CN103073029B - Method for processing and producing potassium chloride by using magnesium sulfate subtype or sulfate chloride transitional-type potassium-containing salt lake brine - Google Patents
Method for processing and producing potassium chloride by using magnesium sulfate subtype or sulfate chloride transitional-type potassium-containing salt lake brine Download PDFInfo
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- CN103073029B CN103073029B CN201310046820.XA CN201310046820A CN103073029B CN 103073029 B CN103073029 B CN 103073029B CN 201310046820 A CN201310046820 A CN 201310046820A CN 103073029 B CN103073029 B CN 103073029B
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- bittern
- sylvite
- potassium
- carnallitite
- chloride
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Abstract
The invention relates to a method for processing and producing potassium chloride by using magnesium sulfate subtype or sulfate chloride transitional-type potassium-containing salt lake brine. According to the method, the potassium-containing salt lake brine as a raw material contains Na, K, Mg, Cl, SO4 ions, wherein the weight ratio of SO4 to K is (0.5-3.5): 1. The method disclosed by the invention comprises the following steps of: introducing a modifying agent to a halite stage in a brine evaporation process, wherein the weight ratio of SO4 to K in the modified brine is (2.0-0.1): 1; continuously evaporating the modified brine by insolation to obtain sylvine and carnallite; and carrying out potassium chloride flotation on the sylvine and carnallite mixture, and washing and drying flotation concentrate to obtain a potassium chloride product. The method disclosed by the invention solves the problem of processing and producing the potassium chloride by using the potassium mixed salt obtained by the insolation of the magnesium sulfate subtype or transitional-type potassium-containing salt lake brine, is used for processing and producing the potassium chloride from the sylvine and carnallite obtained by using the modified brine and is good in product quality and high in sylvine yield.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to inorganic salt phase chemistry isolation technique, be specifically related to a kind of magnesium sulfate contains sylvite lake bittern water processing high-quality Repone K method containing sylvite lake bittern water or vitriol muriate transition type.
Background technology
Repone K is a kind of important industrial chemicals, industrially has purposes widely; Be again one of large fertilizer of the necessary N P and K three of crop growth, more important to the effect of agriculture production, China is as a large agricultural country, and the market demand of potash fertilizer is very large simultaneously.China is again the country of a potassium resource famine, verified that potassium resource reserves account for world's potassium resource total amount 2%, solubility salt lake potassium resource is the main source that China produces sylvite product, be distributed in the ground such as Qinghai, Xinjiang, Tibet, the Inner Mongol, the distributional region condition of salt lake potassium resource, the difference of Resource environmental condition and weather condition etc., determine the difference of the development technique route of salt lake potassium resource, magnesium sulfate and muriate transition type are one of important sources producing Repone K containing sylvite lake bittern water.
The difference that magnesium sulfate and muriate transition type form because of it containing sylvite lake bittern water, its bittern composition point is at Na, K, Mg//Cl, SO
4-H
2phase region residing on O quinary system metastable phase diagram is different, general salt lake brine many places are in white sodium magnesium vanadium phase region, Shoenite phase region, epsom salt phase region or sylvite phase region, sylvite lake bittern water is contained to the part of sulfuric acid magnesium hypotype or transition type that are in Shoenite phase region, epsom salt phase region or sylvite phase region, its potassium mixed salt intermediates obtained through salt pan evaporative crystallization are directly used in production potassium sulfate, its sulfate radical is not enough, for the production of Repone K, then its vitriol is too high, gained Potassium Chloride Product is second-rate, and potassium yield is lower.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, there is provided a kind of technological design more reasonable, produce the method containing sylvite lake bittern water processing Repone K by magnesium sulfate or vitriol muriate transition type that the Potassium Chloride Product quality obtained is good, sylvite yield is high.
Technical problem to be solved by this invention is realized by following technical scheme.The present invention is a kind of method that magnesium sulfate or vitriol muriate transition type contain sylvite lake bittern water processing Repone K, and be characterized in, its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 0.5 ~ 3.5:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 0% ~ 85%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 2.0 ~ 0.1:1, (SO in bittern after crystal gypsum and halite are separated out
4 2-ion is with CaSO
42H
2o form is separated out in advance), be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is the evaporated waste ammonia liquid in soda manufacture process, or the concentrated solution of evaporated waste ammonia liquid, or other is containing calcium solution;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:0.5 ~ 2.0; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
Above-described the present invention produces in the method for Repone K:
1. in step (1): described other contains calcium solution preferably from calcium chloride solution or milk of lime.
