CN111847611A - Method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid - Google Patents
Method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid Download PDFInfo
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- CN111847611A CN111847611A CN202010512117.3A CN202010512117A CN111847611A CN 111847611 A CN111847611 A CN 111847611A CN 202010512117 A CN202010512117 A CN 202010512117A CN 111847611 A CN111847611 A CN 111847611A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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Abstract
The invention provides a method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid, which comprises four steps of hydrochloric acid detection, modulation treatment, separation and purification and preparation of solid polyferric chloride. On one hand, the method has simple operation process and high ion separation and recovery operation efficiency, and the prepared polyferric chloride has high purity and is not easy to oxidize and deteriorate, so that the efficiency and the quality of the process for extracting the polyferric chloride from the waste hydrochloric acid are greatly improved; on the other hand, in the operation of the invention, the centralized treatment capacity of the solid waste is effectively realized, the pollution of the solid waste to the environment is reduced, and simultaneously the recycling rate of the solid waste is effectively improved, thereby further reducing the operation risk and the cost of the process.
Description
Technical Field
The invention relates to a method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid, belonging to the technical field of waste acid treatment.
Background
At present, in the purification and recycling of waste hydrochloric acid containing ferrous chloride, the preparation of a water purifying agent by recycling iron ions in the hydrochloric acid is one of the main treatment methods at present, but in the practical application of the technology, although products such as ferrous chloride, ferric chloride and the like can be obtained to a certain extent, on one hand, the obtained ferrous chloride product is mostly in a liquid state, the concentration is relatively low, and the product quality and the yield of the product which is used as a raw material to prepare the ferric chloride are seriously influenced due to deterioration caused by oxidation; on the other hand, in the process of obtaining the ferrous chloride, a large amount of solid wastes are generated, and the solid wastes are often not effectively treated, so that the current purification and recovery technology for the industrial waste hydrochloric acid containing the ferrous chloride is still difficult to effectively popularize, and has great hidden troubles.
Therefore, in order to meet the current situation, a brand-new method for preparing the polymeric ferric chloride for water treatment from the iron-containing waste hydrochloric acid needs to be developed to meet the actual use requirement.
Disclosure of Invention
The invention aims to provide a method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention discloses a method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid, which comprises the following steps:
s1, detecting hydrochloric acid, namely firstly introducing the iron-containing waste hydrochloric acid to be treated into an acid storage tank, keeping the depth of the acid liquid to be 0.3-1.5 m, standing for 4-24 hours, then sampling and detecting the acid liquid, measuring the content of ferrous chloride and the content of free acid in the iron-containing waste hydrochloric acid at present, and comparing the content of ferrous chloride and the content of free acid with a set value;
s2, modulating, namely modulating the ion concentration of the iron-containing waste hydrochloric acid according to the detection parameters and the comparison result obtained in the step S1, vertically inserting a plurality of iron columns into the acid liquor of the acid storage pool at intervals of 0.3-1.5 meters around the axis of the acid storage pool when modulating the ion concentration, enabling the interval between the lower end surface of the iron column and the bottom of the acid storage pool to be 0.1-0.2 meter, standing for 1-24 hours after the iron column is immersed into the acid liquor, detecting the content of ferrous chloride and the content of free acid in the acid liquor of the acid storage pool at the frequency of once detection per hour in the standing process, separating the iron column from the acid liquor and cleaning the surface of the iron column by deionized water until the set standard is reached, and returning the cleaned deionized water to the acid storage pool;
S3, separating and purifying, after the step S2 is completed, pressurizing the clarified acid liquor in the acid storage pool by a booster pump, conveying the acid liquor to a filtering device for solid-liquid separation, returning the separated solid filter residue to the step S1, injecting the solid filter residue into the acid storage pool, and conveying the filtered filtrate to a reaction kettle for reaction to obtain liquid ferrous chloride;
s4, preparing solid polyferric chloride, firstly evacuating the air in the reaction kettle, making the oxygen content in the reaction kettle not more than 10%, then heating the liquid ferrous chloride in the air to 85-95 ℃ by the reaction kettle, keeping the temperature, simultaneously injecting 50-80% sodium carbonate solution to the top of the liquid level of the reaction kettle, injecting 28% hydrochloric acid solution to the bottom of the reaction kettle, adding alkali liquor and acid liquor, simultaneously detecting the concentration of ferrous iron ions in the liquid ferrous chloride in the reaction kettle, stopping adding the alkali liquor when the concentration is less than or equal to 0.15%, stopping adding the hydrochloric acid solution when the salt concentration reaches 5-10%, simultaneously introducing high-pressure inert gas into the mixed liquid in the reaction kettle for unidirectional uniform stirring, and conveying the mixture in the reaction kettle to a crystallization reaction kettle for crystallization after stirring for 3-10 minutes, thus obtaining the finished product of the solid polyferric chloride.
