CN104355983A - Crystallization method of coarse particle nickel acetate - Google Patents
Crystallization method of coarse particle nickel acetate Download PDFInfo
- Publication number
- CN104355983A CN104355983A CN201410550869.3A CN201410550869A CN104355983A CN 104355983 A CN104355983 A CN 104355983A CN 201410550869 A CN201410550869 A CN 201410550869A CN 104355983 A CN104355983 A CN 104355983A
- Authority
- CN
- China
- Prior art keywords
- nickel acetate
- crystallization method
- solution
- coarse particles
- crystal
- 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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- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229940078494 nickel acetate Drugs 0.000 title claims abstract description 53
- 238000002425 crystallisation Methods 0.000 title claims abstract description 18
- 239000011362 coarse particle Substances 0.000 title claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 229960000583 acetic acid Drugs 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 4
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 claims description 2
- 230000003381 solubilizing effect Effects 0.000 claims description 2
- 239000006200 vaporizer Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 11
- 239000000428 dust Substances 0.000 abstract description 4
- 230000009323 psychological health Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000010413 mother solution Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical compound [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002889 sympathetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a crystallization method of coarse particle nickel acetate. A nickel acetate crystal obtained through evaporating and condensing of a nickel acetate solution, adding of glacial acetic acid to regulate pH, cooling and crystalizing is regular in crystal form, as well as coarse, large and uniform in particles, and the crystal with the length between 0.5-1.0mm accounts for more than 75%. The process is simple and reliable, and is strong in operability. The nickel acetate product produced through the process is coarse and large in particle, dust pollution is avoided in the use process, and the physical and psychological health of an operator is not jeopardized.
Description
Technical field
The invention belongs to nickel acetate crystallization technique field, be specifically related to a kind of crystallization method of coarse particles shape nickel acetate.
Background technology
Nickel acetate (another name nickelous acetate) is organo-nickel compounds, and molecular formula is C
4h
6o
4ni4H
2o or Ni (CH
3cOO)
24H
2o, blue-greenish colour monoclinic crystal or powder, tool water absorbability.There is acetic acid smell, be heated to fusing point and decompose, soluble in water, ethanol and ammoniacal liquor.Nickel acetate is widely used in the industrial production, is mainly used as catalyzer, produces the encapsulant of aluminium alloy extrusions, the siccative of paint, print and dye agent, glass reinforced plastic curing catalyst and sympathetic ink etc.Now also be applied to the plating etc. of accuracy electroplate, high-end electronic material.
At present, domestic most enterprise is with nickel hydroxide or basic nickel carbonate and the direct composite powder powder of Glacial acetic acid or fine particulate nickel acetate crystal, but there is following shortcoming in this method: 1) Powdered or fine particulate nickel acetate at production and use procedure dust pollution seriously, has very large harm to the respiratory system of operator; 2) synthesize liquid directly cool after because of degree of supersaturation lower, nickel acetate percent crystallization in massecuite is low, and production efficiency is low.
Summary of the invention
Technical problem to be solved by this invention is the crystallization method overcoming deficiency of the prior art and provide a kind of coarse particles shape nickel acetate, adopt the method can obtain the nickel acetate crystal that crystal growth is good, particle length is 0.5-1.5mm, solve Powdered or fine particulate nickel acetate at the dust pollution question produced and exist in use procedure simultaneously.
Following technical scheme is adopted for solving technical problem of the present invention:
A crystallization method for coarse particles shape nickel acetate, comprises the following steps:
A). solution preparation: basic nickel carbonate being added to mass concentration is in the acetum of 15%-20%, under normal temperature, abundant solubilizing reaction obtains that pH is 3.8-4.2, proportion is the nickel acetate solution of 1.06 ~ 1.08; The nickel acetate solution chemical constitution of preparation: Ni:40 ~ 50g/L, Co≤0.002g/L, Cu≤0.002g/L, Fe≤0.002g/L, Pb≤0.002g/L, Zn≤0.002g/L, Mn≤0.002g/L, Cd≤0.002g/L, Ca≤0.5g/L, Mg≤0.5g/L, Na≤0.5g/L, SO
4 2-:≤5.0g/L.
B). evaporation concentration: step a nickel acetate solution is concentrated into proportion 1.13-1.17 at vaporizer;
C). regulate pH: step a concentrated solution is delivered to crystallizer tank, start stir, add Glacial acetic acid regulate pH be 3.4-3.6, be heated to 80-90 DEG C, then 80-90 DEG C insulation 40-50 minute as clear as crystal to concentrated solution;
D). crystallisation by cooling: made by step c concentrated solution temperature slowly be down to 22 DEG C-24 DEG C from 80-90 DEG C in 10-12 hour, then at 22 DEG C-24 DEG C insulation 10-12 hour;
E). centrifugation: use whizzer by the centrifugation of steps d magma, be the finished product after the drying of gained crystal, mother liquor returns nickel acetate synthesis procedure.
Described step b) mixing speed is 22-24r/min.
