CN102951659B - The method preparing refined brine and side-product thereof - Google Patents
The method preparing refined brine and side-product thereof Download PDFInfo
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- CN102951659B CN102951659B CN201210517699.XA CN201210517699A CN102951659B CN 102951659 B CN102951659 B CN 102951659B CN 201210517699 A CN201210517699 A CN 201210517699A CN 102951659 B CN102951659 B CN 102951659B
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- brine
- salt
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Abstract
The method that the present invention relates to prepare refined brine and side-product thereof；Use three refined, secondary salt, the processes of a step denitration, comprise the steps: to add crude salt in salt dissolving tank, being simultaneously introduced a certain amount ofization salt water dissolution crude salt carrying out salt, recycling reactor, settling tank carry out that three times refined, secondary salt, a step denitration prepare refined brine.Engineering earth dispensing can be prepared by three mud of washing and a mud.Light calcium carbonate product is prepared by washing secondary mud.
Description
Technical field
The present invention relates to a kind of method preparing refined brine, a kind of method preparing refined brine and side-product thereof.
Background technology
Refined brine is needed raw material during ammonia-soda process soda manufacture, prepares refined brine and need to be dissolved by crude salt and remove Ca therein
2+
、Mg
2+
、SO
4
2-
.Dissolve crude salt, can preferentially to utilize rich in NaCl composition in concentrated seawater with fresh water or concentrated seawater.The currentization salt refining commonly used one-step method of refined brine technique, two step method salt refining technique, but all can affect NaCl concentration in refined brine to some extent.Especially Ca in concentrated seawater
2+
、Mg
2+
、SO
4
2-
NaCl concentration impact in refined brine, apparently higher than fresh water, is become apparent from when using one-step method, two step method refinedization salt to prepare refined brine by content.
Summary of the invention
The purpose of the present invention aims to solve the problem that the problem that background technology exists, and provide a kind of use that three times refined, secondary salt, the method for refined brine of a step denitration；During this refined brine and side-product can be produced.
The technical scheme realizing foregoing invention purpose is:
1, a kind of method preparing refined brine, comprises the steps:
A, in salt dissolving tank I add crude salt, being simultaneously introduced salt water dissolution crude salt, make a crude brine；
B, crude brine is sent in reactor I, in reactor I, add lime cream simultaneously, then enter settling tank I；
The Mg (OH) that c, settling tank I are isolated in reactant liquor after being sufficiently stirred for reaction
2
And CaSO
4-
And form a mud, one time mud is sent in mud cleaning bucket I, is sent to brine sludge filter pressing operation after changing saline washing, washed once the light salt brine of mud formation for once changing saline；
Supernatant liquid 4～8% (percent by volume) after the clarification of clarified bucket I return settling tank I, and remaining enters reactor II as primary brine；Complete primary purification and complete denitration；
D, heat alkali liquid and lime cream are sent into causticization settling tank in react, clarified bottom generates CaCO
3
Mud, Na is formed at top
2
CO
3
Solution；
E, top Na
2
CO
3
Solution enters and fully reacts the Ca removed in primary brine in reactor II
2+
, then utilize settling tank II to isolate the CaCO in reactant liquor
3
And form secondary mud and secondary brine, complete secondary refining；Wherein in secondary mud 55～65% (percent by volume) Returning reactor II do crystal seed use；
F, secondary brine deliver to salt dissolving tank II, add crude salt in salt dissolving tank II, utilize secondary brine to dissolve crude salt, send in reactor III, complete second timeization salt after making secondary crude brine；
G, in the ratio of 1:2～3, lime cream and soda liquid are sent into causticizing tank in react, and with the CaCO from causticization settling tank
3
Mud mixes, and the causticization liquid of formation is sent in reactor III；
H, reactor III remove the Mg in secondary crude brine
2+
、Ca
2+
、SO
4
2-
, then inject settling tank III；
I, settling tank III are carried out be sufficiently stirred for reaction, isolate the Mg (OH) in reactant liquor
2
、CaCO
3
And forming three mud, 2～5% (percent by volume) in the supernatant returns settling tank III, and remainder goes to inhale ammonia operation and carbonation process prepares qualified refined brine；Complete three times to refine.
