CN101168444A - Technique for producing sodium nitrate by chilisaltpeter adverse current circulation leaching - Google Patents
Technique for producing sodium nitrate by chilisaltpeter adverse current circulation leaching Download PDFInfo
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- CN101168444A CN101168444A CNA2006101506618A CN200610150661A CN101168444A CN 101168444 A CN101168444 A CN 101168444A CN A2006101506618 A CNA2006101506618 A CN A2006101506618A CN 200610150661 A CN200610150661 A CN 200610150661A CN 101168444 A CN101168444 A CN 101168444A
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Abstract
The invention relates to a process for producing sodium nitrate by using nitratine reverse-flow circulation extraction, which comprises steps as follows: (1) breaking ores into the grains smaller not larger than 5cm, (2) reverse-flow circulation leaching: after 2-6 stages of reverse-flow circulation immerge, the sodium nitrate content of extraction solution is increased from 300-380g/l to 390-500g/l, (3) separating, washing and drying at low temperature that exchanges heat between the extraction solution and low-temperature separation mother liquid, to reduce temperature, mixing and reducing temperature to -10-20DEG C, and keeping temperature for 100-140min, separating solid and liquid, filtering and washing via a saturated sodium nitrate, according to the mass ratio between product and sodium nitrate solution as 6/1-5/1, then drying to obtain sodium nitrate product, and feeding the separated mother liquid into the step (2), to process next circulation. The invention can save water more than 40%, and save energy more than 25%, while the single-process collecting rate is more than 25% and the total collecting rate of sodium nitrate in ore is more than 95.0%. The product obtained by low-temperature separation contains sodium nitrate more than 92%, and the washed product contains sodium nitrate more than 98%. The invention can use low-grade nitratine mine to produce sodium nitrate.
Description
One, technical field:
The present invention relates to a kind of production technique of SODIUMNITRATE, especially a kind of technology with preparing sodium nitrate with soda niter.
Two, background technology:
SODIUMNITRATE is water white transparency or faint yellow rhomboidan, can make chemical analysis reagent, oxygenant, chemical fertilizer, and system fireworks, system nitric acid, dyestuff are synthetic etc.Being mainly used in and making saltpetre, explosive, picric acid and other nitrate, also be widely used in glass industry, porcelain enamel industry, dyestuffs industries, medicine industry and agricultural, is a kind of important Inorganic Chemicals.
In the known technology, the technology of directly utilizing sodium nitre processing SODIUMNITRATE is based on having the higher nitre of the SODIUMNITRATE of containing ore deposit, content even more than 60%, in this case, can directly add water extraction in ore, saltwater brine can obtain the SODIUMNITRATE product through condensing crystal again.Along with the decline of ore grade, complete processing develops into the pond by direct water logging and soaks and add leaching, solar pond and concentrate molten slagging-off, leaching solution evaporating, concentrating and crystallizing, the output SODIUMNITRATE product of soaking of work in-process.But ore advances the pond granularity requirements below 8 centimeters during leaching, and ore grade must be more than 10%.
Though China has abundant sodium nitre ore resources, its reserves are only second to Chile and occupy the second in the world, and the nitrate ore grade is generally below 8%.It is reported that Xinjiang SODIUMNITRATE distant view stock number reaches 1.7 hundred million tons.Xinjiang saliter stone ore mainly is distributed in little careless lake and areas to the south and ground such as seven Ke Tai and Tu Yugou-Sai Ergaifu.Its ore is made up of fragmental products and saline minerals.Saline minerals mainly contains sodium nitre, darapskite, halite, sylvite, gypsum, semi-hydrated gypsum, thenardite, bloedite, hanksite.Bed top is a loose sandy gravel coverture, with ore bed obvious limit is arranged, and is mixed by compositions such as sand, clay, gravels.Seam floor is the sand gravel layer that contains halite, is the gradual transition relation with ore bed.
China carries out quite early, intermittently so far the exploitation processing of saliter stone ore, existing nearly 50 years history, but method for producing is very outmoded mostly, promptly stirs leaching with water, separate, the leaching liquid that obtains is with the pan concentrated recrystallize of getting salt by evaporation of sea-water, boil the salt off the water again, process recovery ratio only 30～40%.
