CN1223553C - Iron powder reducing method for simultaneously producing organic product and ferric oxide black - Google Patents
Iron powder reducing method for simultaneously producing organic product and ferric oxide black Download PDFInfo
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- CN1223553C CN1223553C CN 03128113 CN03128113A CN1223553C CN 1223553 C CN1223553 C CN 1223553C CN 03128113 CN03128113 CN 03128113 CN 03128113 A CN03128113 A CN 03128113A CN 1223553 C CN1223553 C CN 1223553C
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Abstract
The present invention discloses a method for producing organic products and synchronously producing iron oxide black by an iron powder reduction method. The method comprises reduction, filtration, washing, sieving, refiltration and drying, wherein in the reduction reaction, a reduction reaction tank with paddle stirrer is adopted, iron powder, water and reaction media are added in the reduction reaction tank, suspension liquid of iron powder is indirectly heated by vapour, organic raw materials are continuously added dropwise after activation is carried out for 0.5 to 1 hour, iron powder, reaction media and water are discontinuously replenished in reaction, and ratio of the feeding amounts of organic raw materials, iron powder, the reaction media and water is always kept to be 1: 0.5 to 1.5: 0.01 to 0.1: 2 to 5. Suspension liquid of organic products and iron mud are continuously discharged from a discharge port of the reduction reaction tank. The present invention can realize continuous production, lower consumption, and improve the utilization rate of resources. All processes that iron powder is used as reducing agents for producing organic products can use the present invention for synchronously producing iron oxide black.
Description
Technical Field
The invention relates to a method for producing black iron oxide, in particular to a method for synchronously producing black iron oxide by producing organic products by an iron powder reduction method.
Background
The reduction reaction of iron powder reducing agent to produce organic products is a conventional reduction process. The process has the characteristics of simplicity, low requirement on equipment, less side reaction and the like, the iron powder is finally oxidized into iron oxide (the main components are adducts of ferroferric oxide and ferric oxide) by organic raw materials, and the traditional process adopts a discontinuous production mode, so that the production efficiency is low, and the generated iron mud has low grade and is often discarded, thereby easily causing resource waste and environmental pollution.
Disclosure of Invention
The invention aims to provide a method for synchronously producing iron oxide black by producing organic products by an iron powder reduction method, and the iron oxide black prepared by the method has excellent performance and low treatment cost.
The purpose of the invention is realized as follows: a method for synchronously producing iron oxide black by producing organic products by an iron powder reduction method comprises the processes of reduction reaction, filtration, water washing, screening, filtration, drying and grinding, and comprises the following steps:
(1) reduction reaction: putting iron powder, a reaction medium and water into a reduction reaction tank, heating and activating for 0.5-1 hour by steam, wherein the reaction temperature is 50-95 ℃, the reaction pressure is normal pressure, the stirring speed is 60-120 r/min, the pH value in the reduction reaction tank is 5-8, an aromatic nitro compound or a quinone compound is continuously dripped in the reaction process, iron powder, the reaction medium and water are discontinuously supplemented, the weight ratio of the aromatic nitro compound or the quinone compound, the iron powder, the reaction medium and the water is always maintained to be 1: 0.5-1.5: 0.01-0.1: 2-5, and the suspended substance of the aromatic amino compound or the phenol compound and the iron mud is continuously discharged from a discharge port of the reduction reaction tank;
(2) and (3) filtering: filtering suspended matters generated in the reaction in the step (1) to obtain a solid-phase substance A;
(3) washing: washing the solid-phase substance A in the step (2) by heating water until supernatant liquor is colorless, wherein the temperature of the heating water is 50-90 ℃;
(4) screening: screening the suspension B washed in the step (3) by a drum screen, wherein the screen mesh is 200-500 meshes, and obtaining a screen underflow B;
(5) and (3) filtering: filtering the undersize product B in the step (4) to obtain a solid phase product B;
(6) and (3) drying: and drying the solid phase substance B to obtain an iron oxide black product, wherein the drying temperature is 50-250 ℃, and the drying time is 30-90 minutes.
(1) The reaction medium is one or more of ferrous sulfate, ferrous chloride, dilute hydrochloric acid, dilute nitric acid, ferrous nitrate and ammonium chloride.
(2) The main components of the solid-phase substance A are iron mud and iron powder, and the main component of the iron mud is ferroferric oxide.
(4) The suspension B is the water suspension of iron mud and iron powder, and the undersize B is the water suspension of iron mud.
(5) The solid-phase material B is iron mud, and the main component of the iron mud is ferroferric oxide.
