CN203173931U - Device for increasing concentration of iron ions in artificial rutile mother liquor - Google Patents

Device for increasing concentration of iron ions in artificial rutile mother liquor Download PDF

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Publication number
CN203173931U
CN203173931U CN 201320158574 CN201320158574U CN203173931U CN 203173931 U CN203173931 U CN 203173931U CN 201320158574 CN201320158574 CN 201320158574 CN 201320158574 U CN201320158574 U CN 201320158574U CN 203173931 U CN203173931 U CN 203173931U
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iron
mother liquor
gas
artificial rutile
bed reactor
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CN 201320158574
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颜华
邓科
张定明
唐勇
孙永贵
周高明
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Yibin Tianyuan Group Co Ltd
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Yibin Tianyuan Group Co Ltd
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Abstract

The utility model discloses a device for increasing concentration of iron ions in artificial rutile mother liquor, which comprises a mother liquor pre-treatment system, a gas inlet system, a discharging system, a circulation system, a tail gas treatment system and a fluidized bed reactor. The fluidized bed reactor comprises a conical section, a reaction section, an expansion section and a settling section arranged in sequence from the bottom to top; the fluidized bed reactor is provided with a gas feed port, a solid and liquid slurry feed port, a liquid outlet and a tail gas outlet. By the device, the concentration of iron in the artificial rutile mother liquor is increased, and simultaneously, the nitrogen element in the mother liquor is recycled, so that recycle of resources and energy is realized, energy consumption is saved, and the device can be continuously produced.