The public use of improvement technology is also arranged in the known technology, build heap, brine sparge leaching removal of impurities as ore; Salt pan evaporation separates sodium-chlor, output SODIUMNITRATE or claims the darapskite work in-process, work in-process through moltenly soak, the novel process of evaporating, concentrating and crystallizing output SODIUMNITRATE product.This technology is compared with complete processing before, has not only solved the separation problem in extracting, and has saved the mine water, and made full use of low grade ore; The mode of shining with the beach, salt pan is separated the associated mineral in the leaching liquid, concentrates the purpose mineral, has saved the energy, has reduced cost, has improved benefit.Present this technology is answered can be more extensive, built up many covers production equipment, and throughput reaches 100,000 tons.But this process water amount is still bigger than normal, and the influence that sprays wind-engaging when leaching is bigger, and sodium nitrate concentration is low in the leaching liquid, and it is relatively large that the salt pan construction investment is shone on the beach, and energy consumption is higher during salt pan work in-process production SODIUMNITRATE.
Three, summary of the invention:
It is few that technical problem to be solved by this invention is to propose a kind of water consumption, less energy consumption, be not subjected to the weather condition restriction, be easy to realize large-scale industrial production, the service temperature gentleness, production cost is low, and economic benefit is better produced the production technique of SODIUMNITRATE with the saliter stone ore, promptly a kind of technology with sodium nitre circulated in countercurrent leaching production SODIUMNITRATE.
The measure that the present invention solves above technical problem is, takes the circulated in countercurrent leaching technology, specifically may further comprise the steps: (1) ore reduction: become particle diameter to≤5cm particle the ore reduction of saliter stone ore; (2) circulated in countercurrent leaching: the ore that fragmentation is the good counter-current extraction column of packing into, after adjusted low ternperature separation process mother liquor is warming up to 35 ℃～70 ℃, provide its energy to enter by header tank or pump from adverse current extraction column bottom, flow out from the counter-current extraction column upper isopipe again, through 2～6 stage countercurrents circulation leaching, the content of SODIUMNITRATE will rise to 390～500g/l from 300～380g/l in the leaching liquid, and the leaching liquid of this moment is leaching and finishes liquid; (3) low ternperature separation process, washing, drying: leaching is finished liquid after lowering the temperature with the heat exchange of low ternperature separation process mother liquor, under agitation condition, be cooled to-10 ℃～20 ℃ again, be incubated 100 minutes simultaneously-140 minutes, carry out solid-liquid separation thereafter, after about 6/1～5/1 weight ratio was carried out filtration washing by product/sodium nitrate solution, drying promptly got the SODIUMNITRATE product to head product after the separation through saturated sodium nitrate solution, mother liquor after the separation then enters step (2), circulates next time.
The invention has the advantages that technical process is short, water consumption is existing can economize on water more than 40% with saliter stone ore production SODIUMNITRATE technology, and energy-conservation more than 25%, simple to operate, once through yield is more than 25%, and the total recovery of SODIUMNITRATE is more than 95.0% in the ore.The product that low ternperature separation process obtains contains SODIUMNITRATE more than 92%, and product contains SODIUMNITRATE more than 98% after washing.The present invention is particularly suitable for low-grade saliter stone ore production SODIUMNITRATE, and its production cost is low, and is very economical worthwhile.
Four, embodiment:
Embodiment 1: take the circulated in countercurrent leaching technology, specifically may further comprise the steps:
(1) SODIUMNITRATE content 6% saliter stone ore ore is crushed to particle diameter≤5cm particle with jaw crusher;
(2) to be loaded into aspect ratio be in 5 the counter-current extraction column for ore that fragmentation is good, flush to ore and extraction column are suitable for reading, after the leaching bittern that contains SODIUMNITRATE 355g/L for preparing is heated to 45 ℃, leaching bittern injects counter-current extraction column from header tank to be ended when liquid level floods mineral surface through the bottom, and leaching bittern residence time in post is 10 hours; After then being heated to 45 ℃ equally by the leaching bittern that contains SODIUMNITRATE 355g/L again, through bottom injecting second stage counter-current extraction column from second stage header tank from header tank through the leaching dope that bottom injection counter-current extraction column stops the front 10 hours is flow to intercepting basin to be preheated to 45 ℃ again by upper isopipe after ends when liquid level floods mineral surface, the injection speed of leaching liquid steadily rises to suitable with liquid level in the post, leaching bittern residence time in the post of the second stage is 10 hours, after step was carried out 4 times altogether according to this, resulting leaching was finished liquid and is contained SODIUMNITRATE 475g/L;
(3) leaching that will contain SODIUMNITRATE 475g/L is finished liquid carry out low ternperature separation process in 5 ℃ environment.Earlier liquid being finished in leaching stirred 120 minutes in 5 ℃ environment, carry out solid-liquid separation again, resulting head product butt contains SODIUMNITRATE 92wt%, after saturated sodium nitrate solution carries out filtration washing by the weight ratio of product/sodium nitrate solution 6/1, the products obtained therefrom drying, promptly get the SODIUMNITRATE product, contain SODIUMNITRATE 98wt% butt, the mother liquor after the separation solid phase then enters operation steps (2) after adjusting;
The mine tailings carrying out washing treatment: ore is through behind 4 counter-current extractions, the washing water of using lower concentration instead carry out laundry operation 2 times to the slag after leaching, wash water enters circulation leaching system through circulation cleaning and after concentrating, again at last once with clear water washing slag, the contents on dry basis of SODIUMNITRATE will be reduced to below 0.4% in the slag at this moment, and tailings promptly reaches emission request.
