CN1245142A - Process for preparing potassium ferrocyanide - Google Patents
Process for preparing potassium ferrocyanide Download PDFInfo
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- CN1245142A CN1245142A CN 99112416 CN99112416A CN1245142A CN 1245142 A CN1245142 A CN 1245142A CN 99112416 CN99112416 CN 99112416 CN 99112416 A CN99112416 A CN 99112416A CN 1245142 A CN1245142 A CN 1245142A
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- CN
- China
- Prior art keywords
- ferrocyanide
- potassium
- reaction
- potassium ferrocyanide
- sodium
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- 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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- 239000000276 potassium ferrocyanide Substances 0.000 title claims abstract description 62
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000000047 product Substances 0.000 claims abstract description 26
- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000264 sodium ferrocyanide Substances 0.000 claims abstract description 25
- 235000012247 sodium ferrocyanide Nutrition 0.000 claims abstract description 25
- 239000001103 potassium chloride Substances 0.000 claims abstract description 24
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- NYRAVIYBIHCEGB-UHFFFAOYSA-N [K].[Ca] Chemical compound [K].[Ca] NYRAVIYBIHCEGB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000279 calcium ferrocyanide Substances 0.000 claims abstract description 11
- 235000012251 calcium ferrocyanide Nutrition 0.000 claims abstract description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 20
- 239000012452 mother liquor Substances 0.000 claims description 19
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 230000002950 deficient Effects 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010517 secondary reaction Methods 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract 1
- 238000011426 transformation method Methods 0.000 abstract 1
- 229960002816 potassium chloride Drugs 0.000 description 20
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 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 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Removal Of Specific Substances (AREA)
Abstract
A process for preparing potassium ferrocyanide includes the reaction of sodium ferrocyanide on potassium chloride in mole ratio of 1.1-1.2 to obtain the coarse potassium ferrocyanide, adding potassium chloride (10-20 wt.%), and reaction to obtain finished product with high content of potassium ferrocyanide 98.5% or more. The mother liquid resulted from the first reaction is treated by potassium calcium ferrocyanide transformation method to recover potassium ferrocyanide and return it back to the second reactor. The mother liquid in the second reactor is directly returned back to the first reactor. Its advantages are high output rate up to over 95%, by-products of sodium chloride and calcium carbonate, and no waste liquid discharge.
Description
The invention relates to a production process of potassium ferrocyanide, in particular to a production process for preparing potassium ferrocyanide by using sodium ferrocyanide.
The potassium ferrocyanide is mainly used for manufacturing pigments, printing and dyeing oxidation auxiliaries, paints, printing ink, potassium ferrocyanide, explosives and chemical reagents, and is also used for steel heat treatment, lithography, carving and pharmaceutical industry. As food additive, it is mainly used as anticaking agent for salt.
The method for industrially producing potassium ferrocyanide in China comprises the following steps: the cyanide smelting method, the sodium cyanide method, the sodium ferrocyanide conversion method, the potassium cyanide method, the method for preparing the cyanide sludge by using the waste gas purifying agent and the cyanide-containing waste water recovery method. Although the method is different in China, the method is basically a potassium calcium ferrocyanide conversion method, and the method has long flow, waste time and waste chemical industry. The method for converting sodium ferrocyanide and potassium chloride directly needs to add a large amount of potassium chloride in the reaction process, generally more than twice of the theoretical amount, and the crystallized potassium ferrocyanide contains 20% of sodium ferrocyanide. The process conditions are difficult to control, and the high-purity potassium ferrocyanide product is difficult to obtain. And the product yield is low, the production cost is high, and the method has larger wastewater discharge and pollutes the environment.
The invention aims to provide a process for producing potassium ferrocyanide, which has the advantages of simple process, low production cost, high product purity and high yield.
The production process for preparing potassium ferrocyanide from sodium ferrocyanide provided by the invention is a preferred method with low cost. The invention has the important characteristic that the finished product of the high-purity potassium ferrocyanide can be obtained by reacting sodium ferrocyanide with potassiumchloride twice.
