CN1298635C - Method of preparing chromium sulphate - Google Patents
Method of preparing chromium sulphate Download PDFInfo
- Publication number
- CN1298635C CN1298635C CN 200510053373 CN200510053373A CN1298635C CN 1298635 C CN1298635 C CN 1298635C CN 200510053373 CN200510053373 CN 200510053373 CN 200510053373 A CN200510053373 A CN 200510053373A CN 1298635 C CN1298635 C CN 1298635C
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- CN
- China
- Prior art keywords
- chromic anhydride
- formaldehyde
- chromium
- sulfuric acid
- chromium sulphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 17
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 title claims abstract description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 39
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 claims 1
- 230000002829 reductive effect Effects 0.000 claims 1
- 239000011651 chromium Substances 0.000 abstract description 13
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052804 chromium Inorganic materials 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003760 magnetic stirring Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- RAGLTCMTCZHYEJ-UHFFFAOYSA-K azanium;chromium(3+);disulfate Chemical compound [NH4+].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RAGLTCMTCZHYEJ-UHFFFAOYSA-K 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种用甲醛还原铬酐制备硫酸铬的方法。该方法以铬酐为原料，在硫酸存在、水浴加热、磁力搅拌下，以甲醛作还原剂制备硫酸铬。该方法工艺简便、无杂质，产品无需任何处理即可在电沉积铬生产中使用。The invention discloses a method for preparing chromium sulfate by reducing chromic anhydride with formaldehyde. The method uses chromic anhydride as a raw material, and prepares chromium sulfate by using formaldehyde as a reducing agent in the presence of sulfuric acid, heating in a water bath, and magnetic stirring. The method has simple process and no impurities, and the product can be used in the production of electrodeposited chromium without any treatment.
Description
技术领域technical field
本发明涉及一种制备硫酸铬的方法，特别是电沉积铬中甲醛还原铬酐制备硫酸铬的方法。The invention relates to a method for preparing chromium sulfate, in particular to a method for preparing chromium sulfate by reducing chromic anhydride with formaldehyde in electrodeposited chromium.
背景技术Background technique
硫酸铬是三价铬电沉积铬中的一种主要原料，由于其具有对环境污染较小、反应条件温和、电解效率较高等优点而引起人们的极大关注。但由于硫酸铬价格较高，且市场供应不足。而铬酐纯度高，市场供应充足，价格较低廉，因而用还原铬酐法获取三价铬源不失为一种经济、快速、高效的方法。目前，还原铬酐常用的还原剂有FeSO4、NaHSO3、Na2SO3、SO2、水合肼、蔗糖、甲醇等。但这些还原方法常存在引入有害离子、反应难以控制、使用对环境有污染的气体等缺陷，难以满足电沉积铬源的要求。关于甲醛还原铬酐制备硫酸铬的方法研究未见报导。Chromium sulfate is one of the main raw materials for trivalent chromium electrodeposition. It has attracted great attention because of its advantages such as less environmental pollution, mild reaction conditions, and high electrolysis efficiency. However, due to the high price of chromium sulfate and insufficient market supply. However, the purity of chromic anhydride is high, the market supply is sufficient, and the price is relatively low. Therefore, it is an economical, fast and efficient method to obtain trivalent chromium source by reducing chromic anhydride method. At present, the commonly used reducing agents for reducing chromic anhydride include FeSO 4 , NaHSO 3 , Na 2 SO 3 , SO 2 , hydrazine hydrate, sucrose, methanol, etc. However, these reduction methods often have defects such as the introduction of harmful ions, the difficulty in controlling the reaction, and the use of gases that pollute the environment, which make it difficult to meet the requirements of the chromium source for electrodeposition. There is no report about the method research on the reduction of chromic anhydride by formaldehyde to prepare chromium sulfate.
发明内容Contents of the invention
本发明的目的是提供一种反应产物无污染、无杂质的硫酸铬铵电沉积铬生产中甲醛还原铬酐制备硫酸铬的方法。The purpose of the present invention is to provide a method for preparing chromium sulfate by formaldehyde reduction of chromic anhydride in the production of ammonium chromium sulfate electrodeposited chromium with no pollution and no impurities in the reaction product.
本发明制备硫酸铬的工艺方法是：以分析纯铬酐为原料，用一定量的水溶解，缓慢加入反应计量所需的硫酸，在90～100℃水浴、磁力搅拌下逐滴加入甲醛，甲醛的用量控制为反应计量的180％即过量80％。滴加完毕后继续加热10分钟，使铬酐还原完全。该反应液可直接用于硫酸铬铵电沉积铬的基础溶液，也可将反应液蒸发浓缩使硫酸铬以水合结晶形式结晶出来，以备各种实验或生产所需。The process for preparing chromium sulfate in the present invention is as follows: use analytically pure chromic anhydride as a raw material, dissolve it in a certain amount of water, slowly add sulfuric acid required for reaction metering, add formaldehyde dropwise in a water bath at 90-100°C and magnetic stirring, formaldehyde The consumption control is 180% that is excessive 80% of reaction metering. After the dropwise addition, continue heating for 10 minutes to completely reduce the chromic anhydride. The reaction solution can be directly used as the basic solution for chromium ammonium sulfate electrodeposition chromium, and the reaction solution can also be evaporated and concentrated to crystallize the chromium sulfate in the form of hydrated crystals for various experiments or production needs.
