CN109650409A - A kind of higher solid cyanamide preparation method of safety - Google Patents
A kind of higher solid cyanamide preparation method of safety Download PDFInfo
- Publication number
- CN109650409A CN109650409A CN201910112094.4A CN201910112094A CN109650409A CN 109650409 A CN109650409 A CN 109650409A CN 201910112094 A CN201910112094 A CN 201910112094A CN 109650409 A CN109650409 A CN 109650409A
- Authority
- CN
- China
- Prior art keywords
- cyanamide
- crystal
- safety
- water
- preparation
- 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.)
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Links
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000007787 solid Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 6
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000002631 hypothermal effect Effects 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 150000001298 alcohols Chemical class 0.000 abstract description 3
- 239000000383 hazardous chemical Substances 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- -1 cyanogen Amine Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/16—Cyanamide; Salts thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of higher solid cyanamide preparation methods of safety, method is the following steps are included: squeeze into crystallizer for liquid single-cyandiamide, coarse crystal cyanamide is obtained by frozen cooling, it is again dissolved in water after being dried using centrifuge, it is completely dissolved to crystal, impurity is removed using filter plant, the chilled cooling of filtrate obtains crystal, low temperature drying is carried out after crystal is separated, obtain high-purity solid cyanamide, filtrate is again introduced into dissolution kettle for dissolving coarse crystal, can be recycled.The present invention relates to a kind of preparation methods of solid cyanamide, have the characteristics that simple process, high income, at low cost, acquisition cyanamide crystal purity is high, solve the problems, such as that the solid cyanamide of separating out alcohol method production is difficult to store and transport, water is recrystallized as solvent simultaneously, is eliminated using hazardous chemicals such as alcohols as solvent security risk in process of production and to the pollution of air.
Description
Technical field
The present invention relates to a kind of preparation methods of solid cyanamide, and in particular to a kind of solid cyanamide that technique is safer
Preparation method.
Background technique
Cyanamide, English name Cyanamide also known as cyanamide, cyanamide, amino first cyanogen, are the raw materials of organic synthesis.Single cyanogen
Amine contains cyano and amino, is all active group, the multiple reaction performance with above-mentioned functional group, Yi Fasheng addition, substitution, contracting
The reaction such as conjunction.When the purity of solid cyanamide is less than 95%, when moisture content is higher, performance is extremely unstable, is storing and is transporting
Polymerization or decomposition reaction easily occur in the process, can occur to burn when violent or explodes.
Existing high-purity solid cyanamide production method is separating out alcohol method, and concrete technology is: by high concentration liquid cyanamide
92% or more coarse crystal is obtained through low temperature crystallization, coarse crystal, which is added to organic solvent methanol, (can also be used ethyl alcohol, propyl alcohol, second
Ether) in dissolution, by filtering remove impurity after again crystallization obtain solid, use vacuum drying method obtain content 99% with
On product.
The product purity that above method obtains can achieve 99% or more, but organic solvent becomes new impurity, is producing
There are problems that security risk and pollution air in the process, while properties of product are still unstable, in storage and transportational process
Polymerization easily occurs or decomposes, or even spontaneous combustion or explosion occurs, cause product in production, storage, transport and use process not
Safety.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides one kind is easy to operate, at low cost, product purity is high, product storage
A kind of safer solid cyanamide preparation method.
A kind of higher solid cyanamide preparation method of safety, specific steps are as follows:
Liquid single-cyandiamide is squeezed into crystallizer, obtains coarse crystal cyanamide by frozen cooling, after drying using centrifuge again
It is soluble in water, it is completely dissolved to crystal, removes impurity using filter plant, the chilled cooling of filtrate obtains crystal, by crystal
Low temperature drying is carried out after separating, and obtains high-purity solid cyanamide, filtrate is again introduced into dissolution kettle and is used to dissolve coarse crystal,
It can be recycled.
The concentration of the liquid single-cyandiamide be 45%~65%, the coarse crystal cyanamide purity that frozen cooling obtains be 90~
96%。
The coarse crystal cyanamide completely dissolves in water, and feed concentration is 50%~70%, and wherein water is eliminated as solvent
When using hazardous chemicals such as alcohols as solvent, in process of production existing for security risk and pollution to air；Together
When dissolution with water use tap water, the higher deionized water of quality, pure water, distilled water also can be used.
The frozen cooling method cools down using hypothermic saline staged.
The temperature of the low temperature drying is lower than 40 DEG C, and wherein drier uses low-temperature drying equipment, and freezing also can be used
Drying equipment, this method solve moisture in solid cyanamide to be not easy the problem of removing, while used low temperature drying method,
It is lower compared with freeze-drying method energy consumption.
The low temperature drying method is dried using purified compressed air, is reduced impurity and is entered in product, improves
The production of product, storage, the safety used.
The cyanamide content of the solid cyanamide of the high-purity is 99% or more, due to using water conduct in production process
Solvent is dried through recrystallizing, and with purified compressed air, and production is safer, solves consolidating for separating out alcohol method production
Unsafe problem is transported and is used in the storage of body cyanamide.
