CN1026226C - Preparation method of cuprous cyanide - Google Patents
Preparation method of cuprous cyanide Download PDFInfo
- Publication number
- CN1026226C CN1026226C CN 92105092 CN92105092A CN1026226C CN 1026226 C CN1026226 C CN 1026226C CN 92105092 CN92105092 CN 92105092 CN 92105092 A CN92105092 A CN 92105092A CN 1026226 C CN1026226 C CN 1026226C
- Authority
- CN
- China
- Prior art keywords
- sodium
- cuprous
- cyanide
- chlor
- cuprous cyanide
- 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.)
- Expired - Fee Related
Links
- DOBRDRYODQBAMW-UHFFFAOYSA-N copper(i) cyanide Chemical compound [Cu+].N#[C-] DOBRDRYODQBAMW-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 13
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 7
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229940045803 cuprous chloride Drugs 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000005554 pickling Methods 0.000 claims abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract 6
- 239000011780 sodium chloride Substances 0.000 claims abstract 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 8
- 150000003839 salts Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Abstract
The invention relates to a preparation process of cuprous cyanide. Mixing metallic copper, crystalline copper sulfate, sodium chloride and a proper amount of water together, reacting for 3-4 hours at the temperature of 80-120 ℃ to prepare cuprous salt, namely complex solution generated by cuprous chloride and sodium chloride, reacting with sodium cyanide at room temperature to generate cuprous cyanide precipitate, pickling, washing with water, and drying at the temperature of 110 ℃ to obtain pure white monoclinic cuprous cyanide. The invention has the advantages of simple equipment, short process flow, easy control, low cost and high product quality, and is suitable for large-scale industrial production.
Description
Cuprous cyanide is a kind of important chemical material.At present the traditional method of domestic production cuprous cyanide is to be the main raw material preparation with copper sulfate, S-WAT and sodium cyanide.Foreign patent RU62089, RO67960 have also reported the preparation method of cuprous cyanide, and main raw material is S-WAT, yellow soda ash, copper sulfate and sodium cyanide.Above-mentioned method technical process is long, and the reference mark is many in the actual production, the cost height, and the cuprous cyanide quality product of particularly producing is low and outward appearance is relatively poor.
The purpose of this invention is to provide a kind of technology of new generation cuprous cyanide, prepare the quality height, the cuprous cyanide product that outward appearance is good, and operation is few, and equipment is simple, and is with low cost.
The present invention is mainly by two step synthesis techniques.At first select metallic copper for use, cupric sulfate crystals and sodium-chlor reaction generate cuprous salt, promptly generate the complex solution of cuprous chloride and sodium-chlor, and this complex solution generates cuprous cyanide with the sodium cyanide reaction again.
The present invention selects metallic copper, cupric sulfate crystals and the sodium-chlor of technical grade for use, their weight ratio that feeds intake is 1-1.3: 1-1.3: 2-2.3, adding 10 times of water to the crystalline sulfuric acid weight of copper dissolves copper sulfate and sodium-chlor, heat 80-120 ℃, reacted 3-4 hour, the complex solution that obtains at room temperature reacts with sodium cyanide solution, generate the cuprous cyanide crystalline precipitation, through pickling (dilute hydrochloric acid of pH=2 or dilute sulphuric acid), be washed to neutrality, after the solid-liquid separation under 110 ℃ of temperature drying crystalline, promptly get purified cuprous cyanide.
The present invention is the complex solution and the reaction of sodium cyanide solution that degree Beaume is 10-20Be ' of the cuprous salt of 25-30Be ' with degree Beaume, the cuprous cyanide precipitation that generates is through a pickling (dilute hydrochloric acid of pH=2 or dilute sulphuric acid), wash four times to neutral, drying can obtain to contain the white monoclinic crystal powder of cuprous cyanide more than 99%.
The resulting product of the present invention identifies that by analysis every index all reaches ministerial standard.
Table 1 be product of the present invention with the mass ratio of produced in conventional processes cuprous cyanide.
Production process of the present invention is few, and equipment is simple, and the reference mark is few in the actual production operation, and raw material is easy to get, and is with low cost, and the quality product height is applicable to large-scale industrial production.
Substantial characteristics that the present invention gives prominence to and exploitativeness can be embodied from following embodiment.