In the first reaction, a solution of 60-70% (by weight) sodium ferrocyanide is added with a slight excess of solid potassium chloride and the reaction is carried out at 90-95 ℃. The addition amount of the potassium chloride is 1.1 to 1.2 times of the sodium ferrocyanide in terms of molar ratio. After the reaction is completed, removing impurities by decoloring and filtering, cooling the filtrate to 10 ℃, crystallizing and separating out potassium ferrocyanide, and performing centrifugal separation to obtain a primary product potassium ferrocyanide and a primary mother solution. In this case, the defective potassium ferrocyanide product obtained contains about 20% of sodium ferrocyanide. The primary mother liquor mainly contains potassium ferrocyanide, partial excessive potassium chloride, a small amount of unreacted sodium ferrocyanide and sodium chloride produced in the primary reaction.
Then, the first-time product potassium ferrocyanide is prepared into a potassium ferrocyanide solution with the concentration of 70-80% (weight percent), solid potassium chloride is added for secondary reaction, the reaction temperature is 90-95 ℃, and the addition amount of the potassium chloride is equivalent to 10-20% of the weight of the potassium ferrocyanide. The potassium chloride added at this time can make the sodium ferrocyanide remained in the primary product potassium ferrocyanide quickly react to produce potassium ferrocyanide. After the reaction is completed, filtering to remove impurities, cooling the filtrate to 10 ℃, crystallizing to separate out potassium ferrocyanide, and carrying out centrifugal separation to obtain a potassium ferrocyanide finished product with the content of more than 98.5 percent and secondary mother liquor. The product quality meets the requirements of GB3448-82 standard (see Table 1).
TABLE-analysis of potassium ferrocyanide products
| Item | GB-3448-82 First grade standard | The product |
| Potassium ferrocyanide content K4Fe(N)6.3H2O％≥ | 98.5 | 98.7 |
| Chloride (Cl)% > is less than or equal to | 0.4 | 0.01 |
| The water insoluble substance content is less than or equal to | 0.03 | 0.008 |
The other important characteristic of the invention is that the mother liquor separated in the two reactions is returned and used as the proportioning liquid respectively. The secondary mother liquor mainly contains a small amount of potassium ferrocyanide, excessive potassium chloride and a small amount of sodium chloride generated in the secondary reaction. Therefore, the secondary mother liquor is directly returned to the primary reactor for preparing the solution of the sodium ferrocyanide.
The primary mother liquor discharged from the primary reaction mainly contains potassium ferrocyanide, a small amount of unreacted sodium ferrocyanide, a part of excess potassium chloride and a large amount of sodium chloride generated in the primary reaction. The primary mother liquor is treated as follows: the calculated amount of calcium chloride was added to the primary mother liquor, calculated as the saturation of the potassium ferrocyanide solution at 10 ℃. The reaction is carried out at 30-40 ℃, and the potassium ferrocyanide and the sodium ferrocyanide in the mother liquor are subjected to the following precipitation reaction:
filtering and separating to obtain potassium calcium ferrocyanide and sodium chloride solution. Since this is a precipitation reaction, little ferrocyanide remains in solution at this point. And because potassium chloride is added in a little excess amount in one reaction, the residual potassium chloride in the mother liquor is less, and the residual amount of potassium chloride in the mother liquor is further reduced through the precipitation reaction. Therefore, the sodium chloride crystals recovered after the filtrate is evaporated in vacuum and cooled for crystallization contain only a small amount of potassium chloride, the content of potassium chloride is less than 5%, and the recovered sodium chloride can be used for industrial water softening treatment. The cooling water evaporated in vacuum and the residual mother liquid after recovering sodium chloride can be returned to the primary reactor for preparing the sodium ferrocyanide solution.