2. in step (1): preferably introduce properties-correcting agent when precipitated sodium chloride 50% ~ 85%.
3. in step (1): properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 1.5 ~ 0.5:1.
Compared with prior art, the inventive method carries out modification by introducing properties-correcting agent to magnesium sulfate salt lake brine, adjustment bittern forms, control vitriol segmentation to separate out, make it in the solar evaporation crystallisation process of salt pan, obtain high-quality sylvite and carnallitite, so that processing high-quality potassium chloride product.Thus solve magnesium sulfate or the transition type difficult problem containing the processing Repone K of the potassium mixed salt of sylvite lake bittern water Exposure to Sunlight gained.The sylvite obtained with modified making from brine again and carnallitite processing Repone K, good product quality, sylvite yield is high.
Accompanying drawing explanation
Fig. 1 is a kind of process flow diagram of the present invention.
Embodiment
Referring to accompanying drawing, further describe concrete technical scheme of the present utility model, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, with reference to Fig. 1, a kind of magnesium sulfate or vitriol muriate transition type contain the method for sylvite lake bittern water processing Repone K, and its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 0.5:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 0%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 0.1:1, after crystal gypsum and halite are separated out, be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is the evaporated waste ammonia liquid in soda manufacture process;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:0.5; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
Embodiment 2, with reference to Fig. 1, a kind of magnesium sulfate or vitriol muriate transition type contain the method for sylvite lake bittern water processing Repone K, and its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 3.5:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 85%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 2.0:1, after crystal gypsum and halite are separated out, be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is the evaporated waste ammonia liquid in soda manufacture process, or the concentrated solution of evaporated waste ammonia liquid, or other is containing calcium solution;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:2.0; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
Embodiment 3, with reference to Fig. 1, a kind of magnesium sulfate or vitriol muriate transition type contain the method for sylvite lake bittern water processing Repone K, and its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 2.0:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 50%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 1.5:1, after crystal gypsum and halite are separated out, be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is the evaporated waste ammonia liquid in soda manufacture process, or the concentrated solution of evaporated waste ammonia liquid, or other is containing calcium solution;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:1; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
Embodiment 4, with reference to Fig. 1, a kind of magnesium sulfate or vitriol muriate transition type contain the method for sylvite lake bittern water processing Repone K, and its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 1.5:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 70%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 0.5:1, after crystal gypsum and halite are separated out, be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is calcium chloride solution or milk of lime;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:1.1; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
Embodiment 5, contains the experiment one of sylvite lake bittern water processing Repone K by magnesium sulfate or vitriol muriate transition type:
Certain magnesium sulfate salt lake brine is containing Na
+7.06%, K
+0.67%, Mg
2+1.41%, Cl
-14.98%, SO
4 2-1.68%, its SO
4 2-: K
+(weight ratio) is 2.51:1, and this bittern is after the sodium-chlor that evaporative crystallization separates out 85%, and add evaporated waste ammonia liquid clear liquor, control section vitriol and sodium-chlor are separated out jointly, regulates bittern composition, Na
+2.39%, K
+2.26%, Mg
2+5.01%, Cl
-18.41%, SO
4 2-2.26%, its SO
4 2-: K
+ratio is 1.00:1, bittern evaporation crystallization, obtains sylvite (composition NaCl 58.36%, KCl 26.65%, MgCl respectively
23.39%, MgSO
40.72%) and carnallitite (composition NaCl 9.46%, KCl14.30%, MgCl
228.53%, MgSO
45.73%); Normal temperature decomposes carnallitite, mixes with sylvite slip in 1:1 ratio, flotation Repone K, and flotation concentrate must Potassium Chloride Product through washing, after drying, KCl content 96.23%.
Embodiment 6, contains the experiment two of sylvite lake bittern water processing Repone K by magnesium sulfate or vitriol muriate transition type:
Certain salt lake brine is containing Na
+6.82%, K
+0.77%, Mg
2+1.73%, Cl
-15.90%, SO
4 2 -0.76%, its SO
4 2-: K
+(weight ratio) is 0.99:1, and bittern is after the sodium-chlor that evaporative crystallization separates out 70%, and add evaporated waste ammonia liquid clear liquor, control section vitriol and sodium-chlor are separated out jointly, regulates bittern composition, Na
+3.58%, K
+1.60%, Mg
2+3.50%, Cl
-17.58%, SO
4 2-0.18%, its SO
4 2-: K
+ratio is 0.11:1, and after bittern evaporation crystallization part halite, crystallization obtains sylvite (composition NaCl 45.73%, KCl 35.20%, MgCl respectively
25.33%) and carnallitite (composition NaCl 12.33%, KCl16.74%, MgCl
230.33%), normal temperature decomposes carnallitite, mixes with sylvite slip in 1:1.2 ratio, flotation Repone K, and flotation concentrate must Potassium Chloride Product through washing, after drying, KCl content 96.92%.