Description

A kind of device that increases iron concentration in the artificial rutile mether liquor
Technical field
The utility model relates to a kind of device that increases concentration of iron in the artificial rutile mether liquor, belongs to chemical field.
Background technology
Artificial rutile means the chemical process method of utilizing, with the most of ferrous components in the ilmenite separate produce a kind of on the composition with structure properties on the rich titanium material identical with natural rutile.Producing with the hydrochloric acid leaching ilmenite concentrate in the process of artificial rutile, can remove impurity iron in the ilmenite concentrate and most of CaO, MgO, Al effectively 2O 3, MnO etc., obtain to contain TiO 2The high-grade artificial rutile of 88%-96% is particularly suitable for handling various types of ilmenite concentrates.But, to make in the artificial rutile process with the hydrochloric acid leaching ilmenite concentrate, dissolvings such as the iron compound in the ilmenite concentrate and calcium magnesium oxide formation chlorate enters and forms artificial rutile mether liquor in the hydrochloric acid.
Shown in the classical group of artificial rutile mether liquor becomes to see the following form:
Figure 687374DEST_PATH_IMAGE001
Owing to contain multiple metal chloride in the artificial rutile mether liquor, particularly contain a large amount of iron(ic) chloride and iron protochloride, add the unreacted hydrochloric acid of part in addition, make its very difficult recycling.
Publication number is to disclose a kind of method for recovery and treatment components from mother liquid of artificial rutile in the utility application specification sheets of CN1657426A.This method is after the artificial rutile mether liquor heating is concentrated, ferric chloride concn is wherein improved, spray into the roasting kiln roasting then, iron(ic) chloride generation pyrolysis under high temperature oxidation atmosphere, form hydrogen chloride gas and based on the soild oxide of ferric oxide, hydrogen chloride gas then water absorption obtains the hydrochloric acid of regenerating.Though this method has realized the recycle of chlorion, energy consumption is very high, and the mother liquor that one ton of artificial rutile of every processing produces needs the heat of about 6,400,000 kilocalories, and needing Sweet natural gas is 800Nm 3About, and 70% heat all consumes on evaporation of water latent heat, advocates for a long time under the energy-conservation policies and regulations in country always, this method obviously is unsustainable property.
The patent No. is that the utility model patent of ZL 90105886.6 discloses a kind of method of obtaining through refining ultrafine iron oxide from dilute hydrochloric acid method rutile mether liquor.This method is to be the swarf of 2-25 millimeter with adding particle diameter in the rutile mether liquor, when under 30-100 ℃, handling to PH3.8, add the polyacrylamide postprecipitation again, behind the logical chlorine oxidation of clear liquid, the oxidation liquid that will contain iron(ic) chloride is when semi continuous adds ammoniacal liquor to PH5-8 under 25-70 ℃ of temperature strong mixing, generate amorphous ferric hydroxide colloidal precipitation, this precipitation is made the slurry that contains Fe 0.5-15%, add iron filings successively, trivalent iron salt, tensio-active agent and positively charged mass treatment, filter, the filter cake drying is ground and is made the ultrafine iron oxide Huang, the gained iron oxide yellow is calcined then in calcining furnace can be obtained brown iron oxide.Though this method has added the concentration of iron that swarf has increased mother liquor in mother liquor, but this method technical process complexity, need to use poisonous chlorine swarf that acidolysis reaction could take place in the process, and this acidolysis reaction needs more condition, reaction not exclusively, and the chlorine element fails to obtain to recycle in the artificial rutile mether liquor, and the waste liquid of a large amount of chloride ion-containings of by product brings severe contamination to environment.
Prior art is less to the Processing Technology Research of artificial rutile mether liquor at present, basically the utilization of artificial rutile mether liquor is all just reclaimed iron and do not consider the recycling of chlorine element, and contain a large amount of moisture content in the artificial rutile mether liquor, method energy consumption concentrated by heating, spray roasting is higher, environmental protection cost height.Therefore for the processing of artificial rutile mether liquor, press for a kind of method and device that improves concentration of iron in the mother liquor of research, avoid a large amount of heating roasting process, energy efficient, simultaneously the chlorine element in the mother liquor is recycled, take full advantage of the tail gas in the treating processes, realize resource, energy recycling.
The utility model content
The purpose of this utility model just is at the deficiencies in the prior art, and a kind of device that increases concentration of iron in the artificial rutile mether liquor is provided.
To achieve these goals, the utility model adopts following technical scheme:
A kind of device that increases concentration of iron in the artificial rutile mether liquor, comprise the mother liquor pretreatment system, gas enters system, discharge system, the recycle system, exhaust treatment system and fluidized-bed reactor, described fluidized-bed reactor comprises the conical section that is disposed in order from bottom to top, conversion zone, expanding reach and settling section, be provided with the gas feed mouth, solid-liquid slurry feed mouth, liquid exit and tail gas outlet, the mother liquor pretreatment system is connected with solid-liquid slurry feed mouth, gas enters system and is connected with the gas opening for feed, discharge system is connected with liquid exit, outlet is connected the recycle system and mother liquor pretreatment system to exhaust treatment system with tail gas, exhaust treatment system connects.
Described gas feed mouth is arranged on the bottom of described conical section, and solid-liquid slurry feed mouth is arranged on the bottom of described conversion zone, and liquid exit is arranged on the bottom of described settling section, and the tail gas outlet arranges the fluidized-bed reactor top.
Described mother liquor pretreatment system comprises preevaporator, hydrochloric acid pump, source of iron feed bin, premix groove and anti-corrosive pulp pump.
Described gas enters system and comprises air compressor and hydrogen chloride gas gas compressor.
Described discharge system comprises surge tank, strainer and anticorrosion mortar pump.
Described exhaust treatment system comprises condenser, water wash column and soda-wash tower.
The described recycle system comprises mother liquor storage tank and Recycling Mother Solution pump.The process of using the utility model device processing artificial rutile mether liquor is as described below:
At first the recycle system is carried pending mother liquor to preevaporator, and preevaporator utilizes the ilmenite concentrate oxidized tail gas that mother liquor is heated up, and the pre-concentration mother liquor promotes Fe in the mother liquor simultaneously 3+Concentration, be delivered in the premix groove by the artificial rutile mether liquor of hydrochloric acid pump after with prevapourising then, fully mix formation solid-liquid mixed slurry with the source of iron of from the source of iron feed bin, getting off, by the anti-corrosive pulp pump solid-liquid mixed slurry is delivered in the fluidized-bed reactor again.Simultaneously, gas enters system hydrogen chloride gas is delivered in the fluidized-bed reactor through the gas feed mouth, and solid-liquid mixed slurry and hydrogen chloride gas are in fluidized state in fluidized-bed reactor, and acidolysis reaction is complete.After treating that acidolysis reaction reaches standard, acid hydrolysis solution passes through filter from the liquid exit discharge and filters, and acid non-soluble substance is delivered to the cement mill, and the mistake cleaner liquid is delivered to subsequent handling and handled.In the fluidizing reactor the gaseous phase materials of complete reaction discharge from tail gas outlet, HCl forms hydrochloric acid through water wash column washing back and returns the HCl content that the mother liquor storage tank replenishes mother liquor, all the other are emptying after the exhaust treatment system processing is up to standard then.The mother liquor storage tank mainly stores the artificial rutile mether liquor after the Crystallization Separation, and utilizes Recycling Mother Solution to be pumped to recycle in preevaporator and the water wash column, and the high mother liquor of small portion foreign matter content is delivered to outside the system and handled simultaneously.
