CN102139921A - Preparation method for producing chromate by continuous liquid-phase oxidation reaction tower - Google Patents

Preparation method for producing chromate by continuous liquid-phase oxidation reaction tower Download PDF

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CN102139921A
CN102139921A CN2011100356421A CN201110035642A CN102139921A CN 102139921 A CN102139921 A CN 102139921A CN 2011100356421 A CN2011100356421 A CN 2011100356421A CN 201110035642 A CN201110035642 A CN 201110035642A CN 102139921 A CN102139921 A CN 102139921A
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tower
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reaction tower
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李守昌
李正国
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Chongqing Changyuan Chemical Corp Ltd
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Chongqing Changyuan Chemical Corp Ltd
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Abstract

The invention relates to a preparation method for producing chromate by a continuous liquid-phase oxidation reaction tower, which comprises the following steps of: mixing sodium hydroxide (potassium hydroxide) and chromium mineral powder (chromium iron powder), which serve as raw materials, and heating to prepare blended slurry; and adding caustic soda liquid which is preheated to the temperature of between 300 and 450 DEG C from a feed inlet of the continuous liquid-phase oxidation reaction tower, introducing compressed air of which the flow is between 10 and 60 m<3>/minute and of which the temperature is between 150 and 300 DEG C from the bottom of the reaction tower, adding the preheated blended slurry from the top of the reaction tower, performing a continuous liquid-phase oxidizing reaction at the temperature of between 250 and 350 DEG C under the inlet pressure of between 0.45 and 0.80 MPa of the compressed air in the reaction tower for 1.5 to 6 hours, diluting reaction material liquid which is separated initially in the tower, and performing solid-liquid separation to obtain the chromate. The method has the advantages of relieving the labor strength of production workers, along with continuous production process, safety, environmental protection, economic operation, low production cost, low energy consumption, few waste residues, no exhaust gas and waste water and the like, and can be widely used for producing the chromate.

Description

A kind of continuous liquid phase oxidation reaction tower is produced the preparation technology of chromic salt
Technical field
The invention belongs to the preparation technology of chromic salt, saying so with sodium hydroxide (potassium), chromite ore fine or siderochrome powder etc. in more detail is raw material, through the preparation technology of continuous liquid phase oxidation reaction tower production chromic salt.
Background technology
Chromic salt is important Inorganic Chemicals, generally is applied to industries such as chemical industry, metallurgical industry, plating, process hides.Existing chromic salt suitability for industrialized production technology is to add in chromite ore fine after yellow soda ash and rhombspar, Wingdale mix, and in temperature roasting more than 1000 ℃, reaction back grog obtains chromium acid sodium alkaline liquid through leaching at rotary kiln.It has energy consumption height, chromium yield low, seriously polluted, weak points such as direct labor's labour intensity height.
At CN10152476.1, denomination of invention be " chromic salt efficient, energy-conservation, the cleaning manufacture method " document in, disclosing a kind of employing ferrochrome is raw material, carrying out oxidation at High Temperature High Pressure alkali lye in mutually melts, through after the decrease temperature and pressure, solid-liquid separation, the mixture of acquisition chromatedsolution, water and ferric oxide, chromic oxide.It has advantages such as energy-conservation, no waste gas, no waste residue, no waste water generation, its weak point is in process of production, need at 4MP-22MP, preferably oxidation stripping in the high-temperature high-pressure reaction kettle of the highly compressed belt stirrer of 8MP-12MP, have in production technique, increased unsafe factor, sealing material and part requirement performance high and can not continuous production etc. weak point.
At CN101481144A, denomination of invention be in the document of " a kind of clean preparation method of preparing potassium chromate from chromic iron " and the CN101659444A denomination of invention in the document of " a kind of clean preparation method of preparing sodium chromate from chromite ", chromite is disclosed at KOH-KNO 3-H 2Oxidizing gas reacts in the O medium, and nitrate only uses as catalyzer, obtains the reaction product mixture of alkali lye, Sodium chromate (potassium) and scum after the reaction.Reaction product mixture is separated with the liquid-solid of brilliant slag mixture through leaching, alkali lye, the dissolving of scum and Sodium chromate (potassium) mixture, the solid-liquid separation of scum and Sodium chromate (potassium) solution, Sodium chromate (potassium) is carried out evaporative crystallization, and to after Sodium chromate (potassium) the crystal drip washing and drying that obtain, make Sodium chromate (potassium), crystalline mother solution recycles with alkali lye, is used to decompose chromite.Its temperature that responds low (280 ℃-400 ℃), chromium transformation efficiency height, chromium content is low in the slag, bed drain purge is few, can not produce advantages such as environmentally harmful dust and exhaust emission.Its weak point has complex manufacturing, reaction times long etc.
