CN101734694B - Method for excluding sodium oxalate and carbonate from Bayer process solution by adopting ultra-concentration method - Google Patents
Method for excluding sodium oxalate and carbonate from Bayer process solution by adopting ultra-concentration method Download PDFInfo
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Abstract
The invention discloses a method for excluding sodium oxalate and carbonate from Bayer process solution by adopting an ultra-concentration method. The method comprises the steps of: concentrating the mother liquor of an alumina system, sending liquor in the concentrated mother liquor to an alumina production system, and then send to a first segment causticization tank for causticizing for 2 to 4 hours to obtain seriflux B after solid phase dissolution; cooling the seriflux B to 50 to 70 DEG C and send to a second segment causticization tank for causticizing for 1.5 to 3 hours at 50 to 70 DEG C to obtain seriflux C; sending the seriflux C into a separating and washing machine, sending washed liquid to the alumina production system, and sending residues an alumina red mud washing system. The invention not only has the advantages of good excluding effect, simple process, less investment and low production and operation cost, but also achieves less loss of alumina, and has good use value and economic value.
Description
Technical field
The present invention relates to a kind of method that adopts the ultra concentrated method from Bayer process solution, to get rid of sodium oxalate and carbonate, belong to the technical field of getting rid of Bayer process solution oxalate and carbonate.
Background technology
The source of alumina producing flow process mesoxalic acid sodium is mainly carrying of bauxite, secondly is to contain organic subsidiary material (as: flocculation agent, lubricant, antifoams etc.) for what satisfy that the production needs add.Because of sodium oxalate constantly accumulation on stream;, accumulation will bring great harm after reaching certain concentration to alumina producing; Its main harm is: 1, reduce quality product: the solubleness of sodium oxalate in sodium aluminate solution is along with the reduction of temperature reduces; Decomposition in the bayer's process production is a temperature-fall period, and this just separates out for the sodium oxalate crystalline and has created convenience, thereby has a strong impact on quality product.2, sodium oxalate impels the generation of fine particle aluminum hydroxide crystals; Thereby cause product granularity defective; Separate out simultaneously with white lake at decomposition course mesoxalic acid sodium; Therefore will cause the further refinement of product granularity at the hydroxide roasting process, sodium oxalate and white lake are separated out jointly, can cause the content of aluminum hydroxide crystals alkali to increase.3, reduced the speed of agglomeration efficient and crystal growth in the decomposition course, made and decompose output capacity and reduce and the cycle efficiency reduction.4, contain the higher solution of sodium oxalate and can produce a large amount of foams, cause equipment can not satisfy load operation at conveying and storage process.5, sodium oxalate reaches capacity after the concentration; Will be at the seed vertical-disk filter, separate out the positions such as hot face of the heat-transfer surface of seminal fluid heat exchange, decomposer inner peripheral wall and vaporizer, and this not only causes the production capacity of equipment own to reduce; And can cause the equipment cleaning cycle to shorten, operation rate is low; Can cause the heat-transfer effect of vaporizer, heat exchanging apparatus to reduce in addition.6, a large amount of normal pressure equipment is arranged in the alumina producing, alkali lye or slip overflow in company with the organism foam together in careless slightly this this equipment, influence industrial hygiene and environment protection.