In steps S1 and S2, the acid storage tank comprises a bearing groove, a bearing cover, a lifting driving mechanism, an adjusting iron rod, a displacement sensor and a control circuit, the bearing groove is of a structure with an axial section of a groove shape, the upper end surface of the bearing cover is connected with the bearing cover and coaxially distributed to form a closed cavity structure, a plurality of positioning holes are uniformly distributed on the bearing cover, the axes of the positioning holes are distributed in parallel with the axis of the bearing groove and the positioning holes are uniformly distributed around the axis of the bearing groove, the adjusting iron rods which are coaxially distributed with the positioning holes are arranged in the positioning holes and are in sliding connection with the wall of the positioning hole through a lifting driving mechanism, a displacement sensor is additionally arranged on the side wall of the positioning hole and is additionally connected with the side surface of the adjusting iron rod, the control circuit is connected with the upper end face of the bearing cover and is respectively and electrically connected with the lifting driving mechanism and the displacement sensor.
The bearing cover is hinged with the upper end face of the bearing groove through a ratchet mechanism, and the lower end face of the ratchet mechanism is connected with the upper end face of the bearing groove through a lifting driving mechanism.
The setting values in step S1 are: the content of ferrous chloride is more than or equal to 20wt percent, and the content of free acid is less than or equal to 5wt percent.
And step S3, returning the solid filter residue to the acid storage pool, and purifying the solid residue when the thickness of the solid residue in the acid storage pool reaches 0.1-0.2 m.
The purification treatment specifically comprises the following steps:
firstly, performing filter pressing operation, namely performing filter pressing operation on solid residues in an acid storage pool, performing solid-liquid separation, returning acid liquor obtained by filter pressing to the acid storage pool again for later use, cleaning solid residues obtained by filter pressing by using clear water, and conveying cleaned water to the acid storage pool for later use after solid-liquid separation;
and secondly, drying, namely adding the cleaned solid residues into a forming grinding tool, then carrying out extrusion forming on the solid residues, and after demolding, carrying out centralized collection on the formed solid residues.
In step S3, during solid-liquid separation, the pressure of the liquid material above the filter layer is at least 3 times the pressure below the filter layer.
On one hand, the method has simple operation process and high ion separation and recovery operation efficiency, and the prepared polyferric chloride has high purity and is not easy to oxidize and deteriorate, so that the efficiency and the quality of the process for extracting the polyferric chloride from the waste hydrochloric acid are greatly improved; on the other hand, in the operation of the invention, the centralized treatment capacity of the solid waste is effectively realized, the pollution of the solid waste to the environment is reduced, and simultaneously the recycling rate of the solid waste is effectively improved, thereby further reducing the operation risk and the cost of the process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the process of the present invention;
FIG. 2 is a flow diagram of a solid residue treatment process; a
FIG. 3 is a schematic view of the acid storage tank.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing polymeric ferric chloride for water treatment based on waste hydrochloric acid containing iron as shown in fig. 1 to 3, comprising the following steps:
s1, detecting hydrochloric acid, namely firstly introducing the iron-containing waste hydrochloric acid to be treated into an acid storage tank, keeping the depth of the acid liquid to be 0.3-1.5 m, standing for 4-24 hours, then sampling and detecting the acid liquid, measuring the content of ferrous chloride and the content of free acid in the iron-containing waste hydrochloric acid at present, and comparing the content of ferrous chloride and the content of free acid with a set value;
S2, modulating, namely modulating the ion concentration of the iron-containing waste hydrochloric acid according to the detection parameters and the comparison result obtained in the step S1, vertically inserting a plurality of iron columns into the acid liquor of the acid storage pool at intervals of 0.3-1.5 meters around the axis of the acid storage pool when modulating the ion concentration, enabling the interval between the lower end surface of the iron column and the bottom of the acid storage pool to be 0.1-0.2 meter, standing for 1-24 hours after the iron column is immersed into the acid liquor, detecting the content of ferrous chloride and the content of free acid in the acid liquor of the acid storage pool at the frequency of once detection per hour in the standing process, separating the iron column from the acid liquor and cleaning the surface of the iron column by deionized water until the set standard is reached, and returning the cleaned deionized water to the acid storage pool;
