CN100503440C - Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype - Google Patents
Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype Download PDFInfo
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- CN100503440C CN100503440C CN 200710017628 CN200710017628A CN100503440C CN 100503440 C CN100503440 C CN 100503440C CN 200710017628 CN200710017628 CN 200710017628 CN 200710017628 A CN200710017628 A CN 200710017628A CN 100503440 C CN100503440 C CN 100503440C
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Abstract
The present invention provides process of preparing potassium sulfate with potassium containing subtype magnesium sulfate bittern. The process includes naturally evaporating potassium containing subtype magnesium sulfate bittern from salt lake to crystallize and separate out potassium containing sulfate and sulfate radical containing carnallite successively; grinding the potassium containing sulfate, decomposing to convert and floating to obtain picromerite; decomposing sulfate radical containing carnallite to convert and floating to obtain coarse potassium chloride; mixing picromerite, coarse potassium chloride and potassium sulfate mother liquid to obtain slurry, washing, filtering, decomposing to convert and filtering separation to obtain potassium sulfate. The present invention has low production cost, high yield and high product quality.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of flotation separation and the isolating interleaving techniques of inorganic salt phase chemistry, be specifically related to that a kind of to combine, contain potassium bittern with magnesium sulfate with flotation partition method and inorganic salt phase chemistry technology be the method that raw material is produced vitriolate of tartar.
Background technology
Potash fertilizer is non-renewable scarce resource, and potash fertilizer also is one of main fertilizer of agriculture production, particularly has the effect of strong stem stalk for stem stalk class crop, in case lack appearance lodging, the underproduction; Potash fertilizer also is one of three big raw materials of production composite fertilizer, and the potash fertilizer price is very big to the influence of fertilizer price, and the potash fertilizer security relationship further is related to national food safety to chemical fertilizer safety.China's potassium resource is limited, and wherein magnesium sulfate contains that the potassium resource reserves account for 60% of China's bittern potassium resource total reserves in the potassium bittern, has great value of exploiting and utilizing.But, because magnesium sulfate contains potassium bittern system salt pan mineralogical composition that solar evaporation is separated out and is subjected to regional Temperature Influence bigger, the magnesium sulfate of different areas contains potassium bittern and analyses the phase chemistry relation that has in the salt process than complicated in the salt pan evaporation, the composition of the mineral of separating out changes greatly, determine that thus the elasticity of its processing technology is bigger, magnesium sulfate is contained the degree that potassium bittern develops thereby limited China.
Utilize the existing a lot of reports of method of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype, Chinese patent 02143641.X (applicant: Luobubo K Salt Tech Development Co Ltd, Xinjiang; Changsha Design ﹠ Research Inst., Ministry of Chemical Industry) discloses a kind of usefulness and contained the method that potassium magnesium sulfate bittern is produced vitriolate of tartar: earlier former halogen has been imported the evaporation of sodium-chlor pond and remove sodium, when bittern is evaporated in the sodium pond vitriol when saturated vitriol saturated bittern and the old bittern of saturated magnesium chloride are mixed different substances together by a certain percentage, bittern after mixing different substances together imports the epsom salt pond and evaporates, separate out salts such as epsom salt, sylvite magnesium vanadium, carnallitite then successively, utilize technological processs such as sylvite magnesium navajoite ore grinding, decomposition and inversion, flotation to obtain the soft potassium magnesium of higher-grade vanadium; Utilize carnallite, C point bittern, soft potassium magnesium vanadium decomposed solution decomposition and inversion carnallitite, carnallitite decomposition and inversion slip obtains rough Repone K through flotation, and rough Repone K carries out twice transformation with soft potassium magnesium vanadium and obtains vitriolate of tartar behind potassium sulfate mother liquid washing dehalogenation.The complex process of this scheme, flow process be long, to convert the halogen energy consumption in a large number also higher because of need.
Summary of the invention
Purpose of the present invention is in order to overcome the defective that exists in the prior art, provides that a kind of technology is fairly simple, flow process is short, energy consumption is lower, and containing potassium bittern with magnesium sulfate is the method that raw material is produced vitriolate of tartar.
