CN105523572A - System for direct-heat-exchange production of cyanamide by utilization of low-boiling-point organic solvent and method thereof - Google Patents
System for direct-heat-exchange production of cyanamide by utilization of low-boiling-point organic solvent and method thereof Download PDFInfo
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- CN105523572A CN105523572A CN201510894868.5A CN201510894868A CN105523572A CN 105523572 A CN105523572 A CN 105523572A CN 201510894868 A CN201510894868 A CN 201510894868A CN 105523572 A CN105523572 A CN 105523572A
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- organic solvent
- cyanamide
- boiling point
- low boiling
- point organic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/16—Cyanamide; Salts thereof
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Abstract
The invention discloses a system for direct-heat-exchange production of cyanamide by the utilization of a low-boiling-point organic solvent and a method thereof. According to the method, crushed lime nitrogen, a low-boiling-point organic solvent and carbon dioxide gas are introduced into a reactor and uniformly dispersed; temperature in the reactor is controlled to below 60 DEG C, and the low-boiling-point organic solvent is vaporized to directly absorb heat released from a reaction for cyanamide production; when pH of the reaction liquid is 9-10, the reaction is finished; organic solvent steam formed after heat absorption of the organic solvent is condensed by a condenser and the condensed product returns to an organic solvent storage tank to be recycled; reaction products are filtered to remove filter residue; and after filtrate phase-splitting treatment, a cyanamide aqueous solution and a low-boiling-point organic solvent are obtained. by boiling of the low-boiling-point organic solvent, heat released from the reaction is directly absorbed, temperature gradient in the reactor is eliminated, reaction temperature is controlled to below 60 DEG C, and generation of dicyandiamide is reduced. Without cooling water, equipment scaling problem caused by indirect cooling is avoided, energy consumption is lowered, and water resources are saved.
Description
Technical field
The present invention relates to a kind of system and method utilizing low boiling point organic solvent direct heat exchange manufacture order cyanamide.
Background technology
Cyanamide is widely used in agricultural chemicals and medical material industry as industrial raw material, is used as epoxy curing agent, dye fixing agent, flocculation agent etc.Crystal cyanamide is mainly used in medicine, healthcare product, the synthesis of fodder additives and the synthesis of pesticide intermediate, and the cyanamide aqueous solution can make the defoliant of fruit fruit tree, nontoxic insecticide.Cyanamide is also the intermediate product in synthesis Dyhard RU 100 technique.Dyhard RU 100, has another name called cyanamid dimerization, abbreviation DICY or DCD, chemical formula C2H4N4.White crystalline powder, being the dimer of cyanamide, is also the cyano derivative of guanidine, and in water, solubleness is 4.13g/100g (298.15K).Dyhard RU 100 is typically used as the raw materials for production of trimeric cyanamide and medical and dyestuff intermediate, is a kind of very important fine chemical material.In medicine industry, for producing Guanidinium nitrate and sulfa drugs etc.Also can be used for producing guanidine, thiocarbamide, nitrocellulose stablizer, steel surface stiffening agent, thiofide, printing and dyeing laking agent, leatheroid filler and tackiness agent etc.Existing manufacture order cyanamide and Dyhard RU 100 technology are the cyanogen ammonia hydrogen calcium suspension being hydrolyzed gained by calcium cyanamide (having another name called lime nitrogen), through filtration under diminished pressure removing calcium hydroxide filter residue, pass into carbonic acid gas to filtrate again calcium is precipitated out as calcium carbonate, obtain the cyanamide aqueous solution.Make it be polymerized in the basic conditions, more after filtration, crystallisation by cooling, separation, drying, obtain Dyhard RU 100.Its equation is as follows:
2CaCN
2+2H
2O→Ca(HCN
2)
2+Ca(OH)
2
Ca(HCN
2)
2+CO
2+H
2O→2NH
2CN+CaCO
3
2NH
2CN→(NH
2CN)
2
Lime nitrogen hydrolysis decalcification can release amount of heat, because cyanamide is unstable, temperature is too high can be polymerized, easy formation Dyhard RU 100, so, when temperature controls bad, what obtain is cyanamide and Dyhard RU 100 mixture, due in now mixed solution containing waste residue, therefore the Dyhard RU 100 of this step generation can only be got rid of with waste residue.Therefore, at present by additional cooling water control temperature, highly purified cyanamide is obtained.In existing technique, adopt recuperative heat exchanger cooling, cause in reactor and there is very large thermograde, reactor hot(test)-spot temperature can not be avoided to generate Dyhard RU 100 more than 60 DEG C, heat-exchange equipment fouling can be caused simultaneously, cause heat transfer effect to reduce.