s3, separating and purifying, after the step S2 is completed, pressurizing the clarified acid liquor in the acid storage pool by a booster pump, conveying the acid liquor to a filtering device for solid-liquid separation, returning the separated solid filter residue to the step S1, injecting the solid filter residue into the acid storage pool, and conveying the filtered filtrate to a reaction kettle for reaction to obtain liquid ferrous chloride;
s4, preparing solid polyferric chloride, firstly evacuating the air in the reaction kettle, making the oxygen content in the reaction kettle not more than 10%, then heating the liquid ferrous chloride in the gas by the reaction kettle to 85-95 ℃ and keeping the temperature, then simultaneously, on the one hand, injecting hydrochloric acid aqueous solution with the concentration not more than 28% to the top of the liquid level of the reaction kettle, on the other hand, detecting the concentration of ferrous iron ions in the liquid ferrous chloride in the reaction kettle and stopping adding the alkali liquid when the concentration is not more than 0.15% while adding the alkali liquid and the acid liquid, when the salt concentration reaches 5-10%, stopping adding the hydrochloric acid aqueous solution, simultaneously introducing high-pressure inert gas into the mixed liquid in the reaction kettle for unidirectional uniform stirring, and after stirring for 3-10 minutes, conveying the mixture in the reaction kettle to a crystallization reaction kettle for crystallization, thus obtaining the finished product of the solid polyferric chloride.
It is important to point out that in the steps S1 and S2, the acid storage tank includes a bearing tank 1, a bearing cover 2, a lifting driving mechanism 3, an adjusting iron rod 4, a displacement sensor 5 and a control circuit 6, the bearing tank 1 is of a structure with an axial cross section of a shape of a trough, the upper end surface of the bearing cover is connected with the bearing cover 2 and coaxially distributed to form a closed cavity structure, a plurality of positioning holes 7 are uniformly distributed on the bearing cover 2, the axes of the positioning holes 7 are distributed in parallel with the axis of the bearing groove 1, all the positioning hole rings 7 are uniformly distributed around the axis of the bearing groove 1, an adjusting iron rod 4 coaxially distributed with the positioning holes 7 is arranged in each positioning hole 7, the adjusting iron rod 4 is in sliding connection with the wall of the positioning hole 7 through a lifting driving mechanism 3, a displacement sensor 5 is additionally arranged on the side wall of each positioning hole 7, the displacement sensor 5 is connected with the side surface of the adjusting iron rod 4, and the control circuit 6 is connected with the upper end surface of the bearing cover 2 and is respectively and electrically connected with the lifting driving mechanism 3 and the displacement sensor 5.
Further preferably, the bearing cover 2 is hinged with the upper end face of the bearing groove 1 through a ratchet mechanism 8, and the lower end face of the ratchet mechanism 8 is connected with the upper end face of the bearing groove 1 through a lifting driving mechanism 3.
In this embodiment, the set values in step S1 are: the content of ferrous chloride is more than or equal to 20wt percent, and the content of free acid is less than or equal to 5wt percent.
And simultaneously, returning the solid filter residue in the step S3 to the acid storage pool, and purifying the solid residue when the thickness of the solid residue in the acid storage pool reaches 0.1-0.2 m.
It should be noted that the purification treatment specifically includes the following steps:
firstly, performing filter pressing operation, namely performing filter pressing operation on solid residues in an acid storage pool, performing solid-liquid separation, returning acid liquor obtained by filter pressing to the acid storage pool again for later use, cleaning solid residues obtained by filter pressing by using clear water, and conveying cleaned water to the acid storage pool for later use after solid-liquid separation;
and secondly, drying, namely adding the cleaned solid residues into a forming grinding tool, then carrying out extrusion forming on the solid residues, and then carrying out centralized collection on the formed solid residues after demoulding.
In this embodiment, in the step S3, when solid-liquid separation is performed, the pressure of the liquid material above the filter layer is at least 3 times of the pressure below the filter layer.