The advantage of the embodiment of the invention is that technical process is short, and water consumption is existing can economize on water more than 40% with saliter stone ore production SODIUMNITRATE technology, and energy-conservation more than 25%, simple to operate, once through yield is more than 25%, and the total recovery of SODIUMNITRATE is more than 95.0% in the ore.The product that low ternperature separation process obtains contains SODIUMNITRATE more than 92%, and product contains SODIUMNITRATE more than 98% after washing.The present invention is particularly suitable for low-grade saliter stone ore production SODIUMNITRATE, and its production cost is low, and is very economical worthwhile.
Embodiment 2: take the circulated in countercurrent leaching technology, specifically may further comprise the steps:
(1) SODIUMNITRATE content 6% saliter stone ore ore is crushed to particle diameter≤5cm particle with jaw crusher;
(2) to be loaded into aspect ratio be in 3 the counter-current extraction column for ore that fragmentation is good, flush to ore and extraction column are suitable for reading, after the leaching bittern that contains SODIUMNITRATE 365g/L for preparing is heated to 65 ℃, leaching bittern injects counter-current extraction column from header tank to be ended when liquid level floods mineral surface through the bottom, and leaching bittern residence time in post is 8 hours; After then being heated to 65 ℃ equally by the leaching bittern that contains SODIUMNITRATE 365g/L again, through bottom injecting second stage counter-current extraction column from second stage header tank from header tank through the leaching dope that bottom injection counter-current extraction column stops the front 8 hours is flow to intercepting basin to be preheated to 65 ℃ again by upper isopipe after ends when liquid level floods mineral surface, the injection speed of leaching liquid steadily rises to suitable with liquid level in the post, leaching bittern residence time in the post of the second stage is 8 hours, after step was carried out 3 times altogether according to this, resulting leaching was finished liquid and is contained SODIUMNITRATE 480g/L;
(3) leaching that will contain SODIUMNITRATE 480g/L is finished liquid carry out low ternperature separation process in 10 ℃ environment.Earlier liquid being finished in leaching stirred 120 minutes in 5 ℃ environment, carry out solid-liquid separation again, resulting head product contains SODIUMNITRATE butt 93wt%, filter by the weight ratio of product/sodium nitrate solution 5/1 through saturated sodium nitrate solution, the products obtained therefrom drying, promptly get the SODIUMNITRATE product, contain SODIUMNITRATE 98wt% butt, the mother liquor after the separation solid phase then enters operation steps (2) after adjusting.
The mine tailings carrying out washing treatment: ore is through behind 3 counter-current extractions, the washing water of using lower concentration instead carry out laundry operation 3 times to the slag after leaching, wash water enters circulation leaching system through circulation cleaning and after concentrating, again at last once with clear water washing slag, the content of SODIUMNITRATE will be reduced to butt below 0.4% in the slag at this moment, and tailings promptly reaches emission request.
Embodiment 3: preferred implementation is: (1) ore reduction: become particle diameter to≤5cm particle the ore reduction of saliter stone ore; (2) circulated in countercurrent leaching: the ore that fragmentation is the good counter-current extraction column of packing into, extraction column aspect ratio scope is preferably 1～5, preferred 3～4, after adjusted low ternperature separation process mother liquor is warming up to 45 ℃～60 ℃, provide its energy to enter, flow out from the counter-current extraction column upper isopipe again from adverse current extraction column bottom by header tank or pump, through 3-4 stage countercurrent circulation leaching, the content of SODIUMNITRATE will rise to 390～500g/L from 300～380g/L in the leaching liquid, and the leaching liquid of this moment is leaching and finishes liquid; (3) low ternperature separation process, washing, drying: leaching is finished liquid after lowering the temperature with the heat exchange of low ternperature separation process mother liquor, under agitation condition, be cooled to 5 ℃～10 ℃ again, be incubated 120 minutes simultaneously, carry out solid-liquid separation thereafter, after about 6/1～5/1 weight ratio was carried out filtration washing by product/sodium nitrate solution, drying promptly got purity 98% above SODIUMNITRATE product to the head product that contains SODIUMNITRATE 92-95% after the separation through saturated sodium nitrate solution, mother liquor after the separation then enters step (2), circulates next time.
