CN112299463B - Method for producing polyaluminium chloride by constant temperature and constant acid - Google Patents
Method for producing polyaluminium chloride by constant temperature and constant acid Download PDFInfo
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- CN112299463B CN112299463B CN202011119459.5A CN202011119459A CN112299463B CN 112299463 B CN112299463 B CN 112299463B CN 202011119459 A CN202011119459 A CN 202011119459A CN 112299463 B CN112299463 B CN 112299463B
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- C01—INORGANIC CHEMISTRY
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- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
Abstract
The invention discloses a production method for producing polyaluminium chloride by constant temperature and constant acid, which comprises the following steps: step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion; step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously; and step S3: simultaneously adding water for spraying; and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the indexes of the mixed liquid meet the planned proportioning requirement; step S5: when the mixed liquid index is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, transferring the mixed liquid into a reaction kettle; step S6: according to the transfer amount and the detection result, hydrochloric acid and the mixed solution are continuously added in proportion for reaction, and the qualified product is continuously removed. The invention has the advantages of more uniform and sufficient reaction, reaction time reduction, effective reduction of reaction heat loss, sufficient reaction, less energy consumption, effective reduction of residue amount, difficult occurrence of too large local temperature difference and defective rate reduction.
Description
Technical Field
The invention relates to the technical field of polyaluminium chloride production, in particular to a production method for producing polyaluminium chloride by constant temperature and constant acid.
Background
The production flow and the method for producing the polyaluminium chloride in the current industry are as follows: firstly, adding hydrochloric acid and water in proportion in a reaction kettle for stirring, starting to gradually add raw materials (calcium aluminate powder, bauxite and the like) containing aluminum oxide in proportion after uniformly stirring, still stirring in the process, generating temperature rise in the reaction, needing operations such as steam pumping cooling and the like, then reacting for 2-3 hours at a relatively constant temperature of about 100 ℃, sampling, adjusting slag removal according to needs, and warehousing.
However, the prior art has the following disadvantages in the production process:
1. as a solid powdery aluminum-containing raw material, a large amount of heat can be generated at a contact point in the reaction process of the solid powdery aluminum-containing raw material and a diluted hydrochloric acid solution, so that raw material powder is easily pumped away by an exhaust fan along with hot gas, raw material loss is caused, the difficulty of a rear-end cooling system is increased, and the overhauling frequency is high;
2. the product belongs to a flocculating agent, and the product is easy to flocculate solid powder serving as flocculated matters in the reaction process to form large-particle precipitates which are finally treated as sediments, so that the consumption of raw materials is increased, and the treatment difficulty of waste residues is increased;
3. defective products are easily generated and adjustment is difficult.
4. The production is not continuous, which causes high energy consumption, unstable product quality and large fluctuation.
Therefore, a constant temperature and constant acid production method for producing the polyaluminium chloride is provided for solving the problems.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for producing polyaluminium chloride by constant temperature and constant acid.
The invention provides a production method for producing polyaluminum chloride by constant temperature and constant acid, which comprises the following steps:
step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion;
step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously;
and step S3: simultaneously adding water for spraying;
and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the index of the mixed liquid meets the planned proportioning requirement;
step S5: when the index of the mixed liquid is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, the mixed liquid is transferred to a reaction kettle;
step S6: adding hydrochloric acid in proportion according to the transfer amount and the detection result to react;
step S7: controlling the initial reaction temperature of the reaction kettle at 40 ℃;
step S8: after 50% of required hydrochloric acid is added into the reaction kettle, the temperature of the reaction kettle gradually rises, the temperature of the reaction kettle is observed in real time in the process, and the heating is stopped in time when the temperature of the reaction kettle is overhigh;
step S9: when the temperature in the reaction kettle rises to 95 ℃, controlling the acid adding speed, and not enabling the temperature to rise to exceed 105 ℃;
step S10: keeping the reaction kettle at 103 ℃ for stable reaction for 1-2 hours;
step S11: sampling and detecting whether the product is qualified;
step S12: quantitatively removing the finished product from the bottom of the reaction kettle after the product is qualified, and then quantitatively and continuously adding the mixed solution and the hydrochloric acid to balance the inlet and outlet amount;
step S13: and after the product is detected to be qualified, deslagging, cooling and then feeding into a finished product.
Preferably, in the step S1, the raw materials of the polyaluminum chloride include aluminum-containing powder raw materials, hydrochloric acid, and water, and the mixture ratio is 1: (2-3): (0.6-0.8), wherein the concentration of the hydrochloric acid is 28-36%.
