CN102020551A - Production process of superfine powdery nickel acetate - Google Patents
Production process of superfine powdery nickel acetate Download PDFInfo
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- CN102020551A CN102020551A CN2010106132311A CN201010613231A CN102020551A CN 102020551 A CN102020551 A CN 102020551A CN 2010106132311 A CN2010106132311 A CN 2010106132311A CN 201010613231 A CN201010613231 A CN 201010613231A CN 102020551 A CN102020551 A CN 102020551A
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- CN
- China
- Prior art keywords
- acetic acid
- glacial acetic
- nickelous acetate
- final stage
- nickel carbonate
- 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.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 title abstract 5
- 229940078494 nickel acetate Drugs 0.000 title abstract 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229960000583 acetic acid Drugs 0.000 claims abstract description 26
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims abstract description 17
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000004064 recycling Methods 0.000 claims abstract description 4
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical compound [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 3
- 230000002459 sustained effect Effects 0.000 claims description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 230000003407 synthetizing effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- SAEBCFDIJRQJQB-UHFFFAOYSA-N carbonic acid;nickel Chemical compound [Ni].OC(O)=O SAEBCFDIJRQJQB-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a production process of superfine powdery nickel acetate, which comprises the following steps of: synthetizing: reacting glacial acetic acid and basic nickel carbonate under agitation conditions by a molar ratio, adding the glacial acetic acid and the basic nickel carbonate in batch and continuously reacting until reaction is completed; dewatering: carrying out liquid-solid separation for synthetized nickel acetate, and recycling mother liquor; and drying to obtain the superfine powdery nickel acetate. Industrial first-grade glacial acetic acid with more than 99.5% content and the basic nickel carbonate in which the Ni content is from 18% to 20% are adopted as raw materials, and the reaction ratio, namely the molar ratio of the basic nickel carbonate to the glacial acetic acid is 1: 1.1-1.5. The invention has the advantages of simple production process, small environment pollution, high production efficiency, high primary recovery rate, no special requirement for production equipment, low work intensity and small process consumption. All process parameters are easy to control. The quality of the product is largely improved over that of the traditional nickel acetate powder on the market, and the quality is stable and reliable. Large-scale industrial production proves that the process has excellent repeatability.
Description
Technical field
The present invention relates to a kind of production technique of ultrafine powder final stage nickelous acetate.
Background technology
Nickelous acetate (Nicrel aceatate) is generally green crystallization formula powder, and according to general production technique production, formed product is in the majority with fine crystallization and powder.But growing along with science and technology, the application of nickelous acetate not only is confined to fabric mordant on the general industry, plating, face list processing and ceramic colour glaze etc., now also be applied to the plating of accuracy electroplate, high-end electronic material, so the specification of quality to acetic acid product is more and more higher, only the fine crystallization shape can not satisfy market demand.
The great advantage of ultrafine powder final stage nickelous acetate is, mixes with other material easily, mixes the back material and is evenly distributed.Some there is the production technique (as physical mixed) of particular requirement, in order to guarantee its uniform distributivity, need be broken in advance to crystalloid nickelous acetate, do like this and will bring a lot of shortcomings, the one, can increase production cost, the 2nd, particle size after cracking often can not reach processing requirement, and the 3rd, bigger process loss is arranged, also can bring environmental pollution.Therefore, production ultrafine powder final stage nickelous acetate just seems very important.
Nickelous acetate powder (granularity 100-200 order) can run into a lot of difficulties in process of production, mainly shows synthetic and dry link.The powder nickelous acetate is easy to caking, and the caking back can cause inside and outside humidity inhomogeneous when drying.Degree of drying is not enough, and the inner content of block is not enough, causes packing back secondary caking; Excessively dry, can cause surperficial dehydration, influence the solvability of product.Owing to do not solve these technological problemses well, and cause most in the market nickelous acetate unstable product quality.The invention of ultrafine powder final stage nickelous acetate (granularity 300-400 order) production technique solves these problems effectively, has increased substantially the quality of product.Have higher requirement, as the pH value of solution, generated time, drying mode, drying temperature etc.
