CN101780961B - Energy saving, consumption reduction and high efficiency process for manufacturing borax with carbon alkaline method - Google Patents
Energy saving, consumption reduction and high efficiency process for manufacturing borax with carbon alkaline method Download PDFInfo
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- CN101780961B CN101780961B CN2010101188575A CN201010118857A CN101780961B CN 101780961 B CN101780961 B CN 101780961B CN 2010101188575 A CN2010101188575 A CN 2010101188575A CN 201010118857 A CN201010118857 A CN 201010118857A CN 101780961 B CN101780961 B CN 101780961B
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 125
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 61
- 230000008569 process Effects 0.000 title claims abstract description 50
- 229910021538 borax Inorganic materials 0.000 title claims abstract description 44
- 239000004328 sodium tetraborate Substances 0.000 title claims abstract description 44
- 235000010339 sodium tetraborate Nutrition 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 230000009467 reduction Effects 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000005406 washing Methods 0.000 claims abstract description 27
- 239000002893 slag Substances 0.000 claims abstract description 26
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims description 26
- 238000001914 filtration Methods 0.000 claims description 21
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 20
- 229910052796 boron Inorganic materials 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 14
- 239000006200 vaporizer Substances 0.000 claims description 11
- 239000012452 mother liquor Substances 0.000 claims description 10
- 239000011435 rock Substances 0.000 claims description 8
- 235000017550 sodium carbonate Nutrition 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 4
- 230000000994 depressogenic effect Effects 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 230000008929 regeneration Effects 0.000 claims description 3
- 238000011069 regeneration method Methods 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 230000009897 systematic effect Effects 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 9
- 238000002425 crystallisation Methods 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 5
- 238000010926 purge Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 61
- 239000011734 sodium Substances 0.000 description 10
- 239000003513 alkali Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- Y02P20/121—
Landscapes
- Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
Abstract
The invention relates to a carbon alkaline process for manufacturing borax with energy saving, consumption reduction and high efficiency, belonging to the field of chemical engineering science. The process for manufacturing borax comprises: 1, CO2 with high temperature (145-165 DEG C), high pressure (0.8-1.2MPa) and high volume concentration (98-99%) is used for deep carbonate decomposition; 2, a hot carbonate catalyzing method is used for enriching CO2 in conventional carbonate decomposition tail gas, and the regenerated heat is provided by water vapor and evaporated end effect vapor in the tail gas; 3, CO2 in decompressed gas and purge gas in the discharging process is recycled, and the water vapor is used for heating slag washing water; and 4, the heat (65-75 DEG C) before evaporation concentration liquid enters a crystallization cooler is used for heating borax mother liquid and washing water. The process can shorten the carbonate decomposition time to 7-10 hours, enable the carbonate decomposition rate to exceed 1-3% of activity, reduce tail gas CO2 to 0.5-5%, consume 2.6-3.5 tons of vapor of 0.7MPa and obtain 0.7-1.2 tons of byproduct vapor of 0.03-0.15MPa.
Description
Technical field
The present invention relates to a kind of carbon alkaline process for manufacturing borax of energy saving, consumption reduction and high efficiency, belong to chemical engineering subject field.
Background technology
From fibre-bearing szaibelyite (2MgOB
2O
3H
2O) or suanite (2MgOB
2O
3) the class boron rock is directly made borax that two class methods were once arranged; Alkaline process (NaOH) and carbon alkaline process (CO
2+ Na
2CO
3) the decomposition boron rock.The carbon alkaline process is light with flow process weak point, less investment, corrosion, advantages such as little and cost is lower have replaced alkaline process gradually and become domestic manufacturing borax and be close to unique method to environmental disruption a little less than the boron mud alkalescence.But also there are several big shortcomings in the carbon alkaline process: 1. long reaction time, generally want 15～20 hours; 2. the leaching of boron (decomposition) rate is low, and is lower more than 5% than pressure alkali decomposition; 3. CO
2Utilization ratio is low, is generally 50～60%; 4. energy consumption height.
