CN100412049C - Method for production of potassium diformate - Google Patents
Method for production of potassium diformate Download PDFInfo
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- CN100412049C CN100412049C CNB2006100437697A CN200610043769A CN100412049C CN 100412049 C CN100412049 C CN 100412049C CN B2006100437697 A CNB2006100437697 A CN B2006100437697A CN 200610043769 A CN200610043769 A CN 200610043769A CN 100412049 C CN100412049 C CN 100412049C
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Abstract
The present invention discloses a method for producing potassium diformate. In the method, formic acid and potassium oxide are used as raw materials; firstly, the aminic acid solution with a percentage concentration of 80 to 99% reacts with a matched equivalent weight of solid potassium oxide for 1 to 6 hours at a temperature of 20 to 90 DEG C; then the temperature of the obtained reaction solution is lowered to below a room temperature of 25 DEG C to precipitate crystals; the potassium diformate is obtained after centrifugal separation and drying. Because the formic acid solution directly reacts with the solid potassium oxide, and the raw materials only contain more than 80% of formic acid solution and less than 20% of water, from the whole reaction course, water consumption is little; the obtained solution after the reaction need not be condensed by reducing pressure and can be directly separated and dried to reduce energy consumption.
Description
Technical field
The present invention relates to a kind of method of producing Potassium hydrogen diformate.
Background technology
Potassium hydrogen diformate is that calendar year 2001 BASF releases a kind of novel microbiotic growth promoter surrogate product, and intestinal bacteria, Salmonellas etc. are had good effect.In the same year, as first kind of non-antibiotic fodder additives, in Swine Production, played antibiotic effect by European Union's approval.Use the feed that adds Potassium hydrogen diformate can save the cost of raising pigs, improve the healthy state of pig and can improve the sanitary conditions on farm.Because European Union forbids to use microbiotic in animal-feed, this new additive agent that can replace the microbiotic effect will have enormous and latent market.
The Chinese Ministry of Agriculture ratified Potassium hydrogen diformate and was used for pig feed as a kind of novel fodder additive on March 22nd, 2005.This will quicken the further popularization of this novel, green, high efficiency products.
Chinese patent on December 7th, 2005 also disclosed a kind of among the CN1704394A be the technology of feedstock production Potassium hydrogen diformate by aqueous formic acid and salt of wormwood or potassium hydroxide aqueous solution, the shortcoming of this technology is that water consumption is big, need concentrating under reduced pressure, the energy consumption height increases production cost.
Summary of the invention
Technical problem to be solved by this invention is: the method that the production Potassium hydrogen diformate that a kind of water consumption is few, energy consumption is low and the purity of Potassium hydrogen diformate is high is provided.
For solving the problems of the technologies described above, technical scheme of the present invention is: the method for producing Potassium hydrogen diformate, with formic acid and potassium oxide is raw material, at first be that 80～99% formic acid solution and solid oxidation potassium were 20～90 ℃ of reactions 1～6 hour with mass percent concentration, the mol ratio of described formic acid and potassium oxide is 4～6: 1, then the reaction soln that obtains is cooled to the room temperature that is lower than 25 ℃ and separates out crystal, after centrifugation, drying, obtain Potassium hydrogen diformate.
As preferred embodiment, the mass percent concentration of formic acid solution is 85～95%;
As preferred embodiment, potassium oxide solid purity is 〉=98%;
The present invention adopts formic acid solution and solid oxidation potassium direct reaction.Has only in the raw material and contain water in the formic acid solution, and the concentration of formic acid solution is more than 80%, thus the water content in the formic acid below 20%, from entire reaction course, its water consumption is few.The solution that obtains after the reaction need not concentrating under reduced pressure, just can directly separate and drying, has reduced energy consumption.In reaction process, formic acid and potassium oxide direct reaction generate Potassium hydrogen diformate and water, and the formic acid solution of high density and highly purified potassium oxide have guaranteed the high purity of Potassium hydrogen diformate, and through detecting, the purity of Potassium hydrogen diformate is more than 98%, and its fusing point is 100～110 ℃.