Compared with the prior art, the method realizes continuous production, and the method can be used for synchronously producing the iron oxide black in all processes of producing organic products by taking the iron powder as the reducing agent. According to the experiment, 1 ton of iron powder reducing agent can prepare 1.2 ton of iron oxide black by the method, and the obtained product has high tinting strength, high content and good performance and meets the national relevant standards. Improves the resource utilization rate and reduces the environmental pollution caused by the waste of the iron mud.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a process flow diagram of the present invention.
FIG. 1 is also taken as an abstract figure.
Detailed Description
As shown in fig. 1, a method for synchronously producing iron oxide black by producing organic products by an iron powder reduction method comprises the processes of reduction reaction, filtration, water washing, screening, filtration, drying and grinding, and comprises the following steps:
(1) reduction reaction: putting iron powder, a reaction medium and water into a reduction reaction tank, heating and activating for 0.5-1 hour by steam, wherein the reaction temperature is 50-95 ℃, the reaction pressure is normal pressure, the stirring speed is 60-120 r/min, the pH value in the reduction reaction tank is 5-8, an aromatic nitro compound or a quinone compound is continuously dripped in the reaction process, iron powder, the reaction medium and water are discontinuously supplemented, the weight ratio of the aromatic nitro compound or the quinone compound, the iron powder, the reaction medium and the water is always maintained to be 1: 0.5-1.5: 0.01-0.1: 2-5, and the suspended substance of the aromatic amino compound or the phenol compound and the iron mud is continuously discharged from a discharge port of the reduction reaction tank;
(2) and (3) filtering: filtering suspended matters generated in the reaction in the step (1) to obtain a solid-phase substance A;
(3) washing: washing the solid-phase substance A in the step (2) by heating water until supernatant liquor is colorless, wherein the temperature of the heating water is 50-90 ℃;
(4) screening: screening the suspension B washed in the step (3) by a drum screen, wherein the screen mesh is 200-500 meshes, and obtaining a screen underflow B;
(5) and (3) filtering: filtering the undersize product B in the step (4) to obtain a solid phase product B;
(6) and (3) drying: and drying the solid phase substance B to obtain an iron oxide black product, wherein the drying temperature is 50-250 ℃, and the drying time is 30-90 minutes.
(1) The reaction medium is one or more of ferrous sulfate, ferrous chloride, dilute hydrochloric acid, dilute nitric acid, ferrous nitrate and ammonium chloride.
(2) The main components of the solid-phase substance A are iron mud and iron powder, and the main component of the iron mud is ferroferric oxide.
(4) The suspension B is the water suspension of iron mud and iron powder, and the undersize B is the water suspension of iron mud.
(5) The solid-phase material B is iron mud, and the main component of the iron mud is ferroferric oxide.
The reaction formula is exemplified:
example 1:
taking 85 g of iron powder, 8 g of ferrous nitrate and 150 ml of water, simultaneously adding the iron powder, the ferrous nitrate and the water into a 2000 ml container (with a discharge port at the upper part), starting a paddle stirrer to stir and disperse, heating to react for 1 hour, controlling the pH of the solution to be 5, slowly dropwise adding 770 ml of 10% p-benzoquinone solution into the solution, supplementing 85 g of ironpowder, 8 g of ferrous nitrate and 150 ml of water once after the p-benzoquinone solution is completely dripped, and then continuously dropwise adding 770 ml of the p-benzoquinone solution. The stirring speed was controlled at 80 rpm. And filtering 900 ml of the discharged suspension, washing a filter cake by adding hot water until the supernatant is colorless after washing, then sieving (the aperture of a sieve mesh is less than 45 microns), filtering, putting solid-phase iron mud into a CLS101-E type oven, drying at 65-75 ℃, and grinding to obtain a finished product of ferroferric oxide of 102 g. The tinting strength is detected to be 100 percent (compared with the standard sample), and the content of ferroferric oxide is detected to be 95 percent.
Example 2:
adding 1.4 tons of iron powder, 40 kilograms of ferrous chloride, 40 kilograms of ferrous sulfate and 2500 liters of water into a 5000 liter stainless steel reaction tank, starting a paddle type stirrer to stir and disperse, heating to 80 ℃, reacting for 2 hours, controlling the pH of the solution to be 6, slowly dropwise adding 1000 liters of nitrobenzene solution into the reaction tank, supplementing 1.4 tons of iron powder, 40 kilograms of ferrous chloride, 40 kilograms of ferrous sulfate and 2500 liters of water for one time after all nitrobenzene is dropwise added, and then continuously dropwise adding 1000 liters of nitrobenzene solution. The stirring speed was controlled at 85 rpm. Filtering 3800L of the discharged suspension, washing a filter cake with hot water until the supernatant is colorless, sieving (the mesh size is less than 45 micrometers), filtering, and drying the solid-phase iron mud in a GSX800 type flash evaporation dryer at the temperature of 200 ℃ to obtain 1.68 tons of finished ferroferric oxide. The detected tinting strength is 105 percent (compared with a standard sample), and the ferroferric oxide content is 94 percent.
Claims (5)
1. A method for synchronously producing iron oxide black by producing organic products by an iron powder reduction method comprises the processes of reduction reaction, filtration, water washing, screening, filtration, drying and grinding, and is characterized in that:
(1) reduction reaction: putting iron powder, a reaction medium and water into a reduction reaction tank, heating and activating for 0.5-1 hour by steam, wherein the reaction temperature is 50-95 ℃, the reaction pressure is normal pressure, the stirring speed is 60-120 r/min, the pH value in the reduction reaction tank is 5-8, an aromatic nitro compound or a quinone compound is continuously dripped in the reaction process, iron powder, the reaction medium and water are discontinuously supplemented, the weight ratio of the aromatic nitro compound or the quinone compound, the iron powder, the reaction medium and the water is always maintained to be 1: 0.5-1.5: 0.01-0.1: 2-5, and the suspended substance of the aromatic amino compound or the phenol compound and the iron mud is continuously discharged from a discharge port of the reduction reaction tank;
(2) and (3) filtering: filtering suspended matters generated in the reaction in the step (1) to obtain a solid-phase substance A;
(3) washing: washing the solid-phase substance A in the step (2) by heating water until supernatant liquor is colorless, wherein the temperature of the heating water is 50-90 ℃;
(4) screening: screening the suspension B washed in the step (3) by a drum screen, wherein the screen mesh is 200-500 meshes, and obtaining a screen underflow B;
(5) and (3) filtering: filtering the undersize product B in the step (4) to obtain a solid phase product B;
(6) and (3) drying: and drying the solid phase substance B to obtain an iron oxide black product, wherein the drying temperature is 50-250 ℃, and the drying time is 30-90 minutes.
2. The method for synchronously producing the black iron oxide by producing the organic products by the iron powder reduction method according to claim 1, which is characterized in that: (1) the reaction medium is one or more of ferrous sulfate, ferrous chloride, dilute hydrochloric acid, dilute nitric acid, ferrous nitrate and ammonium chloride.
3. The method for synchronously producing the black iron oxide by producing the organic products by the iron powder reduction method according to claim 1, which is characterized in that: (2) the main components of the solid-phase substance A are iron mud and iron powder, and the main component of the iron mud is ferroferric oxide.
4. The method for synchronously producing the black iron oxide by producing the organic products by the iron powder reduction method according to claim 1, which is characterized in that: (4) the suspension B is the water suspension of iron mud and iron powder, and the undersize B is the water suspension of iron mud.
5. The method for synchronously producing the black iron oxide by producing the organic products by the iron powder reduction method according to claim 1, which is characterized in that: (5) the solid-phase material B is iron mud, and the main component of the iron mud is ferroferric oxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03128113 CN1223553C (en) | 2003-06-03 | 2003-06-03 | Iron powder reducing method for simultaneously producing organic product and ferric oxide black |
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| CN 03128113 CN1223553C (en) | 2003-06-03 | 2003-06-03 | Iron powder reducing method for simultaneously producing organic product and ferric oxide black |
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| CN1223553C true CN1223553C (en) | 2005-10-19 |
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| CN 03128113 Expired - Fee Related CN1223553C (en) | 2003-06-03 | 2003-06-03 | Iron powder reducing method for simultaneously producing organic product and ferric oxide black |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100422088C (en) * | 2004-12-23 | 2008-10-01 | 湖北开元化工科技股份有限公司 | Method for preparing iron oxide black by reducing nitrobenzene using ferrous powder with side product of aniline sulfate salts |
| CN102616864A (en) * | 2012-04-17 | 2012-08-01 | 河南创力新能源科技有限公司 | Method for manufacturing ferroferric oxide for iron electrode |
| CN106629862B (en) * | 2016-12-22 | 2019-03-19 | 广州市群笑化工颜料有限公司 | With the method for fluorine titanium mother liquor production iron oxide black |
| CN109761860A (en) * | 2019-02-28 | 2019-05-17 | 河北诚信集团有限公司 | A method of reduction nitryl aromatic race substituent prepares amino aromatic series substituent |
| CN111233045B (en) * | 2019-12-25 | 2021-09-07 | 河北彩客化学股份有限公司 | Method for preparing iron oxide red pigment and synchronously producing aromatic amine |
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