Once used or proposed many measures and overcame above-mentioned shortcoming:
1) existing factory adopts and strengthens the kiln gas flow, improves carbon and separates tail gas CO
2Concentration shortens the carbon dioxide-soda reaction time, perhaps suitably reduces carbon and separates rate to increase output;
2) carbon is separated jar and to be adopted series connection or series-multiple connection to operate in groups to reduce CO
2Consume;
3) high concentration CO
2Carbon is separated;
4) under the condition that equipment allows, suitably improve kiln gas pressure to improve CO
2Dividing potential drop;
5) carbon is separated CO in the tail gas
2Recovery is carried and is returned carbon after dense and separate, and for example reclaims CO with pressure swing adsorption process
2, it can obviously shorten carbon and separate the time, but separates the DeGrain of rate to improving carbon;
6) make NaHCO earlier by kiln gas and soda ash
3, use NaHCO then
3Decompose boron rock, the carbon time of separating can significantly shorten, and the carbon rate of separating can suitably improve, and brings up to more than the 6.5MPa but require retort to bear pressure;
7) suitably improve carbon and separate tail gas CO
2Concentration to 21.3%, the tail gas Na that adds activator
2CO
3Solution is made NaHCO
3, use NaHCO then
3Decompose boron rock together with kiln gas;
8) in order to reclaim a large amount of low temperature exhaust heats, water vapor heat energy and the magnanimous water for cooling crystalline sensible heat now carbon separated in the tail gas use for boron mud filter cake washing by heat exchange mode heating clear water.Carbon after cooling is separated tail gas pressure 0.2～0.25MPa and is used for force feed liquid object, realizes that pressure can utilize.
Summary of the invention
In order to overcome above-mentioned problems of the prior art, the invention provides a kind of carbon alkaline process for manufacturing borax of energy saving, consumption reduction and high efficiency, this technology should be lacked the leaching of boron (decomposition) rate height, CO in the reaction times
2The utilization ratio height, energy consumption is low.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of carbon alkaline process for manufacturing borax of energy saving, consumption reduction and high efficiency, the batching that it adopts is mainly szaibelyite and soda ash, and successively through material-compound tank, carbon separate secondary jar, carbon separate main jar, press filtration and washery slag process, cooling crystallizer, separate with wash the boron process after obtain borax, kiln gas enters carbon and separates main jar after the kiln gas compression process.Between described carbon is separated main jar and press filtration and washery slag process, be provided with a degree of depth carbon and separate jar, between described press filtration and washery slag process and cooling crystallizer, be provided with vaporizer and interchanger; The off-gas that described degree of depth carbon is separated jar enters CO behind cooling tower
2Basin, described carbon are separated secondary jar tail gas through CO
2Enriching apparatus enters CO
2Basin, CO
2CO in the basin
2Through CO
2Enter degree of depth carbon after the compression process and separate jar; It is to use high concentration CO that described degree of depth carbon is separated jar
2Carbon is separated still unreacted boron ore powder slip in main jar, and reaction conditions is: CO
2Volumetric concentration 95～99%, pressure 0.8～1.2MPa, 140～165 ℃ of temperature, 1～2 rev/min of mixing speed reacted 1～4 hour; Behind the stopped reaction, the CO in the off-gas of earlier degree of depth carbon being separated jar
2Reclaim with water vapor, with overbottom pressure tail gas degree of depth carbon is separated a jar interior slip then and be pressed into press filtration and washery slag process,, wash the back filter cake and discharge the field of removing slag through press filtration, filter cake washing; Filtrate and wash water head concentrate through vaporizer, the borax concentrated solution enters cooling crystallizer after interchanger is cooled to 65～75 ℃, enter at last to separate and go out borax with the washing process centrifugation, after washing decon with water, obtain the product borax, the borax mother liquor and the wash water that are heated to 75～85 ℃ return material-compound tank.