On one hand, the method has simple operation process and high ion separation and recovery operation efficiency, and the prepared polyferric chloride has high purity and is not easy to oxidize and deteriorate, so that the efficiency and the quality of the process for extracting the polyferric chloride from the waste hydrochloric acid are greatly improved; on the other hand, in the operation of the invention, the centralized treatment capacity of the solid waste is effectively realized, the pollution of the solid waste to the environment is reduced, and simultaneously the recycling rate of the solid waste is effectively improved, thereby further reducing the operation risk and the cost of the process.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. A method for preparing polyferric chloride for water treatment based on iron-containing waste hydrochloric acid is characterized by comprising the following steps: the method comprises the following steps:
s1, detecting hydrochloric acid, namely firstly introducing the iron-containing waste hydrochloric acid to be treated into an acid storage tank, keeping the depth of the acid liquid to be 0.3-1.5 m, standing for 4-24 hours, then sampling and detecting the acid liquid, measuring the content of ferrous chloride and the content of free acid in the iron-containing waste hydrochloric acid at present, and comparing the content of ferrous chloride and the content of free acid with a set value;
s2, modulating, namely modulating the ion concentration of the iron-containing waste hydrochloric acid according to the detection parameters and the comparison result obtained in the step S1, vertically inserting a plurality of iron columns into the acid liquor of the acid storage pool at intervals of 0.3-1.5 meters around the axis of the acid storage pool when modulating the ion concentration, enabling the interval between the lower end surface of the iron column and the bottom of the acid storage pool to be 0.1-0.2 meter, standing for 1-24 hours after the iron column is immersed into the acid liquor, detecting the content of ferrous chloride and the content of free acid in the acid liquor of the acid storage pool at the frequency of once detection per hour in the standing process, separating the iron column from the acid liquor and cleaning the surface of the iron column by deionized water until the set standard is reached, and returning the cleaned deionized water to the acid storage pool;
S3, separating and purifying, after the step S2 is completed, pressurizing the clarified acid liquor in the acid storage pool by a booster pump, conveying the acid liquor to a filtering device for solid-liquid separation, returning the separated solid filter residue to the step S1, injecting the solid filter residue into the acid storage pool, and conveying the filtered filtrate to a reaction kettle for reaction to obtain liquid ferrous chloride;
s4, preparing solid polyferric chloride, firstly evacuating the air in the reaction kettle, making the oxygen content in the reaction kettle not more than 10%, then heating the liquid ferrous chloride in the air to 85-95 ℃ by the reaction kettle, keeping the temperature, simultaneously injecting 50-80% sodium carbonate solution to the top of the liquid level of the reaction kettle, injecting 28% hydrochloric acid solution to the bottom of the reaction kettle, adding alkali liquor and acid liquor, simultaneously detecting the concentration of ferrous iron ions in the liquid ferrous chloride in the reaction kettle, stopping adding the alkali liquor when the concentration is less than or equal to 0.15%, stopping adding the hydrochloric acid solution when the salt concentration reaches 5-10%, simultaneously introducing high-pressure inert gas into the mixed liquid in the reaction kettle for unidirectional uniform stirring, and conveying the mixture in the reaction kettle to a crystallization reaction kettle for crystallization after stirring for 3-10 minutes, thus obtaining the finished product of the solid polyferric chloride.
2. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 1, wherein the method comprises the following steps: in steps S1 and S2, the acid storage tank comprises a bearing groove, a bearing cover, a lifting driving mechanism, an adjusting iron rod, a displacement sensor and a control circuit, the bearing groove is of a structure with an axial section of a groove shape, the upper end surface of the bearing cover is connected with the bearing cover and coaxially distributed to form a closed cavity structure, a plurality of positioning holes are uniformly distributed on the bearing cover, the axes of the positioning holes are distributed in parallel with the axis of the bearing groove and the positioning holes are uniformly distributed around the axis of the bearing groove, the adjusting iron rods which are coaxially distributed with the positioning holes are arranged in the positioning holes and are in sliding connection with the wall of the positioning hole through a lifting driving mechanism, a displacement sensor is additionally arranged on the side wall of the positioning hole and is additionally connected with the side surface of the adjusting iron rod, the control circuit is connected with the upper end face of the bearing cover and is respectively and electrically connected with the lifting driving mechanism and the displacement sensor.
3. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 2, wherein the method comprises the following steps: the bearing cover is hinged with the upper end face of the bearing groove through a ratchet mechanism, and the lower end face of the ratchet mechanism is connected with the upper end face of the bearing groove through a lifting driving mechanism.
4. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 1, wherein the method comprises the following steps: the setting values in step S1 are: the content of ferrous chloride is more than or equal to 20wt percent, and the content of free acid is less than or equal to 5wt percent.
5. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 1, wherein the method comprises the following steps: and step S3, returning the solid filter residue to the acid storage pool, and purifying the solid residue when the thickness of the solid residue in the acid storage pool reaches 0.1-0.2 m.
6. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 5, wherein the method comprises the following steps: the purification treatment specifically comprises the following steps:
firstly, performing filter pressing operation, namely performing filter pressing operation on solid residues in an acid storage pool, performing solid-liquid separation, returning acid liquor obtained by filter pressing to the acid storage pool again for later use, cleaning solid residues obtained by filter pressing by using clear water, and conveying cleaned water to the acid storage pool for later use after solid-liquid separation;
and secondly, drying, namely adding the cleaned solid residues into a forming grinding tool, then carrying out extrusion forming on the solid residues, and after demolding, carrying out centralized collection on the formed solid residues.
7. The method for preparing the polyferric chloride for water treatment based on the iron-containing waste hydrochloric acid as claimed in claim 1, wherein the method comprises the following steps: in step S3, during solid-liquid separation, the pressure of the liquid material above the filter layer is at least 3 times the pressure below the filter layer.
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| CN1266819A (en) * | 1999-03-11 | 2000-09-20 | 中国科学院生态环境研究中心 | Flocculant of polyiron chloride prepared from waste hydrochloric acid as pickling liquid of iron and steel and its preparing process |
| CN101037233A (en) * | 2007-02-28 | 2007-09-19 | 天津市聚鑫源水处理技术开发有限公司 | Method for producing solid polymeric ferric chloride using ferrous chloride crystal as raw material |
| CN101462776A (en) * | 2009-01-07 | 2009-06-24 | 金月祥 | Process for preparing poly ferric chloride |
| CN101891258A (en) * | 2009-05-20 | 2010-11-24 | 北京紫光英力化工技术有限公司 | Novel production process of polyferric chloride |
| CN103073067A (en) * | 2013-02-02 | 2013-05-01 | 梁锡明 | Method for producing ferric chloride by using pickle liquor |
| CN103145196A (en) * | 2013-03-28 | 2013-06-12 | 青岛新世纪环境工程有限公司 | Method for producing polymerization ferric chloride by utilizing waste hydrochloric acid and waste ferrous mud |
| CN104229902A (en) * | 2014-07-23 | 2014-12-24 | 浙江富春环保新材料有限公司 | Method for preparing liquid ferrous chloride for water treatment by taking waste hydrochloric acid as raw material |
| CN104817118A (en) * | 2015-05-18 | 2015-08-05 | 陈雷 | Simple and quick method for preparing polyferric chloride |
-
2020
- 2020-06-08 CN CN202010512117.3A patent/CN111847611A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1266819A (en) * | 1999-03-11 | 2000-09-20 | 中国科学院生态环境研究中心 | Flocculant of polyiron chloride prepared from waste hydrochloric acid as pickling liquid of iron and steel and its preparing process |
| CN101037233A (en) * | 2007-02-28 | 2007-09-19 | 天津市聚鑫源水处理技术开发有限公司 | Method for producing solid polymeric ferric chloride using ferrous chloride crystal as raw material |
| CN101462776A (en) * | 2009-01-07 | 2009-06-24 | 金月祥 | Process for preparing poly ferric chloride |
| CN101891258A (en) * | 2009-05-20 | 2010-11-24 | 北京紫光英力化工技术有限公司 | Novel production process of polyferric chloride |
| CN103073067A (en) * | 2013-02-02 | 2013-05-01 | 梁锡明 | Method for producing ferric chloride by using pickle liquor |
| CN103145196A (en) * | 2013-03-28 | 2013-06-12 | 青岛新世纪环境工程有限公司 | Method for producing polymerization ferric chloride by utilizing waste hydrochloric acid and waste ferrous mud |
| CN104229902A (en) * | 2014-07-23 | 2014-12-24 | 浙江富春环保新材料有限公司 | Method for preparing liquid ferrous chloride for water treatment by taking waste hydrochloric acid as raw material |
| CN104817118A (en) * | 2015-05-18 | 2015-08-05 | 陈雷 | Simple and quick method for preparing polyferric chloride |
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Application publication date: 20201030 |