CN112573584A - Treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on surface of metal product - Google Patents
Treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on surface of metal product Download PDFInfo
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- CN112573584A CN112573584A CN202011086507.5A CN202011086507A CN112573584A CN 112573584 A CN112573584 A CN 112573584A CN 202011086507 A CN202011086507 A CN 202011086507A CN 112573584 A CN112573584 A CN 112573584A
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- sulfuric acid
- waste sulfuric
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- ferric sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
Abstract
The invention discloses a treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, which comprises the steps of pickling, adding heated waste sulfuric acid into a reaction kettle, adding scrap iron into the reaction kettle, filtering the waste sulfuric acid, adding a filtrate into a stirrer, adding an oxidant into the stirrer to obtain a ferric iron solution, adding the ferric iron solution into the reaction stirrer, introducing water vapor under the environment of 100-110 ℃, setting the rotating speed to be 180-, the preparation method is simple in preparation process, the finally obtained polymeric ferric sulfate has higher acquisition rate than that of a traditional mode, the stability is better, the environment is protected, no pollution is caused, and the resource recycling is realized.
Description
Technical Field
The invention relates to the technical field of preparation of polymeric ferric sulfate from waste acid, in particular to a treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product.
Background
The traditional treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product is complex, the finally obtained polymeric ferric sulfate has low acquisition rate and poor stability, and therefore, an improved technology is urgently needed to solve the problem in the prior art.
Disclosure of Invention
The invention aims to provide a treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, which is simple to operate, the finally obtained polymeric ferric sulfate has higher acquisition rate than that of a traditional mode, better stability, environmental friendliness and no pollution, and the resource recycling is realized so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 80-90 deg.C for 2-3h, and naturally cooling to room temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding scrap iron into the reaction kettle, setting the temperature at 120-;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: then adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature to be 60-70 ℃, setting the rotating speed to be 200-;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor under the environment with the temperature of 100-110 ℃, setting the rotating speed as 180-200r/min, continuing for 25-30min, carrying out primary hydrolysis, then increasing the temperature to 150-160 ℃, introducing water vapor again, setting the rotating speed as 250-300r/min, continuing for 10-15min, then reducing the temperature to 60-70 ℃, introducing water vapor, setting the rotating speed as 100-120r/min, continuing for 1-2h, and completely carrying out hydrolysis reaction to obtain polymeric ferric sulfate.
Preferably, the acid washing in the first step is performed by using 60% sulfuric acid.
Preferably, the iron filings in the third step are added into the reaction kettle after being washed by water.
Preferably, in the fifth step, sodium nitrite is used as the oxidizing agent.
Preferably, in the sixth step, a steam vent pipe is arranged in the reaction stirrer.
Compared with the prior art, the invention has the beneficial effects that:
the method is simple to operate, the obtaining rate of the finally obtained polymeric ferric sulfate is higher than that of the traditional mode, the stability is better, the method is environment-friendly and pollution-free, and the resource recycling is realized.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides a technical scheme that: a treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 80-90 deg.C for 2-3h, and naturally cooling to room temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron chips subjected to washing operation into the reaction kettle, setting the temperature at 120-;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: then adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature to be 60-70 ℃, setting the rotating speed to be 200-;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor through a steam vent pipe under the environment with the temperature of 100-110 ℃, setting the rotation speed to be 180-200r/min, continuing for 25-30min, carrying out primary hydrolysis, then increasing the temperature to be 150-160 ℃, introducing the water vapor again, setting the rotation speed to be 250-300r/min, continuing for 10-15min, then reducing the temperature to be 60-70 ℃, introducing the water vapor, setting the rotation speed to be 100-120r/min, continuing for 1-2h, and completely carrying out hydrolysis reaction to obtain the polymeric ferric sulfate.