Preferably, in the step S7, when the initial temperature of the reaction kettle does not reach 40 ℃, the reaction kettle is heated by a steam heating method.
Preferably, in the step S7, when the initial reaction temperature of the reaction kettle is controlled, the temperature error range is plus or minus 1 ℃.
Preferably, in the step S8, heating is stopped when the temperature of the mixed liquid in the reaction kettle is higher than 103 ℃.
Preferably, in the step S9, after the temperature in the reaction kettle rises to 95 ℃, the adding rate of the hydrochloric acid is controlled to be 1-2% per minute of the total volume.
Preferably, in the step S10, the error of the stable reaction temperature of the reaction kettle is controlled to be plus or minus 2 ℃.
Preferably, in the step S11, the product qualification standard is 10% ± 0.5% aluminum and the basicity is 30-9.
Preferably, the material inlet and outlet in the step S12 need to reach a balance.
The production method for producing the polyaluminum chloride by the constant temperature and the constant acid has the beneficial effects that:
(1) In order to accelerate the reaction of products, reduce the production period, reduce the energy consumption and have strong continuous production type. The production process of the product is groped and tested, and finally the original production flow is changed: firstly, dissolving solid powdery aluminum-containing raw material in a dissolving tank, and adding water and the raw material according to a proportion;
(2) Stirring to form a solution, pumping into a reaction kettle, gradually adding hydrochloric acid in proportion, stirring simultaneously, reacting at about 100 ℃ for 1-2 hours after the hydrochloric acid is added, adjusting according to a detection result, adding a mixed solution and hydrochloric acid according to the output of a finished product to reach the balance of the reaction kettle in and out, removing the product to remove slag, cooling, and then feeding into a finished product tank;
the invention has the advantages of more uniform and sufficient reaction, energy consumption reduction, continuous production, loss reduction effect on materials during steam extraction and cooling in the heating process, difficulty in causing large-particle flocculate, sufficient reaction, effective reduction of residue amount, difficulty in causing too large local temperature difference and reduction of defective rate.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
A production method for producing polyaluminum chloride by constant temperature and constant acid comprises the following steps:
step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion;
step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously;
and step S3: simultaneously adding water for spraying;
and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the index of the mixed liquid meets the planned proportioning requirement;
step S5: when the index of the mixed liquid is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, transferring the mixed liquid into a reaction kettle;
step S6: adding hydrochloric acid in proportion according to the transfer amount and the detection result to react;
step S7: the initial reaction temperature of the reaction kettle is controlled at 40 ℃;
step S8: after 50% of required hydrochloric acid is added into the reaction kettle, the temperature of the reaction kettle gradually rises, the temperature of the reaction kettle is observed in real time in the process, and the heating is stopped in time when the temperature of the reaction kettle is overhigh;
step S9: when the temperature in the reaction kettle rises to 95 ℃, controlling the acid adding speed, and preventing the temperature from rising to more than 105 ℃;
step S10: keeping the reaction kettle to react stably for 1 hour at 103 ℃;
step S11: sampling and detecting whether the product is qualified;
step S12: quantitatively removing the finished product from the bottom of the reaction kettle after the product is qualified, then quantitatively and continuously adding the mixed solution and the hydrochloric acid, and balancing the inlet and outlet amount;
step S13: and after the product is detected to be qualified, deslagging, cooling and then feeding into a finished product.
In this embodiment, in step S1, the raw materials of the polyaluminum chloride include aluminum-containing powder, hydrochloric acid, and water, and the mixture ratio is 1:2:0.6, wherein the concentration of hydrochloric acid is 32%, in step S7, when the initial temperature of the reaction kettle does not reach 40 ℃, heating is carried out in a steam heating mode, in step S7, when the initial reaction temperature of the reaction kettle is controlled, the temperature error range is plus or minus 1 ℃, in step S8, heating is stopped when the temperature of the mixed liquid in the reaction kettle is higher than 103 ℃, in step S9, after the temperature in the reaction kettle rises to 95 ℃, the adding speed of the hydrochloric acid is controlled to be 1% per minute of the total volume, in step S10, the stable reaction temperature error of the reaction kettle is controlled to be plus or minus 2 ℃. In step S12, the reactor inlet and outlet amounts must be balanced.