Example 1:
In 3000 milliliters beaker, add 1800 ml waters, add 330 gram sodium-chlor again, 100 gram red copper bits and 170 grams contain the copper sulfate of five crystal water, heating, reaction is 4 hours under 110-120 ℃ of temperature, the complex solution (degree Beaume is 25Be ') that the cuprous chloride that obtains and sodium-chlor are generated is that the sodium cyanide solution of 10Be ' (20%) carries out replacement(metathesis)reaction to reacting completely with degree Beaume at room temperature, stir, the cuprous cyanide precipitation that generates is washed once with the dilute sulfuric acid aqueous solution of pH=2, wash four times then with water to neutral, solid-liquid separation, drying crystalline under 110 ℃ of temperature gets cuprous cyanide finished product 100 grams.
Example 2:
The water that in the enamel still of 2,000 liters, adds 1.7 tons, add 0.33 ton of sodium cyanide, add 0.14 ton of red copper bits and 0.17 ton of cupric sulfate crystals again, steam heating, reaction is 3 hours under 110-120 ℃ of temperature, the complex compound (degree Beaume is 30Be ') that the cuprous chloride that obtains and sodium-chlor are generated is transferred in the enamel still of another 2,000 liter then, at room temperature drip the sodium cyanide solution that degree Beaume is 12Be ', be stirred to and react completely, the white precipitate that generates is washed once with the dilute sulfuric acid aqueous solution of pH=2, washed four times again to neutral, solid-liquid separation, dry under 110 ℃ of temperature, get 1 ton of cuprous cyanide product.
Table 1:
Yang Zhuan Shanghai, Tianjin Tao Pu
Test event the present invention
Chemical plant, sub-chemical plant
CuCN（%，≥） 99.05 98 98.5
CN
-（%，≥） 28.72 28.4 28.5
Fe（%，≤） 0.005 0.03 0.01
Cl
-（%，≤） 0.01 0.05 0.05
Na
2CO
3（%，≤） 0.08 0.4 0.4
The pure white greyish white Huang of outward appearance is greyish white
Claims (2)
1, a kind of is the method that main raw material prepares cuprous cyanide with copper sulfate and sodium cyanide, it is characterized in that metallic copper, cupric sulfate crystals and the sodium-chlor of technical grade are put together, adding weight is to decuple the water of cupric sulfate crystals with cupric sulfate crystals and sodium-chlor dissolving, heat 80-120 ℃, reacted 3-hour, the complex solution that cuprous chloride that makes and sodium-chlor generate at room temperature generates the cuprous chloride precipitation with the sodium chloride aqueous solution reaction, to precipitate pickling, be washed to neutrality, solid-liquid separation, drying crystalline under 110 ℃ of temperature promptly gets the cuprous cyanide product; The weight ratio of metallic copper, cupric sulfate crystals and sodium-chlor is 1-1.3: 1-1.3: 2-2.3; The complex solution that cuprous chloride and sodium-chlor generate is 5-6: 2-4 with the ratio of the degree Beaume of sodium cyanide solution.
2,, it is characterized in that said pickling is to use diluted hydrochloric acid aqueous solution or the dilute sulfuric acid aqueous solution of pH=2 according to the said method for preparing cuprous cyanide of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92105092 CN1026226C (en) | 1992-06-27 | 1992-06-27 | Preparation method of cuprous cyanide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92105092 CN1026226C (en) | 1992-06-27 | 1992-06-27 | Preparation method of cuprous cyanide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1066636A CN1066636A (en) | 1992-12-02 |
| CN1026226C true CN1026226C (en) | 1994-10-19 |
Family
ID=4941176
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92105092 Expired - Fee Related CN1026226C (en) | 1992-06-27 | 1992-06-27 | Preparation method of cuprous cyanide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1026226C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211088A (en) * | 2014-09-10 | 2014-12-17 | 杭州青化社化工有限公司 | Preparation method of cuprous cyanide |
| CN107758694A (en) * | 2017-09-30 | 2018-03-06 | 杭州青化社化工有限公司 | A kind of high-purity cuprous cyanide environment-friendly type preparation method |
| CN107758693A (en) * | 2017-09-30 | 2018-03-06 | 杭州青化社化工有限公司 | A kind of method that cuprous cyanide is prepared using high cyanide containing wastewater |
| CN111392944A (en) * | 2020-03-24 | 2020-07-10 | 宁波神化特种化学品集成有限公司 | Treatment method of cuprous cyanide production wastewater |
| CN111392747A (en) * | 2020-03-24 | 2020-07-10 | 宁波神化特种化学品集成有限公司 | Preparation method of cuprous cyanide |
-
1992
- 1992-06-27 CN CN 92105092 patent/CN1026226C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1066636A (en) | 1992-12-02 |
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