CN102485650A - Preparation method for nickel borate - Google Patents
Preparation method for nickel borate Download PDFInfo
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- CN102485650A CN102485650A CN2010105754191A CN201010575419A CN102485650A CN 102485650 A CN102485650 A CN 102485650A CN 2010105754191 A CN2010105754191 A CN 2010105754191A CN 201010575419 A CN201010575419 A CN 201010575419A CN 102485650 A CN102485650 A CN 102485650A
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- trihydroxyborane
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Abstract
The invention discloses a green synthetic method for nickel orthoborate. According to the method, nickel salt and boric acid are put in a mortar and mixed with water to form paste, the paste is then subjected to roasting at a certain temperature for a certain period of time after full grinding and drying, and a product of nickel orthoborate is directly obtained after a reaction is finished. The preparation method provided in the invention has the advantages of a low synthesis temperature, a simple process, cheap and easily available raw materials, good repeatability, high reaction yield, a short period of reaction time, no need for any organic solvent, safe operation, greenness, environmental friendliness and easy industrial production.
Description
Technical field
The invention belongs to technical field of inorganic material, what be specifically related to is to be the process method of feedstock production nickelous borate with nickel salt and boric acid.
Background technology
Borate cpd has the abundant structures type, is widely used as nonlinear optical material and laser, luminous host material.Moreover, nickelous borate also is applied in the other field, as joins and make the additive for improving tribological property in the lubricating oil, can in lithium cell, substitute the 3d-MOX as anode material, and nickelous borate also has magnetic and catalytic performance.Particularly Trihydroxyborane nickel has good magnetic and antiwear and friction reduction property, and the production of Trihydroxyborane nickel is had very important significance.
The compound method of existing Trihydroxyborane nickel mainly contains following several kinds: (1) high temperature solid-state method: with NiO or Ni (OH)
2And B
2O
3Synthetic Trihydroxyborane nickel under 1200 ℃ or 1100 ℃, this method temperature is too high, if want to reduce temperature of reaction, generally needs to add solubility promoter, is not suitable for industrial production.(J.Pardo, M.Martinez-Ripoll, S.Garc í a-Blanco.Acta Crystallog., 1974, B30:37-40; H.Effenberger, F.Pertlik.Zeitschrift f ü r Kristallographie, 1984; 166:129-140.) (2) reverse micelle method: adopt the synthetic precursor of nickelous nitrate and Peng Qinghuana and multiple organic raw material, obtain Trihydroxyborane nickel 800 ℃ of following roastings then, though this kind method temperature decreases; But the preparation process is complicated; Need many organic solvents, raw materials cost is high, is unfavorable for environmental protection.(Menaka, S.E.Lofland, K.V.Ramanujachary; A.K.Ganguli, J.Organomet.Chem., 2010; 695 (7): 1002-1005) (3) coprecipitation method: post precipitation is 55 ℃ of dryings in the aqueous solution to adopt nickelous chloride, borax and boric acid, and 800 ℃ of following roastings several days, this method was simple then; But required time is oversize, lacks commercial competitiveness.(A.Débart，B.Revel，L.Dupont，L.Montagne，J.B.Leriche，M.Touboul，and?J.M.Tarascon.Chem.Mater.，2003，15(19)：3683-3691)
Summary of the invention
The green synthesis method that the purpose of this invention is to provide a kind of Trihydroxyborane nickel, this method technological process is simple, reaction yield is high, the time is short, cost is low, do not have by product, and products obtained therefrom purity is high.
The present invention realizes through following technical measures:
A kind of synthesis technique of Trihydroxyborane nickel is characterized in that: 1) nickel salt and boric acid are put into mortar, Ni in the nickel salt
2+With BO in the boric acid
3 3-Mol ratio be 1: 0.66～0.8; 2) add water furnishing pasty state, the amount of water is 0～3 times of Trihydroxyborane nickel theoretical yield; 3) behind the abundant mill-drying, the crucible of packing into is placed in the retort furnace, temperature programming, and 700 ℃～800 ℃ following roasting for some time, cooling obtains Trihydroxyborane nickel product.The XRD spectra of this product is consistent with the standard spectrogram of Trihydroxyborane nickel, and utilizes ir spectra and UV spectrum to prove that further the conclusion of XRD is correct, and the product that obtains from above analysis explanation this patent is purified Trihydroxyborane nickel.