本发明与其它相关制备技术相比，最显著的特点是生产设备简单，过程简短，反应条件易于控制，反应产物无污染、无杂质，能直接用作电沉积铬的铬源，满足电沉积铬生产中对硫酸铬的要求。Compared with other related preparation technologies, the present invention has the most notable features of simple production equipment, short process, easy control of reaction conditions, no pollution and no impurities in the reaction product, and can be directly used as a chromium source for electrodeposited chromium to meet the requirements of electrodeposited chromium. Requirements for chromium sulfate in production.
具体实施方式Detailed ways
实施例1Example 1
称取5.00g铬酐于100mL小烧杯中，加入20mL蒸馏水，缓慢加入相对密度为1.83g/cm3含量为95％的浓硫酸4.3mL，置90℃水浴中，在磁力搅拌下逐滴加入甲醛2.5mL，滴加完毕后继续在水浴中加热10分钟，使铬酐充分还原，浓缩干燥，可得17.78g紫色Cr2SO4·18H2O，收率为99.3％。Weigh 5.00g of chromic anhydride into a 100mL small beaker, add 20mL of distilled water, slowly add 4.3mL of concentrated sulfuric acid with a relative density of 1.83g/ cm3 and a content of 95%, put it in a water bath at 90°C, and add formaldehyde drop by drop under magnetic stirring 2.5 mL, continue heating in a water bath for 10 minutes after the dropwise addition to fully reduce the chromic anhydride, concentrate and dry to obtain 17.78 g of purple Cr 2 SO 4 ·18H 2 O with a yield of 99.3%.
实施例2Example 2
称取15.00g铬酐于400mL烧杯中，加入50mL蒸馏水，缓慢加入相对密度为1.78g/cm380％浓硫酸15.5mL，置95℃水浴中，在磁力搅拌下逐滴加入甲醛7.5mL，滴加完毕后继续在水浴中加热10分钟，使铬酐充分还原，浓缩干燥，可得53.25g紫色Cr2SO4·18H2O，收率为99.2％。Weigh 15.00g of chromic anhydride in a 400mL beaker, add 50mL of distilled water, slowly add 15.5mL of 80% concentrated sulfuric acid with a relative density of 1.78g/cm 3 , put it in a water bath at 95°C, add 7.5mL of formaldehyde dropwise under magnetic stirring, drop After the addition, continue heating in a water bath for 10 minutes to fully reduce the chromic anhydride, concentrate and dry to obtain 53.25 g of purple Cr 2 SO 4 ·18H 2 O with a yield of 99.2%.
实施例3Example 3
称取25.00g铬酐于500mL烧杯中，加入120mL蒸馏水，缓慢加入相对密度为1.84g/cm398％浓硫酸20.4mL，置100℃水浴中，在磁力搅拌下逐滴加入甲醛12.5mL，滴加完毕后继续在水浴中加热10分钟，使铬酐充分还原，浓缩干燥，可得88.52g紫色Cr2SO4·18H2O，收率为98.9％。Weigh 25.00g of chromic anhydride in a 500mL beaker, add 120mL of distilled water, slowly add 20.4mL of 98% concentrated sulfuric acid with a relative density of 1.84g/cm 3 , put it in a water bath at 100°C, add 12.5mL of formaldehyde dropwise under magnetic stirring, drop After the addition, continue heating in a water bath for 10 minutes to fully reduce the chromic anhydride, concentrate and dry to obtain 88.52 g of purple Cr 2 SO 4 ·18H 2 O, with a yield of 98.9%.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510053373 CN1298635C (en) | 2005-03-11 | 2005-03-11 | Method of preparing chromium sulphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510053373 CN1298635C (en) | 2005-03-11 | 2005-03-11 | Method of preparing chromium sulphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1718545A CN1718545A (en) | 2006-01-11 |
| CN1298635C true CN1298635C (en) | 2007-02-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200510053373 Expired - Fee Related CN1298635C (en) | 2005-03-11 | 2005-03-11 | Method of preparing chromium sulphate |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2395463C9 (en) * | 2008-08-13 | 2010-10-10 | Федеральное государственное унитарное предприятие "Калужский научно-исследовательский институт телемеханических устройств" | Method of neutralising chromium-(+6)-containing spent solutions |
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- 2005-03-11 CN CN 200510053373 patent/CN1298635C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1718545A (en) | 2006-01-11 |
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