Claims (2)
1. contain a method for sylvite lake bittern water processing Repone K by magnesium sulfate or vitriol muriate transition type, it is characterized in that, its concrete steps are as follows:
(1) raw material sulphuric acid magnesium hypotype contains Na containing sylvite lake bittern water or vitriol muriate transition type containing in sylvite lake bittern water
+, K
+, Mg
2+, Cl
-, SO
4 2-ion, and wherein SO
4 2-with K
+weight ratio be 2.0:1; Introduce properties-correcting agent in the halite stage of this bittern evaporation process, namely introduce properties-correcting agent when its precipitated sodium chloride 50%, make SO in bittern
4 2-ion is separated out in advance; Properties-correcting agent add-on is to control modified bittern SO
4 2-: K
+weight ratio at 1.5:1, after crystal gypsum and halite are separated out, be separated to obtain modified bittern, modified bittern continues solar evaporation in salt pan, obtains sylvite and carnallitite respectively; Described properties-correcting agent is the evaporated waste ammonia liquid in soda manufacture process, or the concentrated solution of evaporated waste ammonia liquid, or other is containing calcium solution;
(2) hydrolyzable carnallitite under normal temperature condition, prepares sylvite slip with carnallite decomposition liquid, and mixes with carnallitite decomposing materials, and the weight ratio of sylvite and carnallitite is 1:1; Flotation Repone K, flotation concentrate obtains Potassium Chloride Product after washing, drying.
2. the method for production Repone K according to claim 1, is characterized in that, in step (1): described other is calcium chloride solution containing calcium solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310046820.XA CN103073029B (en) | 2013-02-06 | 2013-02-06 | Method for processing and producing potassium chloride by using magnesium sulfate subtype or sulfate chloride transitional-type potassium-containing salt lake brine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310046820.XA CN103073029B (en) | 2013-02-06 | 2013-02-06 | Method for processing and producing potassium chloride by using magnesium sulfate subtype or sulfate chloride transitional-type potassium-containing salt lake brine |
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| Publication Number | Publication Date |
|---|---|
| CN103073029A CN103073029A (en) | 2013-05-01 |
| CN103073029B true CN103073029B (en) | 2015-04-22 |
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| CN103991884B (en) * | 2014-05-27 | 2016-01-20 | 中国科学院青海盐湖研究所 | From low-grade vitriol hypotype containing the method preparing Repone K potassium mine tailing |
| CN111392746B (en) * | 2020-03-30 | 2021-10-08 | 中国科学院过程工程研究所 | Resourceful treatment system and method for mixed salt solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335260A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Halogenation process of preparing KCl |
| CN1886338A (en) * | 2003-12-31 | 2006-12-27 | 科学与工业研究委员会 | Simultaneous recovery of potassium chloride and KC1 enriched edible salt |
| CN101857467A (en) * | 2010-05-20 | 2010-10-13 | 广东南方碱业股份有限公司 | Process method for preparing potassic fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar |
| CN102583446A (en) * | 2012-02-13 | 2012-07-18 | 河北工业大学 | Method for preparing potassium chloride through decomposing carnallite by concentrated brine |
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2013
- 2013-02-06 CN CN201310046820.XA patent/CN103073029B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335260A (en) * | 2001-09-07 | 2002-02-13 | 中信国安锂业科技有限责任公司 | Halogenation process of preparing KCl |
| CN1886338A (en) * | 2003-12-31 | 2006-12-27 | 科学与工业研究委员会 | Simultaneous recovery of potassium chloride and KC1 enriched edible salt |
| CN101857467A (en) * | 2010-05-20 | 2010-10-13 | 广东南方碱业股份有限公司 | Process method for preparing potassic fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar |
| CN102583446A (en) * | 2012-02-13 | 2012-07-18 | 河北工业大学 | Method for preparing potassium chloride through decomposing carnallite by concentrated brine |
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