Weak point in view of above technology, present inventors are through with keen determination research for many years, discovery is a raw material with sodium hydroxide (potassium) and chromite ore fine etc., feeds preheated air and can prepare chromic salt continuously under continuously liquid phase oxidation reaction tower and certain temperature, pressure, has so far finished the present invention.
Summary of the invention
The purpose of this invention is to provide that a kind of raw material ore deposit consumption is low, sodium hydroxide (potassium) alkali lye can recycle, the transformation efficiency height of chromium sesquioxide, Chrome-free dust, no waste gas, no Cr 6+The preparation technology of the chromic salt of residue contamination.
It is low that second purpose of the present invention provides a kind of production energy consumption, production security height, but the preparation technology of the continuous production chromic salt of the labour intensity that the reduction workman produces.
But the preparation technology of the continuous production chromic salt that the 3rd purpose of the present invention provides that a kind of production technique is easy, the reaction times is short, production cost is low etc.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is:
A kind of continuous liquid phase oxidation reaction tower is produced the preparation technology of chromic salt, and its production technique mainly contains:
(1) in mixed powder container (52) with sodium hydroxide (potassium) with contain Cr 2O 3Chromite ore fine more than 35% is made the slip that is mixed, its sodium hydroxide (potassium): chromite ore fine: the mixing quality percentage of water is 10%-30%: 40%-10%: 50%-60%, and the slip that will be mixed in chromium powder preheating bucket (5) is preheating to 50-200 ℃;
(2) be to be pumped in the continuous liquid phase oxidation reaction tower (26) with pump after sodium hydroxide (potassium) more than 48% is preheated to 300~450 ℃ massfraction, when temperature in the tower reached 180 ℃-250 ℃, sending into flow from the inlet mouth (30) of tower was 10-60M 3/ min, temperature are 150-300 ℃ pressurized air;
(3) add the slip that is mixed of preheating from the top (33) of reaction tower, keeping the pressurized air intake pressure is 0.45-0.8MPa, tower top pressure 0.18-0.36MPa, chromite ore fine (ferrochrome powder): sodium hydroxide (potassium) mass ratio is 1: 0.75-5, carried out under 250-350 ℃ of temperature oxidizing reaction 1.5-6 hour;
(4) store the bucket (41) to low level from outlet (29) discharging of reaction tower through the chromic salt feed liquid of initial gross separation, after using water in rare bucket (51) to be diluted to the 25-70% mass percent concentration then, with pump low level is stored material after bucket (41) dilution and pump in the solid-liquid separator (44) and carry out solid-liquid separation.
A kind of preparation technology of chromic salt, it is characterized in that continuous adding is preheating to 50-200 ℃ the slip that is mixed, is preheating to 300~450 ℃ sodium hydroxide (potassium) and is preheating to 150-300 ℃ pressurized air in continuous liquid phase oxidation reaction tower, is to produce chromic salt under 250-350 ℃ continuously keeping continuous liquid phase oxidation reaction tower temperature.
A kind of preparation technology of chromic salt is characterized in that the described slip that is mixed can be mixed with the slip that is mixed with washing chromium slag or other alkali lye, sodium hydroxide (potassium) alkali lye and chromite ore fine of producing diluted alkaline water, recycle.
A kind of preparation technology of chromic salt, it is characterized in that alkali lye that chromic salt mixture through continuous liquid phase oxidation reaction production is containing the 20-45% mass percent concentration store be cooled to 90-120 ℃ of temperature in the bucket (41) after, carry out solid-liquid separation with concentrated, crystallisation by cooling sedimentation method for separating.
A kind of preparation technology of chromic salt, it is characterized in that with the stack gas after the dedusting (23) and stack gas (14) respectively to chromium powder preheating bucket (5), alkali lye preheating bucket (6), continuously liquid phase oxidation reaction tower (26), pressurized air (36) heats and be incubated.
Perhaps when adopting the ferrochrome powder, can adopt following steps:
(1) in mixed powder container (52) with sodium hydroxide (potassium) with contain Cr 2O 3Ferrochrome powder more than 60% is made the slip that is mixed, its sodium hydroxide (potassium): ferrochrome powder: the mixing quality percentage of water is 10%-30%: 40%-10%: 50%-60%, and the slip that will be mixed in chromium powder preheating bucket (5) is preheating to 50-200 ℃;
(2) be to be pumped in the continuous liquid phase oxidation reaction tower (26) with pump after sodium hydroxide (potassium) more than 48% is preheated to 300~450 ℃ concentration, when temperature in the tower reached 180 ℃-250 ℃, sending into flow from the inlet mouth (30) of tower was 10-60M 3/ min, temperature are 150-300 ℃ pressurized air;
(3) add the preheating slip that is mixed from the top (33) of reaction tower, keeping the pressurized air intake pressure is that 0.45-0.8MPa, tower top pressure are 0.18-0.36MPa, carries out under 250-350 ℃ of temperature oxidizing reaction 1.5-6 hour;
(4) be diluted to the 25-70% mass percent concentration through the chromic salt feed liquid of initial gross separation and carry out solid-liquid separation.