Summary of the invention
The objective of the invention is to: propose a kind of novel process of producing nickelous acetate, the products obtained therefrom outward appearance is a ultrafine powder, and the common nickelous acetate powder of mass ratio is greatly improved, and production process is simple, and environmental pollution is little.
Technological process of the present invention is as follows: may further comprise the steps:
A), synthetic: glacial acetic acid and basic nickel carbonate are reacted under stirring condition in molar ratio, according to response situation, add glacial acetic acid and basic nickel carbonate in batches, sustained reaction is to reacting completely;
B), dehydration: will synthesize good nickelous acetate and carry out liquid-solid separation, Recycling Mother Solution is used;
C), drying makes.
Raw material selection content of the present invention is more than 99.5%, the basic nickel carbonate of the glacial acetic acid of industrial one-level and Ni content 19% ± 1%, and both reaction ratios are alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.1～1.5 in molar ratio.
Stir speed (S.S.) 80～85r/min in the technology of the present invention, control reaction temperature is no more than 40 ℃.
The present invention judges by the pH value of monitoring end reaction liquid whether reaction is complete, control pH=4.0 ± 0.1.
The present invention carries out liquid-solid separation by whizzer to synthetic good nickelous acetate.
The present invention's back nickelous acetate solid that will dewater carries out atomization drying, comes to determine the single dry amount greatly according to equipment, to reach optimum efficiency, controls 55～85 ℃ of inlet temperature, time of drying 20～30min.
Technology of the present invention possesses following advantage: the operational path that the present invention proposes a production ultrafine powder final stage nickelous acetate, production process is simple, each processing parameter is controlled easily, compare with traditional technology, environmental pollution is little, the production efficiency height, disposable rate of recovery height does not have particular requirement to production unit, labour intensity is low, process consumption is few, and products obtained therefrom is compared with existing nickelous acetate powder on the market, and quality greatly improves, and it is reliable and stable, prove that by large-scale industrial production process repeatability is fine, be worth promoting in the industry.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
Embodiment 1: the production process of ultrafine powder final stage nickelous acetate is described below:
1, synthetic: (content is more than 99.5% to add a certain amount of glacial acetic acid earlier in synthesis reaction vessel, the industry one-level), add basic nickel carbonate (Ni content 19% ± 1%) again, control alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰, 1.1～1.5(mol ratio), stir speed (S.S.) 80～85r/min is according to response situation, add glacial acetic acid and basic nickel carbonate in batches, sustained reaction to reacting completely, notices that control reaction temperature is no more than 40 ℃.PH value by monitoring end reaction liquid judges whether reaction is complete.Should control pH=4.0 ± 0.1, the pH value is too high, makes nickelous acetate emulsification easily, and the pH value is low excessively, and product is difficult for evenly dry.
2, dehydration: will synthesize good nickelous acetate and carry out liquid-solid separation by whizzer, Recycling Mother Solution is used.
3, drying: the back nickelous acetate solid that will dewater carries out atomization drying, comes to determine the single dry amount greatly according to equipment, to reach optimum efficiency.55～85 ℃ of inlet temperature of control, time of drying 20～30min.
Embodiment 2
Selected raw material glacial acetic acid (content 99.6%, industrial one-level), basic nickel carbonate (Ni content 19%), alkali formula carbonic acid nickel ︰ glacial acetic acid=1 ︰ 1.4(mol ratio), stir speed (S.S.) 80～85r/min, technological process and other processing parameter are identical with embodiment 1.
Embodiment 3:
Selected raw material glacial acetic acid (content 99.8%, industrial one-level), basic nickel carbonate (Ni content 20%), alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.3(mol ratio), stir speed (S.S.) 80～85r/min, temperature of reaction 30-40 ℃, technological process and other processing parameter are identical with embodiment 1.
Embodiment 4:
Selected raw material glacial acetic acid (content more than 99.6%, industrial one-level), basic nickel carbonate (Ni content 18%), alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.2(mol ratio), stir speed (S.S.) 80～85r/min, temperature of reaction 35-48 ℃, technological process and other processing parameter are identical with embodiment 1.
Embodiment 5:
Selected raw material glacial acetic acid (content more than 99.6%, industrial one-level), basic nickel carbonate (Ni content 18%), alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.5(mol ratio), stir speed (S.S.) 80～85r/min, temperature of reaction 30-40 ℃, technological process and other processing parameter are identical with embodiment 1.
