CN100436322C - 一种纯碱制备方法 - Google Patents
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- CN100436322C CN100436322C CNB2006101353364A CN200610135336A CN100436322C CN 100436322 C CN100436322 C CN 100436322C CN B2006101353364 A CNB2006101353364 A CN B2006101353364A CN 200610135336 A CN200610135336 A CN 200610135336A CN 100436322 C CN100436322 C CN 100436322C
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 title claims abstract description 44
- 229910000029 sodium carbonate Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 24
- 239000000460 chlorine Substances 0.000 claims abstract description 21
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000047 product Substances 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000011780 sodium chloride Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 5
- 238000005649 metathesis reaction Methods 0.000 claims abstract description 5
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000009615 deamination Effects 0.000 claims description 6
- 238000006481 deamination reaction Methods 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005194 fractionation Methods 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 26
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- NBFQLHGCEMEQFN-UHFFFAOYSA-N N.[Ni] Chemical compound N.[Ni] NBFQLHGCEMEQFN-UHFFFAOYSA-N 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 abstract 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 7
- 239000002699 waste material Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 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 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Manufacture And Refinement Of Metals (AREA)
- Fertilizers (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
一种纯碱制备方法，涉及一种采用氨镍法制备纯碱的工艺。提供一种原料易得，媒体氨和镍损耗小并可循环利用，排污少，产物品质高，含氯可控在0.1%以内的纯碱制法。NiO溶于CO2和氨水混合溶液，吸氨至饱和，加NaCl复分解，过滤分离出Na2CO3氨水溶液和Ni(NH3)6Cl2；Na2CO3氨水溶液蒸馏脱氨过滤出沉淀物Ni2(OH)2CO3，滤液浓缩结晶得纯碱产品。Ni(NH3)6Cl2加热脱氨得NiCl2；NiCl2加热与水蒸汽反应得NiO和氯化氢与水蒸汽混合物，或与空气中的O2反应得NiO和Cl2与空气混合物，NiO回收，氯化氢与水蒸汽混合物经冷凝得盐酸，Cl2与空气混合气经冷冻得液氯。
Description
技术领域
本发明涉及一种钠、钾或一般碱金属的碳酸盐，尤其是涉及一种采用氨镍法制备纯碱的工艺。
背景技术
传统的制碱工艺主要有氨碱法、联碱法和天然碱精制法，基中氨碱法制碱的优点是原料易得，工艺既成熟又简单，但NaCl的利用率较低，同时产生大量废液。联碱法虽然解决了氨碱法中所存在的问题，但是其设备要求较高，副产品的NH4Cl作为化肥在国外受到限制，在国内则受制于其他氮肥的市场价格，其附加值不高。
李忠在公开号为CN1308020的发明专利申请中提供一种新的纯碱生产工艺，通过将蒸氨母液中CaCl2重新转化为CaO，返回蒸氨系统。以彻底消除氨碱法纯碱生产中大量废液废渣并降低消耗。其理论依据如下式：CaCl2+H2O→CaO+2HCl↑。
徐贵义在公开号为CN1814548的发明专利申请中提供一种无废排放氨碱法纯碱工艺，它是将蒸氨工序出来的废渣液进行处理，废渣液经分离工序分离除渣并经洗涤得工程土产品；上清液在反应工序中与冻硝(Na2SO4)反应得精石膏产品；反应工序出来的循环液进入盐水工序循环使用；多余的循环液进入制盐工序制取精盐产品。
发明内容
本发明的目的在于针对现有的制碱工艺所存在的诸多问题，提供一种原料易得，媒体氨和镍的损耗小并可循环利用，中间无废弃物产生，排污量少，制得的目标产物品质高，含氯可控制在0.1％以内的纯碱制备方法。
本发明的技术方案是以NaCl、工业CO2、水和空气为原料，以氨和镍为媒体，制得纯碱和盐酸或氯气。
本发明包括以下步骤：
1)将NiO溶解于CO2和氨水混合溶液中，吸氨至饱和，再加入NaCl进行复分解、过滤、分离出Na2CO3氨水溶液和Ni(NH3)6Cl2；
2)将Na2CO3氨水溶液蒸馏脱氨，过滤出沉淀物Ni2(OH)2CO3，滤液再浓缩结晶得纯碱产品；
3)将Ni(NH3)6Cl2加热至150～200℃，脱氨得NiCl2；
4)将NiCl2加热至500～1000℃，与水蒸汽反应得NiO以及氯化氢与水蒸汽混合物，或者与空气中的O2反应得NiO以及Cl2与空气混合物，NiO回收到步骤1中的浸出工序循环利用，而氯化氢与水蒸汽混合物经冷凝得盐酸产品，Cl2与空气的混合气经冷冻分离出液氯产品。
按质量比NiO∶CO2∶NaCl＝100∶62∶162，NiCl2∶水蒸汽＝100∶200。