Summary of the invention
The object of the invention is the deficiency overcoming the high energy consumption poor efficiency that prior art exists, provide a kind of flow process simply to utilize the system of low boiling point organic solvent direct heat exchange manufacture order cyanamide.
Second object of the present invention is to provide a kind of low, the energy-conservation method utilizing low boiling point organic solvent direct heat exchange manufacture order cyanamide of process cost
Technical scheme of the present invention is summarized as follows:
Utilize the system of low boiling point organic solvent direct heat exchange manufacture order cyanamide, comprise reactor 1, reactor by pipeline successively with strainer 2, phase splitter 3, cyanamide solution storage tank 4 connects, and described phase splitter 3 is connected with organic solvent storage tank 5, reactor 1 successively by pipeline; Described reactor is connected with condenser 6, organic solvent storage tank 5 successively by pipeline; Reactor 1 is provided with carbon dioxide adds entrance, lime nitrogen adds entrance and water adds entrance; Described strainer 2 is provided with waste residue relief outlet; Described organic solvent storage tank 5 is provided with organic solvent and adds entrance.
Utilize the method for low boiling point organic solvent direct heat exchange manufacture order cyanamide, comprise the steps: the lime nitrogen that will pulverize, water, low boiling point organic solvent and carbon dioxide to pass in reactor and are uniformly dispersed, temperature in control reactor is below 60 DEG C, utilize low boiling point organic solvent to vaporize and directly absorb generation cyanamide reaction liberated heat, reaction is terminated as the pH=9-10 of reaction solution, the organic vapor that organic solvent heat absorption is formed recycles by returning organic solvent storage tank after condenser condenses, reaction product is crossed and is filtered filter residue, after filtrate phase-splitting process, obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% and low boiling point organic solvent, the described cyanamide aqueous solution passes into cyanamide solution storage tank, described low boiling point organic solvent passes into organic solvent storage tank Posterior circle and uses, described low boiling point organic solvent be under normal pressure boiling point at 57.3 DEG C and following solvent.
Under normal pressure boiling point 57.3 DEG C and following solvent preferred: Skellysolve A, iso-pentane, neopentane, sherwood oil, ether, methylene dichloride, acetone or 1,1-ethylene dichloride.
A kind of method utilizing low boiling point organic solvent direct heat exchange manufacture order cyanamide, comprise the steps: the lime nitrogen that will pulverize, water, in low boiling point organic solvent and the continuous input reactor of carbon dioxide, temperature in control reactor is below 60 DEG C, utilize low boiling point organic solvent to vaporize and directly absorb generation cyanamide reaction liberated heat, control carbon dioxide flow, make the pH=9-10 of reaction solution, the organic vapor that organic solvent heat absorption is formed recycles by returning organic solvent storage tank after condenser condenses, reaction product is crossed and is filtered filter residue, after filtrate phase-splitting process, obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% and low boiling point organic solvent, the described cyanamide aqueous solution passes into cyanamide solution storage tank, described low boiling point organic solvent passes into organic solvent storage tank Posterior circle and uses, described low boiling point organic solvent be under normal pressure boiling point at 57.3 DEG C and following solvent.
Under normal pressure boiling point 57.3 DEG C and following solvent preferred: Skellysolve A, iso-pentane, neopentane, sherwood oil, ether, methylene dichloride, acetone or 1,1-ethylene dichloride.
System of the present invention is simple, method of the present invention utilizes low boiling point organic solvent to seethe with excitement direct absorption reaction liberated heat, and the thermograde in eliminative reaction device, can control temperature of reaction preferably, equal control temperature of reaction, below 60 DEG C, decreases the generation of Dyhard RU 100; Do not need water coolant, avoid the equipment scaling problem of cooling indirectly, save energy consumption and water resources.
Accompanying drawing explanation
Fig. 1 is the system schematic utilizing low boiling point organic solvent direct heat exchange manufacture order cyanamide.