Embodiment 6:
Selected raw material glacial acetic acid (content more than 99.6%, industrial one-level), basic nickel carbonate (Ni content 18%), alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.3(mol ratio), stir speed (S.S.) 80～85r/min, temperature of reaction 30-40 ℃, technological process and other processing parameter are identical with embodiment 1.
By the present invention, the quality standard such as the following table of prepared ultrafine powder final stage nickelous acetate:
Claims (6)
1. the production technique of a ultrafine powder final stage nickelous acetate is characterized in that: may further comprise the steps:
A), synthetic: glacial acetic acid and basic nickel carbonate are reacted under stirring condition in molar ratio, according to response situation, add glacial acetic acid and basic nickel carbonate in batches, sustained reaction is to reacting completely;
B), dehydration: will synthesize good nickelous acetate and carry out liquid-solid separation, Recycling Mother Solution is used;
C), drying makes.
2. ultrafine powder final stage nickelous acetate production technique according to claim 1, it is characterized in that: raw material selection content is more than 99.5%, the industry glacial acetic acid of one-level and the basic nickel carbonate of Ni content 19% ± 1%, both reaction ratios are alkali formula carbonic acid Nie ︰ glacial acetic acid=1 ︰ 1.1～1.5 in molar ratio.
3. the production technique of ultrafine powder final stage nickelous acetate according to claim 1 and 2 is characterized in that: stir speed (S.S.) 80～85r/min, control reaction temperature is no more than 40 ℃.
4. the production technique of ultrafine powder final stage nickelous acetate according to claim 1 and 2 is characterized in that: the pH value by monitoring end reaction liquid judges whether reaction is complete, control pH=4.0 ± 0.1.
5. the production technique of ultrafine powder final stage nickelous acetate according to claim 1 and 2 is characterized in that: will synthesize good nickelous acetate and carry out liquid-solid separation by whizzer.
6. the production technique of ultrafine powder final stage nickelous acetate according to claim 1 and 2, it is characterized in that: the back nickelous acetate solid that will dewater carries out atomization drying, comes to determine the single dry amount greatly according to equipment, to reach optimum efficiency, 55～85 ℃ of inlet temperature of control, time of drying 20～30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106132311A CN102020551A (en) | 2010-12-30 | 2010-12-30 | Production process of superfine powdery nickel acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106132311A CN102020551A (en) | 2010-12-30 | 2010-12-30 | Production process of superfine powdery nickel acetate |
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| Publication Number | Publication Date |
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| CN102020551A true CN102020551A (en) | 2011-04-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN2010106132311A Pending CN102020551A (en) | 2010-12-30 | 2010-12-30 | Production process of superfine powdery nickel 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 |
| CN110937990A (en) * | 2018-09-21 | 2020-03-31 | 荆门市格林美新材料有限公司 | Preparation method for continuously and efficiently preparing nickel acetate crystals |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1097604A1 (en) * | 1982-07-09 | 1984-06-15 | Уральский ордена Трудового Красного Знамени политехнический институт им.С.М.Кирова | Process for preparing acetates of bivalent nickel or cobalt |
| CN201678609U (en) * | 2010-02-09 | 2010-12-22 | 吉林市弗兰达科技股份有限公司 | Nickel acetate or cobalt production equipment with acetic acid recovery unit |
-
2010
- 2010-12-30 CN CN2010106132311A patent/CN102020551A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1097604A1 (en) * | 1982-07-09 | 1984-06-15 | Уральский ордена Трудового Красного Знамени политехнический институт им.С.М.Кирова | Process for preparing acetates of bivalent nickel or cobalt |
| CN201678609U (en) * | 2010-02-09 | 2010-12-22 | 吉林市弗兰达科技股份有限公司 | Nickel acetate or cobalt production equipment with acetic acid recovery unit |
Non-Patent Citations (1)
| Title |
|---|
| 段长强等: "《现代化学试剂手册》", 30 June 1988 * |
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 |
| CN110937990A (en) * | 2018-09-21 | 2020-03-31 | 荆门市格林美新材料有限公司 | Preparation method for continuously and efficiently preparing nickel acetate crystals |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20110420 |