Example two
A production method for producing polyaluminium chloride by constant temperature and constant acid comprises the following steps:
step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion;
step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously;
and step S3: simultaneously adding water for spraying;
and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the index of the mixed liquid meets the planned proportioning requirement;
step S5: when the mixed liquid index is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, the mixed liquid is transferred to a reaction kettle;
step S6: adding hydrochloric acid in proportion according to the transfer amount and the detection result to react;
step S7: controlling the initial reaction temperature of the reaction kettle at 40 ℃;
step S8: after 50% of required hydrochloric acid is added into the reaction kettle, the temperature of the reaction kettle gradually rises, the temperature of the reaction kettle is observed in real time in the process, and the heating is stopped in time when the temperature of the reaction kettle is overhigh;
step S9: when the temperature in the reaction kettle rises to 95 ℃, controlling the acid adding speed, and not enabling the temperature to rise to exceed 105 ℃;
step S10: keeping the reaction kettle to react stably for 1.5 hours at 103 ℃;
step S11: sampling and detecting whether the product is qualified;
step S12: quantitatively removing the finished product from the bottom of the reaction kettle after the product is qualified, then quantitatively and continuously adding the mixed solution and the hydrochloric acid, and balancing the inlet and outlet amount;
step S13: and after the product is detected to be qualified, deslagging, cooling and then feeding into a finished product.
In this embodiment, in step S1, the raw materials of the polyaluminum chloride include aluminum-containing powder, hydrochloric acid, and water, and the mixture ratio is 1:2:0.8, wherein the concentration of hydrochloric acid is 34%, in step S7, when the initial temperature of the reaction kettle does not reach 40 ℃, heating is carried out in a steam heating mode, in step S7, when the initial reaction temperature of the reaction kettle is controlled, the temperature error range is plus or minus 1 ℃, in step S8, heating is stopped when the temperature of a mixed liquid in the reaction kettle is higher than 103 ℃, in step S9, after the temperature in the reaction kettle rises to 95 ℃, the adding speed of the hydrochloric acid is controlled to be 1.5% per minute of the total volume, in step S10, the stable reaction temperature error of the reaction kettle is controlled to be plus or minus 1 ℃. In step S12, the reactor inlet and outlet amounts must be balanced.
EXAMPLE III
A production method for producing polyaluminium chloride by constant temperature and constant acid comprises the following steps:
step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion;
step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously;
and step S3: simultaneously adding water for spraying;
and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the index of the mixed liquid meets the planned proportioning requirement;
step S5: when the index of the mixed liquid is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, the mixed liquid is transferred to a reaction kettle;
step S6: adding hydrochloric acid in proportion according to the transfer amount and the detection result to react;
step S7: the initial reaction temperature of the reaction kettle is controlled at 40 ℃;
step S8: after 50% of required hydrochloric acid is added into the reaction kettle, the temperature of the reaction kettle gradually rises, the temperature of the reaction kettle is observed in real time in the process, and the heating is stopped in time when the temperature of the reaction kettle is overhigh;
step S9: when the temperature in the reaction kettle rises to 95 ℃, controlling the acid adding speed, and not enabling the temperature to rise to exceed 105 ℃;
step S10: keeping the reaction kettle to react stably for 2 hours at 103 ℃;
step S11: sampling and detecting whether the product is qualified;
step S12: quantitatively removing the finished product from the bottom of the reaction kettle after the product is qualified, then quantitatively and continuously adding the mixed solution and the hydrochloric acid, and balancing the inlet and outlet amount;
step S13: and after the product is detected to be qualified, deslagging, cooling and then feeding into a finished product.
In this embodiment, in step S1, the raw materials of the polyaluminum chloride include aluminum-containing powder, hydrochloric acid, and water, and the mixture ratio is 1:3:0.6, wherein the concentration of hydrochloric acid is 36%, in the step S7, when the initial temperature of the reaction kettle does not reach 40 ℃, heating is carried out in a steam heating mode, in the step S7, when the initial reaction temperature of the reaction kettle is controlled, the temperature error range is plus or minus 1 ℃, in the step S8, heating is stopped when the temperature of a mixed liquid in the reaction kettle is higher than 103 ℃, in the step S9, after the temperature in the reaction kettle rises to 95 ℃, the adding speed of the hydrochloric acid is controlled to be 2% per minute of the total volume. In step S12, the reactor inlet and outlet amounts must be balanced.