Embodiment
Below in conjunction with specific embodiment and Figure of description, the present invention is further illustrated.Embodiments of the invention understand the present invention better to enable those skilled in the art to, but do not impose any restrictions the present invention.
Utilize the system of low boiling point organic solvent direct heat exchange manufacture order cyanamide, comprise reactor 1, reactor by pipeline successively with strainer 2, phase splitter 3, cyanamide solution storage tank 4 connects, and described phase splitter 3 is connected with organic solvent storage tank 5, reactor 1 successively by pipeline; Described reactor is connected with condenser 6, organic solvent storage tank 5 successively by pipeline; Reactor 1 is provided with carbon dioxide adds entrance, lime nitrogen adds entrance and water adds entrance; Described strainer 2 is provided with waste residue relief outlet; Described organic solvent storage tank 5 is provided with organic solvent and adds entrance.
Embodiment 1
Utilize a method for low boiling point organic solvent direct heat exchange batch production cyanamide, comprise the steps:
By the lime nitrogen of the pulverizing of 1.5kg nitrogen content 20wt%, 3L water, 2L Skellysolve A and carbon dioxide to pass in reactor 1 and are uniformly dispersed, temperature in control reactor is below 60 DEG C, the flow controlling carbon dioxide is 6L/min, utilization utilizes the vaporization of low boiling point organic solvent Skellysolve A directly to absorb and generates cyanamide reaction liberated heat, reaction is terminated as the pH=9 of reaction solution, Skellysolve A heat absorption formed Skellysolve A steam recycle by returning organic solvent storage tank 5 after condenser 6 condensation, reaction product is at strainer 2 inner filtration removing filter residue 2.1kg, filtrate is in phase splitter 3 after phase-splitting process, obtain the cyanamide aqueous solution and Skellysolve A that massfraction is 24.5%, the cyanamide aqueous solution passes into cyanamide solution storage tank 4, Skellysolve A passes into organic solvent storage tank circulation 5 and uses.
Experiment proves, as pH=10, instruction terminates reaction, and other same the present embodiment, can obtain the cyanamide aqueous solution that massfraction is 22.5%.
The flow of carbon dioxide can control within the scope of 5-10L/min, and the large reaction of flow is fast, and the little reaction of flow is slow.
Experiment proves, substitutes the Skellysolve A of the present embodiment, other same the present embodiment, can obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% with iso-pentane, neopentane, sherwood oil, ether, methylene dichloride, acetone or 1,1-ethylene dichloride.Embodiment 2
Utilize a method for low boiling point organic solvent direct heat exchange continuous seepage cyanamide, comprise the steps:
In the continuous input reactor 1 of lime nitrogen nitrogen content 20wt% pulverized by 15kg/h, 30L/h water, 20L/h Skellysolve A and carbon dioxide, temperature in control reactor is below 60 DEG C, utilize low boiling point organic solvent Skellysolve A to vaporize and directly absorb generation cyanamide reaction liberated heat, the amount controlling carbon dioxide, within the scope of 5-10L/min, makes reaction system at pH=9-10; Skellysolve A heat absorption formed steam recycle by returning organic solvent storage tank 5 after condenser 6 condensation, the reaction product of discharging from reactor filters waste calcium carbonate excessively by strainer 2, after filtrate carries out phase-splitting process in phase splitter 3, obtain the cyanamide aqueous solution and Skellysolve A that massfraction is 21.17%, the cyanamide aqueous solution passes into cyanamide solution storage tank 4, and Skellysolve A passes into organic solvent storage tank 5 and recycles.
Experiment proves, substitutes the Skellysolve A of the present embodiment, other same the present embodiment, can obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% with iso-pentane, neopentane, sherwood oil, ether, methylene dichloride or acetone.
Claims (5)
1. utilize the system of low boiling point organic solvent direct heat exchange manufacture order cyanamide, comprise reactor (1), it is characterized in that described reactor by pipeline successively with strainer (2), phase splitter (3), cyanamide solution storage tank (4) connects, and described phase splitter (3) is connected with organic solvent storage tank (5), reactor (1) successively by pipeline; Described reactor is connected with condenser (6), organic solvent storage tank (5) successively by pipeline; Reactor (1) is provided with carbon dioxide adds entrance, lime nitrogen adds entrance and water adds entrance; Described strainer (2) is provided with waste residue relief outlet; Described organic solvent storage tank (5) is provided with organic solvent and adds entrance.