The first embodiment is as follows:
the treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 80 ℃, continuing for 2h, and then naturally cooling to the normal temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron scraps subjected to washing operation into the reaction kettle, setting the temperature to be 120 ℃, setting the rotating speed to be 200r/min and the negative pressure to be 0.25MPa, and continuously reacting for 20 min;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature at 60 ℃ and the rotating speed at 200r/min, and continuing for 1h to obtain a ferric iron solution;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor through a steam vent pipeline under the environment of 100 ℃, setting the rotating speed at 180r/min for 25min, performing primary hydrolysis, then increasing the temperature to 150 ℃, introducing water vapor again, setting the rotating speed at 250r/min for 10min, then reducing the temperature to 60 ℃, introducing water vapor, setting the rotating speed at 100r/min for 1h, and completely performing hydrolysis reaction to obtain the polymeric ferric sulfate.
Example two:
the treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 90 ℃, keeping for 2 hours, and then naturally cooling to the normal temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron scraps subjected to washing operation into the reaction kettle, setting the temperature to be 130 ℃, setting the rotating speed to be 150r/min and the negative pressure to be 0.25MPa, and continuously reacting for 30 min;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature to be 70 ℃, setting the rotating speed to be 250r/min, and continuing for 1.5 hours to obtain a ferric iron solution;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor through a steam vent pipeline under the environment of 110 ℃, setting the rotating speed at 200r/min for 30min, performing primary hydrolysis, then increasing the temperature to 160 ℃, introducing water vapor again, setting the rotating speed at 300r/min for 15min, then reducing the temperature to 70 ℃, introducing water vapor, setting the rotating speed at 120r/min, and continuing for 2h, so that hydrolysis reaction completely occurs, and obtaining the polymeric ferric sulfate.
Example three:
the treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 80 ℃, continuing for 3 hours, and then naturally cooling to the normal temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron scraps subjected to washing operation into the reaction kettle, setting the temperature at 130 ℃, the rotating speed at 200r/min and the negative pressure at 0.25MPa, and continuously reacting for 30 min;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature at 60 ℃ and the rotating speed at 200r/min, and continuing for 1h to obtain a ferric iron solution;
step six: adding a ferric iron solution into a reaction stirrer, introducing steam through a steam ventilation pipeline under the environment of 100 ℃, setting the rotating speed at 200r/min for 30min, carrying out primary hydrolysis, then increasing the temperature to 160 ℃, introducing the steam again, setting the rotating speed at 250r/min for 15min, then reducing the temperature to 60 ℃, introducing the steam, setting the rotating speed at 100r/min for 1h, and completely carrying out hydrolysis reaction to obtain the polymeric ferric sulfate.
Example four:
the treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 85 ℃, continuing for 2.5h, and then naturally cooling until the temperature is normal;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron scraps subjected to washing operation into the reaction kettle, setting the temperature to be 125 ℃, setting the rotating speed to be 170r/min and the negative pressure to be 0.25MPa, and continuously reacting for 25 min;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature to be 65 ℃ and the rotating speed to be 220r/min, and continuing for 1h to obtain a ferric iron solution;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor through a steam vent pipeline under the environment of 105 ℃, setting the rotating speed to be 190r/min for 25min, carrying out primary hydrolysis, then increasing the temperature to 155 ℃, introducing water vapor again, setting the rotating speed to be 280r/min for 10min, then reducing the temperature to 65 ℃, introducing water vapor, setting the rotating speed to be 110r/min, and continuing for 1h, so that hydrolysis reaction completely occurs, and obtaining the polymeric ferric sulfate.
Example five:
the treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid on the surface of the metal product comprises the following steps:
the method comprises the following steps: pickling the metal product, reacting with 60% sulfuric acid, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 85 ℃, continuing for 3 hours, and then naturally cooling to the normal temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding the iron scraps subjected to washing operation into the reaction kettle, setting the temperature to be 125 ℃, setting the rotating speed to be 200r/min and the negative pressure to be 0.25MPa, and continuously reacting for 30 min;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature at 60 ℃ and the rotating speed at 250r/min, and continuing for 1.5 hours to obtain a ferric iron solution;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor through a steam vent pipeline under the environment of 105 ℃, setting the rotating speed to be 190r/min for 25min, carrying out primary hydrolysis, then increasing the temperature to 150 ℃, introducing water vapor again, setting the rotating speed to be 300r/min for 15min, then reducing the temperature to be 60 ℃, introducing water vapor, setting the rotating speed to be 100r/min for 2h, and completely carrying out hydrolysis reaction to obtain the polymeric ferric sulfate.
