CN104607128A - Reactor and method used for preparing iron oxide via circulation precipitation - Google Patents
Reactor and method used for preparing iron oxide via circulation precipitation Download PDFInfo
- Publication number
- CN104607128A CN104607128A CN201310535232.2A CN201310535232A CN104607128A CN 104607128 A CN104607128 A CN 104607128A CN 201310535232 A CN201310535232 A CN 201310535232A CN 104607128 A CN104607128 A CN 104607128A
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- Prior art keywords
- retort
- reaction
- inner core
- main shaft
- paddle
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001556 precipitation Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 238000005273 aeration Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 7
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 13
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 35
- 235000013980 iron oxide Nutrition 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00184—Controlling or regulating processes controlling the weight of reactants in the reactor vessel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a reactor and a method used for preparing iron oxide via circulation precipitation. The reactor is composed of a reaction tank, an inner barrel body, a variable frequency motor, a main shaft, stirring paddles, a heating coil pipe, and bottom aeration discs; the inner barrel body is arranged in the reaction tank; the top of the reaction tank is provided with the variable frequency motor and the main shaft; the main shaft is provided with two sets of the stirring paddles; the bottom of the reaction tank is provided with the aeration discs and the heating coil pipe; stirring speed is controlled by the variable frequency motor, and the variable frequency motor is controlled by a frequency converter, so that mixing uniformity of liquid in the reaction tank is controlled; air needed by reaction is delivered through the bottom aeration discs; reaction liquid in the inner barrel body is driven by rising of air, and overflows the inner barrel body; reaction liquid outside the inner barrel body flows downward so as to form a circulation loop; reaction materials in the reaction tank are mixed fully, after a certain time of reaction, reaction is stopped until states of color paste in the reaction tank accords with needed states.
Description
Technical field
The present invention relates to the reactor preparing iron in a kind of inorganic pigment iron oxide production system and technique, be specifically related to reactor and technique that a kind of circulation type precipitation method prepare iron oxide.
Background technology
Iron oxide is a kind of important inorganic chemistry pigment, is widely used in coating, the fields such as building and traffic.At present, the production method of iron oxide pigment comprises dry method and wet method.Produce a large amount of waste gas in the process of dry production iron oxide, environmental pollution is more serious; Wet method is the industrial method generally adopted at present, manufactures in the production technology of iron oxide, generally adopt cylindric retort to react in wet method.Reaction raw materials copperas solution adds in retort, adds sodium hydroxide solution and regulates pH value, at a certain temperature, air is passed into bottom retort, and constantly stirring makes it reaction, progressively add iron filings and participate in reaction, until mill base reaches required state in retort.Now, stop reaction, reaction material is pumped into filter element, after through washing.Drying and packaging, be finished product.
In the process of wet method reaction production iron oxides inorganic pigment, the mixability of reaction raw materials has important impact to reaction efficiency and product quality, only has gas-liquid-solid fully to contact, and just can reach the consumption that economizes in raw materials, and raises the efficiency the object with product quality.In order to reach the object stirred, usual retort is equipped with the very large motor of power and drives paddle, and operation energy consumption is higher.Along with the demand of iron oxide constantly increases, the volume of the retort of newly-built employing also increases gradually.In the case, require that in reactor, gas-liquid-solid Flow Field Distribution is very even, requires reaction technology and the device of design novel energy-conserving on the other hand on the one hand.And in report disclosed at present, rarely have the reactor design preparing iron oxide, such as patent of invention " wet method manufactures technique and the preparation of iron oxide red " (CN1143049A) discloses a kind of production technology of iron oxide red, but requires simpler to consersion unit.Along with the increase of retort, the paddle shaft power that device adopts significantly promotes, and plant running energy consumption strengthens gradually, needs the reactor to preparing iron oxide to carry out appropriate design.
Summary of the invention
The object of the present invention is to provide a kind of circulation type precipitation method to prepare the reactor of iron oxide, to substitute traditional high-power stirring reaction bucket, significantly reduce speed of agitator, realize the effect reducing energy consumption; Another object of the present invention be to provide the technique utilizing above-mentioned reactor to prepare iron oxide.
Technical scheme of the present invention: a kind of circulation type precipitation method prepare the reactor of iron oxide, is made up of retort, inner core, variable-frequency motor, main shaft, paddle, heat(ing) coil, aeration plate, pollution discharge joint and thermometer; Wherein, be provided with inner core in retort, inner core lower side has return port.Retort center is provided with main shaft, spindle top installs variable-frequency motor, first paddle is installed in the middle part of main shaft, main shaft bottom is provided with the second paddle, bottom retort, aeration plate is housed, and is provided with heat(ing) coil above aeration plate, second paddle is positioned at above heat(ing) coil, first paddle is positioned at the middle and upper part of inner core, is provided with blowdown interface below retort side, and thermometer is arranged on middle and upper part outside retort.Utilize Frequency Converter Control variable-frequency motor, realize different stir speed (S.S.), control reaction pot liquid mixture homogeneity; Bottom aeration plate passes into the air needed for reaction, and air rises and drives inner barrel reactant liquor rise and overflow to outside inner core, and outside inner core, reactant liquor flows downward and forms backflow.