Compared with prior art, advantage of the present utility model is:
(1) fluidized-bed reactor can be realized the continuous input and output of solid materials, and the motion of fluid and particle simultaneously makes reaction bed have the good heat transfer performance, and the bed internal temperature is even, is easy to control, is convenient to carry out cyclical operation.Acidolysis reaction is put in the fluidized-bed reactor carries out, the HCl gas that feeds is not only as reaction mass, and provide power for the fluidization of solid-liquid mixed slurry, make the source of iron particle in reactor, can carry out fluidisation uniformly and effectively, the liquid-solid--gas three-phase is fully contacted, improve heat transfer, rate of mass transfer and reaction efficiency, react completely.Enter the flow of air and HCl gas in the system by adjustments of gas, can use the fluidisation of different grain size source of iron, not high to the source of iron granularity requirements.Guarantee its continous-stable charging and discharging, realized the serialization production of device.
(2) tail gas of fluidized-bed reactor forms hydrochloric acid and returns the mother liquor storage tank and the hydrogen chloride tail gas that iron trichloride pyrolysis in the artificial rutile mether liquor subsequent disposal operation produces is fed in the fluidized-bed reactor after water washing, has realized the recycling of chlorine element in the mother liquor.
(3) utilize the preheating of ilmenite concentrate oxidized tail gas that mother liquor is heated in pre-concentration and the hydrogen chloride tail gas feeding fluidized-bed reactor with iron trichloride pyrolysis generation in the artificial rutile mether liquor subsequent disposal operation, resource and energy recycling have been realized, energy efficient.
Description of drawings
Fig. 1 is the structure iron of the utility model device;
Fig. 2 is the structural representation of fluidized-bed reactor among Fig. 1.
Marginal data:
The 1-preevaporator; 2-hydrochloric acid pump; 3-source of iron feed bin; 4-premix groove; 5-anti-corrosive pulp pump; The 6-fluidized-bed reactor; The 7-air compressor; 8-hydrogen chloride gas gas compressor; The 9-surge tank; The 10-strainer; The anticorrosion mortar pump of 11-; The 12-condenser; The 13-water wash column; The 14-soda-wash tower; 15-mother liquor storage tank; 16-Recycling Mother Solution pump.
The 601-conical section; The 602-conversion zone; 603-amplifies section; The 604-settling section; The 605-wash tube; 606-gas feed mouth; The 607-gas distributor; The 608-valve; 609-solid-liquid slurry feed mouth; The 610-liquid exit; The outlet of 611-tail gas.
Embodiment
In order to be expressly understood the purpose of this utility model, technical scheme and beneficial effect more, below in conjunction with accompanying drawing the utility model is described further, but protection domain of the present utility model is not limited in following examples.
Referring to Fig. 1, the utility model provides a kind of device that increases concentration of iron in the artificial rutile mether liquor, comprises that mother liquor pretreatment system, gas enter system, discharge system, the recycle system, exhaust treatment system and fluidized-bed reactor 6.
(1) described mother liquor pretreatment system comprises preevaporator 1, hydrochloric acid pump 2, source of iron feed bin 3, premix groove 4 and anti-corrosive pulp pump 5, is used for that artificial rutile mether liquor is heated pre-concentration and mixes backward current fluidized bed reactor conveying solid-liquid mixed slurry with source of iron.Preevaporator 1 mainly utilizes the ilmenite concentrate oxidized tail gas that artificial rutile mether liquor is heated pre-concentration, promotes Fe3+ concentration in the mother liquor, simultaneously mother liquor is heated up; 2 of hydrochloric acid pumps are delivered to the artificial rutile mether liquor behind the prevapourising in the premix groove 4, mix the formation slurry with the sulfate slag that gets off from source of iron feed bin 3 or other sources of iron, anti-corrosive pulp pump 5 is delivered to the solid-liquid slurry feed mouth 609 of slurry from fluidized-bed reactor 6 that configures in the premix groove 4 in the reactor again.Can use this area equipment commonly used as preevaporator, hydrochloric acid pump, feed bin, premix groove and the anti-corrosive pulp pump of the pretreatment system in the fluidization reaction unit of the present utility model here.
(2) described gas enters system and comprises air compressor 7 and hydrogen chloride gas gas compressor 8.Gas feed mouth 606 after the air mixed of coming out by hydrogen chloride gas gas compressor 8 compression backs and air compressor 7 from the hydrogen chloride tail gas of iron trichloride pyrolysis from fluidized-bed reactor 6 is delivered in the reactor, and the flow by regulating two kinds of gases and ratio are as thermal barrier and the propulsion source of reactor.Can use this area equipment commonly used as the compressor of the gas feed system in the fluidization reaction unit of the present utility model here.
(3) described discharge system comprises surge tank 9, strainer 10 and anticorrosion mortar pump 11.Reacted acid hydrolysis solution enters into surge tank 9 from liquid exit 610 in the fluidized-bed reactor 6, separates through entering strainer 10 after the buffering, and the acid non-soluble substance after the separation is delivered to the cement mill, separates clear liquid and delivers to the subsequent handling processing through anticorrosion mortar pump 11.
(4) described exhaust treatment system comprises condenser 12, water wash column 13 and soda-wash tower 14.Be mainly used in the vent gas treatment of reactor for treatment back up to standard is being discharged, can use this area equipment commonly used as exhaust treatment system required equipment in this device.
(5) the described recycle system comprises mother liquor storage tank 15 and Recycling Mother Solution pump 16.Be used for the mother liquor after the Crystallization Separation is delivered to water wash column 13 and preevaporator 1 recycle, the mother liquor that the small portion foreign matter content is high is delivered to outside the system.
(6) referring to Fig. 2, below explain in detail fluidized-bed reactor 6.
Described fluidized-bed reactor 6 comprises conical section 601, conversion zone 602, expanding reach 603 and the settling section 604 that is disposed in order from bottom to top, be provided with gas feed mouth 606, solid-liquid slurry feed mouth 609, liquid exit 610 and tail gas outlet 611, the mother liquor pretreatment system is connected with solid-liquid slurry feed mouth 609, gas enters system and is connected with gas opening for feed 606, discharge system is connected with liquid exit 610, and exhaust treatment system is connected with tail gas outlet 611.Described gas feed mouth 606 is arranged on the bottom of described conical section 601, solid-liquid slurry feed mouth 609 is arranged on the bottom of described conversion zone 602, liquid exit 610 is arranged on the bottom of described settling section 604, and tail gas outlet 611 is arranged on the fluidized-bed reactor top.
The conical section 601 of fluidized-bed reactor 6 is lower cone section, and cone angle is 30 °-50 °, is provided with wash tube 605 in the bottom of conical section, is convenient to regularly purge flow fluidized bed reactor 6 inside.
The bottom of the conversion zone 602 of fluidized-bed reactor 6 is provided with solid-liquid slurry feed mouth 609, be furnished with gas distributor 607 in the bottom, gas distributor comprises a plurality of valves 608, enters the conversion zone 602 after will evenly distributing from the mixed gas that the gas feed mouth is come in.
The expanding reach 603 of fluidized-bed reactor 6 is upper cone section, and cone angle is 100 °-150 °.
The bottom of the settling section 604 of fluidized-bed reactor 6 is provided with liquid exit 610, reacted acid hydrolysis solution flows in the surge tank 9 from here, be provided with tail gas outlet 611 at the top of settling section 604, tail gas enters exhaust treatment system from here in the reactor, treated back emptying up to standard.