A kind of method preparing light calcium carbonate product, will in step e obtain secondary mud in 35～45% part to prepare light calcium carbonate product after concentrated seawater, multiplexing water counter current washes.
A kind of engineering earth dispensing preparation method, after being mixed with a mud in step c by three mud isolated in step i, utilize concentrated seawater, wash with water again after carry out filter pressing and obtain.
Compared with prior art, refining effect is good for the present invention, and refined brine concentration is high, can produce side-product, do not produce process waste while preparing refined brine.
The preferred version of the method preparing refined brine is:
Change saline in step a be secondary mud is washed by concentrated seawater or fresh water or step e wash after use water.
The concentration of the crude brine made in step a is 90～108Ti.
In step d, in heat alkali liquid, ratio with lime cream percent by volume is 10～15:1.
In described step d heat alkali liquid, the ratio with lime cream percent by volume is 10:1.
In described step f, the concentration of secondary crude brine is 106～108Ti.
3% return settling tank III in described step i clear liquid at the middle and upper levels.
Described step h adds in reactor III Mg that settling agent is sufficiently stirred in reaction removing secondary crude brine
2+
、Ca
2+
、SO
4
2-
, then inject settling tank III.
The settling agent added in described reactor III is the secondary mud in step e.
Add settling agent in reactor III in described step h, dissolution aids is sufficiently stirred for reaction and removes the Mg in secondary crude brine
2+
、Ca
2+
、SO
4
2-
, then inject settling tank III；Dissolving settling agent is the supernatant generated in step i.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment describe in detail the present invention:
Embodiment 1:
Under the conditions of 20～60 DEG C, after utilizing 990L concentrated seawater to be dissolved by 265Kg crude salt in salt dissolving tank I, make a crude brine.One time crude brine is sent in reactor I, and in reactor I, addition 50L concentration is the lime cream of 180Ti, makes Mg
2+
、SO
4
2-
With OH
-
、Ca
2+
Reaction, then utilizes the Mg (OH) that settling tank I is isolated in reactant liquor under 20g settling agent effect
2
And CaSO
4
, supernatant liquid having 65L for dissolving outside settling agent, remaining is as primary brine dereaction device II.It is that 100Ti heat alkali liquid reacts, with the lime cream that 5L concentration is 105Ti, the Na formed by 50L concentration in causticization settling tank
2
CO
3
Solution is sent in reactor II, with Ca in primary brine
2+
Reaction, then utilizing settling tank II to isolate main constituent in reactant liquor is water and CaCO
3
Secondary mud, secondary mud has 70L Returning reactor II do crystal seed use, remaining 47L after 60L concentrated seawater, multiplexing water counter current washes, output 10Kg light calcium carbonate product after machine solid-liquid separation by centrifugation.
The isolated filtrate in rear water and mud of washing of washing mud formation is used as once to change salt water.Under the conditions of 20～60 DEG C, in salt dissolving tank II, add the supernatant liquid of settling tank II, be simultaneously introduced 35Kg crude salt, and the crude brine of secondary salt formation is sent in reactor III.To be sent in reactor III with lime cream in the mixed liquor of 2.5:1 ratio (percent by volume) by 3L soda liquid in causticizing tank, with the Mg in the crude brine of secondary salt formation
2+
、Ca
2+
Reaction, then clarification forms the saturated refined brine of 1100L.Isolated for settling tank III three mud and a mud are collected, utilize 200L concentrated seawater, wash with water again after carry out filter pressing, the brine sludge that filter pressing is formed makes dispensing needed for engineering earth.What washing, filter pressing were formed washes rear water and filter pressing filtrate as concentrated seawater needed for change salt.
