CN107162037A - It is a kind of while preparing the method for cuprous oxide and nickel chloride - Google Patents
It is a kind of while preparing the method for cuprous oxide and nickel chloride Download PDFInfo
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- CN107162037A CN107162037A CN201710470780.XA CN201710470780A CN107162037A CN 107162037 A CN107162037 A CN 107162037A CN 201710470780 A CN201710470780 A CN 201710470780A CN 107162037 A CN107162037 A CN 107162037A
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- Prior art keywords
- nickel
- cuprous oxide
- chloride
- hydrochloric acid
- acid solution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/08—Halides
- C01G53/09—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of while preparing the method for cuprous oxide and nickel chloride, it is characterised in that obtain cuprous oxide and nickel chloride with the reaction of stannous chloride hydrochloric acid solution in the presence of the compound of acid-soluble nickel by reducing agent of copper powder.The preparation method of the present invention is simple to operate, it is easy to control, and product purity is high, and greatly reduces liquid phase reduction and prepare the cost of cuprous oxide and solve the problem of chloride emission.
Description
Technical field
Cuprous oxide and chlorination are prepared the present invention relates to a kind of preparation method of metal oxide, more particularly to one kind simultaneously
The method of nickel.
Background technology
Cuprous oxide（Cu2O）Powder is a kind of Inorganic Chemicals, is widely used in anti-fouling ship paint, glass porcelain glaze and
Toner, organic catalyst compound, agriculture chemicals fungicide and electronic material etc..As a kind of p-type semiconductor material, cuprous oxide exists
Good application prospect is shown in fields such as solar cell, hydrogen storage battery, lithium ion battery, photocatalysis.Nickel chloride is extensive
For electroplating, breathing mask ammonia absorbent, also serve as catalyst and nickel compound.At present, nickel chloride mainly uses liquid phase method
Prepare.
At present, preparing cuprous oxide mainly has solid phase method, electrolysis and liquid phase reduction, and solid phase method is by copper powder and oxidation
Copper is mixed, and 800-9000C is heated in calcining furnace and is sintered into cuprous oxide, then crushes finished product is made.Electrolysis is with casting
Copper coin is anode, and copper plate is negative electrode, and potassium chromate is additive, and sodium chloride is made up of electrolyte.Liquid phase method mainly has glucose
Reducing process, hydrazine reducing process, sulfite reduction method, copper reduction method etc..Liquid phase reduction prepare cuprous oxide compared to solid phase method and
The advantages of electrolysis, its product purity height, good dispersion, size tunable, be the main method for preparing cuprous oxide at present.
Chinese invention patent 90105244.2 is disclosed a kind of makees reducing agent in the presence of sodium chloride also using sodium sulfite
The method that former cupric sulfate pentahydrate prepares cuprous oxide.Chinese invention patent 201010119206.8 discloses a kind of cuprous oxide
Preparation method, metallic copper or reducing agent are carried out reaction and prepare oxygen by it with sodium chloride and copper-containing compound under 30-2000C
Change cuprous.Chinese invention patent 201510013497.5 discloses a kind of method that cuprous oxide is prepared under copper chloride system,
It uses the copper chloride of printed substrate restored acid etching waste liquor for copper source, and sulphite and alkali metal chloride are reduction
Agent, cuprous oxide is prepared in the presence of alkali and inert gas.Chinese invention patent 201610201276.5 discloses one kind
The preparation method of purple cuprous oxide, it uses copper for reducing agent, in surfactant, sodium hydroxide or potassium hydroxide or ammoniacal liquor
In the presence of, cuprous oxide is prepared into mantoquita reduction.Chinese invention patent 201610345864.6 discloses a kind of cuprous oxide
Environment-friendly preparation method thereof, this method is by solvent of alkylamine, particle-stabilised dose and reducing agent, using ultrasonic technique be prepared for oxidation
It is cuprous.Chinese invention patent 201410337558.9 disclose it is a kind of using carried out after nickelous carbonate and hydrochloric acid reaction concentration prepare it is excellent
The preparation method of the pure nickel chloride of level.These prepare the method for cuprous oxide using various types of mantoquitas as copper source, using difference
Reducing agent can prepare cuprous oxide, however, anion and reducing agent or additive formation in the mantoquita used
Product such as chloride, sulfate etc. are discharged by modes such as filtering, washings, cause environmental pollution, and processing cost is high.Using printing
Copper chloride in circuit board etching waste liquor is copper source, and cost is low, how not to cause chloride dirty while cuprous oxide is prepared
Dye thing is the problem of present invention endeavours solution.