The treatment process for preparing the polymeric ferric sulfate from the waste sulfuric acid in the first to fifth embodiments is simple to operate, the finally obtained polymeric ferric sulfate has a higher obtaining rate than that of a traditional mode, the stability is better, the environment is protected, no pollution is caused, and the resource recycling is realized.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product is characterized in that: the method comprises the following steps:
the method comprises the following steps: pickling the metal product, and collecting waste sulfuric acid obtained after pickling;
step two: heating to 80-90 deg.C for 2-3h, and naturally cooling to room temperature;
step three: adding heated waste sulfuric acid into a reaction kettle, adding scrap iron into the reaction kettle, setting the temperature at 120-;
step four: discharging the waste sulfuric acid into a filter, filtering the waste sulfuric acid, and collecting filtrate;
step five: then adding the filtrate into a stirrer, adding an oxidant into the stirrer, setting the temperature to be 60-70 ℃, setting the rotating speed to be 200-;
step six: adding a ferric iron solution into a reaction stirrer, introducing water vapor under the environment with the temperature of 100-110 ℃, setting the rotating speed as 180-200r/min, continuing for 25-30min, carrying out primary hydrolysis, then increasing the temperature to 150-160 ℃, introducing water vapor again, setting the rotating speed as 250-300r/min, continuing for 10-15min, then reducing the temperature to 60-70 ℃, introducing water vapor, setting the rotating speed as 100-120r/min, continuing for 1-2h, and completely carrying out hydrolysis reaction to obtain polymeric ferric sulfate.
2. The treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, according to claim 1, is characterized in that: in the first step, sulfuric acid with the concentration of 60% is adopted for acid washing to carry out reaction.
3. The treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, according to claim 1, is characterized in that: and step three, adding the iron filings into the reaction kettle after the washing operation.
4. The treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, according to claim 1, is characterized in that: and in the fifth step, sodium nitrite is used as an oxidant.
5. The treatment process for preparing polymeric ferric sulfate from waste sulfuric acid on the surface of a metal product, according to claim 1, is characterized in that: and a steam vent pipeline is arranged in the reaction stirrer in the sixth step.
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Citations (6)
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| KR101572914B1 (en) * | 2015-04-15 | 2015-12-01 | 넥스테크(주) | Poly ferric sulfate manufacture method using disuse sulfuric acid of semiconductor production process |
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| CN108455684A (en) * | 2018-02-09 | 2018-08-28 | 无锡日月水处理有限公司 | Environment-friendly type polyaluminum sulfate process for making iron |
| CN108557901A (en) * | 2018-05-10 | 2018-09-21 | 湘潭湘钢瑞兴公司 | A kind of production technology of steel mill's spent acid production bodied ferric sulfate |
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2020
- 2020-10-12 CN CN202011086507.5A patent/CN112573584A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| KR101572914B1 (en) * | 2015-04-15 | 2015-12-01 | 넥스테크(주) | Poly ferric sulfate manufacture method using disuse sulfuric acid of semiconductor production process |
| CN106395925A (en) * | 2016-06-23 | 2017-02-15 | 江门市江海区炜洁净水材料有限公司 | A method of preparing a polyferricsulfate water purifier |
| CN105948210A (en) * | 2016-07-11 | 2016-09-21 | 哈尔滨辰能工大环保科技股份有限公司 | Method for producing polymeric ferric sulfate from raw materials industrial waste acid and scrap iron |
| CN207108517U (en) * | 2017-07-12 | 2018-03-16 | 南京云泰化工总厂 | A kind of pyrite slag prepares the device of polymerization iron sulfate water-purifying agent |
| CN108455684A (en) * | 2018-02-09 | 2018-08-28 | 无锡日月水处理有限公司 | Environment-friendly type polyaluminum sulfate process for making iron |
| CN108557901A (en) * | 2018-05-10 | 2018-09-21 | 湘潭湘钢瑞兴公司 | A kind of production technology of steel mill's spent acid production bodied ferric sulfate |
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