Embodiment
Embodiment 1: with purity is that 99% 470kg potassium oxide pressed powder is put in the reactor that has whipping appts, at ambient temperature, slowly add the 1100kg mass percent concentration while stirring and be 85% formic acid solution, the reinforced time was with 2 hours, temperature of reaction is controlled at about 40 ℃, behind reinforced the finishing, keep about 40 ℃ of temperature and continue stirring 4 hours; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1210kg Potassium hydrogen diformate finished product 75 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.5%, and the yield of whole process is 93.1%, fusing point: 104～109 ℃.
Embodiment 2: at ambient temperature, with mass percent concentration is that 85% formic acid solution 1100kg puts in the reactor that has whipping appts, be that 99% 470kg potassium oxide pressed powder slowly joins in the reactor then with purity, the reinforced time was with about 1.5 hours, temperature of reaction is controlled at about 40 ℃, behind reinforced the finishing, keep about 40 ℃ of temperature and continue stirring 4 hours; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1200kg Potassium hydrogen diformate finished product 75 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.5%, and the yield of whole process is 92.3%, fusing point: 103.5～108.5 ℃.
Embodiment 3: with purity is that 99% 470kg potassium oxide pressed powder is put in the reactor that has whipping appts, at ambient temperature, slowly add 1100kg, mass percent concentration while stirring and be 85% formic acid solution, the reinforced time was with 40 minutes, temperature of reaction is controlled at about 80 ℃, behind reinforced the finishing, keep about 80 ℃ of temperature and continue stirring 1 hour; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1203kg Potassium hydrogen diformate finished product 75 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.2%, and the yield of whole process is 92.5%, fusing point: 102.5～107.5 ℃.
Embodiment 4: at ambient temperature, with mass percent concentration is that 85% formic acid solution 1100kg puts in the reactor that has whipping appts, be that 99% 470kg potassium oxide solid powder joins in the reactor while stirring then with purity, the reinforced 30 minutes time, temperature of reaction is controlled at about 80 ℃, behind reinforced the finishing, keep about 80 ℃ of temperature and continue stirring 1 hour; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1206kg Potassium hydrogen diformate finished product 55 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.7%, and the yield of whole process is 92.8%, fusing point: 102～107 ℃.
Embodiment 5: with purity is that 99% 470kg potassium oxide pressed powder is put in the reactor that has whipping appts, at ambient temperature, slowly add 985kg, mass percent concentration while stirring and be 95% formic acid solution, the reinforced time was with 2 hours, temperature of reaction is controlled at about 60 ℃, behind reinforced the finishing, keep about 60 ℃ of temperature and continue stirring 2 hours; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1230kg Potassium hydrogen diformate finished product 55 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.5%, and the yield of whole process is 94.6%, fusing point: 103～108 ℃.
Embodiment 6: at ambient temperature, with mass percent concentration is that 85% formic acid solution 1100kg puts in the reactor that has whipping appts, be that 99% 470kg potassium oxide pressed powder joins in the reactor while stirring then with purity, the reinforced 2 hours time, temperature of reaction is controlled at about 60 ℃, behind reinforced the finishing, keep about 60 ℃ of temperature and continue stirring 2 hours; Then reaction soln is reduced to room temperature (20～25 ℃), separate out white, needle-shaped crystals, isolate the Potassium hydrogen diformate crystal, obtain 1225kg Potassium hydrogen diformate finished product 55 ℃ of dryings by whizzer.
The purity that detects Potassium hydrogen diformate through HPLC is 98.7%, and the yield of whole process is 94.2%, fusing point: 104～109 ℃.
The present invention is not limited to the foregoing description, experimental results show that repeatedly, as long as with the formic acid solution of high density and highly purified potassium oxide solid according to molar weight 4～6: 1 ratio (theoretical value is 4: 1) mixes, make it reaction, separate out crystal, centrifugation and drying step through cooling then and just can obtain highly purified Potassium hydrogen diformate finished product.The most significant effect is water saving in reaction process, but (potassium hydroxide with 60% replaces potassium oxide to feed intake to produce 1000kg Potassium hydrogen diformate water saving 305kg, reaction yield is 94%), the solution that obtains after the reaction need not concentrating under reduced pressure, just can directly separate and drying, reduce energy consumption.