Described szaibelyite is selected for use through szaibelyite type boron rock after the activation treatment and the szaibelyite type, the granularity that contain ludwigite stone and is passed through 150 purpose breezes 90% or more.
Described carbon is separated secondary jar tail gas employing catalysis hot potash method, BV method or the enrichment of activation sodium carbonate method; Absorb CO
2After tail gas CO
2Volumetric concentration is 0.5～5%, absorbs CO
2Rich solution heating evict CO from
2Make solution regeneration, recover to absorb CO
2Ability; The used heat energy of regenerating is imitated steam by the end of water vapor in the tail gas and vaporizer and is suitably boosted to the heat energy that 0.05～0.15MPa emits and provide, and is absorbed CO
2After the tail gas overbottom pressure still at 0.45～5.5MPa, be stored in the overbottom pressure gas tank.
The CO that described degree of depth carbon discharges when separating jar discharging
2All recycle with water vapor, unload the gas that is depressed into before 0.65～0.75MPa and directly be disposed to main carbon through offgas duct and separate jar, the gas that 0.65～0.75MPa to 0.02～0.05MPa gives off contains the CO that discharges out in the solution
2Gas and the water vapor that flashes off enter the direct contact type cooling tower with atmospheric operation, with the water coolant counter-current operation, enter CO behind gas cooling to 30～40 ℃
2Basin is heated to 75～85 ℃ hot water inflow press filtration and the hot water tank in the washery slag process and uses for slag filter cake wash water.
Described vaporizer adopts multiple-effect evaporation to keep systematic water balance, and vapor pressure is imitated according to enrichment CO in the end
2Solution regenerated temperature levels in the operation and deciding is at 0.01～0.07MPa; Evaporation structure is provided with Despumation device.
Technique scheme is to set up a degree of depth carbon to separate jar after the carbon of traditional carbon alkali reaction system is separated main jar, and it uses CO
2Volumetric concentration is that 98～99% gas comes carbon to separate the main jar boron ore powder of complete reaction not as yet.Its reaction conditions is pressure 0.8～1.2MPa, 145～165 ℃ of temperature, and 1～4 hour time, the leaching yield of boron (carbon is separated rate) reaches on the boron rock activity 1～3%.
Carbon in traditional reactive system separates secondary jar and carbon is separated the still reservation of main jar.The unstripped gas of reaction mainly is the CO that contains in limestone kiln
2Volumetric concentration is 35～40% gases, the tail gas that degree of depth carbon is separated jar and (or) dense CO more than needed
2Gas also feeds main jar, discharges from secondary jar and is sent to CO
2The enrichment operation.It is that feed temperature is risen to 130～135 ℃ that carbon is separated a secondary jar main task, and 0.55～0.6MPa keep-ups pressure; It is 0.6～0.65MPa that carbon is separated a main jar reaction conditions, 135～140 ℃ of temperature.Carbon is separated main jar and carbon and is separated the total reacting weight of secondary jar and account for 3/4～4/5, and promptly carbon is separated rate 65～75%.
The condition of batching is with the requirement of conventional carbon alkaline process.Slip such as boron ore powder, soda ash joins carbon and separates secondary jar.Three jars are separated pair jar--carbon is separated main jar---degree of depth carbon according to carbon and are separated jar order circulation switching in 2.5～4 hours once.
Degree of depth carbon is separated a jar reaction and is finished, and stops to feed CO
2After the gas, at first release gas feeds carbon and separates main jar, unloads to be depressed into 0.65～0.7MPa and to stop to separate main jar exhaust to carbon; Discharge and flash gas leads to the direct contact type water cooling tower, ℃ be sent to CO with cold water cooling condensation to 30～40
2The CO of gas-reservoir jar and enrichment
2Go degree of depth carbon to separate jar through overdraft together.Cold water is heated to 80 ℃, uses as the filter cake wash water.Reduce to 0.03～0.05MPa when the jar internal pressure, close the pneumatic outlet valve, slip is depressed into the press filtration operation with pressurized gas.