A kind of preparation technology of chromic salt, it is characterized in that through the alkali lye that the chromic salt mixture that continuous liquid phase oxidation reaction generates is containing the 20-45% mass percent concentration store be cooled to 90-120 ℃ of temperature in the bucket (41) after, carry out solid-liquid separation with concentrated, crystallisation by cooling sedimentation method for separating.
A kind of preparation technology of chromic salt, it is characterized in that with the stack gas after the dedusting (23) and stack gas (14) respectively to chromium powder preheating bucket (5), alkali lye preheating bucket (6), continuously liquid phase oxidation reaction tower (26), pressurized air (36) heats and be incubated.
Table 1 is an effect comparison table of the present invention
Table 1
Figure BSA00000432098800031
The preparation technology that a kind of continuous liquid phase oxidation reaction tower of the present invention is produced chromic salt, production technique continuously, safety, environmental protection, economical operation, production cost is low, energy consumption is low, alleviated direct labor's labour intensity, waste residue is few, advantages such as no waste gas, no waste water can be widely used in the production of chromic salt salt.
Description of drawings
Accompanying drawing 1 is a process flow sheet of the present invention
Accompanying drawing 2 is structure iron of continuous liquid phase oxidation reaction device of the present invention
1. induced draft fan; 2. flue gas outlet; 3. the chromium powder slurry outlet that is mixed; 4 chromium powder mixed ingredients slurry inlets; 5. chromium powder preheating bucket; 6. alkali lye preheating bucket; 7. flue gas outlet; 8. alkali lye import; 9. agitator; 10. alkali lye outlet; 11. pre-thermal jacket; 12. stack gas import; 13. secondary kitchen range cleaning apparatus; 14. secondary kitchen range reciprocating furnace flue gas outlet; 15. secondary kitchen range; 16. reciprocating furnace; 17. secondary pot 1; 18. secondary pot 2; 19. main kitchen range; 20. reciprocating furnace; 21. main pot 1; 22. main pot 2; 23. main kitchen range reciprocating furnace flue gas outlet; 24. main kitchen range cleaning apparatus; 25. reaction mass alkali lye import; 26. continuous liquid phase oxidation reaction tower; 27. heat required chuck outward; 28. stack gas import; 29. reacted material outlet; 30. participate in the gas feed of reaction; 31. tapered tower tray; 32. flue gas outlet; 33. reaction mass chromium powder import; 34. reaction back pneumatic outlet; 35. air preheater; 36. air intlet; 37. reacted gas feed; 38. pneumatic outlet; 39. material outlet; 40. gas-liquid separator; 41. store bucket; 42. material inlet; 43. material outlet; 44. separator; 45. material outlet; 46. separator stack gas import; 47. the pre-thermal jacket of separator; 48. material inlet; 49. material outlet; 50. separator flue gas outlet; 51. rare bucket; 52. mix the powder container.
By embodiment the present invention is given further instruction below in conjunction with accompanying drawing
Embodiment 1:
With 3.96 tons of water, 1.04 tons of massfractions is that 96% NaOH adds to mix in the powder container and is mixed with 20%NaOH solution.
With 5 tons of 20%NaOH solution and content is Cr 2O 335.58%, Fe 2O 314.00%, Al 2O 310.09%, CaO0.48%, MgO 22.36%, SiO 212.13% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 315.81%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 200 ℃.
8 tons of NaOH liquid caustic soda that are preheated to 300 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 180 ℃ in tower, sends into 150 ℃, 10m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 250 ℃, keeps intake pressure 0.45Mpa, tower top pressure 0.18Mpa reaction 6 hours down, discharges Na from the discharge port of tower 2CrO 43.544 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 19.34%, the content 48.55% of NaOH.Feed liquid is diluted with water to 57.21% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 120 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
Get 3.04m 3Contain diluted alkaline water, 1.3m in the rare bucket of 2%NaOH 3The NaOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 20%NaOH solution
With 5 tons of 20%NaOH solution and content is Cr 2O 335.58%, Fe 2O 314.00%, Al 2O 310.09%, CaO0.48%, MgO 22.36%, SiO 212.13% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 315.81%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 200 ℃.