Described steps d) falling temperature gradient is 5.5-6.5 DEG C/h.
Described step e) in centrifuge be separated time rotating speed be 500-700r/min.
The principle of nickel acetate solution evaporation concentration, interpolation acetum tune pH, crystallisation by cooling coarse particles shape nickel acetate is by the present invention: by nickel acetate solution evaporation concentration, make its degree of supersaturation in Metastable zone, then add Glacial acetic acid, nickel acetate crystal is separated out when lower pH; In sufficiently long crystallization time, falling temperature gradient is less, and solution degree of supersaturation is lower, and crystal growth rate is greater than nucleus generating rate, thus obtains coarse particles shape nickel acetate crystal.
The crystallization method of coarse particles shape nickel acetate of the present invention, by nickel acetate synthesis liquid evaporation concentration, to add acetum adjusts pH, the method for crystallisation by cooling obtains nickel acetate crystal habit rule, particle thick and even, and particle length is that 0.5-1.5mm(particle length accounts for more than 75% between the crystal of 0.5-1.0mm).Present invention process is simple, reliable, workable.Not only particle is thick to use the nickel acetate product of present invention process output, and use procedure no dust pollution, can not endanger the physical and mental health of operator.
Embodiment
Below by specific embodiment, treatment process of the present invention is described further:
embodiment 1
Under normal temperature condition, be 5.0m by 1.0 tons of basic nickel carbonates and volume number
3, mass concentration be 15% the acetic acid synthesized nickel of acetum, filter, output pH4.2, proportion are the nickel acetate solution of 1.06; Get 5.0m
3it is deliver to crystallizer tank after 1.15 that synthetic nickel acetate solution is concentrated into proportion, and start and stir, mixing speed is 23r/min, adds Glacial acetic acid and adjusts concentrated solution pH 3.5, be incubated 50 minutes (80 DEG C); Then with the gradient cooling to 23 DEG C of 5.5 DEG C/h, 12 hours are incubated; Namely obtain after slurry centrifugation (centrifuge speed: 600r/min), drying particle length be 0.5-1.5mm(wherein length account for 77% between the crystal of 0.5-1.0mm) nickel acetate product, crystalline mother solution then returns nickel acetate synthesis procedure.
embodiment 2
Under normal temperature condition, be 5.0m by 1.0 tons of basic nickel carbonates and volume number
3, mass concentration be 18% the acetic acid synthesized nickel of acetum, filter, output pH4.0, proportion are the nickel acetate solution of 1.08; Get 5.0m
3it is deliver to crystallizer tank after 1.13 that synthetic nickel acetate solution is concentrated into proportion, and start and stir, mixing speed is 22r/min, adds Glacial acetic acid and adjusts concentrated solution pH3.6, be incubated 40 minutes (90 DEG C); Then with the gradient cooling to 22 DEG C of 6.5 DEG C/h, 10 hours are incubated; Slurry namely obtain after centrifugation (centrifuge speed: 700r/min), drying again particle length be 0.5-1.5mm(wherein length account for 75% between the crystal of 0.5-1.0mm) nickel acetate product, crystalline mother solution then returns nickel acetate synthesis procedure.
embodiment 3
Under normal temperature condition, be 5.0m by 1.0 tons of basic nickel carbonates and volume number
3, mass concentration be 20% the acetic acid synthesized nickel of acetum, filter, output pH3.8, proportion are the nickel acetate solution of 1.07; Get 5.0m
3it is deliver to crystallizer tank after 1.17 that synthetic nickel acetate solution is concentrated into proportion, and start and stir, mixing speed is 24r/min, adds Glacial acetic acid and adjusts concentrated solution pH3.4, be incubated 46 minutes (85 DEG C); Then with the gradient cooling to 24 DEG C of 6.0 DEG C/h, 11 hours are incubated; Slurry namely obtain after centrifugation (centrifuge speed: 500r/min), drying again particle length be 0.5-1.5mm(wherein length account for 83% between the crystal of 0.5-1.0mm) nickel acetate product, crystalline mother solution then returns nickel acetate synthesis procedure.
embodiment 4
Under normal temperature condition, be 5.0m by 1.0 tons of basic nickel carbonates and volume number
3, mass concentration be 17% the acetic acid synthesized nickel of acetum, filter, output pH4.0, proportion are the nickel acetate solution of 1.07; Get 5.0m
3it is deliver to crystallizer tank after 1.16 that synthetic nickel acetate solution is concentrated into proportion, and start and stir, mixing speed is 23r/min, adds Glacial acetic acid and adjusts concentrated solution pH 3.5, be incubated 45 minutes (83 DEG C); Then with the gradient cooling to 22 DEG C of 5.5 DEG C/h, 12 hours are incubated; Slurry namely obtain after centrifugation (centrifuge speed: 600r/min), drying again particle length be 0.5-1.5mm(wherein length account for 81% between the crystal of 0.5-1.0mm) nickel acetate product, crystalline mother solution then returns nickel acetate synthesis procedure.
