CN101423231A - Purification method of solid cyanamide - Google Patents
Purification method of solid cyanamide Download PDFInfo
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- CN101423231A CN101423231A CNA2008102338106A CN200810233810A CN101423231A CN 101423231 A CN101423231 A CN 101423231A CN A2008102338106 A CNA2008102338106 A CN A2008102338106A CN 200810233810 A CN200810233810 A CN 200810233810A CN 101423231 A CN101423231 A CN 101423231A
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- cyanamide
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- temperature
- solid cyanamide
- purification
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Abstract
The invention relates to a purification method of solid cyanamide, and the purification process is as follows: the solid cyanamide to be purified is added in a container which contains an organic solvent and is provided with a stirring device under the stirring state, the temperature is kept at the temperature of 20-40 DEG C, the solid cyanamide is filtered after full dissolution, filtrate is put in a container with cooling and stirring devices, the stirring is continuously carried out simultaneously when decreasing the temperature, when the temperature is decreased to minus 10-5 DEG C, the stirring is carried out for 20-60 minutes, then cyanamide crystals are filtered out, a finished product is obtained after drying, and the filtrate is recycled, and one part of solid cyanamide is dissolved in 0.2-1.5 parts of organic solvent. The purification method solves the problem of instability when the water content in the solid cyanamide is higher and is characterized by simple process, low production cost and good effect, thereby being applicable to large-scale industrial production and solving the problems of storage and transportation of liquid cyanamide at the natural environmental temperature, which confuse people for a long time.
Description
Technical field
The present invention relates to the method for purification of solid cyanamide.
Background technology
Cyanamide has another name called cyanamide, cyanamide, when the purity of solid cyanamide less than 95%, when moisture content is high, its performance is extremely unstable, easily polymerization or decomposition in storage and transportation, burning or blast can take place when violent, and the stability of the higher cyanamide of purity better, but owing to the purification to solid cyanamide does not at present also have good method, particularly can't use conventional means to remove to the moisture in the solid cyanamide, this has brought very large difficulty just for the storage and the transportation of cyanamide manufacturing enterprise.
Summary of the invention
The method of purification that the purpose of this invention is to provide a kind of solid cyanamide by improving the purity of solid cyanamide, improves the stability of solid cyanamide.
For achieving the above object, technical scheme of the present invention is: a kind of method of purification of solid cyanamide, its purifying technique is: in the container of the band whipping appts that organic solvent is housed, under whipped state, add the solid cyanamide that needs purification, maintain the temperature under 20-40 ℃ the condition, after solid cyanamide is fully dissolved, filter, filtrate is put into the container of being with cooling and whipping appts, in cooling, continue to stir, when temperature is reduced to-10-5 ℃, stirred 20-60 minutes, and filtered out the crystal of cyanamide then, be finished product after the oven dry, filtrate cycle is used, and wherein 1 part of solid cyanamide is dissolved in 0.2-1.5 parts of organic solvents.
Above-mentioned organic solvent is methyl alcohol, ethanol, ether, acetone.
Above-mentioned oven dry is to adopt vacuum drying.
The present invention has adopted with cyanamide and has not reacted, and be easy to low temperature evaporable organic solvent and remove impurity and moisture in the solid cyanamide, solved because moisture when higher in the solid cyanamide, problem of unstable, it is simple to have technology, low, the good effectiveness of production cost is applicable to large-scale commercial production, has solved long-term puzzlement people's storage and the transportation problem of liquid single-cyandiamide under the physical environment temperature.
Embodiment
Embodiment 1:
The methyl alcohol (purity 99.5%) of getting 60g joins in the there-necked flask of the 500mL that agitator and thermometer are housed, the solid cyanamide of making by the liquid single-cyandiamide crystallisation by cooling (purity 93.0%) that adds 300g while stirring, heating in water bath to 25 ℃, solid cyanamide is fully dissolved, filter then, contaminant filter in the cyanamide is fallen, the gained filtrate collection is in the there-necked flask of the 500mL that agitator and thermometer are housed, there-necked flask is put into the chilled brine crystallisation by cooling, starts agitator simultaneously.When temperature drops to below-5 ℃, continue to stir 20 minutes, filter the crystal of separating out, mother liquid recycling.With the crystal vacuum-drying that leaches, obtain the stable solid cyanamide of white.
Embodiment 2:
The methyl alcohol (purity 99.5%) of getting 110g joins in the there-necked flask of the 500mL that agitator and thermometer are housed, the solid cyanamide of making by the liquid single-cyandiamide crystallisation by cooling (purity 93.0%) that adds 200g while stirring, heating in water bath to 40 ℃, solid cyanamide is fully dissolved, filter then, the gained filtrate collection is in the there-necked flask of the 500mL that agitator and thermometer are housed, and there-necked flask is put into the chilled brine crystallisation by cooling, starts agitator simultaneously.When temperature drops to below 5 ℃, filter the crystal of separating out, mother liquid recycling.With the crystal vacuum-drying that leaches, obtain the stable solid cyanamide of white.