Discharging will be preheated to 300 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge Na from the discharge port of tower 2CrO 45.438 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 25.21%, the content 38.45% of NaOH.Feed liquid is diluted to 57.21% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 300 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 200 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge Na from the discharge port of tower 2CrO 44.888 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 28.05%, the content 33.57% of NaOH.Feed liquid is diluted to 57.21% mass percent concentration with the diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 300 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge all Na from the discharge port of tower 2CrO 48.982 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 22.89%, the content 42.43% of NaOH.Feed liquid is diluted to 57.21% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 120 ℃ carries out solid-liquid separation, the chromium slag is through repeatedly washing, slag washing water and system recoveries water are stored in rare bucket, with the slag specimen sampling analysis, contain chromium 5.48%, iron 22.41%, aluminium 16.15%, calcium 0.77%, magnesium 35.79%, silicon 19.41%, Cr in oxide compound 2O 3Transformation efficiency is 90.38%, and this produces Sodium chromate (not contain crystal water) 4.792 tons.
Embodiment 2:
With 4.219 tons of water, 0.781 ton of massfraction is that 96% NaOH adds to mix in the powder container and is mixed with 15%NaOH solution.
With 5 tons of 15%NaOH solution and content is Cr 2O 343.31%, Fe 2O 328.00%, Al 2O 314.24%, MgO 11.02%, SiO 24.49% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 319.25%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 150 ℃.
8 tons of NaOH liquid caustic soda that are preheated to 358 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 200 ℃ in tower, sends into 200 ℃, 11m from the inlet mouth of tower 3The pressurized air of/Min, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃ from the top of reaction tower, temperature heating in the tower is brought up to 280 ℃, keep intake pressure 0.60Mpa, tower top pressure 0.24Mpa to react 4.5 hours down, discharge Na from the discharge port of tower 2CrO 43.553 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 23.98%, the content 44.76% of NaOH.Feed liquid is diluted with water to 48.38% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 110 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 3.64m 3Contain diluted alkaline water, 0.9m in the rare bucket of 2%NaOH 3The NaOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 15%NaOH solution.
With 5 tons of 15%NaOH solution and content is Cr 2O 343.31%, Fe 2O 328.00%, Al 2O 314.24%, MgO 11.02%, SiO 24.49% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 20 319.25%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 150 ℃.
Discharging will be preheated to 358 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃.In tower, reacted 4.5 hours under 280 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge Na from the discharge port of tower 2CrO 45.455 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 31.23%, the content 33.55% of NaOH.Feed liquid is diluted to 48.38% mass percent concentration with the diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 358 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 150 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 4.5 hours under 280 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge Na from the discharge port of tower 2CrO 44.905 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 34.73%, the content 28.14% of NaOH.Feed liquid is diluted to 48.38% mass percent concentration with the diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 358 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃.In tower, reacted 4.5 hours under 280 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge all Na from the discharge port of tower 2CrO 49.008 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 28.37%, the content 37.97% of NaOH.Feed liquid is diluted to 48.38% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 110 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket, with the slag specimen sampling analysis through repeatedly washing, contain chromium 7.35%, iron 45.83%, aluminium 23.31%, magnesium 18.04%, silicon 7.35%, Cr in oxide compound 2O 3Transformation efficiency is 92.27%, and this produces Sodium chromate (not contain crystal water) 6.309 tons.
Embodiment 3:
With 3.698 tons of water, 1.302 tons of massfractions is that 96% NaOH adds to mix in the powder container and is mixed with 25%NaOH solution.
With 5 tons of 25%NaOH solution and content is Cr 2O 346.10%, Fe 2O 322.27%, Al 2O 318.36%, CaO1.09%, MgO 9.35%, SiO 22.83% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 320.49%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 100 ℃.
8 tons of NaOH liquid caustic soda that are preheated to 408 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 220 ℃ in tower, sends into 250 ℃, 13m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 310 ℃, keeps intake pressure 0.72Mpa, tower top pressure 0.30Mpa reaction 3 hours down, discharges Na from the discharge port of tower 2CrO 43.681 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 25.13%, the content 45.37% of NaOH.Feed liquid is diluted with water to 38.23% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 100 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 2.6m 3Contain diluted alkaline water, 1.6m in the rare bucket of 2%NaOH 3The NaOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 25%NaOH solution.
With 5 tons of 25%NaOH solution and content is Cr 2O 346.10%, Fe 2O 322.27%, Al 2O 318.36%, CaO1.09%, MgO 9.35%, SiO 22.83% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 320.49%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 100 ℃.