Press filtration and filter cake washing are with the conventional carbon alkali process.
Different with the conventional carbon alkaline process, the magnanimous water that press filtration obtains need concentrate through vaporizer, adopts double-effect evaporation.Point of the present invention is to improve the end and imitates evaporating pressure greater than barometric point.According to CO
2The requirement of enrichment operation is imitated steam with the end and is pressurized to 0.1～0.15MPa with vapour compressor, the usefulness of heat supply alkali liquid regeneration.
Concentrated solution cooling, crystallization, centrifugation, washing borax etc. are identical substantially with traditional technology.Of the present invention point is that hot concentrated solution advances before the crystallizer earlier borax mother liquor and the wash water heat exchange with batching usefulness, and cold fluid is heated to 75～85 ℃, and concentrated solution is cooled to 65～75 ℃.
The invention has the beneficial effects as follows: the carbon alkaline process for manufacturing borax of this energy saving, consumption reduction and high efficiency comprises: 1. adopt high temperature (145～165 ℃), high pressure (0.8～1.2MPa), high density (98～99%) CO
2Degree of depth carbon is separated; 2. the conventional carbon of the hot carbonation enrichment of employing catalysis is separated the CO in the tail gas
2, its reactivation heat is imitated steam by the end of water vapor in the tail gas and evaporation and is provided; 3. CO in release gas and the off-gas when recycling discharging
2, water vapor is used for heating slag washing water; 4. evaporation concentration liquid advances that the heat of (65～75 ℃) is used for heating borax mother liquor and wash water before the crystallization water cooler.Thereby make the carbon time of separating shorten to 7～10 hours, carbon is separated rate and is surpassed activity 1～3%, tail gas CO
2To arrive 0.5～5%, 2.6～3.5 tons of steam consumption 0.7MPa steam, 0.7～1.2 ton of by-product 0.03～0.15MPa steam.
Description of drawings
Fig. 1 is a kind of carbon alkaline process for manufacturing borax schema of energy saving, consumption reduction and high efficiency.
Embodiment
Fig. 1 shows a kind of carbon alkaline process for manufacturing borax of energy saving, consumption reduction and high efficiency.Among the figure, szaibelyite and soda ash batching successively through material-compound tank, carbon separate that secondary jar, carbon separate that main jar, dark carbon are separated jar, press filtration and washery slag process, vaporizer, interchanger, cooling crystallizer and separate with washing process after obtain borax, kiln gas enters carbon and separates main jar after the kiln gas compression process.The off-gas that degree of depth carbon is separated jar enters CO behind cooling tower
2Basin, carbon are separated secondary jar tail gas through CO
2Enriching apparatus enters CO
2Basin, CO
2CO in the basin
2Through CO
2Enter degree of depth carbon after the compression process and separate jar; It is to use high concentration CO that degree of depth carbon is separated jar
2Carbon is separated still unreacted boron ore powder slip in main jar, and reaction conditions is: CO
2Volumetric concentration 95～99%, pressure 0.8～1.2MPa, 140～165 ℃ of temperature, 1～2 rev/min of mixing speed reacted 1～4 hour; Behind the stopped reaction, the CO in the off-gas of earlier degree of depth carbon being separated jar
2Reclaim with water vapor, with overbottom pressure tail gas degree of depth carbon is separated a jar interior slip then and be pressed into press filtration and washery slag process,, wash the back filter cake and discharge the field of removing slag through press filtration, filter cake washing.Filtrate and wash water head concentrate through vaporizer, the borax concentrated solution enters cooling crystallizer after interchanger is cooled to 65～75 ℃, enter at last to separate and go out borax with the washing process centrifugation, after washing decon with water, obtain the product borax, the borax mother liquor and the wash water that are heated to 75～85 ℃ return material-compound tank.Clear water one tunnel is through cooling tower, press filtration and the laggard material-compound tank of washery slag process, and material-compound tank is also advanced in another road behind separation and washing process.