Claims (4)
1. the technology with sodium nitre circulated in countercurrent leaching production SODIUMNITRATE is characterized in that, takes the circulated in countercurrent leaching technology, specifically may further comprise the steps: (1) ore reduction: become particle diameter to≤5cm particle the ore reduction of saliter stone ore; (2) circulated in countercurrent leaching: the ore that fragmentation is the good counter-current extraction column of packing into, after adjusted low ternperature separation process mother liquor is warming up to 35 ℃～70 ℃, provide its energy to enter by header tank or pump from adverse current extraction column bottom, flow out from the counter-current extraction column upper isopipe again, through 2～6 stage countercurrents circulation leaching, the content of SODIUMNITRATE will rise to 390～500g/l from 300～380g/l in the leaching liquid, and the leaching liquid of this moment is leaching and finishes liquid; (3) low ternperature separation process, washing, drying: leaching is finished liquid after lowering the temperature with the heat exchange of low ternperature separation process mother liquor, under agitation condition, be cooled to-10 ℃～20 ℃ again, be incubated 100 minutes simultaneously-140 minutes, carry out solid-liquid separation thereafter, after about 6/1～5/1 weight ratio was carried out filtration washing by product/sodium nitrate solution, drying promptly got the SODIUMNITRATE product to head product after the separation through saturated sodium nitrate solution, mother liquor after the separation then enters step (2), circulates next time.
2. a kind of technology as claimed in claim 1 with sodium nitre circulated in countercurrent leaching production SODIUMNITRATE, it is characterized in that, take the circulated in countercurrent leaching technology, specifically may further comprise the steps: (1) is crushed to particle diameter≤5cm particle with SODIUMNITRATE content 6% saliter stone ore ore with jaw crusher; (2) to be loaded into aspect ratio be in 5 the counter-current extraction column for ore that fragmentation is good, flush to ore and extraction column are suitable for reading, after the leaching bittern that contains SODIUMNITRATE 355g/L for preparing is heated to 45 ℃, leaching bittern injects counter-current extraction column from header tank to be ended when liquid level floods mineral surface through the bottom, and leaching bittern residence time in post is 10 hours; After then being heated to 45 ℃ equally by the leaching bittern that contains SODIUMNITRATE 355g/L again, through bottom injecting second stage counter-current extraction column from second stage header tank from header tank through the leaching dope that bottom injection counter-current extraction column stops the front 10 hours is flow to intercepting basin to be preheated to 45 ℃ again by upper isopipe after ends when liquid level floods mineral surface, the injection speed of leaching liquid steadily rises to suitable with liquid level in the post, leaching bittern residence time in the post of the second stage is 10 hours, after step was carried out 4 times altogether according to this, resulting leaching was finished liquid and is contained SODIUMNITRATE 475g/L; (3) leaching that will contain SODIUMNITRATE 475g/L is finished liquid carry out low ternperature separation process in 5 ℃ environment.Earlier liquid being finished in leaching stirred 120 minutes in 5 ℃ environment, carry out solid-liquid separation again, resulting head product butt contains SODIUMNITRATE 92wt%, after saturated sodium nitrate solution carries out filtration washing by the weight ratio of product/sodium nitrate solution 6/1, the products obtained therefrom drying, promptly get the SODIUMNITRATE product, contain SODIUMNITRATE 98wt% butt, the mother liquor after the separation solid phase then enters operation steps (2) after adjusting.