Purpose of the present invention realizes by following measure:
The present invention contains the method that potassium bittern is the raw material production vitriolate of tartar with magnesium sulfate, comprises following processing step:
1. utilize salt pan solar evaporation technology to obtain successively based on the sulfuric acid salt mine that contains potassium vitriol with based on the carnallite of the sulfur-bearing hydrochlorate of carnallitite;
2. with described sulfuric acid salt mine process ore grinding, decomposition and inversion, flotation, flotation concentrate separates through dense thickening after-filtration, makes soft potassium magnesium vanadium;
3. with carnallite process decomposition and inversion, the flotation of sulfur-bearing hydrochlorate, flotation concentrate makes rough Repone K through dense thickening after-filtration;
4. with soft potassium magnesium vanadium, rough Repone K potassium sulfate mother liquid pulp washing, filtration, decomposition and inversion, filtering separation, filter cake is wet vitriolate of tartar.
Step 2. in, the Grinding procedure of described sulfuric acid salt mine be will contain potassium sulfuric acid salt mine and water with the weight ratio batching of 1:0.2～1:1.0, and in grinding machine ore grinding, grinding particle size is 80～100 orders; Described decomposition and inversion operation is that ore grinding is finished slip in the decomposition and inversion groove, and decomposition and inversion is 0.5～4.0 hour under 8～30 ℃ of temperature; Described flotation is decomposition and inversion to be finished slip send into the flotation machine flotation; Flotation institute with medicament is a fat polyamine, and its consumption is 0.005～0.015% of a slip.
Step 3. in, the decomposition and inversion operation of described carnallite is with carnallite and the water weight ratio batching with 1:0.3～1:1.0, reacts 0.5～4.0 hour under 8～30 ℃ of temperature; Described flotation institute with medicament is an aliphatic amide, and its consumption is 0.0005～0.0015% of a slip.
Step 4. in, with soft potassium magnesium vanadium, rough Repone K and the potassium sulfate mother liquid weight ratio pulp washing with 1:1:1～1:1.5:6, temperature of reaction is 8～30 ℃, washing is 0.2～2.0 hour the adjustment time; Described decomposition and inversion is that mixture behind the pulp washing and water are prepared burden with the weight ratio of 1:1～1:2, and 0.2～2.0 hour 20～80 ℃ of following reaction times of temperature.
Step 4. in, the filtering filtrate of pulp washing can be turned back to carnallite decomposition and inversion operation and prepare burden: carnallite and water and pulp washing filtrate with the weight ratio batching of 1:0.3:0.3～1:1:1, were reacted 0.5～4.0 hour under 8～30 ℃ of temperature; Described flotation institute with medicament is an aliphatic amide, and its consumption is 0.005～0.015% of a slip.
Step 4. in, decomposition and inversion slurry filtration separated filtrate can be turned back to soft potassium magnesium vanadium, rough Repone K pulp washing operation batching.
The present invention compared with prior art has the following advantages:
1, the cost of the vitriolate of tartar of the present invention's preparation is low, yield is high, the product grade height: the present invention directly utilizes magnesium sulfate to contain the evaporative crystallization salting out law of sylvite lake bittern water nature, separate out the carnallitite of potassic vitriol and sulfur-bearing acid group successively salt Tanaka, utilize potassic vitriol to obtain soft potassium magnesium vanadium then through ore grinding, decomposition and inversion, flotation; Utilize the carnallitite of sulfur-bearing acid group to get rough Repone K through decomposition and inversion, flotation; Again with soft potassium magnesium vanadium and rough Repone K potassium sulfate mother liquid pulp washing, filtration, decomposition and inversion, filtering separation and get.Because the rough Repone K that technology of the present invention obtains improves 5～10% than the grade of utilizing carnallite, C point bittern, soft potassium magnesium vanadium decomposed solution decomposition and inversion, flotation to obtain rough Repone K in the prior art, resulting vitriolate of tartar yield has improved 5～10%, and the grade that decomposition and inversion is filtered the wet vitriolate of tartar that directly obtains has improved 2-5%; Because the treatment capacity of this operation slip reduces by 10～20%, cause the working efficiency of equipment to improve 10～20% simultaneously, effectively reduce production cost, reduced energy consumption.
2, technological process of the present invention is mated mutually because of need not more material, and technological process is simple relatively, and is easy to operate; Technical process is short, stable, easy to control, the production efficiency height; The investment of founding the factory will be reduced about 5～10% relatively.