Original carbon alkali process is lower than 70% in the carbon rate of separating, CO
2Under volumetric concentration 35%, 130～135 ℃ of conditions of temperature of reaction, CO
2Uptake rate and szaibelyite rate of decomposition be suitable, neither be too slow.Conditioned response time length mainly is the reaction later stage.The simple CO that improves
2Concentration though can shorten the time of whole process, can not change the shape of speed of reaction and time curve.Improve temperature of reaction and can improve speed of reaction, but Ying Yineng guarantees CO
2By enough uptake rates for guaranteeing, promptly improve temperature should with the supporting use of pressurize.
Embodiment 1
Used three carbon separate jar pattern and size is all identical, for steam jacket and whipping appts are arranged, design the pot type pressurized vessel of withstand voltage 1.2MPa, volume 18M
3
Used breeze is to contain B after the activated roasting of wide pasture szaibelyite
2O
314%, active 88% ripe boron powder is planned the every jar of 4275kg that feeds intake, and joins alkali by 103%, allocates slag washing lotion (moderate water), borax wash water and borax mother liquor at 1.8: 1 by liquid-solid ratio.Identical with the conventional carbon alkali process, raw material be pressed into carbon separate secondary jar (promptly emptying degree of depth carbon separate jar), switch each gas tube valve, with the CO of 98% volumetric concentration
2Gas feeds degree of depth carbon and separates jar, contains CO
2The tail gas that 37～39% kiln gas and degree of depth carbon are separated jar feeds main carbon in the lump and separates jar.The tail gas that secondary carbon is separated jar send CO
2Enriching apparatus.The processing condition of each jar are: degree of depth carbon is separated pressure tank 1.0MPa, 155～160 ℃ of temperature; Main carbon is separated pressure tank 0.65MPa, 135～140 ℃ of temperature; Secondary carbon is separated pressure tank 0.55～0.60MPa, 130～135 ℃ of temperature.Degree of depth carbon is separated CO in the jar
2Concentration reaches at 97.5% o'clock, turns down CO
2Intake valve, or take to be interrupted the tonifying Qi way and keep pressure.When temperature at 160 ℃, stopped tonifying Qi 20 minutes.The jar internal pressure does not have obvious decline, and reaction promptly comes to an end.The degree of depth carbon time of separating has been used 2 hours 40 minutes.Begin subsequently degree of depth carbon is separated a jar release, gas unloads to main carbon and separates jar, when pressure is reduced to 0.7MPa, stops to main jar exhaust.Cooling tower is led in unlatching, and this tower is a packing tower, direct contact cooling off-gas of water and water vapor.The control Outlet Gas Temperature is at 35～40 ℃, and it is CO
2Gas is sent to CO
2Gas holder.80 ℃ of heated hot water, the hot water tank of inflow filter wash cake.When the jar internal pressure was reduced to 0.05MPa, recovering discharging gas finished.
By the operating method of conventional carbon alkaline process, with the overbottom pressure gas of 0.45MPa degree of depth carbon is separated a jar interior slip and press to the press filtration operation, adopt filter cake cover washing method washing leaching cake.Slip filtrate and " wash water head " obtain magnanimous water behind controlled filter, it contains Na
2B
4O
712.71%, total amount 7836kg.Draw off slag, weight in wet base 6350kg.Slag drying rate of weight loss 28% contains B in the dried slag
2O
3Acid molten 1.44%, water-soluble 0.26%.
Amount to reaction 8 hours 10 minutes from being dosed to release.Heating and insulation 0.7MPa steam 2480kg.Consumption contains CO
238% kiln gas 1185NM
3
Magnanimous water is sent to the double-effect evaporator evaporation concentration to Na
2B
4O
716.73%, dope 5946kg, 139 ℃ of temperature. vapor pressure 0.03MPa, 106 ℃ of temperature are imitated in the end.Evaporative process consumes 0.7MPa steam 1508kg, by-product 0.03MPa steam 1076kg.