Claims (5)
1. produce the method for Potassium hydrogen diformate, it is characterized in that: with formic acid and potassium oxide is raw material, at first be that 80～99% formic acid solution and solid oxidation potassium were 20～90 ℃ of reactions 1～6 hour with mass percent concentration, the mol ratio of described formic acid and potassium oxide is 4～6: 1, then the reaction soln that obtains is cooled to the room temperature that is lower than 25 ℃ and separates out crystal, after centrifugation, drying, obtain Potassium hydrogen diformate.
2. the method for production Potassium hydrogen diformate as claimed in claim 1 is characterized in that: the mass percent concentration of described formic acid solution is 85～95%.
3. the method for production Potassium hydrogen diformate as claimed in claim 1 or 2 is characterized in that: described potassium oxide solid purity 〉=98%.
4. the method for production Potassium hydrogen diformate as claimed in claim 1 is characterized in that: the temperature of reaction of described formic acid solution and potassium oxide is 30～60 ℃.
5. the method for production Potassium hydrogen diformate as claimed in claim 1 is characterized in that: the temperature of described drying step is 40～90 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100437697A CN100412049C (en) | 2006-04-26 | 2006-04-26 | Method for production of potassium diformate |
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| CNB2006100437697A CN100412049C (en) | 2006-04-26 | 2006-04-26 | Method for production of potassium diformate |
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| CN1844074A CN1844074A (en) | 2006-10-11 |
| CN100412049C true CN100412049C (en) | 2008-08-20 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125809B (en) * | 2007-07-31 | 2010-05-19 | 厦门大学 | Solvent-free heating-free method for synthesizing potassium diformate |
| CN110642703A (en) * | 2019-09-18 | 2020-01-03 | 山东凯米科环保科技有限公司 | Method for producing potassium diformate |
| CN113754529B (en) * | 2021-08-31 | 2024-05-10 | 潍坊加易加生物科技有限公司 | Method for preparing potassium diformate and sodium diformate by using organic carboxylic acid potassium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1187807A (en) * | 1995-05-12 | 1998-07-15 | 诺尔斯海德公司 | Method for manufacture of products containing disalts of formic acid |
| CN1428325A (en) * | 2001-12-27 | 2003-07-09 | 徐林坤 | Production method of potassium diformate |
| CN1452882A (en) * | 2003-05-23 | 2003-11-05 | 黄逸强 | Feed additive |
| CN1704394A (en) * | 2004-05-26 | 2005-12-07 | 北京挑战农业科技有限公司 | Method for production of potassium diformate |
-
2006
- 2006-04-26 CN CNB2006100437697A patent/CN100412049C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1187807A (en) * | 1995-05-12 | 1998-07-15 | 诺尔斯海德公司 | Method for manufacture of products containing disalts of formic acid |
| CN1428325A (en) * | 2001-12-27 | 2003-07-09 | 徐林坤 | Production method of potassium diformate |
| CN1452882A (en) * | 2003-05-23 | 2003-11-05 | 黄逸强 | Feed additive |
| CN1704394A (en) * | 2004-05-26 | 2005-12-07 | 北京挑战农业科技有限公司 | Method for production of potassium diformate |
Non-Patent Citations (2)
| Title |
|---|
| 二甲酸钾的合成. 梁平，石波.中国畜牧兽医，第31卷第2期. 2004 |
| 二甲酸钾的合成. 梁平，石波.中国畜牧兽医，第31卷第2期. 2004 * |
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| CN1844074A (en) | 2006-10-11 |
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Effective date of registration: 20160323 Address after: 262737 Shandong city of Weifang province Lingang Industrial Park, Binhai Economic Development Zone, Binhai Avenue No. 0199 Patentee after: SHANDONG SUNWIN BIOTECHNOLOGY CO., LTD. Address before: 261061 Shandong city of Weifang province high tech Development Zone East Road sail business in Hong Kong, room 701 Patentee before: Sunwin Chemicals Co., Ltd. |