3. a kind of technology as claimed in claim 1 with sodium nitre circulated in countercurrent leaching production SODIUMNITRATE, it is characterized in that, take the circulated in countercurrent leaching technology, specifically may further comprise the steps: (1) is crushed to particle diameter≤5cm particle with SODIUMNITRATE content 6% saliter stone ore ore with jaw crusher; (2) to be loaded into aspect ratio be in 3 the counter-current extraction column for ore that fragmentation is good, flush to ore and extraction column are suitable for reading, after the leaching bittern that contains SODIUMNITRATE 365g/L for preparing is heated to 65 ℃, leaching bittern injects counter-current extraction column from header tank to be ended when liquid level floods mineral surface through the bottom, and leaching bittern residence time in post is 8 hours; After then being heated to 65 ℃ equally by the leaching bittern that contains SODIUMNITRATE 365g/L again, through bottom injecting second stage counter-current extraction column from second stage header tank from header tank through the leaching dope that bottom injection counter-current extraction column stops the front 8 hours is flow to intercepting basin to be preheated to 65 ℃ again by upper isopipe after ends when liquid level floods mineral surface, the injection speed of leaching liquid steadily rises to suitable with liquid level in the post, leaching bittern residence time in the post of the second stage is 8 hours, after step was carried out 3 times altogether according to this, resulting leaching was finished liquid and is contained SODIUMNITRATE 480g/L; (3) leaching that will contain SODIUMNITRATE 480g/L is finished liquid carry out low ternperature separation process in 10 ℃ environment.Earlier liquid being finished in leaching stirred 120 minutes in 5 ℃ environment, carry out solid-liquid separation again, resulting head product contains SODIUMNITRATE butt 93wt%, filter by the weight ratio of product/sodium nitrate solution 5/1 through saturated sodium nitrate solution, the products obtained therefrom drying, promptly get the SODIUMNITRATE product, contain SODIUMNITRATE 98wt% butt, the mother liquor after the separation solid phase then enters operation steps (2) after adjusting.
4. a kind of technology with sodium nitre circulated in countercurrent leaching production SODIUMNITRATE as claimed in claim 1 is characterized in that extraction column aspect ratio scope is preferably 1～5, preferred 3～4.
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| CN200610150661A CN100595149C (en) | 2006-10-23 | 2006-10-23 | Technique for producing sodium nitrate by chilisaltpeter adverse current circulation leaching |
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| CN200610150661A CN100595149C (en) | 2006-10-23 | 2006-10-23 | Technique for producing sodium nitrate by chilisaltpeter adverse current circulation leaching |
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| CN100595149C CN100595149C (en) | 2010-03-24 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259897A (en) * | 2010-05-31 | 2011-11-30 | 中国中轻国际工程有限公司 | Continuous leaching process of nitratine |
| CN102408118A (en) * | 2011-08-08 | 2012-04-11 | 新疆安华矿业投资有限公司 | Process for producing high-concentration sodium nitrate brine by virtue of counterflow, rotary and dynamic leaching of nitratine ore |
| CN102557083A (en) * | 2012-01-05 | 2012-07-11 | 中国中轻国际工程有限公司 | Process for countercurrent leaching in leaching chamber |
| CN102910651A (en) * | 2012-11-19 | 2013-02-06 | 冯耀礼 | Counterflow circulation washing extraction method by using nitratine |
| CN103523803A (en) * | 2013-10-09 | 2014-01-22 | �隆平 | Method of preparing sodium nitrate bittern by utilization of dewatering screens |
| CN104975174A (en) * | 2014-12-15 | 2015-10-14 | 新疆硝石钾肥有限公司 | Ore continuous circulation spraying fast leaching method and device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU715470A1 (en) * | 1978-03-07 | 1980-02-15 | Предприятие П/Я А-3732 | Method of separate preparation of sodium and potassium nitrates |
-
2006
- 2006-10-23 CN CN200610150661A patent/CN100595149C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259897A (en) * | 2010-05-31 | 2011-11-30 | 中国中轻国际工程有限公司 | Continuous leaching process of nitratine |
| CN102408118A (en) * | 2011-08-08 | 2012-04-11 | 新疆安华矿业投资有限公司 | Process for producing high-concentration sodium nitrate brine by virtue of counterflow, rotary and dynamic leaching of nitratine ore |
| CN102557083A (en) * | 2012-01-05 | 2012-07-11 | 中国中轻国际工程有限公司 | Process for countercurrent leaching in leaching chamber |
| CN102910651A (en) * | 2012-11-19 | 2013-02-06 | 冯耀礼 | Counterflow circulation washing extraction method by using nitratine |
| CN103523803A (en) * | 2013-10-09 | 2014-01-22 | �隆平 | Method of preparing sodium nitrate bittern by utilization of dewatering screens |
| CN104975174A (en) * | 2014-12-15 | 2015-10-14 | 新疆硝石钾肥有限公司 | Ore continuous circulation spraying fast leaching method and device |
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| CN100595149C (en) | 2010-03-24 |
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