Embodiment 2:
Under the conditions of 20～60 DEG C, after utilizing 1020L fresh water to be dissolved by 321Kg crude salt in salt dissolving tank I, make a crude brine.One time crude brine is sent in reactor I, and in reactor I, addition 30L concentration is the lime cream of 180Ti, makes Mg
2+
、SO
4
2-
With OH
-
、Ca
2+
Reaction, then utilizes the Mg (OH) that settling tank I is isolated in reactant liquor under 8g settling agent effect
2
And CaSO
4
, supernatant liquid having 30L outside dissolution aids, remaining is as primary brine dereaction device II.By in causticization settling tank by 30L concentration be 100Ti heat alkali liquid be that 180Ti lime cream reacts the Na formed with 3L concentration
2
CO
3
Solution is sent in reactor II, with Ca in primary brine
2+
Reaction, then utilizing settling tank II to isolate main constituent in reactant liquor is water and CaCO
3
Secondary mud, secondary mud has 46L Returning reactor II do crystal seed to use, remaining 25L is after 40L fresh water washs, and output 6.5Kg light calcium carbonate product after machine solid-liquid separation by centrifugation, the isolated filtrate in rear water and mud of washing of washing mud formation is used as once to change salt water.Under the conditions of 20～60 DEG C, in salt dissolving tank II, add the supernatant liquid of settling tank II, be simultaneously introduced 26Kg crude salt, and the crude brine of secondary salt formation is sent in reactor III.To be sent in reactor III with lime cream in the mixed liquor of 2.5:1 ratio (percent by volume) by 2.5L soda liquid in causticizing tank, with the Mg in the crude brine of secondary salt formation
2+
、Ca
2+
Reaction, then clarification forms the saturated refined brine of 1100L, and wherein 44L removes Returning reactor III after dissolving settling agent；Remainder refined brine goes to inhale ammonia operation and carbonation process.
Isolated for settling tank III three mud and a mud are collected, utilize 137L concentrated seawater, wash with water again after carry out filter pressing, the brine sludge that filter pressing is formed makes dispensing needed for engineering earth；What washing, filter pressing were formed washes rear water and filter pressing filtrate as concentrated seawater needed for change salt.
Claims (6)
1. the method preparing refined brine, comprises the steps:
A, in salt dissolving tank I add crude salt, being simultaneously introduced salt water dissolution crude salt, make a crude brine；
B, crude brine is sent in reactor I, in reactor I, add lime cream simultaneously, then enter settling tank I；
The Mg (OH) that c, settling tank I are isolated in reactant liquor after being sufficiently stirred for reaction2And CaSO4-And form a mud, one time mud is sent in mud cleaning bucket I, is sent to brine sludge filter pressing operation after changing saline washing, washed once the light salt brine of mud formation for once changing saline；Supernatant liquid 4～8% after the clarification of clarified bucket I returns settling tank I, and remaining enters reactor II as primary brine；Complete primary purification and complete denitration；
D, heat alkali liquid and lime cream are sent into causticization settling tank in react, clarified bottom generates CaCO3Mud, Na is formed at top2CO3Solution；
E, top Na2CO3Solution enters and fully reacts the Ca removed in primary brine in reactor II2+, then utilize settling tank II to isolate the CaCO in reactant liquor3And form secondary mud and secondary brine, complete secondary refining；Wherein in secondary mud 55～65% Returning reactor II do crystal seed use；
F, secondary brine deliver to salt dissolving tank II, add crude salt in salt dissolving tank II, utilize secondary brine to dissolve crude salt, send in reactor III, complete second timeization salt after making secondary crude brine；
G, in the ratio of 1:2～3, lime cream and soda liquid are sent into causticizing tank in react, and with the CaCO from causticization settling tank3Mud mixes, and the causticization liquid of formation is sent in reactor III；
H, reactor III remove the Mg in secondary crude brine2+、Ca2+、SO4 2-, then inject settling tank III；
I, settling tank III are carried out be sufficiently stirred for reaction, isolate the Mg (OH) in reactant liquor2、CaCO3And forming three mud, 2～5% in the supernatant return settling tank III, and remainder goes to inhale ammonia operation and carbonation process prepares qualified refined brine；Complete three times to refine.