Discharging will be preheated to 408 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃.In tower, reacted 3 hours under 310 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge Na from the discharge port of tower 2CrO 45.713 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 32.38%, the content 34.84% of NaOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 408 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 100 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 3 hours under 310 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge Na from the discharge port of tower 2CrO 45.163 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 35.83%, the content 29.84% of NaOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 408 ℃ 1 ton of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃.In tower, reacted 3 hours under 310 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge all Na from the discharge port of tower 2CrO 49.394 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 29.54%, the content 38.96% of NaOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 100 ℃ carries out solid-liquid separation, the chromium slag is through repeatedly washing, slag washing water and system recoveries water are stored in rare bucket, with the slag specimen sampling analysis, contain chromium 4.78%, iron 39.34%, aluminium 32.43%, calcium 1.93%, magnesium 16.52%, silicon 5.00%, Cr in oxide compound 2O 3Transformation efficiency is 94.13%, and this produces Sodium chromate (not contain crystal water) 7.013 tons.
Embodiment 4:
With 3.438 tons of water, 1.562 tons of massfractions is that 96% NaOH adds to mix in the powder container and is mixed with 30%NaOH solution.
With 5 tons of 30%NaOH solution and content is Cr 2O 360.10%, Fe 2O 330.40%, C 7.10%, SiO 22.50% ferrochrome powder is mixed with 9 tons of ferrochrome powder mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 326.71%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 50 ℃.
8 tons of NaOH liquid caustic soda that are preheated to 450 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 250 ℃ in tower, sends into 300 ℃, 15m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 350 ℃, keeps intake pressure 0.80Mpa, tower top pressure 0.36Mpa reaction 1.5 hours down, discharges Na from the discharge port of tower 2CrO 44.236 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 29.27%, the content 48.08% of NaOH.Feed liquid is diluted with water to 27.70% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 90 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 1.98m 3Contain diluted alkaline water, 2m in the rare bucket of 2%NaOH 3The NaOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 30%NaOH solution.
With 5 tons of 30%NaOH solution and content is Cr 2O 360.10%, Fe 2O 330.40%, C 7.10%, SiO 22.50% ferrochrome powder is mixed with 9 tons of ferrochrome powder mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 326.71%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 50 ℃.
Discharging will be preheated to 450 ℃ 2 tons of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃.In tower, reacted 1.5 hours under 350 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge Na from the discharge port of tower 2CrO 46.822 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 36.35%, the content 39.92% of NaOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 450 ℃ 2 tons of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons 50 ℃ the ferrochrome powder mixed slurry of being preheated to.In tower, reacted 1.5 hours under 350 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge Na from the discharge port of tower 2CrO 46.272 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 39.54%, the content 36.24% of NaOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 450 ℃ 2 tons of NaOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃.In tower, reacted 1.5 hours under 350 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge all Na from the discharge port of tower 2CrO 49.958 tons of mixed liquors are stored in the bucket, through sampling analysis Na to low level 2CrO 4Content 37.35%, the content 38.75% of NaOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 90 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing, with the slag specimen sampling analysis, contains chromium 5.56%, iron 87.27%, silicon 7.18%, Cr in oxide compound 2O 3Transformation efficiency is 96.78%, and this produces Sodium chromate (not contain crystal water) 9.605 tons.
Embodiment 5:
With 3.913 tons of water, 1.087 tons of massfractions is to be mixed with 20%KOH solution in the mixed powder container of 92%KOH adding.
With 5 tons of 20%KOH solution and content is Cr 2O 335.58%, Fe 2O 314.00%, Al 2O 310.09%, CaO0.48%, MgO 22.36%, SiO 212.13% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 315.81%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 200 ℃.
8 tons of KOH liquid caustic soda that are preheated to 300 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 180 ℃ in tower, sends into 150 ℃, 10m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 250 ℃, keeps intake pressure 0.45Mpa, tower top pressure 0.18Mpa reaction 6 hours down, discharges K from the discharge port of tower 2CrO 43.544 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 23.63%, the content 44.85% of KOH.Feed liquid is diluted with water to 57.21% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 120 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 3.07m 3Contain diluted alkaline water, 1.26m in the rare bucket of 2%KOH 3The KOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 20%KOH solution.
With 5 tons of 20%KOH solution and content is Cr 2O 335.58%, Fe 2O 314.00%, Al 2O 310.09%, CaO0.48%, MgO 22.36%, SiO 212.13% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 315.81%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 200 ℃.