The method for removing of existing sodium oxalate mainly contains: 1, roasting method: bauxite is carried out preroasting; Or the fine particle white lake of aluminum oxide production process carried out roasting; Though this method can effectively be got rid of sodium oxalate, but its construction investment is high, energy consumption height and contaminate environment.2, aluminum hydroxide wash liquor causticizing process: need carry out twice classification and the once sedimentation of thin white lake in order to obtain thin crystal seed; Then settled underflow is separated and washing; Its washing lotion is carried out causticization under the condition that adds excessive lime, realize the eliminating of sodium oxalate.This method first pass is complicated: not only the Operation and Maintenance workload is big, and construction investment is high, and only should be used for two sections decomposition, and limited because of the amount of the thin white lake of aluminum oxide factory, the amount of washing lotion mesoxalic acid sodium is just more limited, so the eliminating amount of sodium oxalate is few; The second, because of having increased the washing procedure of thin white lake,, further increased the difficulty of alumina producing water, and can increase heat energy consumption so need increase water consumption; Three, the washing lotion causticization need add excessive lime, causes aluminum oxide and lime complete reaction generation calcium aluminate solid phase in the washing lotion therefrom, and alumina loss is bigger.3, oxidation style: be in the alumina producing flow process, to select suitable place to add oxygenant, make the sodium oxalate in the Bayer process solution be converted into carbonate.Though this method has the organic effect of tangible eliminating, do not consume a large amount of heat energy and expensive reagent again, can not cause the advantages such as pollution of environment yet, the carbon granules with oxidising process generation is very little, and the shortcoming that is difficult to remove can't be applied in factory at present.4, lime absorption method: it is in mother liquor, to add lime with the organism in the adsorbent solution, gets rid of organic purpose to reach.This method was once tried out in certain factory, facts have proved: the not only weak effect of organism eliminating, and lime can generate calcium aluminate with the sodium aluminate reaction, causes alumina loss.5, ion exchange method: be that Bayer process solution is passed through ion exchange resin, get rid of organic purpose in the solution to reach, this method not only has the ion exchange resin regeneration difficulty, the problem that cost is high, and also organic eliminating amount is also very limited.
Summary of the invention
The technical problem that the present invention will solve provides a kind of sodium oxalate and gets rid of method effective, that flow process simple, less investment, the production and operation cost is low, alumina loss is few employing ultra concentrated method are got rid of sodium oxalate and carbonate from Bayer process solution, can overcome the deficiency of prior art.
Technical scheme of the present invention: this method is that the mother liquor with alumina system concentrates; Make the degree that the causticization sodium oxide is dense in the mother liquor reach 300～370g/l; Liquid through concentrating in the mother liquor of back is sent into the alumina producing system; Solid phase with 80～100 ℃ of hot water or dilute alkaline soln (because of dilute alkaline soln for containing alkali water of condensation or trade effluent, because of may containing certain alkali in these two kinds of water, alkali concn usually 10g/l) to be dissolved into concentration of sodium carbonate be 10～14% A solution; A solution is sent into one section causticizing tank, and in one section causticizing tank, add lime or milk of lime, the amount that adds lime or milk of lime is 1.2～1.4 times of yellow soda ash amount; And causticization got the B slurries in 2～4 hours under 75～95 ℃ condition; Send into two sections causticizing tanks after the B slurries are cooled to 50～70 ℃, and in two sections causticizing tanks, add lime or milk of lime, the amount that adds lime or milk of lime is 0.5～1.0 times of sodium oxalate amount; Causticization got the C slurries in 1.5～3.0 hours under 50～70 ℃ condition; The C slurries are sent into separator-scrubber, and washing lotion is sent into the alumina producing system, and residue is delivered to the alumina laterite washing system.
Concentrating to adopt thickener to concentrate or add the high density liquid caustic and concentrate the mother liquor of alumina system.
When the mother liquor to alumina system concentrates, add sodium oxalate crystal seed or yellow soda ash crystal seed are arranged.
Sodium oxalate crystal seed coefficient is generally 0.5～1.2, and yellow soda ash crystal seed coefficient is generally 0.3～1.0.
Temperature when the mother liquor to alumina system concentrates is 103～110 ℃.
Temperature when the mother liquor to alumina system concentrates is 103～108 ℃.
It is water cooler that the B slurries are carried out the refrigerative system.
In order better to get rid of sodium oxalate and carbonate; The applicant has carried out great deal of experimental: following routine data are part test data of the present invention: wherein Nk representes causticization sodium oxide concentration (Na2Ok) in the solution; Nc representes concentration of sodium carbonate in the solution (Na2Oc); NT representes full alkali concn (Na2OT) in the solution, and AO refers to alumina concentration in the solution (Al2O3).C is meant organic carbon content in the solution mesoxalic acid sodium (Na2C2O4), and
refers to (deposition) rate (%) of separating out that C has.