Preferred described retort height is 2-10m, and retort ratio of height to diameter is 1-3:1.Preferred inner barrel effective depth 10-50cm lower than retort.Preferred reaction tank is 1.2-2:1 with the ratio of inner diameter of steel flue.
At the bottom of described inner core (4) lower side distance tank, 10-100cm place surrounding evenly has return port (7), and the area of each return port is 25-100cm2; The number of return port is 10-200; Sky can be other shapes such as circular hole or square hole.
The material of described retort is carbon steel, the acid-alkali-corrosive-resisting material such as stainless steel or titanium material of inside lining anti-corrosive brick; Inner core material is the acid-alkali-corrosive-resisting material such as stainless steel or titanium material.
Present invention also offers the technique utilizing above-mentioned reactor to prepare iron oxide, its concrete steps are as follows: add in retort by reaction raw materials copperas solution from retort top, add sodium hydroxide solution regulates ph value for 8-10 simultaneously, heat(ing) coil passes into Steam Heating to 75-90 degree, air is passed into aeration plate bottom retort, tolerance is 10-10000L/min, start variable-frequency motor and drive paddle Stirring, speed of agitator is that 5-200 turns/min, the air driven reactant liquor that aeration plate enters bottom retort upwards flows into retort inner core top, after be spilled over to reaction mass in retort and fully mix, after reaction a period of time, until when in retort, mill base reaches required state, stop reaction.
Accompanying drawing explanation
Fig. 1 is the present invention prepares the circulating reactor of iron oxide structural representation for the precipitation method, wherein 1, variable-frequency motor, 2, main shaft, 3, retort, 4, inner core, 5A, the first paddle, 5B, the second paddle, 6, heat(ing) coil, 7, return port, 8, aeration plate, 9, blowdown interface, 10, thermometer.
Detailed description of the invention
Embodiment 1:
The structural representation of reactor of the present invention is as shown in Figure 1: a kind of circulation type precipitation method prepare the reactor of iron oxide, by retort, inner core, variable-frequency motor.Main shaft, paddle, heat(ing) coil, aeration plate, blowdown interface and thermometer composition; Wherein, be provided with inner core in retort, inner core lower side has return port, retort center is provided with main shaft, spindle top installs variable-frequency motor, and install the first paddle in the middle part of main shaft, main shaft bottom is provided with the second paddle, bottom retort, aeration plate is housed, be provided with heat(ing) coil above aeration plate, the second paddle is positioned at above heat(ing) coil, and the first paddle is positioned at the middle and upper part of inner core, be provided with blowdown interface below retort side, thermometer is arranged on middle and upper part outside retort.
Wherein retort height is 2m, and retort ratio of height to diameter is 1; Inner barrel effective depth compares retort urceolus 10cm; At the bottom of inner core side lower distance tank, 10cm place evenly has area is 25cm
2circular hole, empty number is 200; Retort urceolus is 2 with the ratio of inner diameter of steel flue; Retort material is the carbon steel of inside lining anti-corrosive brick, and inner core material is 316L stainless steel.
Reaction raw materials copperas solution is added (liquid level is to inner core top) in retort, adding sodium hydroxide solution regulates ph value to be 8, heat(ing) coil passes into steam to 75 and spends, air is passed into aeration plate bottom retort, tolerance is 10L/min, start variable-frequency motor and drive paddle Stirring, speed of agitator is 5 turns/min, the air driven reactant liquor that aeration plate enters bottom retort upwards flows into retort inner core top, after be spilled over to space between retort and inner core and flow downward, enter inner core inside bottom through the perforate of inner core bottom and form circulation, reaction mass in retort is fully mixed, after reaction 1.5h, when in retort, mill base reaches corresponding standard in GB/T1863-2008, stop reaction, compared with traditional reactor, reaction time shortens 1.5h.
Embodiment 2:
The present embodiment structure of reactor is with embodiment 1, and wherein retort height is 10m, and retort ratio of height to diameter is 3; Inner barrel effective depth compares retort urceolus 50cm; At the bottom of inner core side lower distance tank, 100cm place evenly has area is 1000cm
2circular hole, empty number is 10; Retort urceolus is 1.2 with the ratio of inner diameter of steel flue; Retort material is 316L stainless steel, and inner core material is titanium material.
Reaction raw materials copperas solution is added (liquid level is to inner core top) in retort, adding sodium hydroxide solution regulates ph value to be 10, heat(ing) coil passes into steam to 90 and spends, air is passed into aeration plate bottom retort, tolerance is 10000L/min, start variable-frequency motor and drive paddle Stirring, speed of agitator is 200 turns/min, the air driven reactant liquor that aeration plate enters bottom retort upwards flows into retort inner core top, after be spilled over to space between retort and inner core and flow downward, enter inner core inside bottom through the perforate of inner core bottom and form circulation, reaction mass in retort is fully mixed, after reaction 2.5h, when in retort, mill base reaches corresponding standard in GB/T1863-2008, stop reaction, compared with traditional reactor, reaction time shortens 2h.