Claims (7)

1. device that increases concentration of iron in the artificial rutile mether liquor, it is characterized in that: comprise the mother liquor pretreatment system, gas enters system, discharge system, the recycle system, exhaust treatment system and fluidized-bed reactor, described fluidized-bed reactor comprises the conical section that is disposed in order from bottom to top, conversion zone, expanding reach and settling section, be provided with the gas feed mouth, solid-liquid slurry feed mouth, liquid exit and tail gas outlet, the mother liquor pretreatment system is connected with solid-liquid slurry feed mouth, gas enters system and is connected with the gas opening for feed, discharge system is connected with liquid exit, outlet is connected the recycle system and mother liquor pretreatment system to exhaust treatment system with tail gas, exhaust treatment system connects.
2. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: described gas feed mouth is arranged on the bottom of described conical section, solid-liquid slurry feed mouth is arranged on the bottom of described conversion zone, liquid exit is arranged on the bottom of described settling section, and the tail gas outlet arranges the fluidized-bed reactor top.
3. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: described mother liquor pretreatment system comprises preevaporator, hydrochloric acid pump, source of iron feed bin, premix groove and anti-corrosive pulp pump.
4. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: described gas enters system and comprises air compressor and hydrogen chloride gas gas compressor.
5. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: described discharge system comprises surge tank, strainer and anticorrosion mortar pump.
6. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: described exhaust treatment system comprises condenser, water wash column and soda-wash tower.
7. a kind of device that increases concentration of iron in the artificial rutile mether liquor according to claim 1, it is characterized in that: the described recycle system comprises mother liquor storage tank and Recycling Mother Solution pump.
CN 201320158574 2013-04-02 2013-04-02 Device for increasing concentration of iron ions in artificial rutile mother liquor Expired - Lifetime CN203173931U (en)

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CN 201320158574 CN203173931U (en) 2013-04-02 2013-04-02 Device for increasing concentration of iron ions in artificial rutile mother liquor

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Application Number Priority Date Filing Date Title
CN 201320158574 CN203173931U (en) 2013-04-02 2013-04-02 Device for increasing concentration of iron ions in artificial rutile mother liquor

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Granted publication date: 20130904