Adding 2-3 times of water into the filter cake of potassium calcium ferrocyanide to prepare a suspension with the concentration of 30% (weight), adding a reaction amount of sodium carbonate, and carrying out decalcification reaction at 70-80 ℃. Separating calcium carbonate precipitate to obtain filtrate, i.e. solution containing potassium ferrocyanide and sodium ferrocyanide, returning it into secondary reactor for preparing primary product potassium ferrocyanide reaction liquor and making secondary reaction. The filtered calcium carbonate can be further processed into light calcium carbonate for recycling.
The invention will be further described with reference to fig. 1.
FIG. 1 is a schematic flow chart of the production process of the invention.
In FIG. 1, 1 is a reaction for preparing potassium ferrocyanide. A60-70% (weight%) sodium ferrocyanide solution is added with solid potassium chloride with a molar ratio of 1.1-1.2 times to carry out a primary reaction. The reaction liquid is sent to 2 for first impurity separation, and 3 is a first mother liquid obtained by centrifugal separation of potassium ferrocyanide precipitated by first cooling crystallization and sent to 7 for further treatment. The obtained defective potassium ferrocyanide product is sent to a reactor 4, and 70-80% (weight percent) of potassium ferrocyanide solution is prepared to be added with solid potassium chloride for secondary reaction. 5 is the second impurity separation, 6 is the second cooling crystallization, obtains the finished product of potassium ferrocyanide through centrifugal separation, and the secondary mother liquor that is separated is sent back to 1 andis used for preparing the sodium ferrocyanide solution.
3, feeding the primary mother liquor separated out from the step 7, adding calcium chloride to prepare potassium calcium ferrocyanide, 8, separating the potassium calcium ferrocyanide, feeding the separated filtrate to a step 12 for further sodium chloride recovery, and feeding the separated potassium calcium ferrocyanide to a step 9 for decalcification reaction. The decalcified reaction solution is filtered and separated by 10, the separated precipitate is sent to 13 for recycling calcium carbonate, the filtrate 11 mainly contains potassium ferrocyanide and sodium ferrocyanide, and then the solution is returned to 4 for preparing a primary product of potassium ferrocyanide solution.
By using the present invention, 850kg of potassium ferrocyanide, 470kg of sodium chloride and 100kg of calcium carbonate can be obtained by using 1000kg of sodium ferrocyanide, and the yield of potassium ferrocyanide is more than 95%.
The invention has the obvious advantages that the potassium ferrocyanide is prepared by two reactions, and the mother liquor is treated by a potassium calcium ferrocyanide conversion method, so that the mother liquor in the two reactions is completely recycled, the yield of the potassium ferrocyanide is improved, and the yield of the potassium ferrocyanide is up to more than 95%. The invention can obtain high-quality potassium ferrocyanide with the content of more than 98.5 percent. And two valuable products such as sodium chloride, calcium carbonate and the like can be obtained at the same time. Not only reduces the consumption of raw materials and the cost of products, but also reduces the discharge of waste and reduces the environmental pollution. The method has the advantages of low cost, simple equipment, low investment cost and obvious economic and social benefits.
The invention is further illustrated by the following example.
1500t of water is added into a reaction kettle, 900kg of sodium ferrocyanide and 700kg of potassium chloride are added, the temperature is raised to 90 ℃, the filtration is carried out after the reaction is completed, the filtrate is cooled to 10 ℃, and 580kg of defective potassium ferrocyanide product is generated. And adding 1000t of water and the 580kg of potassium ferrocyanide defective product into a reaction kettle, adding 100kg of potassium chloride, filtering out impurities after complete reaction, and cooling the filtrate to 10 ℃ again to obtain 300kg of finished product potassium ferrocyanide. The product contains K4Fe(CN)6.3H298.5 percent of O, less than 0.05 percent of chloride and less than 0.01 percent of water insoluble matter. Conforms to the GB3448-82 standard. 170kg of sodium chloride crystals can be recovered after the primary mother liquor is treated.