The content of the invention
The problem of to exist more than solving, the present invention proposes a kind of while preparing the method for cuprous oxide and nickel chloride, should
Method has cost low, and product purity is high and without chloride emission pollution problem.
To achieve the above object, the present invention prepares cuprous oxide simultaneously and the preparation method of nickel chloride is：By stannous chloride
Hydrochloric acid solution and copper powder mixing, are heated to 80-1000C, add nickelous carbonate or nickel hydroxide, react 0.5-8h under agitation
Afterwards, filter, the sediment of filtering is dried to obtain cuprous oxide under vacuum drying oven or inert gas shielding, filtrate passes through heating
Condensing crystallizing obtains nickel chloride crystal.Wherein, in nickel salt in the mole of nickel and stannous chloride hydrochloric acid solution chlorine mole it
Than for 1：2, the mol ratio of copper powder and stannous chloride is 1：1.
The pH value of described copper chloride hydrochloric acid solution is between 1-5, pH value is less than 1, then with more hydrochloric acid, more than 5
Then copper chloride facile hydrolysis is precipitated into Kocide SD；
The content of copper chloride is 0.1-2mol/L in described copper chloride hydrochloric acid solution, and less than 0.1mol/L, yield is too low, is higher than
2mol/L, the then cuprous oxide particle generated is too small, it is difficult to filter, and easily adsorbing chlorinated nickel and cause purity to reduce.
Described heating-up temperature is 80-1000C, less than 800C, it is impossible to obtain copper oxidule precipitation, and aqueous temperature is not yet
Can be above the boiling point 1000C；
The described reaction time is 0.5-8h, and less than 0.5h, then partial oxidation copper and copper unreacted completely, can exist in nickel chloride
Substantial amounts of copper and purity is relatively low, higher than 8h, then cuprous oxide particle diameter is big and is easily oxidized to cupric oxide, in addition, energy consumption is also higher.
The preparation method of the present invention is simple to operate, it is easy to control, cuprous oxide yield>98.5%, Nickel dichloride hexahydrate crystal
Yield>98%, product purity is high, greatly reduces liquid phase reduction and prepares the cost of cuprous oxide and solve chloride row
The problem put.
Embodiment
Embodiment 1：By the stannous chloride hydrochloric acid solution 100ml of 0.1mol/L pH=5, copper powder 0.6355g is added, under stirring
1000C is heated to, nickelous carbonate 1.18g is added, 0.5h is reacted, filtering is deposited in vacuum drying under 600C and obtains cuprous oxide（Contain
Amount 98.5%）, filtrate condensing crystallizing under 1000C obtains Nickel dichloride hexahydrate crystal（Content 98%）.
Embodiment 2：By the stannous chloride hydrochloric acid solution 100ml of 2mol/L pH=1, copper powder 12.71g is added, stirring is lower to be added
Heat adds nickel hydroxide 19g to 800C, reacts 8h, and filtering is deposited in vacuum drying under 600C and obtains cuprous oxide（Content
98.7%）, filtrate condensing crystallizing under 1000C obtains Nickel dichloride hexahydrate crystal（Content 99.1%）.
