or 2 into the one-step solution according to the target basicity in a weight ratio of 0.25-1.6: 1, wherein the required weight of the aluminum adhesive is in direct proportion to the target basicity, and the heat is preserved for 0.5-2 hours at 65-95 ℃ to obtain the polyaluminum chloride.
4. The method for preparing polyaluminum chloride according to claim 3, wherein: the heat preservation temperature in the step 2) is 80-90 ℃.
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