Ultra concentrated crystal seed coefficient:
Sodium oxalate crystal seed coefficient=
Yellow soda ash crystal seed coefficient=
(1) with Nk=153g/LC
HaveThe mother liquor of=2.46～8.0g/L (ultra concentrated stoste) ultra concentrated can be found out the crystallization eduction rate of sodium oxalate, with stoste C during to the about 300g/L of Nk
HaveRaising and improve (like table 1):
(2) with Nk=136.8g/L, C
HaveThe mother liquor of=1.44g/L (ultra concentrated stoste) carries out ultra concentrated, and along with the raising of hyper-concentration liquid Nk value, the eduction rate of sodium oxalate improves, and when hyper-concentration liquid Nk value reaches the 360g/L left and right sides, can find out that its eduction rate reaches the peak to value (like table 2)
(3) with Nk=136.8g/LC
HaveThe mother liquor of=1.80g/L (ultra concentrated stoste) carries out ultra concentrated, and result of study shows: at ultra concentrated stoste C
HaveUnder the conditions of higher, along with the raising of hyper-concentration liquid Nk value, the eduction rate of sodium oxalate improves equally, when hyper-concentration liquid Nk value reaches the 360g/L left and right sides, and its eduction rate peaking (like table 3)
(4) with table 2 sequence number
, result of study shows: in causticization stoste
Under t=95 ℃ of T=3 hour the condition, C
HaveDeposition be 76.45%, its ultra concentrated precipitate is through one section causticization C
HaveDeposition (as the table .4)
(5) the causticization slip with test number in the table 4 " 7 "～" 9 " is cooled to 50～70 ℃, and presses
Add lime and carry out two sections causticizations, its C
HaveDeposition improves more than 10% on one section causticization basis.
Example: the slip of test number " 7 " is cooled to 50, and adds lime:
Work as lime adding amount:
(6) test-results of interpolation crystal seed
Sequence number in the table 2 " 3 " and " 4 " condition are added the crystal seed test, and the result shows: add the deposition that crystal seed not only can slightly improve the causticization sodium oxalate
, and make and separate out sodium oxalate and contain crystal water (H
2O
Knot) amount reduction significantly.
(7) the causticization slag that the slip of the causticization slag of test number " 7 " in the table 4 (one section causticization) and this test is carried out two sections causticizations carries out solubility test again, its C as a result of two types of tests
HaveThe basically identical of dissolution law again: the washing process alumina concentration is to C
HaveAgain the dissolution rate influence is little, and opposite temperature is to C
HaveDissolution rate again influence big, causticization slag organic carbon is solubility test result such as table 6 again).
Compare with prior art, this has following advantage:
1, ultra concentrated sodium oxalate crystallization eduction rate is high: as with the mother liquor ultra concentrated during to 360g//l (NK): do not add crystal seed C
HaveEduction rate reaches 81.3%, adds crystal seed (crystal seed coefficient 1.0) C
HaveEduction rate reaches 82.1%.); The ultra concentrated process is added crystal seed can make the content of crystal water in the ultra concentrated slag reduce to for 13% (content that does not add seeded crystallization water is about 30%).Show that promptly adding crystal seed makes the sodium oxalate advantages of good crystallization of separating out, particle is thicker, helps the separation and the washing of slag, has prevented that the slag of particulate from getting into solution system again; The sodium oxalate crystallization of ultra concentrated is through one section causticization, and the deposition that sodium oxalate gets into solid phase can reach 76%, and the total deposition (containing a section) of sodium oxalate can reach 85.7～87.6% after two sections causticizations; Sodium oxalate slag after causticization stability is better washed amount that dissolving again gets into solution only 2.9～3.1% under 60～70 ℃ of temperature; Ultra concentrated stoste is behind ultra concentrated, one section causticization and separating, washing, and total elimination factor of its stoste mesoxalic acid sodium is about 57%; Ultra concentrated stoste is behind ultra concentrated, two sections causticizations and separating, washing, and total elimination factor of its stoste mesoxalic acid sodium is about 67%.