The present invention relates to a kind of preparation methods of solid cyanamide, have simple process, high income, at low cost, acquisition list
The high feature of cyanamide crystal purity solves the problems, such as that the solid cyanamide of separating out alcohol method production is difficult to store and transport, while water
Recrystallized as solvent, eliminate using hazardous chemicals such as alcohols as solvent security risk in process of production and
Pollution to air.
Detailed description of the invention:
Fig. 1 is a kind of higher solid cyanamide preparation method process flow chart of safety.
Specific embodiment:
The present invention will be further explained below with reference to the attached drawings and specific examples, and the embodiment of the present invention is to make this field
Technical staff better understood when the present invention, but the present invention is not imposed any restrictions.
Embodiment 1
A kind of preparation method of the higher solid cyanamide of safety, the specific steps are as follows:
It is that 50~53% liquid single-cyandiamides are squeezed into crystallizer by 1600kg concentration, obtaining content by frozen cooling is 91~94%
Coarse crystal cyanamide 900kg, be again dissolved in deionized water after being dried using centrifuge, crystal is completely dissolved, and obtains concentration
For 63.7% cyanamide liquid, impurity is removed using filter plant, filtrate is cooled to 0 DEG C of obtained crystal through hypothermic saline,
Separation is moved back into drier, under the conditions of temperature is lower than 40 DEG C, is passed through purified compressed air and is dried, obtain purity
99.6% solid cyanamide.Filtrate backs into dissolving tank, and 400kg coarse crystal is added again, dissolved, filtered, with low temperature salt
Water is cooled to 1 DEG C and obtains crystal, and the solid cyanamide that purity is 99.4% is obtained after separation, drying.Filtrate can in above process
Reusability 6~10 times.
Claims (9)
1. a kind of higher solid cyanamide preparation method of safety, preparation step are as follows: liquid single-cyandiamide is squeezed into crystallizer,
Coarse crystal cyanamide is obtained by frozen cooling, is again dissolved in water after being dried using centrifuge, is completely dissolved to crystal, then pass through
It crosses filter plant and removes impurity, the chilled cooling of filtrate obtains crystal, carries out low temperature drying after crystal is separated, obtain height
Pure solid cyanamide, filtrate are again introduced into dissolution kettle for dissolving coarse crystal, can be recycled.
2. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that liquid list cyanogen
The concentration of amine is 45%~65%, and the coarse crystal cyanamide purity that frozen cooling obtains is 90~96%.
3. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that above-mentioned coarse-grain
When body cyanamide completely dissolves in water, feed concentration is 50%~70%.
4. a kind of higher solid cyanamide preparation method of safety as described in claim 1 or 3, it is characterised in that coarse-grain
Body cyanamide is soluble in water, and water used is the tap water either higher deionized water of quality, pure water, distilled water.
5. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that frozen cooling
Method cools down using hypothermic saline staged.
6. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that above-mentioned low temperature
Dry temperature is lower than 40 DEG C, and the drier of use is low-temperature drying equipment or freeze drying equipment, preferably low-temperature drying equipment.
7. the higher solid cyanamide preparation method of a kind of safety as described in claim 1 or 6, it is characterised in that described low
Warm drying process is dried using purified compressed air.
8. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that obtained height
The cyanamide content of pure solid cyanamide is 99% or more.
9. a kind of higher solid cyanamide preparation method of safety as described in claim 1, it is characterised in that made using water
Be recrystallized to give crystal for solvent, reuse the dry crystal of purified compressed air, product obtained storage, transport and
It is more secure when used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910112094.4A CN109650409A (en) | 2019-02-13 | 2019-02-13 | A kind of higher solid cyanamide preparation method of safety |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910112094.4A CN109650409A (en) | 2019-02-13 | 2019-02-13 | A kind of higher solid cyanamide preparation method of safety |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109650409A true CN109650409A (en) | 2019-04-19 |
Family
ID=66122230
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910112094.4A Pending CN109650409A (en) | 2019-02-13 | 2019-02-13 | A kind of higher solid cyanamide preparation method of safety |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109650409A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB628631A (en) * | 1946-02-08 | 1949-09-01 | Ciba Ltd | Process for the recrystallisation of melamine |
| CN101423231A (en) * | 2008-12-15 | 2009-05-06 | 宁夏大荣化工冶金有限公司 | Purification method of solid cyanamide |
| CN107473241A (en) * | 2017-09-06 | 2017-12-15 | 山东益丰生化环保股份有限公司 | A kind of preparation method of solid cyanamide |
-
2019
- 2019-02-13 CN CN201910112094.4A patent/CN109650409A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB628631A (en) * | 1946-02-08 | 1949-09-01 | Ciba Ltd | Process for the recrystallisation of melamine |
| CN101423231A (en) * | 2008-12-15 | 2009-05-06 | 宁夏大荣化工冶金有限公司 | Purification method of solid cyanamide |
| CN107473241A (en) * | 2017-09-06 | 2017-12-15 | 山东益丰生化环保股份有限公司 | A kind of preparation method of solid cyanamide |
Non-Patent Citations (1)
| Title |
|---|
| 宁夏大荣化工冶金有限公司: "高纯医药用固体单氰胺研发" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| PB01 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20190419 |