CN1226188C - 一种卤水制取钾盐和硼酸的工艺 - Google Patents
一种卤水制取钾盐和硼酸的工艺 Download PDFInfo
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- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000004327 boric acid Substances 0.000 title claims abstract description 40
- 241001131796 Botaurus stellaris Species 0.000 title claims abstract description 13
- 150000003839 salts Chemical class 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title description 3
- 241001397173 Kali <angiosperm> Species 0.000 title 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000012452 mother liquor Substances 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000012267 brine Substances 0.000 claims abstract description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 6
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 claims abstract 3
- 229910052736 halogen Inorganic materials 0.000 claims description 27
- 150000002367 halogens Chemical class 0.000 claims description 27
- 238000000354 decomposition reaction Methods 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 12
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 239000006210 lotion Substances 0.000 claims description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000010413 mother solution Substances 0.000 claims 1
- 239000001103 potassium chloride Substances 0.000 abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 4
- 239000011780 sodium chloride Substances 0.000 abstract 2
- 230000032683 aging Effects 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- XLKNMWIXNFVJRR-UHFFFAOYSA-N boron potassium Chemical compound [B].[K] XLKNMWIXNFVJRR-UHFFFAOYSA-N 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000007667 floating Methods 0.000 description 2
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- 239000012047 saturated solution Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
一种卤水制取氯化钾和硼酸的工艺，将卤水用改性老卤兑卤和兑卤母液蒸发提取氯化钠，蒸发完成液除氯化钠后，一段真空冷却分离出光卤石，光卤石分解得氯化钾，二段冷却分离出低温盐，低温盐经洗涤、热溶精制得硼酸，本工艺流程简单明晰、产品品位高、各盐类回收率高。
Description
技术领域：一种卤水制取钾盐和硼酸的工艺，涉及采用卤水为原料生产钾盐及硼酸的技术领域。
背景技术：现有技术中，由卤水制取钾盐和硼酸的工艺是，首先在蒸发器中注入卤水进行蒸发脱钠，脱钠母液继续蒸发后产生硼钾混合盐，硼钾混合盐用浮选法分离得到钾盐和硼酸，现有技术的缺点是工业化生产难以实现，浮选工艺存在当浮钾母液和浮硼母液无法严格分开时，钾硼将无法分离的缺陷，而且产品质量差。
本发明的目的是将兑卤脱钠、蒸发结晶、真空冷却、光卤石控速分解多种工艺进行整合，设计一种采用原料卤水制取钾盐和硼酸的工艺。
发明内容：本发明是通过三个工段实现的，即兑卤蒸发工段、光卤石分解结晶工段、硼酸制取工段；
兑卤蒸发工段：将原料卤水与老卤按比例在兑卤器中兑卤，分离得到副产品氯化钠和兑卤母液，兑卤母液经多效蒸发至规定温度，分离得到含有70-85％氯化钠的高温盐和高温母液；