Claims (4)
1. a crystallization method for coarse particles shape nickel acetate, is characterized in that comprising the following steps:
A). solution preparation: basic nickel carbonate being added to mass concentration is in the acetum of 15%-20%, under normal temperature, abundant solubilizing reaction obtains that pH is 3.8-4.2, proportion is the nickel acetate solution of 1.06 ~ 1.08;
B). evaporation concentration: step a nickel acetate solution is concentrated into proportion 1.13-1.17 at vaporizer;
C). regulate pH: step a concentrated solution is delivered to crystallizer tank, start stir, add Glacial acetic acid regulate pH be 3.4-3.6, be heated to 80-90 DEG C, then 80-90 DEG C insulation 40-50 minute as clear as crystal to concentrated solution;
D). crystallisation by cooling: made by step c concentrated solution temperature slowly be down to 22 DEG C-24 DEG C from 80-90 DEG C in 10-12 hour, then at 22 DEG C-24 DEG C insulation 10-12 hour;
E). centrifugation: use whizzer by the centrifugation of steps d magma, be the finished product after the drying of gained crystal, mother liquor returns nickel acetate synthesis procedure.
2. the crystallization method of a kind of coarse particles shape nickel acetate as claimed in claim 1, is characterized in that: described step b) mixing speed is 22-24r/min.
3. the crystallization method of a kind of coarse particles shape nickel acetate as claimed in claim 1, is characterized in that: described steps d) falling temperature gradient is 5.5-6.5 DEG C/h.
4. the crystallization method of a kind of coarse particles shape nickel acetate as claimed in claim 1, is characterized in that: described step e) in centrifuge when being separated rotating speed be 500-700r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550869.3A CN104355983B (en) | 2014-10-17 | 2014-10-17 | A kind of method for crystallising of coarse granule shape nickel acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550869.3A CN104355983B (en) | 2014-10-17 | 2014-10-17 | A kind of method for crystallising of coarse granule shape nickel acetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104355983A true CN104355983A (en) | 2015-02-18 |
| CN104355983B CN104355983B (en) | 2016-10-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410550869.3A Active CN104355983B (en) | 2014-10-17 | 2014-10-17 | A kind of method for crystallising of coarse granule shape nickel acetate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860811A (en) * | 2015-04-23 | 2015-08-26 | 江西核工业兴中科技有限公司 | Coarse particle nickel acetate and preparation method thereof |
| CN106565459A (en) * | 2016-11-01 | 2017-04-19 | 沧州锐星化学科技有限公司 | Preparation method of battery grade nickel acetate |
| 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 |
|---|---|---|---|---|
| CN102020550A (en) * | 2010-12-30 | 2011-04-20 | 江西核工业兴中科技有限公司 | Production process of coarse particle nickel acetate |
| CN103467272B (en) * | 2013-08-09 | 2014-10-15 | 吉林市弗兰达科技股份有限公司 | Rapid energy-saving and emission-reduction production method for high purity large particle nickel acetate |
-
2014
- 2014-10-17 CN CN201410550869.3A patent/CN104355983B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020550A (en) * | 2010-12-30 | 2011-04-20 | 江西核工业兴中科技有限公司 | Production process of coarse particle nickel acetate |
| CN103467272B (en) * | 2013-08-09 | 2014-10-15 | 吉林市弗兰达科技股份有限公司 | Rapid energy-saving and emission-reduction production method for high purity large particle nickel acetate |
Non-Patent Citations (1)
| Title |
|---|
| 张庆等: "粗颗粒乙酸镍的研制", 《东华理工大学学报（自然科学版）》, vol. 34, no. 4, 31 December 2011 (2011-12-31), pages 389 - 391 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860811A (en) * | 2015-04-23 | 2015-08-26 | 江西核工业兴中科技有限公司 | Coarse particle nickel acetate and preparation method thereof |
| CN104860811B (en) * | 2015-04-23 | 2018-05-01 | 江西核工业兴中新材料有限公司 | Coarse particle nickel acetate and preparation method thereof |
| CN106565459A (en) * | 2016-11-01 | 2017-04-19 | 沧州锐星化学科技有限公司 | Preparation method of battery grade nickel acetate |
| 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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| Publication number | Publication date |
|---|---|
| CN104355983B (en) | 2016-10-05 |
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| CB03 | Change of inventor or designer information |
Inventor after: Xing Xiaozhong Inventor after: Dong Cunwu Inventor after: Li Baoping Inventor after: Ye Jianming Inventor after: Meng Maoyong Inventor after: Zhang Guoyong Inventor after: Sun Zhengde Inventor before: Dong Cunwu Inventor before: Li Baoping Inventor before: Xing Xiaozhong Inventor before: Ye Jianming Inventor before: Meng Maoyong Inventor before: Zhang Guoyong Inventor before: Sun Zhengde |
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Effective date of registration: 20240223 Address after: 737100 No.1 Lanzhou Road, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Salt Co.,Ltd. Country or region after: China Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |