CN1696099A - The preparation method of high-purity zinc acetate - Google Patents
The preparation method of high-purity zinc acetate Download PDFInfo
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- CN1696099A CN1696099A CN 200410038170 CN200410038170A CN1696099A CN 1696099 A CN1696099 A CN 1696099A CN 200410038170 CN200410038170 CN 200410038170 CN 200410038170 A CN200410038170 A CN 200410038170A CN 1696099 A CN1696099 A CN 1696099A
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- zinc acetate
- zinc
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- acetate
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- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000004246 zinc acetate Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 239000012047 saturated solution Substances 0.000 claims abstract description 18
- 239000011701 zinc Substances 0.000 claims abstract description 17
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 17
- 229950003143 basic zinc acetate Drugs 0.000 claims abstract description 14
- JCPDISNOORFYFA-UHFFFAOYSA-H tetrazinc;oxygen(2-);hexaacetate Chemical compound [O-2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O JCPDISNOORFYFA-UHFFFAOYSA-H 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 150000002739 metals Chemical class 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- 239000012452 mother liquor Substances 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
技术领域technical field
本发明是一种高纯度醋酸锌的制法，尤其是指一种可使得制品中不含其它重金属杂质的高纯度醋酸锌的制法。The invention relates to a method for preparing high-purity zinc acetate, in particular to a method for preparing high-purity zinc acetate that can make products free from other heavy metal impurities.
背景技术Background technique
按，传统制造醋酸锌的方法，多是利用将锌氧粉(即氧化锌)添加冰醋酸及水，使其反应生成含结晶水的醋酸锌，其主要反应式如下所示：Press, the traditional method of manufacturing zinc acetate mostly is to utilize zinc oxide powder (being zinc oxide) to add glacial acetic acid and water, make it react to generate zinc acetate containing crystallization water, and its main reaction formula is as follows:
此反应会放热而使得溶液温度上升，待反应经过一段时间而成为醋酸锌的饱和溶液后，将溶液的温度降下，使得醋酸锌溶液由饱和溶液成为过饱和溶液而析出醋酸锌的结晶，再将该醋酸锌的析出结晶经过脱水后即成为所需要的醋酸锌结晶。This reaction will release heat and make the temperature of the solution rise. After the reaction becomes a saturated solution of zinc acetate after a period of time, the temperature of the solution is lowered, so that the zinc acetate solution becomes a supersaturated solution from a saturated solution and crystallization of zinc acetate is precipitated. The precipitated crystals of zinc acetate become required zinc acetate crystals after dehydration.
然而，由于锌氧粉中含有如铅、镉、铜、铁等其它重金属杂质，因此，所得到的醋酸锌粉末中亦同时会混杂有上述的重金属杂质存在，导致产品的醋酸锌结晶纯度无法有效的加以提高。However, since the zinc oxide powder contains other heavy metal impurities such as lead, cadmium, copper, iron, etc., the resulting zinc acetate powder will also be mixed with the above-mentioned heavy metal impurities, resulting in the zinc acetate crystal purity of the product being ineffective. to be improved.
传统上是在醋酸锌的溶液加入少量硫酸锌，使得溶液中的铅杂质置换成硫酸铅沉淀物去除，但对于镉、铜、铁等其它重金属杂质无法去除。Traditionally, a small amount of zinc sulfate is added to the zinc acetate solution to replace the lead impurities in the solution with lead sulfate precipitates, but other heavy metal impurities such as cadmium, copper, and iron cannot be removed.
另外，在上述主要反应进行时，一般会同时进行下列反应：In addition, when the above-mentioned main reactions are carried out, the following reactions are generally carried out at the same time:
由于此反应在进行时，部分的锌离子会形成碱式醋酸锌离子(即盐基性醋酸锌离子)，因此在醋酸根离子与锌离子正常反应成为醋酸锌后，便没有多余的醋酸根离子和此碱式醋酸锌离子反应以生成醋酸锌，因此醋酸锌的产量没有办法加以提升。Since the reaction is in progress, part of the zinc ions will form basic zinc acetate ions (i.e. basic zinc acetate ions), so after the normal reaction of acetate ions and zinc ions to form zinc acetate, there will be no excess acetate ions React with this basic zinc acetate ion to generate zinc acetate, so the yield of zinc acetate cannot be improved.