2, simple, the speed less investment of flow process; In order effectively to get rid of the sodium oxalate in the bayer liquor, this research only is that the flow process and the processing parameter of operations such as benefit alkali in original evaporation in the alumina producing, salt discharge (Na2CO3), causticization and the production are done further optimization and adjustment; Do not increase new operation, only increase a small amount of equipment; Ultra concentrated makes in the Baeyer solution crystallization separate out and generally selects high-efficiency evaporator for use, the process that the sodium oxalate crystallization is separated out be equally an evaporation of water concentration process meanwhile the salts such as yellow soda ash in the solution separate out together, so lifted the effect of killing three birds with one stone; The causticization that most alumina producer all need be provided with carbonate with separate, washing system.The causticization of mesoxalic acid sodium of the present invention with separate, wash and can altogether use a covering device with carbonate system.
Need be provided with all in alumina producer factory that strong liquid caustic (NaOH content 42～48%) stores and delivery system, the present invention's original complete outfit capable of using only need change strong caustic alkali into and is transported to the ultra concentrated system and gets final product.Below what time find out: the method for this eliminating sodium oxalate with data by MoM and MEI is before arranged, not only flow process is simple and the alumina producing system had no negative interaction, and construction investment economizes.
3, the production and operation cost is low; The present invention neither increases new operation and equipment, need not add any medicine and reagent (crystal seed recycles) at the sodium oxalate exclusion process, also none regeneration and recovery problem; Explain that thus enforcement of the present invention not only can not increase production cost, opposite to effectively sodium oxalate being got rid of from flow process, reached and eliminated the harm of sodium oxalate alumina producing, alumina production cost is decreased.
4, alumina loss is few: the crystallization of ultra concentrated sodium oxalate be with solution separating after dissolve causticization then, the solution in the crystal is merely some attached liquids and gets into causticization, so the method alumina loss is less.
Description of drawings:
Fig. 1 is a production scheme of the present invention.
Embodiment:
Embodiment 1: as shown in Figure 1; Earlier the mother liquor in the alumina producing system (Bayer process solution) is injected into ultra concentrated device 1 and carries out ultra concentrated; Temperature when the mother liquor to alumina system concentrates is 103 ℃; After concentrating through ultra concentrated device 1, the causticization oxidation is received the degree of dense (Nk) and is reached 300g/l in the mother liquor.After a super-concentrated and then concentrated to a specified value is a mother liquor (liquor with a high concentration of caustic lye mixture) by the super-concentrated discharge pump 2 to the separation settling tank 3, the separated liquid overflow into alumina production systems , separating the bottom stream (solid phase) flow pump 5 via the bottom filter 6 to the salt was filtered, the filtrate (liquid) is also fed alumina production system, the solid phase (filter cake) was dissolved into water inside the tank 7, with 80 ℃ dissolved in hot water or a dilute alkali solution concentration of 10% sodium carbonate solution A, the use of dilute alkali solution as alkaline condensation water or industrial waste water, because the water may contain both a base, alkali concentration is usually <10g /> l; A solution tank of the solution was transferred to a feed pump 8 causticizing tank 9, in a causticizing tank 9 by adding lime or lime, lime or lime in an amount of 1.2 times the amount of sodium carbonate and 75 ℃ under the conditions of B causticizing slurry for 2 hours; the separated solids (Na2C2O4 mixture and Na2CO3) for the purpose of a causticizing converted to caustic soda (Na2CO3 + Ca (OH) 2 = CaCO3
+2 NaOH ) and try to make the sodium oxalate into calcium oxalate Na2C2O4 + Ca (OH) 2 = CaC2O4
+2 NaOH).The B slurries are delivered to water cooler 11 through pump 10; Water cooler 11 is a water cooler, ℃ after pipeline is sent into two sections causticizing tanks 12, in two sections causticizing tanks, adds lime or milk of lime at water cooler 11 internal cooling to 50; The amount that adds lime or milk of lime is 0.5 times of sodium oxalate amount; The all right one way or the other of sodium oxalate analyzed gained according to spot sampling, and because of in present actual production, per tour will be carried out twice sampling analysis at least; Therefore just can confirm the content of organic carbon in the solution according to sampling analysis, just can calculate solution mesoxalic acid sodium amount according to the molecular formula Na2C2O4 of sodium oxalate.Causticization got the C slurries in 1.5 hours under 50 ℃ condition, and the C slurries are delivered to through pump 13 and separated and washing machine 14, and washing lotion is sent into the alumina producing system, washed the back slag and delivered to the alumina laterite washing system.