Embodiment 3:
The methyl alcohol (purity 99.5%) of getting 150g joins in the there-necked flask of the 500mL that agitator and thermometer are housed, the solid cyanamide of making by the liquid single-cyandiamide crystallisation by cooling (purity 93.0%) that adds 100g while stirring, heating in water bath to 30 ℃, solid cyanamide is fully dissolved, filter then, the gained filtrate collection is in the there-necked flask of the 500mL that agitator and thermometer are housed, and there-necked flask is put into the chilled brine crystallisation by cooling, starts agitator simultaneously.When temperature drops to below 0 ℃, filter the crystal of separating out, mother liquid recycling.With the crystal vacuum-drying that leaches, obtain the stable solid cyanamide of white.
In above-mentioned 3 embodiment, under the constant situation of other condition, will there be methyl alcohol to replace with ethanol, ether, acetone respectively, equally also can obtain highly purified cyanamide.
The stability (depositing under 10 ℃ the temperature) of utilizing we to send out the solid cyanamide of purifying sees the following form.
By last table as can be seen, the cyanamide behind the body alcohol is stable very good.
Claims (3)
1, a kind of method of purification of solid cyanamide, its purifying technique is: in the container of the band whipping appts that organic solvent is housed, under whipped state, add the solid cyanamide that needs purification, maintain the temperature under 20-40 ℃ the condition, after solid cyanamide is fully dissolved, filter, filtrate is put into the container of band cooling and whipping appts, in cooling, continue to stir, when temperature is reduced to-10-5 ℃, stirred 20-60 minutes, filter out the crystal of cyanamide then, be finished product after the oven dry, filtrate cycle is used, and wherein 1 part of solid cyanamide is dissolved in 0.2-1.5 parts of organic solvents.
2,, it is characterized in that above-mentioned organic solvent is methyl alcohol, ethanol, ether, acetone according to the method for purification of claims 1 described solid cyanamide.
3,, it is characterized in that above-mentioned oven dry is to adopt vacuum drying according to the method for purification of claims 1 or 2 described solid cyanamides.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102338106A CN101423231A (en) | 2008-12-15 | 2008-12-15 | Purification method of solid cyanamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102338106A CN101423231A (en) | 2008-12-15 | 2008-12-15 | Purification method of solid cyanamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101423231A true CN101423231A (en) | 2009-05-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102338106A Pending CN101423231A (en) | 2008-12-15 | 2008-12-15 | Purification method of solid cyanamide |
Country Status (1)
| Country | Link |
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| CN (1) | CN101423231A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553080A (en) * | 2013-11-07 | 2014-02-05 | 如皋市中如化工有限公司 | Dicyandiamide content control technology in production of 30% hydrogen cyanamide |
| CN109650409A (en) * | 2019-02-13 | 2019-04-19 | 宁夏大荣化工冶金有限公司 | A kind of higher solid cyanamide preparation method of safety |
| CN109879298A (en) * | 2019-01-30 | 2019-06-14 | 徐建自 | A kind of purification process of cyanamide |
| CN110589853A (en) * | 2019-10-25 | 2019-12-20 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
| CN110697733A (en) * | 2019-11-27 | 2020-01-17 | 山东益丰生化环保股份有限公司 | Method for producing high-purity solid cyanamide |
| CN110921682A (en) * | 2019-12-19 | 2020-03-27 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
-
2008
- 2008-12-15 CN CNA2008102338106A patent/CN101423231A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553080A (en) * | 2013-11-07 | 2014-02-05 | 如皋市中如化工有限公司 | Dicyandiamide content control technology in production of 30% hydrogen cyanamide |
| CN109879298A (en) * | 2019-01-30 | 2019-06-14 | 徐建自 | A kind of purification process of cyanamide |
| CN109650409A (en) * | 2019-02-13 | 2019-04-19 | 宁夏大荣化工冶金有限公司 | A kind of higher solid cyanamide preparation method of safety |
| CN110589853A (en) * | 2019-10-25 | 2019-12-20 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
| CN110697733A (en) * | 2019-11-27 | 2020-01-17 | 山东益丰生化环保股份有限公司 | Method for producing high-purity solid cyanamide |
| CN110697733B (en) * | 2019-11-27 | 2021-06-25 | 山东益丰生化环保股份有限公司 | Method for producing high-purity solid cyanamide |
| CN110921682A (en) * | 2019-12-19 | 2020-03-27 | 山东益丰生化环保股份有限公司 | Purification method of cyanamide solution |
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Open date: 20090506 |