CN101306824A - Cold-separation process of NaNO3 from nitre ore leaching liquid - Google Patents

Cold-separation process of NaNO3 from nitre ore leaching liquid Download PDF

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Publication number
CN101306824A
CN101306824A CNA2007101033765A CN200710103376A CN101306824A CN 101306824 A CN101306824 A CN 101306824A CN A2007101033765 A CNA2007101033765 A CN A2007101033765A CN 200710103376 A CN200710103376 A CN 200710103376A CN 101306824 A CN101306824 A CN 101306824A
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cold analysis
nano
cold
leaching
nacl
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刘利鹏
茆晓宝
郝建委
顾建
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CHANGSHA DESIGN INSTITUTE OF XINJIANG NITER POTASSIUM Co Ltd CHEMICAL DEPART
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CHANGSHA DESIGN INSTITUTE OF XINJIANG NITER POTASSIUM Co Ltd CHEMICAL DEPART
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Abstract

A method for cold separation of NaNO3 from leached solution of sodium nitrate ores comprises the steps of pumping high concentration bittern with NaNO3 content of 450g/L from leaching process (i.e. leached solution) into a cold separation tank, starting up a refrigeration unit and a stirrer, controlling the material temperature in the cold separation tank in a range of 2-18 DEG C, performing constant-temperature cold separation at 2-18 DEG C for 5-15 hours, discharging the material from a discharge valve of the cold separation tank, and performing centrifugal separation. The inventive method conducts solid-liquid separation of the leached solution after cold separation, the obtained initial product has good quality, the content of sodium nitrate is up to 85.11%, and the purity of sodium nitrate (dry basis) is 92.85%. After cold separation and centrifugal separation, the single-pass average yield of sodium nitrate is 34.73%, and the content of sodium nitrate in the mother liquid after cold separation is about 350g/L. The inventive method has the advantages of simple process, and easy operation.