Embodiment 2: as shown in Figure 1; Earlier the mother liquor in the alumina producing system (Bayer process solution) is injected into ultra concentrated device 1 and carries out ultra concentrated; Temperature when the mother liquor to alumina system concentrates is 110 ℃; 108 ℃ of its preferred temperature, after concentrating through ultra concentrated device 1, the causticization oxidation is received the degree of dense (Nk) and is reached 370g/l in the mother liquor.Can also be added to the outlet super-concentrated amount of high concentration of caustic lye (42 ~ 48% NaOH), the mother liquor with a high concentration of caustic lye mixture of caustic sodium oxide concentration (Nk) reaches 370g of / l; Then after a super concentrator mother liquor was concentrated to a specified value (the mother liquor with a high concentration of caustic lye mixture) by the super-concentrated discharge pump 2 to the separation settling tank 3, liquid separation overflow into alumina production systems, separation underflow (solid phase) through the underflow to the salt filter pump 5 6 The filtrate (liquid) is also fed alumina production system, the solid phase (filter cake) was dissolved into water inside the tank 7, with 100 ℃ dissolved in hot water or a dilute alkali solution concentration of 14% sodium carbonate solution A, A dissolving tank solution was fed to the feed pump 8, a causticizing tank 9, in a causticizing tank 9 by adding lime or lime, The amount of lime or lime 1.4 times the amount of sodium carbonate and 95 ℃ for 4 hours under the conditions of lime slurry of B; the separated solids (Na2C2O4 and Na2CO3 mixture) for a period of lime is intended to converted to caustic soda (Na2CO3 + Ca (OH) 2 = CaCO3
+2 NaOH) and try to make the sodium oxalate into calcium oxalate Na2C2O4 + Ca (OH) 2 = CaC2O4
+2 NaOH).The B slurries are delivered to water cooler 11 through pump 10; ℃ after pipeline is sent into two sections causticizing tanks 12, in two sections causticizing tanks, add lime or milk of lime at water cooler 11 internal cooling to 70, the amount that adds lime or milk of lime is 1.0 times of sodium oxalate amount; Causticization got the C slurries in 3.0 hours under 70 ℃ condition; The C slurries are delivered to through pump 13 and are separated and washing machine 14, and washing lotion is sent into the alumina producing system, wash the back slag and deliver to the alumina laterite washing system.
Embodiment 3: as shown in Figure 1; Earlier the mother liquor in the alumina producing system (Bayer process solution) is injected into ultra concentrated device 1 and carries out ultra concentrated; Temperature when the mother liquor to alumina system concentrates is 107 ℃; After concentrating through ultra concentrated device 1, the causticization oxidation is received the degree of dense (Nk) and is reached 360g/l in the mother liquor.Can also be added to the outlet super-concentrated amount of high concentration of caustic lye (42 ~ 48% NaOH), the mother liquor with a high concentration of caustic lye mixture of caustic sodium oxide concentration (Nk) reaches 360g of / l; Then after a super concentrator mother liquor was concentrated to a specified value (the mother liquor with a high concentration of caustic lye mixture) by the super-concentrated discharge pump 2 to the separation settling tank 3, liquid separation overflow into alumina production systems, separation underflow (solid phase) through the underflow to the salt filter pump 5 6 The filtrate (liquid) is also fed alumina production system, the solid phase (filter cake) was dissolved into water inside the tank 7, with 90 ℃ dissolved in hot water or a dilute alkali solution concentration of 12% sodium carbonate solution A, A dissolving tank solution was fed to the feed pump 8, a causticizing tank 9, in a causticizing tank 9 by adding lime or lime, The amount of lime or lime 1.3 times the amount of sodium carbonate, and at 85 ℃ for 3 hours under the conditions of B causticizing slurry; the separated solids (Na2C2O4 and Na2CO3 mixture) for a period of lime is intended to converted to caustic soda (Na2CO3 + Ca (OH) 2 = CaCO3
+2 NaOH) and try to make the sodium oxalate into calcium oxalate Na2C2O4 + Ca (OH) 2 = CaC2O4
+2 NaOH).The B slurries are delivered to water cooler 11 through pump 10; ℃ after pipeline is sent into two sections causticizing tanks 12, in two sections causticizing tanks, add lime or milk of lime at water cooler 11 internal cooling to 60, the amount that adds lime or milk of lime is 0.8 times of sodium oxalate amount; Causticization got the C slurries in 2.2 hours under 60 ℃ condition; The C slurries are delivered to through pump 13 and are separated and washing machine 14, and washing lotion is sent into the alumina producing system, wash the back slag and deliver to the alumina laterite washing system.When mother liquor is carried out ultra concentrated, can in ultra concentrated device 1, add crystal seed through crystal seed pump 4 for the crystallization content that further improves sodium oxalate: the sodium oxalate crystal seed coefficient that wherein adds is generally 0.5～1.2; Yellow soda ash crystal seed coefficient is generally 0.3～1.0; This measure not only makes salt crystallization eduction rate increase, and more efficiently is to make to separate out that crystal water content reduces significantly in the crystallization.