光卤石分解结晶工段：利用真空结晶器将高温母液闪蒸冷却至规定温度，分离得到光卤石和中温母液，光卤石与循环洗液、水按比例加入分解结晶器中进行分解结晶，得到氯化钾，再经洗涤、脱水后进入干燥机干燥后得到氯化钾产品；
硼酸制取工段：中温母液经外冷器冷却后进入冷析结晶器，再经振动筛分离少量光卤石，筛分后将母液固液分离得到低温盐，分离低温盐后老卤返回兑卤工段，低温盐、水、循环洗液按重量比混合、搅拌30分钟，分离得到含40～60％硼酸的粗硼酸；再将粗硼酸、硼酸饱和液按重量比加入盐酸和双氧水混合，经过热溶、冷却后，分离、洗涤、干燥得到优级工业硼酸。
本发明的优点是：工艺流程简单明晰，工业化容易实现，产品品位高，各盐类回收率高，该工艺实行全封闭流程，基本不对环境造成影响。
图1为本发明的工艺流程图。
具体实施方法：下面结合附图给出发明的最佳实施例子：本发明是通过三个工段实现的，即兑卤蒸发工段、光卤石分解结晶工段和硼酸制取工段：
1.兑卤蒸发工段：兑卤蒸发工段的原料富钾卤水与含氯化镁25～35％的老卤按1∶(1.2～1.6)进行兑卤，兑卤后的母液依次进入II效蒸发器和I效蒸发器进行蒸发，II效蒸发器蒸发室压力-0.05～-0.09MPa、料液温度60～75℃，I效蒸发器蒸发室控制压力0.02MPa、料液温度120～130℃；蒸发完成液分离出含70～85％氯化钠的高温盐和高温母液，分离出的高温盐固体返回兑卤工段的兑卤器中洗涤，然后分离出纯度为90～99％的氯化钠产品并回收氯化钾和硼酸，分离后的高温母液作为光卤石分解结晶工段的原料；
2.光卤石分解结晶工段：在光卤石分解结晶工段，由兑卤蒸发工段来的高温母液在真空结晶器中闪蒸冷却至50～60℃，真空结晶器蒸发室压力≤-0.08MPa，分离出含4～5％氯化钠的光卤石和中温母液，分离后的中温母液做为硼酸制取工段的原料；将光卤石、水和循环洗液按比例1∶(0.5～1)∶(4～10)的重量比加入分解结晶器分解结晶，分解结晶器内分解母液波美度控制在27～31的范围，得到氯化钾，再经洗涤和脱水后进入干燥机干燥得到纯度为95～98％的氯化钾产品；富余的分解母液返回蒸发工段，回收氯化钾，硼酸和氯化镁；
3.硼酸制取工段：在硼酸制取工段中，由光卤石分解结晶工段来的中温母液经外冷冷却后进入冷析结晶器，冷析结晶器料液温度≤35℃，利用光卤石和硼酸粒度差异，用100～200目筛网振动筛分离出少量含2～3％氯化钠的光卤石和含24～32％硼酸的低温盐；分离低温盐后的老卤返回兑卤工段，将低温盐、水和循环洗液按1∶(0.5～1)∶(4～8)重量比混合后搅拌30～40分钟，分离得到含40～60％的粗硼酸，低温盐的洗涤液返回蒸发工段回收氯化钾、硼酸和氯化镁；再将粗硼酸和硼酸饱和液按1∶(4～8)重量比混合并加入盐酸进行混合，将混合液PH值调至1～3、升温至60～70℃后加入1～10％的双氧水，再热溶至100～110℃，搅拌30分钟、过滤冷却后，分离、洗涤和干燥得到工业硼酸。
Claims (5)
1、一种卤水制取氯化钾和硼酸的工艺，其特征在于：该方法包括以下步骤：
(a).富钾卤水与含氯化镁25～33％的老卤按1∶(1.2～1.6)进行兑卤，然后加入高温盐进行洗涤，分离出纯度为90～99％的氯化钠产品，分离后的兑卤母液作为光卤石分解结晶工段的原料；
(b).兑卤后的母液经多效蒸发至120～130℃，排料分离出含70～85％氯化钠的高温盐固体，分离后的高温母液在真空结晶器中闪蒸冷却至50～60℃分离出含4～5％氯化钠的光卤石和中温母液，中温母液经外冷器冷却后进入冷析结晶器，冷析结晶器料液温度≤35℃，再经振动筛分离得到含24～32％硼酸的低温盐和含2～3％氯化钠的光卤石；
(c).将光卤石、水和循环洗液按1∶(0.5～1)∶(4～10)重量比在分解结晶器中混合，分解结晶器内的分解母液波美度控制在27～31范围，经分离、洗涤、脱水和干燥得到纯度为95～98％的氯化钾产品；
(d).将低温盐、水和循环洗液按1∶(0.5～1)∶(4～10)的重量比混合、搅拌30～40分钟，分离得到含40～60％的粗硼酸。
2、根据权利要求1所述的一种卤水制取氯化钾和硼酸的工艺，其特征在于将蒸发后得到的含70～85％氯化钠的高温盐，返回兑卤工段的兑卤器中洗涤，回收氯化钾和硼酸。
3、根据权利要求1所述的一种卤水制取氯化钾和硼酸的工艺，其特征在于光卤石分解结晶工段的光卤石分解母液返回蒸发工段，回收氯化钾、硼酸和氯化镁。
4、根据权利要求1所述的一种卤水制取氯化钾和硼酸的工艺，其特征在于将光卤石母液再冷却至30～35℃后，利用光卤石和硼酸粒度差异，用100～200目筛网振动筛分离出光卤石。
5、根据权利要求1所述的一种卤水制取氯化钾和硼酸的工艺，其特征在于低温盐洗后的洗涤液回收氯化钾、硼酸和氯化镁。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI383958B (zh) * | 2005-01-28 | 2013-02-01 | Nippoh Chemicals | Wastewater treatment methods |
| CN1319855C (zh) * | 2005-07-17 | 2007-06-06 | 青海中信国安科技发展有限公司 | 从含硼水氯镁石饱和液中生产硼酸的工艺 |
| CN100560491C (zh) * | 2007-08-03 | 2009-11-18 | 乳源瑶族自治县东阳光化成箔有限公司 | 化成废液中硼酸的回收处理方法及其处理*** |
| CN113307299B (zh) * | 2021-06-22 | 2022-10-21 | 中国科学院青海盐湖研究所 | 一种从高钾镁氯化物卤水中提取铷的方法 |
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