Description

Sodium nitre ore leaching liquid NaNO 3Cold analysis technology
One, technical field
The present invention relates to a kind of leaching liquid and carry out cold analysis separation NaNO saltier ore after the pre-treatment 3Deng the technology of solid matter, sodium nitre ore leaching liquid NaNO especially 3Cold analysis technology.
Two, technical background
The evaluation and exploration technology of nitre mineral comes into one's own, and the salt in the nitre mineral mainly is NaNO 3, NaCl and Na 2SO 4Deng, all soluble in water, the variation of the solubility with temperature in their each comfortable water is as SODIUMNITRATE NaNO wherein 3Use very extensive as large industrial or agricultural starting material.SODIUMNITRATE as fertilizer, is specially adapted to shell class crop on agricultural, root crop is as beet, radish etc.It simultaneously also is the raw material of making saltpetre, explosive, picric acid, dyestuff etc.; Also be used as defoamer, discoloring agent, finings and the Aid for Oxidation flux of glass production; Porcelain enamel industry is used to prepare enamel frit as oxygenant and fusing assistant; Mechanical industry is prepared the ferrous metal blueing agent as metal cleaner; Metallurgical industry is as the aluminum alloy heat treatment agent; Light industry is as the tobacco ignition dope; Medicine industry is as the substratum of penicillin; The discoloring agent that also can be used as molten caustic(soda).In addition, also can be used as the chromogenic reagent etc. of refrigerant, canned meat.
The SODIUMNITRATE of China is owing to limit by resource at present, and output is less, based on industrial use.The structure of consumer demand roughly is: light industry accounts for 80%, chemical industry accounts for 9%, mechanical industry accounts for 6%, other industry accounts for 5%.Up to the present, in the known technology by saliter stone ore production SODIUMNITRATE product, its production process route is concluded two kinds: a kind of is after ore leaches, the bittern heating evaporation, behind filtering separation sodium-chlor, the sodium sulfate, crystallisation by cooling is produced SODIUMNITRATE again, and the shortcoming of this technical process is that energy consumption height, production cost height, quality product are low; Another kind is the solar evaporation flow process, i.e. ore reduction, leaching, and bittern send the salt pan solar evaporation, separate back gained crude salt and send finishing department production SODIUMNITRATE, the advantage of this operational path is to make full use of sun power, and helps the development and use of low grade ore, but water loss is big.The production method of extracting SODIUMNITRATE with two-step approach from the SODIUMNITRATE concentrate also claims the Shanks method, operating process comprises the dress ore deposit, leaching, wash and unload the ore deposit, mother liquor after leaching uses liquid from crystallization, the SODIUMNITRATE that contains 450g/l, leaching successively, leach at last and reduce temperature again to the SODIUMNITRATE crystallization in the solution being separated out after the concentration of finishing the liquid SODIUMNITRATE reaches 700g/l near free air temperature, the rate of recovery of its SODIUMNITRATE is greatly about 60%, nitrate radical in the slag is 5%~8%, because this method rate of recovery is low, the energy consumption height, and require the of high grade of ore deposit, up to the present, the SODIUMNITRATE of using this method to produce only accounts for the seldom part of SODIUMNITRATE total amount.Utilize the technology of nitre production SODIUMNITRATE to belong to Na +//NO 3 -, Cl -, SO 4 2--H 2O quaternary salt-water system model is raised.Because the NaNO in the nitre mineral 3, NaCl and Na 2SO 4Deng salt, all soluble in water, the follow-up technology of separating out influences bigger to crystallization precipitate purity from leaching liquid, moiety.
Three, summary of the invention
Goal of the invention of the present invention is, a kind ofly can keep NaNO in the precipitate 3Higher low technology, i.e. the sodium nitre ore leaching liquid NaNO of separating out of other composition that keep simultaneously of content 3Cold analysis technology.
Goal of the invention of the present invention realizes by following measure, will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid pump and is gone in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 2-18 ℃ of scope in the control cold analysis groove, treat temperature of charge reach 2-18 ℃ after constant temperature cold analysis 5-15 hour again, material is discharged from cold analysis groove bleeder valve carry out centrifugation again.
The present invention utilizes leaching to finish liquid cooling and analyses the back solid-liquid separation, and the head product quality of institute's output is better, and SODIUMNITRATE content reaches 85.11%, and its butt purity is 92.85%; After the cold analysis centrifugation, the one way average yield of SODIUMNITRATE is 34.73%, and mother liquor contains SODIUMNITRATE about 350g/l after the cold analysis; With carrying increasing of the water yield in the head product secretly, the content of sodium sulfate increases, and the content of sodium-chlor does not have considerable change, and SODIUMNITRATE content descends in the head product.The average yield of cold analysis sepn process SODIUMNITRATE is 34.73%, and technology is simple and clear, and is easy to implement.
Four, description of drawings
Fig. 1 be in the embodiment of the invention 1 under 0-110 ℃ of differing temps water to NaNO 3, NaCl, NaSO 4Three kinds of component substances changes in solubility synoptic diagram
Fig. 2 is that cold analysis head product of the present invention is carried the influence synoptic diagram of the water yield to the head product quality secretly
Five, embodiment
Embodiment 1: will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 8548.6kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 820kg.
Solid, liquid is distinguished sampling analysis mutually, and liquid phase promptly enters leaching stage.
Mother liquor weight 8548.6kg before the cold analysis, proportion 1.3788g/ml wherein contains 464.7g/lNaNO 3, 160.2g/l NaCl, 36.0g/l Na 2SO 4, mother liquor weight 7263.9kg after the cold analysis, proportion 1.3207g/ml wherein contains 345.7g/l NaNO 3, 180.6g/l NaCl, 25.3g/lNa 2SO 4, obtaining analysing the salt butt is cold analysis head product 820kg, consists of 81.21% NaNO 3, 0.64%NaCl, 6.95%Na 2SO 4, 11.20%H 2O, NaNO 3Yield 23.11%.
The analytical procedure of all conventional elements (ion) is respectively: calcium, magnesium ion adopt the EDTA volumetry; Chlorion adopts the Mercury pernitrate volumetry; Sulfate ion adopts the barium sulfate weighting method; Nitrate ion adopts the potassium dichromate oxidation reductometry; Sodium ions content adopts yin, yang ionic equilibrium method to try to achieve.Relevant analytical procedure in " analytical procedure of bittern and salt " book that concrete operations are write with reference to salt lake, Qinghai institute.The analytical procedure of the SODIUMNITRATE product of producing then adopts among the GB/T4553-2002 corresponding component analytical procedure to analyze and measure.
Embodiment 2: will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 9444.0kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 978kg.
Mother liquor weight 9444.0kg before the cold analysis, proportion 1.3687g/ml wherein contains 491.0g/lNaNO 3, 162.8g/l NaCl, 37.1g/l Na 2SO 4, mother liquor weight 7935.6kg after the cold analysis, proportion 1.3226g/ml wherein contains 344.3g/l NaNO 3, 175.4g/l NaCl, 25.3g/lNa 2SO 4, obtaining analysing the salt butt is cold analysis head product 978kg, consists of 87.77%NaNO 3, 0.54%NaCl, 4.96%Na 2SO 4, 6.73%H 20, NaNO 3Yield 25.34%.
Embodiment 3: will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 9626.4kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 1550kg.
Mother liquor weight 9626.4kg before the cold analysis, proportion 1.3752g/ml wherein contains 458.5g/lNaNO 3, 164.9g/l NaCl, 36.6g/l Na 2SO 4, mother liquor weight 7509.0kg after the cold analysis, proportion 1.3244g/ml wherein contains 354.2g/l NaNO 3, 177.2g/l NaCl, 29.9g/lNa 2SO 4, obtaining analysing the salt butt is cold analysis head product 1550kg, consists of 86.24%NaNO 3, 0.55%NaCl, 5.12%Na 2SO 4, 8.09%H 2O, NaNO 3Yield 41.65%.
Leaching is finished liquid cooling and is analysed solid-liquid separation after 5 ℃, and the head product quality of institute's output is better, and SODIUMNITRATE content reaches 85.11%, and its butt purity is 92.85%; After the cold analysis centrifugation, the one way average yield of SODIUMNITRATE is 34.73%, and mother liquor contains SODIUMNITRATE about 350g/l after the cold analysis; It is poor that the SODIUMNITRATE product purity has certain volume after the centrifugation, and major cause is in centrifugal separation processes, and product is owing to the entrainment mother liquor difference, thus different product purity and the stability of influencing of sodium-chlor in the solid phase with sodium sulphate content.With carrying increasing of the water yield in the head product secretly, the content of sodium sulfate increases, and the content of sodium-chlor does not have considerable change, and SODIUMNITRATE content descends in the head product.