Description of drawings
Fig. 1 produces the process flow sheet of vitriolate of tartar for the present invention
Embodiment
1. will contain the former halogen of potassium magnesium sulfate earlier squeezes into the sodium-chlor salt pan and separates out most of sodium-chlor through solar evaporation, treat bittern evaporation to beginning to separate out when containing potassium vitriol, pour bittern into one section sulfuric acid salt pond and continue evaporation and separate out one section and contain potassium vitriol vitriol is saturated; Treat that one section vitriol precipitate into to a certain degree (determining according to the calphad result), pour this bittern into two sections sulfuric acid salt ponds and continue to separate out two sections and contain potassium vitriol must to contain potassium vitriol be main sulfuric acid salt mine.When two sections sulfate brines are evaporated to carnallitite when saturated, pour bittern into one section carnallitite evaporation tank evaporation, when the carnallitite amount of separating out in the carnallitite pond reaches 80% left and right sides of calculated amount, pour this bittern into two sections carnallitite ponds and continue evaporation, till magnesium chloride in two sections carnallitite ponds is saturated, again the magnesium chloride saturated bittern is poured into the magnesium chloride pond and shone the system bischofite.
2. with two sections ratio batchings that contain potassium sulfuric acid salt mine and water in 1:0.2～1:1.0, and in grinding machine ore grinding (grinding particle size is 80～100 orders; Slip entered in the decomposition and inversion groove after ore grinding was finished, and decomposition and inversion is 0.5～4.0 hour under 8～30 ℃ of temperature; Slip entered the flotation machine flotation (flotation institute with medicament is a fat polyamine after conversion was finished, its consumption is the 0.005-0.015% of slip), flotation concentrate separates after dense thickening, filter cake is soft potassium magnesium vanadium---and standby as the intermediate raw material of producing vitriolate of tartar, filtrate and mine tailing enter tailing treating ponds together and handle.
3. one section carnallite and water are prepared burden with the weight ratio of 1:0.3～1:1.0, under 8～30 ℃ of temperature, react and carried out decomposition and inversion in 0.5～4.0 hour, conversion is finished slip and is entered flotation machine and carry out flotation, flotation concentrate is through dense thickening after-filtration, filter cake is rough Repone K---and standby as the intermediate raw material of producing vitriolate of tartar, filtrate and flotation tailings are squeezed into soft potassium magnesium vanadium mine tailing storage pond and are together handled.
4. soft potassium magnesium vanadium and rough Repone K carry out pulp washing with potassium sulfate mother liquid in steel basin, soft potassium magnesium vanadium, rough Repone K, potassium sulfate mother liquid (can dispose in advance when just beginning potassium sulfate mother liquid as start with) pulp washing ratio of components is 1:1:1～1:1.5:6, the pulp washing temperature is 8～30 ℃, and the time is 0.2～2.0 hour; Pulp washing is finished slurry filtration and is separated, and filtrate is got back to carnallitite decomposition and inversion operation batching, and filter cake is low sodium soft potassium magnesium vanadium and rough potassium chloride mixture; Filter cake and water are prepared burden with the ratio of 1:1～1:2, and under 20～80 ℃ temperature, react and carried out twice transformation in 0.2～2.0 hour, conversion is finished slurry filtration and is separated, filter cake is wet vitriolate of tartar, the drying packing is potassium product, and filtrate is got back to soft potassium magnesium vanadium, the operation batching is adjusted in the washing of rough Repone K.
Claims (8)
1, a kind ofly contain the method that potassium bittern is the raw material production vitriolate of tartar, comprise following processing step with magnesium sulfate:
1. the evaporative crystallization salting out law that utilizes magnesium sulfate to contain potassium bittern nature obtains successively based on the sulfuric acid salt mine that contains potassium vitriol with based on the carnallite of the sulfur-bearing hydrochlorate of carnallitite;
2. with described sulfuric acid salt mine process ore grinding, decomposition and inversion, flotation, flotation concentrate separates through dense thickening after-filtration, makes soft potassium magnesium vanadium;
3. with carnallite process decomposition and inversion, the flotation of sulfur-bearing hydrochlorate, flotation concentrate makes rough Repone K through dense thickening after-filtration;
4. with soft potassium magnesium vanadium, rough Repone K potassium sulfate mother liquid pulp washing, filtration, decomposition and inversion, filtering separation, filter cake is wet vitriolate of tartar.
2, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 2. in, the Grinding procedure of described sulfuric acid salt mine is with described sulfuric acid salt mine and the water weight ratio batching with 1:0.2～1:1.0, and in grinding machine ore grinding, grinding particle size is 80～100 orders; Described decomposition and inversion operation is that ore grinding is finished slip in the decomposition and inversion groove, and decomposition and inversion is 0.5～4.0 hour under 8～30 ℃ of temperature; Described flotation is decomposition and inversion to be finished slip send into the flotation machine flotation; Flotation institute with medicament is a fat polyamine, and its consumption is 0.005～0.015% of a slip.
3, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 3. in, the decomposition and inversion operation of described carnallite is with carnallite and the water weight ratio batching with 1:0.3～1:1.0, reacts 0.5～4.0 hour under 8～30 ℃ of temperature; Described flotation institute with medicament is an aliphatic amide, and its consumption is 0.005～0.015% of a slip.
4, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 3. in, the decomposition and inversion operation of described carnallite be with carnallite and water and step 4. the pulp washing filtrate of potassium sulfate mother liquid reacted 0.5～4.0 hour under 8～30 ℃ of temperature with the weight ratio batching of 1:0.3:0.3～1:1:1; Described flotation institute with medicament is an aliphatic amide, and its consumption is 0.005～0.015% of a slip.
5, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 4. in, with soft potassium magnesium vanadium, rough Repone K and the potassium sulfate mother liquid weight ratio pulp washing with 1:1:1～1:1.5:6, temperature of reaction is 8～30 ℃, and the pulp washing time is 0.2～2.0 hour.
6, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 4. in, described decomposition and inversion is with the mixture behind the pulp washing and the water weight ratio batching with 1:1～1:1.3, and 0.2～2.0 hour 20～80 ℃ of following reaction times of temperature.
7, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 4. in, the filtering filtrate of pulp washing is turned back to carnallite decomposition and inversion operation and prepares burden.
8, produce the method for vitriolate of tartar according to claim 1, it is characterized in that: step 4. in, decomposition and inversion slurry filtration separated filtrate is turned back to soft potassium magnesium vanadium, rough Repone K pulp washing operation batching.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710017628 CN100503440C (en) | 2007-03-30 | 2007-03-30 | Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype |
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| CN 200710017628 CN100503440C (en) | 2007-03-30 | 2007-03-30 | Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype |
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| CN101066770A CN101066770A (en) | 2007-11-07 |
| CN100503440C true CN100503440C (en) | 2009-06-24 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102476075B (en) * | 2010-11-22 | 2014-03-19 | 何建庭 | Combined organic sodium sulfonate salt flotation agent |
| CN102653407B (en) * | 2012-05-03 | 2014-06-04 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride from sulfate type salt lake brine |
| KR101527140B1 (en) * | 2012-12-24 | 2015-06-10 | 주식회사 포스코 | Method for extraction of potassium from brine |
| CN104016379B (en) * | 2014-06-05 | 2016-07-06 | 中国科学院青海盐湖研究所 | A kind of preparation method of potassium sulfate |
| CN104529563A (en) * | 2014-11-20 | 2015-04-22 | 国投新疆罗布泊钾盐有限责任公司 | Method used for preparing potassium sulfate fertilizer from carnallite |
| CN105692657B (en) * | 2016-04-14 | 2017-07-28 | 化工部长沙设计研究院 | A kind of method of use low-sulfur potassium than bittern preparing potassium sulfate |
| CN106083221A (en) * | 2016-06-15 | 2016-11-09 | 古舜起 | Carnallite is utilized to produce the method for potassium sulphate fertilizer magnesium metal PVC and liquid chlorine hydrochloric acid |
| CN113247920A (en) * | 2021-05-24 | 2021-08-13 | 青海联宇钾肥有限公司 | Method for co-producing potash magnesium sulphate fertilizer, potassium chloride and potassium sulphate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439602A (en) * | 2002-09-25 | 2003-09-03 | 新疆罗布泊钾盐科技开发有限责任公司 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
| US6986878B2 (en) * | 2001-12-19 | 2006-01-17 | Dirdal Rand Technologies | Method of producing potassium sulfate via cation exchange |
| CN1789129A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Method for extracting potassium sulphate by magnesium sulfate sub-type potassium-containing salt lake brine water |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6986878B2 (en) * | 2001-12-19 | 2006-01-17 | Dirdal Rand Technologies | Method of producing potassium sulfate via cation exchange |
| CN1439602A (en) * | 2002-09-25 | 2003-09-03 | 新疆罗布泊钾盐科技开发有限责任公司 | Preparation of potassium sulfate from brine containing potassium magnesium sulfate |
| CN1789129A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Method for extracting potassium sulphate by magnesium sulfate sub-type potassium-containing salt lake brine water |
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