Described nickel salt is meant basic nickel carbonate, nickelous oxalate, nickelous nitrate, acetylacetonate nickel or nickel acetate.The productive rate of said product is all more than 95%, some in addition can reach 100%.
Described temperature programming is meant that specifically temperature rise rate is 5 ℃/min～60 ℃/min, can directly rise to 700 ℃～800 ℃, and insulation 3～8h also can temperature-gradient method, rises to a certain lesser temps earlier, insulation for some time, rises to temperature required again.The type of cooling can adopt naturally cooling, also can adopt the programmed cooling type of cooling.
Compared with prior art, adopt technical scheme of the present invention can reach following effect:
Preparing method's technological process of the present invention is simple, and raw material is cheap and easy to get, good reproducibility, and reaction yield high (can reach 100%), time weak point, temperature is low, without any need for organic solvent, operational safety, environmental protection is fit to industrial production.
Description of drawings: accompanying drawing 1 is the contrast of the XRD spectra and the standard spectrogram (JCPDS 75-1809) of the embodiment of the invention 1 products obtained therefrom.
Embodiment:
Embodiment 1
Take by weighing basic nickel carbonate 13.93g, boric acid 4.50g, wherein n (Ni
2+): n (BO
3 3-) be 1: 0.67, basic nickel carbonate and boric acid are put into mortar, fully grind, need 1～2h approximately.Mixture is transferred in the crucible, is placed in the retort furnace, 12 ℃/min of temperature rise rate, rise to 700 ℃ of insulation 3h after, close retort furnace, make furnace body temperature naturally cool to room temperature, open fire door, take out crucible, promptly obtain Trihydroxyborane nickel.The XRD spectra of this product and standard spectrogram (JCPDS 75-1809) (seeing accompanying drawing 1) in full accord can explain that what obtain is purified Trihydroxyborane nickel.
Embodiment 2
Take by weighing nickelous oxalate 14.93g, boric acid 3.54g, wherein n (Ni
2+): n (BO
3 3-) be 1: 0.7, nickelous oxalate and boric acid are put into mortar, add entry while grinding, the furnishing pasty state needs 8mL water approximately, and abundant the grinding powders and drying until mashed prod, needs 1～2h (time of grinding is according to adding how much confirming of the water yield).Mixture is transferred in the crucible, is placed in the retort furnace, 12 ℃/min of temperature rise rate, rise to 800 ℃ of insulation 3h after, close retort furnace, open fire door, treat that furnace body temperature reduces to below 100 ℃, take out crucible, after the cooling, promptly obtain Trihydroxyborane nickel fully.(JCPDS 75-1809) is in full accord for the XRD spectra of this product and standard spectrogram, can explain that what obtain is purified Trihydroxyborane nickel.
Embodiment 3
Take by weighing nickelous oxalate 14.93g, boric acid 3.71g, wherein n (Ni
2+): n (BO
3 3-) be 1: 0.73, nickelous oxalate and boric acid are put into mortar, add entry while grinding, the furnishing pasty state needs 12mL water approximately, fully grinds, and powders and drying until mashed prod, needs 1～2h.Mixture is transferred in the crucible, is placed in the retort furnace, 15 ℃/min of temperature rise rate, rise to 800 ℃ of insulation 8h after, reduce to room temperature with 5 ℃/min, take out crucible, promptly obtain Trihydroxyborane nickel.(JCPDS 75-1809) is in full accord for the XRD spectra of this product and standard spectrogram, can explain that what obtain is purified Trihydroxyborane nickel.