发明内容Contents of the invention
本发明人有鉴于此，乃着手进行研究，以期可以解决上述醋酸锌在制造时所产生的两个问题，经过不断的试验及努力，终于研发出本发明。In view of this, the present inventor started to study in order to solve the two problems in the manufacture of the above-mentioned zinc acetate, and finally developed the present invention through continuous experiments and efforts.
本发明的主要目的在于提供一种产量高，且具有高纯度的醋酸锌的制法。Main purpose of the present invention is to provide a kind of yield height, and have the preparation method of the zinc acetate of high purity.
为了达到上述发明目的，本发明是采取以下的技术手段予以达成，其中本发明包括有：In order to achieve the above-mentioned purpose of the invention, the present invention is achieved by taking the following technical means, wherein the present invention includes:
反应步骤：其乃是将醋酸锌母液、锌氧粉置入反应槽，再适量加入冰醋酸至锌氧粉完全溶解以形成碱式醋酸锌高温饱和溶液；Reaction steps: put zinc acetate mother liquor and zinc oxide powder into the reaction tank, then add glacial acetic acid in an appropriate amount until the zinc oxide powder is completely dissolved to form a high-temperature saturated solution of basic zinc acetate;
纯化步骤：其是将锌制物体浸泡在上述溶液中，使得杂质的重金属离子还原而附着在锌制物体上，而部分的杂质金属形成为沉淀物；Purification step: immerse the zinc object in the above solution, so that the heavy metal ions of the impurities are reduced and attached to the zinc object, and part of the impurity metal forms a precipitate;
分离步骤：其是将醋酸锌饱和溶液抽取分离至另一反应槽；Separation step: it is to extract and separate the zinc acetate saturated solution to another reaction tank;
产量提高步骤：其是在碱式醋酸锌高温饱和溶液中添加冰醋酸，并加以搅拌使之进行后续反应；Yield improving step: it is to add glacial acetic acid to the high-temperature saturated solution of basic zinc acetate, and stir to make it carry out follow-up reaction;
析出步骤：其是将添加冰醋酸后的醋酸锌饱和溶液持续搅拌并降温，使之成为醋酸锌的过饱和溶液以析出醋酸锌结晶；Precipitation step: it is to continuously stir and cool down the zinc acetate saturated solution after adding glacial acetic acid, so that it becomes a supersaturated solution of zinc acetate to precipitate zinc acetate crystals;
脱水步骤：其是将醋酸锌结晶与降温的醋酸锌饱和溶液加以固液分离，醋酸锌结晶经离心脱水成为醋酸锌结晶，而醋酸锌溶液则成为醋酸锌母液回收使用。Dehydration step: it is to separate the zinc acetate crystals from the cooled zinc acetate saturated solution for solid-liquid separation, the zinc acetate crystals are centrifuged and dehydrated to become zinc acetate crystals, and the zinc acetate solution becomes zinc acetate mother liquor for recycling.
经由上述的纯化步骤，使得杂质金属可加以还原成金属粉末而分离，而利用产量提高步骤可使得碱式醋酸锌离子继续反应成为醋酸锌，故可提高醋酸锌的产量。Through the above-mentioned purification steps, the impurity metals can be reduced to metal powders for separation, and the yield-enhancing step can make the basic zinc acetate ions continue to react to form zinc acetate, so the yield of zinc acetate can be increased.
具体实施方式Detailed ways
现就本发明的实施方法加以详细说明。本发明的高纯度醋酸锌的制法包括有反应步骤、纯化步骤、分离步骤、产量提高步骤、析出步骤及过滤干燥步骤，其中各步骤的详细制程如下：Now describe in detail the implementation method of the present invention. The preparation method of high-purity zinc acetate of the present invention comprises reaction step, purification step, separation step, yield improvement step, precipitation step and filter drying step, wherein the detailed process of each step is as follows:
反应步骤：将醋酸锌母液、锌氧粉置入反应槽，再适量加入冰醋酸至锌氧粉完全溶解，此时pH值约为5.5～5，使得温度维持在90℃～100℃以形成碱式醋酸锌高温饱和溶液，其分别具有下述两项反应。Reaction steps: Put zinc acetate mother liquor and zinc oxide powder into the reaction tank, then add glacial acetic acid in an appropriate amount until the zinc oxide powder is completely dissolved, and the pH value is about 5.5~5 at this time, so that the temperature is maintained at 90°C~100°C to form an alkali Formula zinc acetate high temperature saturated solution, it has following two reactions respectively.