Discharging will be preheated to 300 ℃ 1 ton of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge K from the discharge port of tower 2CrO 45.439 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 30.80%, the content 33.62% of KOH.Feed liquid is diluted to 57.21% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 300 ℃ 1 ton of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 200 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge K from the discharge port of tower 2CrO 44.889 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 34.26%, the content 28.21% of KOH.Feed liquid is diluted to 57.21% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 300 ℃ 1 ton of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 200 ℃.In tower, reacted 6 hours under 250 ℃ of temperature, intake pressure 0.45Mpa, the tower top pressure 0.18Mpa, discharge all K from the discharge port of tower 2CrO 48.983 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 27.97%, the content 38.05% of KOH.Feed liquid is diluted to 57.21% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 120 ℃ carries out solid-liquid separation, the chromium slag is through repeatedly washing, slag washing water and system recoveries water are stored in rare bucket, with the slag specimen sampling analysis, contain chromium 4.53%, iron 22.63%, aluminium 16.31%, calcium 0.78%, magnesium 36.15%, silicon 19.61%, Cr in oxide compound 2O 3Transformation efficiency is 92.13%, and this produces potassiumchromate (not contain crystal water) 5.979 tons.
Embodiment 6:
With 4.185 tons of water, 0.815 ton of massfraction is to be mixed with 15%KOH solution in the mixed powder container of 92%KOH adding.
With 5 tons of 15%KOH solution and content is Cr 2O 343.31%, Fe 2O 328.00%, Al 2O 314.24%, MgO 11.02%, SiO 24.49% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 319.25%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 150 ℃.
8 tons of KOH liquid caustic soda that are preheated to 346 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 200 ℃ in tower, sends into 200 ℃, 11m from the inlet mouth of tower 3The pressurized air of/Min is to tower, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃ from the top of reaction tower, temperature heating in the tower is brought up to 270 ℃, keep intake pressure 0.60Mpa, tower top pressure 0.24Mpa to react 4.5 hours down, discharge K from the discharge port of tower 2CrO 43.553 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 28.92%, the content 40.37% of KOH.Feed liquid is diluted with water to 48.38% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 110 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 3.6m 3Contain diluted alkaline water, 0.9m in the rare bucket of 2%KOH 3The KOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 15%KOH solution.
With 5 tons of 15%KOH solution and content is Cr 2O 343.31%, Fe 2O 328.00%, Al 2O 314.24%, MgO 11.02%, SiO 24.49% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 319.25%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 150 ℃.
Discharging will be preheated to 346 ℃ 2 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃.In tower, reacted 4.5 hours under 270 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge K from the discharge port of tower 26.555 tons of CrO4 mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 31.35%, the content 36.90% of KOH.Feed liquid is diluted to 48.38% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 346 ℃ 2 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 150 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 4.5 hours under 270 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge K from the discharge port of tower 2CrO 46.005 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 34.22%, the content 32.79% of KOH.Feed liquid is diluted to 48.38% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 346 ℃ 1.5 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 150 ℃.In tower, reacted 4.5 hours under 270 ℃ of temperature, intake pressure 0.60Mpa, the tower top pressure 0.24Mpa, discharge all K from the discharge port of tower 2CrO 49.558 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 32.25%, the content 35.60% of KOH.Feed liquid is diluted to 48.38% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 110 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket, with the slag specimen sampling analysis through repeatedly washing, contain chromium 5.08%, iron 46.02%, aluminium 23.40%, magnesium 18.11%, silicon 7.38%, Cr in oxide compound 2O 3Transformation efficiency is 92.86%, and this produces potassiumchromate (not contain crystal water) 7.619 tons.
Embodiment 7:
With 3.642 tons of water, 1.358 tons of massfractions is to be mixed with 25%KOH solution in the mixed powder container of 92%KOH adding.
With 5 tons of 25%KOH solution and content is Cr 2O 346.10%, Fe 2O 322.27%, Al 2O 318.36%, CaO1.09%, MgO 9.35%, SiO 22.83% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 320.49%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 100 ℃.
8 tons of KOH liquid caustic soda that are preheated to 396 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 220 ℃ in tower, sends into 250 ℃, 13m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 300 ℃, keeps intake pressure 0.72Mpa, tower top pressure 0.30Mpa reaction 3 hours down, discharges K from the discharge port of tower 2CrO 43.681 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 30.36%, the content 40.74% of KOH.Feed liquid is diluted with water to 38.23% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 100 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 2.55m 3Contain diluted alkaline water, 1.6m in the rare bucket of 2%KOH 3The KOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 25%KOH solution.
With 5 tons of 25%KOH solution and content is Cr 2O 346.10%, Fe 2O 322.27%, Al 2O 318.36%, CaO1.09%, MgO 9.35%, SiO 22.83% chromite ore fine is mixed with 9 tons of chromite ore fine mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 320.49%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 100 ℃.