本发明的基本原理是：由于NiO易溶于(NH4)2CO3溶液，可轻易地形成Ni(NH3)6CO3溶液，而Ni(NH3)6Cl2在浓氨水中的溶解度很小，因此利用上述特性，用NaCl与Ni(NH3)6Cl2进行复分解反应制得Na2CO3，其化学反应式为：
NiO+6NH3+CO2＝Ni(NH3)6CO3
Ni(NH3)6CO3+NaCl＝Na2CO3+Ni(NH3)6Cl2↓
其中氨和镍循环利用，理论上在工艺过程中损耗很小。
本发明解决了现有的氨碱法制纯碱中所存在的问题，所需原料易得，媒体氨和镍的损耗小并可循环利用，中间无废弃物产生，排污量少，制得的目标产物低氯纯碱的含氯在0.1％以下，副产品为盐酸或氯气。
具体实施方式
以下实施例将对本发明作进一步的说明。
将10kgNiO溶解于含6.2kgCO2的CO2和氨水混合溶液中，吸氨至饱和，再加入16.2kgNaCl进行复分解、过滤、分离出Na2CO3氨水溶液和Ni(NH3)6Cl2；将Na2CO3氨水溶液蒸馏脱氨，过滤出沉淀物Ni2(OH)2CO3，滤液再浓缩结晶得纯碱产品；将Ni(NH3)6Cl2加热至150～200℃，脱氨得NiCl2；将NiCl2加热至500～1000℃，与水蒸汽反应得NiO以及氯化氢与水蒸汽混合物，水蒸汽的加入量为NiCl2总量的2倍，NiO回收到步骤1中的浸出工序循环利用，而氯化氢与水蒸汽混合物经冷凝得盐酸产品。
Claims (4)
1.一种纯碱制备方法，其特征在于其化学反应式为：
NiO+6NH3+CO2＝Ni(NH3)6CO3
Ni(NH3)6CO3+2NaCl＝Na2CO3+Ni(NH3)6Cl2↓；
其步骤为：
1)将NiO溶解于CO2和氨水混合溶液中，吸氨至饱和，再加入NaCl进行复分解、过滤、分离出Na2CO3氨水溶液和Ni(NH3)6Cl2；
2)将Na2CO3氨水溶液蒸馏脱氨，过滤出沉淀物Ni2(OH)2CO3，滤液再浓缩结晶得纯碱产品；
按质量比NiO∶CO2∶NaCl＝100∶62∶162。
2.如权利要求1所述的一种纯碱制备方法，其特征在于将Ni(NH3)6Cl2加热至150～200℃，脱氨得NiCl2。
3.如权利要求1所述的一种纯碱制备方法，其特征在于将NiCl2加热至500～1000℃，与水蒸汽反应得NiO以及氯化氢与水蒸汽混合物，或者与空气中的O2反应得NiO以及Cl2与空气混合物，NiO回收到步骤1中的浸出工序循环利用，而氯化氢与水蒸汽混合物经冷凝得盐酸产品，Cl2与空气的混合气经冷冻分离出液氯产品。
4.如权利要求3所述的一种纯碱制备方法，其特征在于按质量比NiCl2∶水蒸汽＝100∶200。
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101353364A CN100436322C (zh) | 2006-12-15 | 2006-12-15 | 一种纯碱制备方法 |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101353364A CN100436322C (zh) | 2006-12-15 | 2006-12-15 | 一种纯碱制备方法 |
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| Publication Number | Publication Date |
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| CN1974388A CN1974388A (zh) | 2007-06-06 |
| CN100436322C true CN100436322C (zh) | 2008-11-26 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101112998B (zh) * | 2007-07-09 | 2010-05-19 | 钟劲光 | 纯碱的制备方法 |
| CN107934964A (zh) * | 2017-12-18 | 2018-04-20 | 青海盐湖工业股份有限公司 | 一种二氧化碳气体综合利用方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113885A (zh) * | 1994-06-01 | 1995-12-27 | 门伟 | 纯碱的生产方法 |
| CN1308020A (zh) * | 2000-10-30 | 2001-08-15 | 李忠 | 绿色化工法纯碱生产工艺 |
| CN1814548A (zh) * | 2005-12-26 | 2006-08-09 | 徐贵义 | 无废排放氨碱法纯碱工艺 |
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2006
- 2006-12-15 CN CNB2006101353364A patent/CN100436322C/zh not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113885A (zh) * | 1994-06-01 | 1995-12-27 | 门伟 | 纯碱的生产方法 |
| CN1308020A (zh) * | 2000-10-30 | 2001-08-15 | 李忠 | 绿色化工法纯碱生产工艺 |
| CN1814548A (zh) * | 2005-12-26 | 2006-08-09 | 徐贵义 | 无废排放氨碱法纯碱工艺 |
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Address after: 200030 room 6, building 829, No. 558, Xuhui District, Shanghai, Yishan Road Patentee after: ZHONGKE YIGONG (SHANGHAI) CHEMICAL TECHNOLOGY CO.,LTD. Address before: Haicang District of Xiamen City, Fujian province 361026 Weng Kok Road No. 289 Chong Building 422 unit Patentee before: Zhongke Yigong (Xiamen) Chemical Technology Co.,Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081126 Termination date: 20211215 |
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| CF01 | Termination of patent right due to non-payment of annual fee |