纯化步骤：其是将锌板、锌条、锌粒、锌球、锌粉等锌制物体浸泡在上述溶液中20～40分钟，使得杂质的金属离子还原成金属粉末而附着在锌制物体上，而部分的杂质金属形成为沉淀物。其中以铅为例其还原反应式如下所示：Purification step: soak zinc objects such as zinc plates, zinc strips, zinc particles, zinc balls, and zinc powder in the above solution for 20 to 40 minutes, so that the metal ions of impurities are reduced to metal powder and attached to the zinc objects , while part of the impurity metals formed as precipitates. Wherein taking lead as an example, its reduction reaction formula is as follows:
分离步骤：其是将醋酸锌饱和溶液抽取分离至另一反应槽。Separation step: it is to extract and separate the zinc acetate saturated solution to another reaction tank.
产量提高步骤：其是在碱式醋酸锌饱和溶液中添加冰醋酸，使其维持在酸碱值4.5～3.5之间，并加以搅拌使之进行后续反应，其反应式如下所示：Yield improvement step: it is to add glacial acetic acid in basic zinc acetate saturated solution, make it maintain between pH value 4.5～3.5, and be stirred to make it carry out follow-up reaction, and its reaction formula is as follows:
析出步骤：其是将添加冰醋酸后的醋酸锌饱和溶液持续搅拌并降温，使之成为醋酸锌的过饱和溶液以析出醋酸锌结晶。Precipitation step: continuously stirring the saturated zinc acetate solution after adding glacial acetic acid and lowering the temperature to make it a supersaturated solution of zinc acetate to precipitate zinc acetate crystals.
脱水步骤：其是将醋酸锌结晶与降温的醋酸锌饱和溶液加以固液分离，醋酸锌结晶经离心脱水成为醋酸锌结晶，而醋酸锌溶液则成为醋酸锌母液回收使用。Dehydration step: it is to separate the zinc acetate crystals from the cooled zinc acetate saturated solution for solid-liquid separation, the zinc acetate crystals are centrifuged and dehydrated to become zinc acetate crystals, and the zinc acetate solution becomes zinc acetate mother liquor for recycling.
另外，上述的回收醋酸锌母液在回收使用的场合时，是先经由纯化步骤以及分离步骤以将母液中的杂质加以去除，再经由上述的反应步骤、产量提高步骤、析出步骤及脱水步骤制造高纯度的醋酸锌。In addition, when the above-mentioned reclaimed zinc acetate mother liquor is reclaimed and used, the impurities in the mother liquor are removed through the purification step and the separation step, and then through the above-mentioned reaction step, yield improvement step, precipitation step and dehydration step. pure zinc acetate.
综上所述，本发明利用纯化步骤，使得杂质金属可加以还原而分离，并利用产量提高步骤可使得碱式醋酸锌离子继续反应成为醋酸锌，故可提高醋酸锌的产量。In summary, the present invention utilizes the purification step to reduce and separate impurity metals, and utilizes the yield improvement step to allow the basic zinc acetate ions to continue to react to become zinc acetate, so the yield of zinc acetate can be increased.
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| CN 200410038170 CN1696099A (en) | 2004-05-11 | 2004-05-11 | The preparation method of high-purity zinc acetate |
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| CN 200410038170 CN1696099A (en) | 2004-05-11 | 2004-05-11 | The preparation method of high-purity zinc acetate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649889A (en) * | 2015-02-09 | 2015-05-27 | 吉林市弗兰达科技股份有限公司 | Acetic acid raw material for producing metal acetate as well as preparation method and special equipment thereof |
| CN105408258A (en) * | 2013-07-16 | 2016-03-16 | 黑达乐格瑞菲工业有限公司 | Preparation and use of zinc compounds |
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- 2004-05-11 CN CN 200410038170 patent/CN1696099A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105408258A (en) * | 2013-07-16 | 2016-03-16 | 黑达乐格瑞菲工业有限公司 | Preparation and use of zinc compounds |
| CN104649889A (en) * | 2015-02-09 | 2015-05-27 | 吉林市弗兰达科技股份有限公司 | Acetic acid raw material for producing metal acetate as well as preparation method and special equipment thereof |
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