Claims (6)

1, sodium nitre ore leaching liquid NaNO 3Cold analysis technology is characterized in that, will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid pump and is gone in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 2-18 ℃ of scope in the control cold analysis groove, treat temperature of charge reach 2-18 ℃ after constant temperature cold analysis 5-15 hour again, material is discharged from cold analysis groove bleeder valve carry out centrifugation again.
2, sodium nitre ore leaching liquid NaNO as claimed in claim 1 3Cold analysis technology is characterized in that, will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 8548.6kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 820kg, mother liquor weight 8548.6kg before the cold analysis, proportion 1.3788g/ml wherein contains 464.7g/l NaNO 3, 160.2g/l NaCl, 36.0g/l Na 2SO 4, mother liquor weight 7263.9kg after the cold analysis, proportion 1.3207g/ml wherein contains 345.7g/l NaNO 3, 180.6g/l NaCl, 25.3g/l Na 2SO 4, obtaining analysing the salt butt is cold analysis head product 820kg, consists of 81.21%NaNO 3, 0.64%NaCl, 6.95% Na 2SO 4, 11.20%H 2O, NaNO 3Yield 23.11%.
3, sodium nitre ore leaching liquid NaNO as claimed in claim 1 3Cold analysis technology is characterized in that, will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 9444.0kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 978kg, mother liquor weight 9444.0kg before the cold analysis, proportion 1.3687g/ml wherein contains 491.0g/l NaNO 3, 162.8g/l NaCl, 37.1g/l Na 2SO 4, mother liquor weight 7935.6kg after the cold analysis, proportion 1.3226g/ml wherein contains 344.3g/l NaNO 3, 175.4g/l NaCl, 25.3g/l Na 2SO 4, obtaining analysing the salt butt is cold analysis head product 978kg, consists of 87.77%NaNO 3, 0.54%NaCl, 4.96%Na 2SO 4, 6.73%H 2O, NaNO 3Yield 25.34%.
4, sodium nitre ore leaching liquid NaNO as claimed in claim 1 3Cold analysis technology is characterized in that, will be from the NaNO in the leaching process 3Content reach the above high density bittern of 450g/l, i.e. leaching is finished liquid 9626.4kg and is pumped in the cold analysis groove, start freezing unit and stirrer, temperature of charge is 5 ± 1 ℃ of scopes in the control cold analysis groove, treat temperature of charge reach 5 ℃ after constant temperature cold analysis 6 hours again, again material is discharged from cold analysis groove bleeder valve and carries out centrifugation to obtain analysing the salt butt be cold analysis head product 1550kg, mother liquor weight 9626.4kg before the cold analysis, proportion 1.3752g/ml wherein contains 458.5g/l NaNO 3, 164.9g/l NaCl, 36.6g/l Na 2SO 4, mother liquor weight 7509.0kg after the cold analysis, proportion 1.3244g/ml wherein contains 354.2g/l NaNO 3, 177.2g/l NaCl, 29.9g/l Na 2SO 4, obtaining analysing the salt butt is cold analysis head product 1550kg, consists of 86.24%NaNO 3, 0.55%NaCl, 5.12%Na 2SO 4, 8.09%H 2O, NaNO 3Yield 41.65%.
5, sodium nitre ore leaching liquid NaNO as claimed in claim 1 3Cold analysis technology is characterized in that, leaching is finished liquid cooling and analysed solid-liquid separation after 5 ℃, and the head product quality of institute's output is better, and SODIUMNITRATE content reaches 85.11%, and its butt purity is 92.85%.
6, sodium nitre ore leaching liquid NaNO as claimed in claim 1 3Cold analysis technology is characterized in that, goes out to carry increasing of the water yield in the head product secretly with cold analysis, and the content of sodium sulfate increases, and the content of sodium-chlor does not have considerable change, and SODIUMNITRATE content descends in the head product.
CNA2007101033765A 2007-05-16 2007-05-16 Cold-separation process of NaNO3 from nitre ore leaching liquid Pending CN101306824A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923737A (en) * 2012-10-18 2013-02-13 新疆硝石钾肥有限公司 Method for dynamically dissolving and preparing nitratine ore leaching solution

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923737A (en) * 2012-10-18 2013-02-13 新疆硝石钾肥有限公司 Method for dynamically dissolving and preparing nitratine ore leaching solution

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Open date: 20081119