Claims (7)
1. method that adopts the ultra concentrated method from Bayer process solution, to get rid of sodium oxalate and carbonate; It is characterized in that: this method is that the mother liquor with alumina system concentrates; Make that causticization sodium oxide concentration reaches 300～370g/l in the mother liquor; Liquid through concentrating in the mother liquor of back is sent into the alumina producing system, and it is 10～14% A solution that solid phase uses 80～100 ℃ of hot water or dilute alkaline soln to be dissolved into concentration of sodium carbonate; A solution is sent into one section causticizing tank, and in one section causticizing tank, add lime or milk of lime, the amount that adds lime or milk of lime is 1.2～1.4 times of yellow soda ash amount; And causticization got the B slurries in 2～4 hours under 75～95 ℃ condition; Send into two sections causticizing tanks after the B slurries are cooled to 50～70 ℃, and in two sections causticizing tanks, add lime or milk of lime, the amount that adds lime or milk of lime is 0.5～1.0 times of sodium oxalate amount; Causticization got the C slurries in 1.5～3.0 hours under 50～70 ℃ condition; The C slurries are sent into separator-scrubber, and washing lotion is sent into the alumina producing system, and residue is delivered to the alumina laterite washing system.
2. employing ultra concentrated method according to claim 1 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: concentrating can adopt thickener to concentrate or add the high density liquid caustic and concentrate the mother liquor of alumina system.
3. employing ultra concentrated method according to claim 1 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: when the mother liquor to alumina system concentrates, adding has sodium oxalate crystal seed or yellow soda ash crystal seed.
4. employing ultra concentrated method according to claim 3 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: sodium oxalate crystal seed coefficient is generally 0.5～1.2, and yellow soda ash crystal seed coefficient is generally 0.3～1.0.
5. employing ultra concentrated method according to claim 1 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: the temperature when the mother liquor to alumina system concentrates is 103～110 ℃.
6. employing ultra concentrated method according to claim 5 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: the temperature when the mother liquor to alumina system concentrates is 103～108 ℃.
7. employing ultra concentrated method according to claim 1 is got rid of the method for sodium oxalate and carbonate from Bayer process solution, it is characterized in that: it is water cooler that the B slurries are carried out the refrigerative system.
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| CN102259903B (en) * | 2011-06-20 | 2013-06-05 | 中国铝业股份有限公司 | Method for reducing content of sodium carbonate in alumina Bayer process solution |
| CN103787392B (en) * | 2014-02-12 | 2015-02-04 | 内蒙古蒙西鄂尔多斯铝业有限公司 | Method for producing aluminium oxide by using clinker dissolving-out liquid subjected to lime desilicication treatment |
| CN112499656A (en) * | 2020-12-16 | 2021-03-16 | 贵州华锦铝业有限公司 | Treatment method of discharged salt causticization slurry in alumina production |
| CN113184889B (en) * | 2021-03-22 | 2023-01-20 | 中国铝业股份有限公司 | Comprehensive utilization method of crystallized sodium oxalate slag in alumina production |
| CN113149048B (en) * | 2021-03-26 | 2022-08-26 | 马朝扬 | Method for treating sodium oxalate solid waste residues in alumina production process |
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