Discharging will be preheated to 396 ℃ 2 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃.In tower, reacted 3 hours under 300 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge K from the discharge port of tower 2CrO 46.813 tons of mixed liquors are stored in the bucket to low level, through the content 32.81% of sampling analysis K2CrO4, and the content 37.43% of KOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 396 ℃ 2 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons 100 ℃ the chromite ore fine mixed slurry of being preheated to.In tower, reacted 3 hours under 300 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge K from the discharge port of tower 2CrO 46.263 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 35.69%, the content 33.53% of KOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 396 ℃ 1.5 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 10 minutes, be pressed into 4.5 tons of chromite ore fine mixed slurries that are preheated to 100 ℃.In tower, reacted 3 hours under 300 ℃ of temperature, intake pressure 0.72Mpa, the tower top pressure 0.30Mpa, discharge all K from the discharge port of tower 2CrO 49.944 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 33.72%, the content 36.20% of KOH.Feed liquid is diluted to 38.23% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 100 ℃ carries out solid-liquid separation, the chromium slag is through repeatedly washing, slag washing water and system recoveries water are stored in rare bucket, with the slag specimen sampling analysis, contain chromium 4.19%, iron 39.59%, aluminium 32.64%, calcium 1.94%, magnesium 16.62%, silicon 5.03%, Cr in oxide compound 2O 3Transformation efficiency is 94.89%, and this produces potassiumchromate (not contain crystal water) 8.496 tons.
Embodiment 8:
With 3.37 tons of water, 1.63 tons of massfractions is to be mixed with 30%KOH solution in the mixed powder container of 92%KOH adding.
With 5 tons of 30%KOH solution and content is Cr 2O 360.10%, Fe 2O 330.40%, C 7.10%, SiO 22.50% ferrochrome powder is mixed with 9 tons of ferrochrome powder mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 326.71%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 50 ℃.
10 tons of KOH liquid caustic soda that are preheated to 436 ℃ are squeezed in the continuous liquid phase oxidation reaction tower with pump, and temperature reaches 250 ℃ in tower, sends into 300 ℃, 15m from the inlet mouth of tower 3The pressurized air of/Min is pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃ from the top of reaction tower, and temperature heating in the tower is brought up to 340 ℃, keeps intake pressure 0.80Mpa, tower top pressure 0.36Mpa reaction 1.5 hours down, discharges K from the discharge port of tower 2CrO 44.786 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 31.39%, the content 47.13% of KOH.Feed liquid is diluted with water to 27.70% mass percent concentration, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 90 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing.
With 1.94m 3Contain diluted alkaline water, 2.0m in the rare bucket of 2%KOH 3The KOH adding that contains 49% recycle mixes in the powder container and is mixed with 5 tons of 30%KOH solution.
With 5 tons of 30%KOH solution and content is Cr 2O 360.10%, Fe 2O 330.40%, C 7.10%, SiO 22.50% ferrochrome powder is mixed with 9 tons of ferrochrome powder mixed slurries for 4 tons in mixed powder container, contain Cr in the slip 2O 326.71%.Be pumped in the chromium powder preheating bucket with pump and be preheated to 50 ℃.
Discharging will be preheated to 436 3 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃.In tower, reacted 1.5 hours under 340 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge K from the discharge port of tower 2CrO 48.472 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 35.47%, the content 42.63% of KOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 436 3 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons 50 ℃ the ferrochrome powder mixed slurry of being preheated to.In tower, reacted 1.5 hours under 340 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge K from the discharge port of tower 2CrO 47.372 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 40.76%, the content 36.78% of KOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Discharging will be preheated to 436 3 tons of KOH liquid caustic soda and squeeze in the continuous liquid phase oxidation reaction tower with pump after 20 minutes, be pressed into 4.5 tons of ferrochrome powder mixed slurries that are preheated to 50 ℃.In tower, reacted 1.5 hours under 340 ℃ of temperature, intake pressure 0.80Mpa, the tower top pressure 0.36Mpa, discharge all K from the discharge port of tower 2CrO 412.158 tons of mixed liquors are stored in the bucket, through sampling analysis K to low level 2CrO 4Content 37.07%, the content 40.86% of KOH.Feed liquid is diluted to 27.70% mass percent concentration with diluted alkaline water in rare bucket, the feed liquid after the dilution is gone in the material storage barrel.
Feed liquid in the material storage barrel is cooled to 90 ℃ carries out solid-liquid separation, the chromium slag is stored in slag washing water and system recoveries water in rare bucket through repeatedly washing, with the slag specimen sampling analysis, contains chromium 3.78%, iron 88.91%, silicon 7.31%, Cr in oxide compound 2O 3Transformation efficiency is 97.85%, and this produces potassiumchromate (not contain crystal water) 11.673 tons.