Embodiment 3：By the stannous chloride hydrochloric acid solution 100ml of 1mol/L pH=3, copper powder 6.355g is added, stirring is lower to be added
Heat adds nickelous carbonate 9.5g to 1000C, reacts 6h, and filtering is deposited in vacuum drying under 600C and obtains cuprous oxide（Content
99.1%）, filtrate condensing crystallizing under 1000C obtains Nickel dichloride hexahydrate crystal（Content 98.7%）.
Embodiment 4：By the stannous chloride hydrochloric acid solution 100ml of 0.5mol/L pH=4, copper powder 3.1775g is added, under stirring
1000C is heated to, nickelous carbonate 4.75g is added, 3h is reacted, filtering is deposited in vacuum drying under 600C and obtains cuprous oxide（Content
99.5%）, filtrate condensing crystallizing under 1000C obtains Nickel dichloride hexahydrate crystal（Content 98.3%）.
Claims (3)
1. a kind of while preparing the method for cuprous oxide and nickel chloride, it is characterised in that using copper powder be reducing agent acid-soluble
Cuprous oxide and nickel chloride are obtained with the reaction of stannous chloride hydrochloric acid solution in the presence of the compound of nickel, is concretely comprised the following steps：By chlorination
Cuprous hydrochloric acid solution and copper powder mixing, is heated to 80-100 under agitation0C, adds acid-soluble nickel compound, reaction
After 0.5-8h, the sediment of filtering is dried to obtain cuprous oxide by filtering under vacuum drying oven or inert gas shielding, and filtrate is led to
Cross heating condensing crystallizing and obtain Nickel dichloride hexahydrate crystal；Wherein, in nickel salt in the mole of nickel and stannous chloride hydrochloric acid solution
The ratio between mole of chlorine is 1：2, the mol ratio of copper powder and stannous chloride is 1：1.
2. it is a kind of while preparing the method for cuprous oxide and nickel chloride described in claim 1, it is characterised in that described chlorination
The pH value of cuprous hydrochloric acid solution is 1-5.
3. it is a kind of while preparing the method for cuprous oxide and nickel chloride described in claim 1, it is characterised in that described chlorination
The content of stannous chloride is 0.1-2mol/L in cuprous hydrochloric acid solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710470780.XA CN107162037A (en) | 2017-06-20 | 2017-06-20 | It is a kind of while preparing the method for cuprous oxide and nickel chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710470780.XA CN107162037A (en) | 2017-06-20 | 2017-06-20 | It is a kind of while preparing the method for cuprous oxide and nickel chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107162037A true CN107162037A (en) | 2017-09-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710470780.XA Pending CN107162037A (en) | 2017-06-20 | 2017-06-20 | It is a kind of while preparing the method for cuprous oxide and nickel chloride |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190327A (en) * | 2010-03-08 | 2011-09-21 | 沈祖达 | Cuprous oxide preparation method |
| CN103993173A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method for removing chlorine from nickel cobalt hydroxide |
| CN104760988A (en) * | 2015-03-11 | 2015-07-08 | 白晓光 | Environmental-protective preparation method of Cu2O and CuCl |
-
2017
- 2017-06-20 CN CN201710470780.XA patent/CN107162037A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190327A (en) * | 2010-03-08 | 2011-09-21 | 沈祖达 | Cuprous oxide preparation method |
| CN103993173A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method for removing chlorine from nickel cobalt hydroxide |
| CN104760988A (en) * | 2015-03-11 | 2015-07-08 | 白晓光 | Environmental-protective preparation method of Cu2O and CuCl |
Non-Patent Citations (2)
| Title |
|---|
| 于冰等编: "《非金属材料大全》", 31 August 1997, 中国物资出版社 * |
| 舒万艮编: "《有色金属精细化工产品生产与应用》", 31 December 1995, 中南工业大学出版社 * |
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Application publication date: 20170915 |
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| RJ01 | Rejection of invention patent application after publication |