The method preparing refined brine the most according to claim 1, it is characterised in that: the change saline in step a be secondary mud is washed by concentrated seawater or fresh water or step e wash after use water.
The method preparing refined brine the most according to claim 1, it is characterised in that: the concentration of the crude brine made in step a is 90～108Ti.
The method preparing refined brine the most according to claim 1, it is characterised in that: in step d, in heat alkali liquid, ratio with lime cream is 10～15:1.
The method preparing refined brine the most according to claim 1, it is characterised in that: in described step f, the concentration of secondary crude brine is 106～108Ti.
The method preparing refined brine the most according to claim 1, it is characterised in that: in described step d heat alkali liquid, the ratio with lime cream is 10:1.
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|---|---|---|---|
| CN201210517699.XA CN102951659B (en) | 2012-12-06 | 2012-12-06 | The method preparing refined brine and side-product thereof |
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|---|---|---|---|
| CN201210517699.XA CN102951659B (en) | 2012-12-06 | 2012-12-06 | The method preparing refined brine and side-product thereof |
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| CN102951659B true CN102951659B (en) | 2016-08-03 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880042B (en) * | 2014-04-14 | 2015-12-02 | 唐山三友化工股份有限公司 | The method of saltcake refined brine and preventing scaring |
| CN107892313A (en) * | 2017-12-30 | 2018-04-10 | 唐山三友化工股份有限公司 | Utilize saltcake refined brine and the process units and production method of by-product dihydrate gypsum |
| CN109485083A (en) * | 2018-12-20 | 2019-03-19 | 四川久大蓬莱盐化有限公司 | A kind of preparation method and preparation system of feed addictive calcium sulfate |
| CN110342547A (en) * | 2019-01-29 | 2019-10-18 | 内蒙古兰太实业股份有限公司 | The method and system of brine are prepared using inferior raw material salt |
Citations (4)
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|---|---|---|---|---|
| WO2003035550A1 (en) * | 2001-10-22 | 2003-05-01 | Council Of Scientific And Industrial Research | Recovery of sodium chloride and other salts from brine |
| CN1765774A (en) * | 2005-09-09 | 2006-05-03 | 唐山三友化工股份有限公司 | Sodium carbonate salt water prerefining and antiscaling process and prerefining reacting trough |
| CN101691239A (en) * | 2009-09-30 | 2010-04-07 | 达州市恒成能源（集团）有限责任公司 | Comprehensive utilization method for bittern |
| CN102795719A (en) * | 2011-05-27 | 2012-11-28 | 王凯勋 | Methods for removing calcium and magnesium and co-producing water and salt by low-cost process during sea water desalination |
-
2012
- 2012-12-06 CN CN201210517699.XA patent/CN102951659B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003035550A1 (en) * | 2001-10-22 | 2003-05-01 | Council Of Scientific And Industrial Research | Recovery of sodium chloride and other salts from brine |
| CN1765774A (en) * | 2005-09-09 | 2006-05-03 | 唐山三友化工股份有限公司 | Sodium carbonate salt water prerefining and antiscaling process and prerefining reacting trough |
| CN101691239A (en) * | 2009-09-30 | 2010-04-07 | 达州市恒成能源（集团）有限责任公司 | Comprehensive utilization method for bittern |
| CN102795719A (en) * | 2011-05-27 | 2012-11-28 | 王凯勋 | Methods for removing calcium and magnesium and co-producing water and salt by low-cost process during sea water desalination |
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