Claims (5)

1. preparation technology that continuous liquid phase oxidation reaction tower is produced chromic salt, its production technique mainly contains:
(1) in mixed powder container (52) with sodium hydroxide (potassium) with contain Cr 2O 3Chromite ore fine more than 35% (ferrochrome powder) is made the slip that is mixed, its chromite ore fine (ferrochrome powder): sodium hydroxide (potassium): the mixing quality percentage of water is 10%-30%: 40%-10%: 50%-60%, and the slip that will be mixed in chromium powder preheating bucket (5) is preheating to 50-200 ℃;
(2) be to be pumped in the continuous liquid phase oxidation reaction tower (26) with pump after sodium hydroxide (potassium) more than 48% is preheated to 300~450 ℃ massfraction, when temperature in the tower reached 180 ℃-250 ℃, sending into flow from the inlet mouth (30) of tower was 10-60M 3/ min, temperature are 150-300 ℃ pressurized air;
(3) add the preheating slip that is mixed from the top (33) of reaction tower, keeping the pressurized air intake pressure is that 0.45-0.8MPa, tower top pressure are 0.18-0.36MPa, chromite ore fine (ferrochrome powder): sodium hydroxide (potassium) mass ratio is 1: 0.75-5, carried out under 250-350 ℃ of temperature oxidizing reaction 1.5-6 hour;
(4) store the bucket (41) to low level from outlet (29) discharging of reaction tower through the chromic salt feed liquid of initial gross separation, use water in rare bucket (51) to be diluted to the 25%-70% mass percent concentration then and carry out solid-liquid separation.
2. the preparation technology of chromic salt according to claim 1, it is characterized in that continuous adding is preheating to 50-200 ℃ the slip that is mixed, is preheating to 300~450 ℃ sodium hydroxide (potassium) and is preheating to 150-300 ℃ pressurized air in continuous liquid phase oxidation reaction tower, is to produce chromic salt under 250-350 ℃ continuously keeping continuous liquid phase oxidation reaction tower temperature.
3. the preparation technology of chromic salt according to claim 1 is characterized in that the described slip that is mixed can be mixed with the slip that is mixed with washing chromium slag or other alkali lye, sodium hydroxide (potassium) alkali lye and chromite ore fine of producing diluted alkaline water, recycle.
4. the preparation technology of chromic salt according to claim 1, it is characterized in that through the alkali lye that the chromic salt mixture that continuous liquid phase oxidation reaction generates is containing the 20-45% mass percent concentration store be cooled to 90-120 ℃ of temperature in the bucket (41) after, carry out solid-liquid separation with concentrated, crystallisation by cooling sedimentation method for separating.
5. the preparation technology of chromic salt according to claim 1, it is characterized in that with the stack gas after the dedusting (23) and stack gas (14) respectively to chromium powder preheating bucket (5), alkali lye preheating bucket (6), continuously liquid phase oxidation reaction tower (26), pressurized air (36) heats and be incubated.
CN2011100356421A 2011-01-27 2011-01-27 Preparation method for producing chromate by continuous liquid-phase oxidation reaction tower Pending CN102139921A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104512928A (en) * 2013-09-30 2015-04-15 湖北振华化学股份有限公司 Bubbling tower three-phase reaction apparatus for liquid-phase oxidation leaching of chromite, and method thereof
CN107758745A (en) * 2017-11-29 2018-03-06 白银昌元化工有限公司 A kind of device of three-phase oxidation production chromate

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CN1410358A (en) * 2001-10-08 2003-04-16 中国科学院过程工程研究所 Clean production method of potassium chromate
US20060188419A1 (en) * 2003-03-19 2006-08-24 Zhikuan Wang Method for production of alkali metal chromates
CN101481144A (en) * 2008-01-09 2009-07-15 中国科学院过程工程研究所 Clean production method for preparing potassium chromate from chromic iron
CN101746830A (en) * 2009-12-29 2010-06-23 重庆昌元化工有限公司 Device for safely producing potassium manganate

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Publication number Priority date Publication date Assignee Title
CN1410358A (en) * 2001-10-08 2003-04-16 中国科学院过程工程研究所 Clean production method of potassium chromate
US20060188419A1 (en) * 2003-03-19 2006-08-24 Zhikuan Wang Method for production of alkali metal chromates
CN101481144A (en) * 2008-01-09 2009-07-15 中国科学院过程工程研究所 Clean production method for preparing potassium chromate from chromic iron
CN101746830A (en) * 2009-12-29 2010-06-23 重庆昌元化工有限公司 Device for safely producing potassium manganate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104512928A (en) * 2013-09-30 2015-04-15 湖北振华化学股份有限公司 Bubbling tower three-phase reaction apparatus for liquid-phase oxidation leaching of chromite, and method thereof
CN107758745A (en) * 2017-11-29 2018-03-06 白银昌元化工有限公司 A kind of device of three-phase oxidation production chromate

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Application publication date: 20110803