By measuring the aluminum content, the basicity and the pH value of the polyaluminum chloride prepared in the above examples, the experimental data are shown in the following table:
| examples | A | II | III |
| Aluminum content | 10.08 | 10.12 | 10.2 |
| Basicity of salt | 80 | 78 | 78 |
| pH value of | 4.5 | 4 | 3.5 |
As can be seen from the above table, the aluminum content, basicity and pH value of the polyaluminum chloride prepared by the present invention all satisfy the national and industrial standards, and three are the best examples.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (1)
1. A production method for producing polyaluminium chloride at constant temperature and constant acid is characterized by comprising the following steps:
step S1: cleaning a dissolving tank, and adding water into the dissolving tank according to a proportion;
step S2: gradually adding an aluminum-containing powder raw material into a dissolving tank according to a proportion, and stirring simultaneously;
and step S3: simultaneously adding water for spraying;
and step S4: detecting a sample in the dissolving tank, and comparing and judging whether the indexes of the mixed liquid meet the planned proportioning requirement;
step S5: when the mixed liquid index is unqualified, adjusting according to the planned proportion; when the index of the mixed liquid is qualified, the mixed liquid is transferred to a reaction kettle;
step S6: adding hydrochloric acid in proportion according to the transfer amount and the detection result to react;
step S7: controlling the initial reaction temperature of the reaction kettle at 40 ℃;
step S8: after 50% of required hydrochloric acid is added into the reaction kettle, the temperature of the reaction kettle gradually rises, the temperature of the reaction kettle is adjusted in real time in the process, and the heating is stopped in time when the temperature of the reaction kettle is overhigh;
step S9: when the temperature in the reaction kettle rises to 95 ℃, controlling the acid adding speed, and preventing the temperature from rising to more than 105 ℃;
step S10: keeping the reaction kettle to react stably for 1-2 hours at 103 ℃;
step S11: sampling and detecting whether the product is qualified;
step S12: quantitatively removing the finished product from the bottom of the reaction kettle after the product is qualified, then quantitatively and continuously adding the mixed solution and the hydrochloric acid, and balancing the inlet and outlet amount;
step S13: removing the product, deslagging, cooling and then entering a finished product tank;
in the step S1, the raw materials of the polyaluminium chloride are aluminum-containing powder raw materials, hydrochloric acid and water, and the mixture ratio is 1: (2-3): (0.6-0.8), wherein the concentration of hydrochloric acid is 28-36%; in the step S7, when the initial temperature of the reaction kettle does not reach 40 ℃, heating is carried out in a steam heating mode; in the step S7, when the initial reaction temperature of the reaction kettle is controlled, the temperature error range is plus or minus 1 ℃; in the step S8, stopping heating when the temperature of the mixed liquid in the reaction kettle is higher than 103 ℃; in the step S9, after the temperature in the reaction kettle rises to 95 ℃, the adding speed of the hydrochloric acid is controlled to be 1-2% per minute of the total volume; in the step S10, the error of the stable reaction temperature of the reaction kettle is controlled to be plus or minus 2 ℃; in the step S11, the qualified standard of the product is 10% +/-0.5% of aluminum and 30-90% of basicity; in the step S12, the finished product is removed and the mixed solution and hydrochloric acid continuously added are to reach the balance of inlet and outlet.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1690834A2 (en) * | 2005-02-14 | 2006-08-16 | Sachtleben Chemie GmbH | Polyaluminum chloride solution |
| CN101172684A (en) * | 2007-10-09 | 2008-05-07 | 王贵明 | Method for industrial production of polymeric aluminum ferric chloride water purification agent with coal ash |
| CN101928031A (en) * | 2009-12-15 | 2010-12-29 | 中南民族大学 | Production method of polyaluminium chloride |
| CN110255595A (en) * | 2019-06-27 | 2019-09-20 | 嘉施利（宜城）化肥有限公司 | The preparation method of aluminium polychloride |
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2020
- 2020-10-19 CN CN202011119459.5A patent/CN112299463B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1690834A2 (en) * | 2005-02-14 | 2006-08-16 | Sachtleben Chemie GmbH | Polyaluminum chloride solution |
| CN101172684A (en) * | 2007-10-09 | 2008-05-07 | 王贵明 | Method for industrial production of polymeric aluminum ferric chloride water purification agent with coal ash |
| CN101928031A (en) * | 2009-12-15 | 2010-12-29 | 中南民族大学 | Production method of polyaluminium chloride |
| CN110255595A (en) * | 2019-06-27 | 2019-09-20 | 嘉施利（宜城）化肥有限公司 | The preparation method of aluminium polychloride |
Non-Patent Citations (2)
| Title |
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| "聚合氯化铝生产工艺的改进";缺;《无机盐工艺》;19830930(第9期);第28页 * |
| 铝酸钙粉制备聚合氯化铝生产条件实验研究;殷洪水等;《哈尔滨商业大学学报(自然科学版)》;20120815;第28卷(第04期);420-423 * |
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