Concentrated solution enters crystallizer earlier preceding and borax mother liquor and wash water 5000kg heat exchange, is heated to more than 80 ℃, and then enters crystallizer.Use the cold water decrease temperature crystalline, reduce to 35 ℃ when temperature and stop crystallization.Centrifugation obtains Na after washing borax with clear water
2B
4O
710H
2O (〉=95%) 1575kg.Mother liquor and wash water return, deallocation material after heating.Consume 40 tons of water coolants.
Embodiment 2
This routine used boron rock is the boron magnesium ore deposit of containing ludwigite, the ripe breeze that activated roasting obtains.Its main component is B
2O
310.2%, MgO 37.0%, and TFe 20.38%, SiO
222.0%, S 0.2%.Active 82%.
Equipment used is with example 1.In material-compound tank, add slag washing lotion, borax mother liquor and borax washing lotion at 1.5: 1 according to liquid-solid ratio, drop into the above-mentioned ripe breeze 5000kg in boron magnesium ore deposit that contains ludwigite again, drop into corresponding Na by joining alkali number 110%
2CO
3Amount.After stirring, slip force feed to the former degree of depth carbon of unsnatching material is separated jar as secondary jar.The switching of three jars and the processing condition of keeping and degree of depth carbon separate that a jar release, off-gas are reclaimed and the slip force feed to the operation of pressure filter with example 1.The tail gas of separating jar from main carbon feeds secondary carbon and separates jar, experiences main carbon and separates with degree of depth carbon and separate etc. till process to release begins, and reacts and lasts 7 hours.Feeding contains CO
238% kiln gas 760NM
3, consume heating and insulation steam 1530kg.
Slip is through press filtration, and filter cake obtains wet cake 7035kg after washing, filter cake sampling oven dry rate of weight loss 27%, and dried slag contains B
2O
3Acid molten 1.59%, water-soluble 0.20%.Obtain containing Na
2B
4O
710.65% magnanimous water 7378kg.Magnanimous water send the double-effect evaporator evaporation concentration, boils off water yield 2370kg, consumes 0.7MPa steam 1810kg, by-product 0.03MPa steam 1284kg.
Processes such as the interchanger cooling of the similar example 1 of concentrated solution 4774kg process, crystallisation by cooling, centrifugation, washing borax obtain containing the Na more than 95%
2B
4O
710H
2O1144kg; Contain Na
2B
4O
74.73% borax mother liquor 3610kg contains Na
2B
4O
73% washing lotion 350kg.Two kinds of fluids return material-compound tank after heating.The crystallisation by cooling process consumes 15.6 tons of water coolants.
Claims (5)
1. the carbon alkaline process for manufacturing borax of an energy saving, consumption reduction and high efficiency, the batching that it adopts is mainly szaibelyite and soda ash, and successively through material-compound tank, carbon separate secondary jar, carbon separate main jar, press filtration and washery slag process, cooling crystallizer, separate with washing process after obtain borax, kiln gas enters carbon and separates main jar after the kiln gas compression process; It is characterized in that: between described carbon is separated main jar and press filtration and washery slag process, be provided with a degree of depth carbon and separate jar, between described press filtration and washery slag process and cooling crystallizer, be provided with vaporizer and interchanger; The off-gas that described degree of depth carbon is separated jar enters CO behind cooling tower
2Basin, described carbon are separated secondary jar tail gas through CO
2Enriching apparatus enters CO
2Basin, CO
2CO in the basin
2Through CO
2Enter degree of depth carbon after the compression process and separate jar; Described degree of depth carbon is separated a jar employing high concentration CO
2Carbon is separated still unreacted boron ore powder slip in main jar, and reaction conditions is: CO
2Volumetric concentration 95～99%, pressure 0.8～1.2MPa, 140～165 ℃ of temperature, 1～2 rev/min of mixing speed reacted 1～4 hour; Behind the stopped reaction, the CO in the off-gas of earlier degree of depth carbon being separated jar
2Reclaim with water vapor, with overbottom pressure tail gas degree of depth carbon is separated a jar interior slip then and be pressed into press filtration and washery slag process,, wash the back filter cake and discharge the field of removing slag through press filtration, filter cake washing; Filtrate and wash water head concentrate through vaporizer, the borax concentrated solution enters cooling crystallizer after interchanger is cooled to 65～75 ℃, enter at last to separate and go out borax with the washing process centrifugation, after washing decon with water, obtain the product borax, the borax mother liquor and the wash water that are heated to 75～85 ℃ return material-compound tank.