Claims (3)
1. the preparation method of Trihydroxyborane nickel comprises the following steps:
1) nickel salt and boric acid are put into mortar, Ni in the nickel salt
2+With B0 in the boric acid
3 3-Mol ratio be 1: 0.66～0.8;
2) add water furnishing pasty state, the amount of water is 0～3 times of Trihydroxyborane nickel theoretical yield;
3) behind the abundant mill-drying, the crucible of packing into is placed in the retort furnace, temperature programming, and 700 ℃～800 ℃ following roasting for some time, cooling obtains Trihydroxyborane nickel product.
2. the synthesis technique of Trihydroxyborane nickel according to claim 1 is characterized in that: described nickel salt is basic nickel carbonate, nickelous oxalate, nickelous nitrate, acetylacetonate nickel or nickel acetate.
3. the synthesis technique of Trihydroxyborane nickel according to claim 1; It is characterized in that: temperature programming is meant that specifically temperature rise rate is 5 ℃/min～60 ℃/min, can directly rise to 700 ℃～800 ℃, insulation 3～8h; Also can temperature-gradient method; Rise to a certain lesser temps earlier, insulation for some time, rise to temperature required again; The type of cooling can adopt naturally cooling, also can adopt the programmed cooling type of cooling.
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| CN2010105754191A CN102485650A (en) | 2010-12-02 | 2010-12-02 | Preparation method for nickel borate |
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| CN2010105754191A CN102485650A (en) | 2010-12-02 | 2010-12-02 | Preparation method for nickel borate |
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| CN102485650A true CN102485650A (en) | 2012-06-06 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626198A (en) * | 2013-11-25 | 2014-03-12 | 哈尔滨理工大学 | Method for synthesizing nickel borate |
| CN104477931A (en) * | 2014-12-16 | 2015-04-01 | 中国科学院青海盐湖研究所 | Preparation method of nano nickel borate crystal |
| CN107681141A (en) * | 2017-09-26 | 2018-02-09 | 福建师范大学 | A kind of anode material of lithium-ion battery of carbon coating boric acid nanosized nickel rods |
| CN109574030A (en) * | 2018-11-30 | 2019-04-05 | 陕西学前师范学院 | It is a kind of to prepare Zn3B7O13The method of X |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845668A (en) * | 2010-02-07 | 2010-09-29 | 浙江工业大学 | Method for preparing nano nickel borate whiskers |
-
2010
- 2010-12-02 CN CN2010105754191A patent/CN102485650A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845668A (en) * | 2010-02-07 | 2010-09-29 | 浙江工业大学 | Method for preparing nano nickel borate whiskers |
Non-Patent Citations (3)
| Title |
|---|
| MENAKA ET AL.: "A new low temperature methodology to obtain pure nanocrystalline nickel borate", 《JOURNAL OF ORGANOMETALLIC CHEMISTRY》 * |
| 娄方等: "纳米硼酸镍的制备、表征及其在水溶液中的摩擦学性能", 《材料导报》 * |
| 郑学家等: "《硼化合物生产与应用》", 31 January 2008 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626198A (en) * | 2013-11-25 | 2014-03-12 | 哈尔滨理工大学 | Method for synthesizing nickel borate |
| CN103626198B (en) * | 2013-11-25 | 2016-01-20 | 哈尔滨理工大学 | A kind of synthetic method of nickelous borate |
| CN104477931A (en) * | 2014-12-16 | 2015-04-01 | 中国科学院青海盐湖研究所 | Preparation method of nano nickel borate crystal |
| CN107681141A (en) * | 2017-09-26 | 2018-02-09 | 福建师范大学 | A kind of anode material of lithium-ion battery of carbon coating boric acid nanosized nickel rods |
| CN109574030A (en) * | 2018-11-30 | 2019-04-05 | 陕西学前师范学院 | It is a kind of to prepare Zn3B7O13The method of X |
| CN109574030B (en) * | 2018-11-30 | 2022-01-04 | 陕西学前师范学院 | Preparation of Zn3B7O13Method of X |
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Application publication date: 20120606 |