Embodiment 3:
The present embodiment structure of reactor is with embodiment 1, and wherein retort height is 5m, and retort ratio of height to diameter is 2; Inner barrel effective depth compares retort urceolus 30cm; At the bottom of inner core side lower distance tank, 50cm place evenly has area is 250cm
2circular hole, empty number is 100; Retort urceolus is 1.6 with the ratio of inner diameter of steel flue; Retort material is titanium material, and inner core material is titanium material.
Reaction raw materials copperas solution is added (liquid level is to inner core top) in retort, adding sodium hydroxide solution regulates ph value to be 9, heat(ing) coil passes into steam to 80 and spends, air is passed into aeration plate bottom retort, tolerance is 4000L/min, start variable-frequency motor and drive paddle Stirring, speed of agitator is 90 turns/min, the air driven reactant liquor that aeration plate enters bottom retort upwards flows into retort inner core top, after be spilled over to space between retort and inner core and flow downward, enter inner core inside bottom through the perforate of inner core bottom and form circulation, reaction mass in retort is fully mixed, after reaction 2.3h, when in retort, mill base reaches corresponding standard in GB/T1863-2008, stop reaction, compared with traditional reactor, reaction time shortens 2h.
Claims (6)
1. the circulation type precipitation method prepare a reactor for iron oxide, are made up of retort (3), inner core (4), variable-frequency motor (1), main shaft (2), paddle, heat(ing) coil (6), aeration plate (8), pollution discharge joint (9) and thermometer (10); Wherein, be provided with inner core (4) in retort (3), inner core (4) lower side has return port (7).Retort (3) center is provided with main shaft (2), variable-frequency motor (1) is installed at main shaft (2) top, the first paddle (5A) is installed at main shaft (2) middle part, main shaft (2) bottom is provided with the second paddle (5B), aeration plate (8) is equipped with in retort (3) bottom, aeration plate (8) top is provided with heat(ing) coil (6), second paddle (5B) is positioned at heat(ing) coil (6) top, first paddle (5A) is positioned at the middle and upper part of inner core (4), blowdown interface (9) is installed below retort (3) side, thermometer (10) is arranged on middle and upper part, retort (3) outside.
2. reactor according to claim 1, it is characterized in that described retort (3) is highly 2-10m, retort (3) ratio of height to diameter is 1-3:1.
3. reactor according to claim 1, is characterized in that described inner core (4) aspect ratio retort (3) low 10-50cm.
4. reactor according to claim 1, it is characterized in that at the bottom of described inner core (4) lower side distance tank, 10-100cm place surrounding evenly has return port (7), the area of each return port is 25-100cm2; The number of return port is 10-200.
5. reactor according to claim 1, is characterized in that described retort and inner diameter of steel flue are than being 1.2-2:1.
6. a reactor according to claim 1 prepares the technique of iron oxide, its concrete steps are as follows: add in retort by reaction raw materials copperas solution from retort top, add sodium hydroxide solution regulates ph value for 8-10 simultaneously, heat(ing) coil passes into Steam Heating to 75-90 degree, air is passed into aeration plate bottom retort, tolerance is 10-10000L/min, start variable-frequency motor and drive paddle Stirring, speed of agitator is that 5-200 turns/min, the air driven reactant liquor that aeration plate enters bottom retort upwards flows into retort inner core top, after be spilled over to reaction mass in retort and fully mix, after reaction a period of time, until when in retort, mill base reaches required state, stop reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310535232.2A CN104607128A (en) | 2013-11-04 | 2013-11-04 | Reactor and method used for preparing iron oxide via circulation precipitation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310535232.2A CN104607128A (en) | 2013-11-04 | 2013-11-04 | Reactor and method used for preparing iron oxide via circulation precipitation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104607128A true CN104607128A (en) | 2015-05-13 |
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ID=53141932
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310535232.2A Pending CN104607128A (en) | 2013-11-04 | 2013-11-04 | Reactor and method used for preparing iron oxide via circulation precipitation |
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| CN (1) | CN104607128A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3581266A4 (en) * | 2017-02-08 | 2020-12-30 | Zhengzhou Gaofu Fertilizer Co., Ltd | Continuous reactor |
| CN115124085A (en) * | 2022-07-27 | 2022-09-30 | 宁波一品生物技术有限公司 | Preparation method and device of iron oxide red |
-
2013
- 2013-11-04 CN CN201310535232.2A patent/CN104607128A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3581266A4 (en) * | 2017-02-08 | 2020-12-30 | Zhengzhou Gaofu Fertilizer Co., Ltd | Continuous reactor |
| CN115124085A (en) * | 2022-07-27 | 2022-09-30 | 宁波一品生物技术有限公司 | Preparation method and device of iron oxide red |
| CN115124085B (en) * | 2022-07-27 | 2024-01-02 | 宁波一品生物技术有限公司 | Preparation method and device of iron oxide red |
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| C06 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150513 |
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| WD01 | Invention patent application deemed withdrawn after publication |