2. according to the carbon alkaline process for manufacturing borax of the described a kind of energy saving, consumption reduction and high efficiency of claim 1, it is characterized in that: described szaibelyite is selected for use through szaibelyite type boron rock after the activation treatment and the szaibelyite type, the granularity that contain ludwigite stone and is passed through 150 purpose breezes 90% or more.
3. according to the carbon alkaline process for manufacturing borax of the described a kind of energy saving, consumption reduction and high efficiency of claim 1, it is characterized in that: described carbon is separated secondary jar tail gas employing catalysis hot potash method or the enrichment of activation sodium carbonate method; Absorb CO
2After tail gas CO
2Volumetric concentration is 0.5～5%, absorbs CO
2Rich solution heating evict CO from
2Make solution regeneration, recover to absorb CO
2Ability; The used heat energy of regenerating is imitated steam by the end of water vapor in the tail gas and vaporizer and is suitably boosted to the heat energy that 0.05～0.15MPa emits and provide, and is absorbed CO
2After the tail gas overbottom pressure still at 0.45～5.5MPa, be stored in the overbottom pressure gas tank.
4. according to the carbon alkaline process for manufacturing borax of the described a kind of energy saving, consumption reduction and high efficiency of claim 1, it is characterized in that: the CO that described degree of depth carbon discharges when separating jar discharging
2All recycle with water vapor, unload the gas that is depressed into before 0.65～0.75MPa and directly be disposed to main carbon through offgas duct and separate jar, the gas that 0.65～0.75MPa to 0.02～0.05MPa gives off contains the CO that discharges out in the solution
2Gas and the water vapor that flashes off enter the direct contact type cooling tower with atmospheric operation, with the water coolant counter-current operation, enter CO behind gas cooling to 30～40 ℃
2Basin is heated to 75～85 ℃ hot water inflow press filtration and the hot water tank in the washery slag process and uses for slag filter cake wash water.
5. according to the carbon alkaline process for manufacturing borax of the described a kind of energy saving, consumption reduction and high efficiency of claim 1, it is characterized in that: described vaporizer adopts multiple-effect evaporation to keep systematic water balance, and vapor pressure is imitated according to enrichment CO in the end
2Solution regenerated temperature levels in the operation and deciding is at 0.01～0.07MPa; Evaporation structure is provided with Despumation device.
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| CN111977661B (en) * | 2020-08-26 | 2023-06-09 | 沈阳工业大学 | Borax production process and device based on circulation energy conservation |
| CN111964446A (en) * | 2020-08-26 | 2020-11-20 | 沈阳工业大学 | Device and method for curing boron-magnesium ore powder based on energy integration |
| CN112044249B (en) * | 2020-08-26 | 2024-04-05 | 沈阳工业大学 | Carbon dioxide tail gas absorbing device and method for carbon dioxide decomposition reaction |
| CN112028084B (en) * | 2020-08-26 | 2023-02-21 | 沈阳工业大学 | Method and equipment for preparing borax |
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| GB1379098A (en) * | 1971-02-17 | 1975-01-02 | Gen Crude Oil Minerals Co Sa | Method for processing water insoluble borate ores |
| US3829553A (en) * | 1972-08-02 | 1974-08-13 | Gen Crude Oil & Minerals Co | Process for treating borocalcic ores |
| CN1007421B (en) * | 1987-12-17 | 1990-04-04 | 铁岭市化学工业局 | Technology for simultaneous prodn. of synthetic ammonia and borax |
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