Claims (6)
1. A method for producing potassium ferrocyanide is characterized in that:
(a) adding solid potassium chloride with the molar ratio of 1.1-1.2 times into 60-70% (weight%) sodium ferrocyanide solution for primary reaction, decoloring and filtering, cooling and crystallizing filtrate to separate out potassium ferrocyanide, and centrifugally separating to obtain potassium ferrocyanide first defective product and primary mother liquor;
(b) preparing a primary product of potassium ferrocyanide into a solution with the concentration of 70-80% (weight percent), adding solid potassium chloride which is 10-20% (weight parts) of potassium ferrocyanide to perform secondary reaction, filtering and separating impurities, cooling and crystallizing the filtrate to separate out potassium ferrocyanide, and performing centrifugal separation to obtain a potassium ferrocyanide finished product and a secondary mother solution;
(c) adding calcium chloride into the primary mother liquor to perform a conversion reaction of potassium calcium ferrocyanide, and filtering and separating to obtain potassium calcium ferrocyanide and a sodium chloride solution;
(d) adding 2-3 times of water into potassium calcium ferrocyanide to prepare suspension with the concentration of 30% (weight percent), adding sodium carbonate to perform decalcification reaction, separating calcium carbonate precipitate, and obtaining filtrate which is solution containing potassium ferrocyanide and sodium ferrocyanide.
2. The process according to claim 1, wherein the reaction temperature in steps a and b is 90 to 95 ℃ and the crystallization temperature of potassium ferrocyanide is 10 ℃.
3. The process according to claim 1, wherein the secondary mother liquor separated in operation b is returned to operation a for preparing a sodium ferrocyanide solution.
4. The method according to claim 1, wherein the filtrate from the decalcification in step d is returned to step b for preparing a defective solution of potassium ferrocyanide.
5. The process according to claim 1, wherein the reaction temperature for converting potassium ferrocyanide in the operation step c is 30-40 ℃.
6. The process according to claim 1, wherein the decalcification reaction temperature in the operation step d is 70 to 80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99112416A CN1079079C (en) | 1999-09-01 | 1999-09-01 | Process for preparing potassium ferrocyanide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99112416A CN1079079C (en) | 1999-09-01 | 1999-09-01 | Process for preparing potassium ferrocyanide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1245142A true CN1245142A (en) | 2000-02-23 |
| CN1079079C CN1079079C (en) | 2002-02-13 |
Family
ID=5275727
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99112416A Expired - Fee Related CN1079079C (en) | 1999-09-01 | 1999-09-01 | Process for preparing potassium ferrocyanide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1079079C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115739A (en) * | 2016-06-29 | 2016-11-16 | 晋城市鸿生化工有限公司 | A kind of production method of yellow sodium prussiate |
| CN108285155A (en) * | 2018-03-13 | 2018-07-17 | 苏州富博宏新材料科技有限公司 | A kind of process for cleanly preparing of potassium ferrocyanide |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO70366A3 (en) * | 1977-02-01 | 1982-02-01 | Institutul De Chimie,Ro | PROCESS FOR THE PREPARATION OF POTASSIUM FERROCYANIDE |
| RO71681A2 (en) * | 1977-10-04 | 1982-10-26 | Intreprinderea Chimica,Ro | PROCESS FOR OBTAINING POTASSIUM FERTILION |
| CN1018525B (en) * | 1985-08-21 | 1992-10-07 | 福里尼迪·布里格里尔公司 | Grinding method and device for carrying out said method |
| CN1012728B (en) * | 1988-03-18 | 1991-06-05 | 丁以钿 | Process for producing potassium ferrocyanide by ion exchange method |
-
1999
- 1999-09-01 CN CN99112416A patent/CN1079079C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115739A (en) * | 2016-06-29 | 2016-11-16 | 晋城市鸿生化工有限公司 | A kind of production method of yellow sodium prussiate |
| CN108285155A (en) * | 2018-03-13 | 2018-07-17 | 苏州富博宏新材料科技有限公司 | A kind of process for cleanly preparing of potassium ferrocyanide |
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| Publication number | Publication date |
|---|---|
| CN1079079C (en) | 2002-02-13 |
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