2. utilize the method for low boiling point organic solvent direct heat exchange manufacture order cyanamide, it is characterized in that comprising the steps: the lime nitrogen by pulverizing, water, low boiling point organic solvent and carbon dioxide to pass in reactor and are uniformly dispersed, temperature in control reactor is below 60 DEG C, utilize low boiling point organic solvent to vaporize and directly absorb generation cyanamide reaction liberated heat, reaction is terminated as the pH=9-10 of reaction solution, the organic vapor that organic solvent heat absorption is formed recycles by returning organic solvent storage tank after condenser condenses, reaction product is crossed and is filtered filter residue, after filtrate phase-splitting process, obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% and low boiling point organic solvent, the described cyanamide aqueous solution passes into cyanamide solution storage tank, described low boiling point organic solvent passes into organic solvent storage tank Posterior circle and uses, described low boiling point organic solvent be under normal pressure boiling point at 57.3 DEG C and following solvent.
3. method according to claim 2, is characterized in that boiling point is Skellysolve A, iso-pentane, neopentane, sherwood oil, ether, methylene dichloride, acetone or 1,1-ethylene dichloride at 57.3 DEG C and following solvent under described normal pressure.
4. one kind utilizes the method for low boiling point organic solvent direct heat exchange manufacture order cyanamide, it is characterized in that comprising the steps: the lime nitrogen by pulverizing, water, in low boiling point organic solvent and the continuous input reactor of carbon dioxide, temperature in control reactor is below 60 DEG C, utilize low boiling point organic solvent to vaporize and directly absorb generation cyanamide reaction liberated heat, control carbon dioxide flow, make the pH=9-10 of reaction solution, the organic vapor that organic solvent heat absorption is formed recycles by returning organic solvent storage tank after condenser condenses, reaction product is crossed and is filtered filter residue, after filtrate phase-splitting process, obtain the cyanamide aqueous solution of massfraction within the scope of 10%-30% and low boiling point organic solvent, the described cyanamide aqueous solution passes into cyanamide solution storage tank, described low boiling point organic solvent passes into organic solvent storage tank Posterior circle and uses, described low boiling point organic solvent be under normal pressure boiling point at 57.3 DEG C and following solvent.
5. method according to claim 4, is characterized in that boiling point is Skellysolve A, iso-pentane, neopentane, sherwood oil, ether, methylene dichloride, acetone or 1,1-ethylene dichloride at 57.3 DEG C and following solvent under described normal pressure.
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| CN201510894868.5A CN105523572B (en) | 2015-12-07 | 2015-12-07 | Utilize the system and method for low boiling point organic solvent direct heat transfer production cyanamide |
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| CN201510894868.5A CN105523572B (en) | 2015-12-07 | 2015-12-07 | Utilize the system and method for low boiling point organic solvent direct heat transfer production cyanamide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500314A (en) * | 2017-09-06 | 2017-12-22 | 山东益丰生化环保股份有限公司 | A kind of preparation method of cyanamide organic solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method of preparing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by calcium cyanamide |
| CN103011200A (en) * | 2012-12-13 | 2013-04-03 | 黄河三角洲京博化工研究院有限公司 | Preparation method of high-concentration cyanamide solution |
| CN103922365A (en) * | 2014-04-10 | 2014-07-16 | 宁夏宝马化工集团有限公司 | Method for efficient synthesis of hydrogen cyanamide employing lime nitrogen |
| CN205346849U (en) * | 2015-12-07 | 2016-06-29 | 上海弗鲁克科技发展有限公司 | System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide |
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- 2015-12-07 CN CN201510894868.5A patent/CN105523572B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016151A (en) * | 2006-08-08 | 2007-08-15 | 芮海平 | Method of preparing cyanamide aqueous solution and dicyandiamide and coproducing carbon and calcium carbonate by calcium cyanamide |
| CN103011200A (en) * | 2012-12-13 | 2013-04-03 | 黄河三角洲京博化工研究院有限公司 | Preparation method of high-concentration cyanamide solution |
| CN103922365A (en) * | 2014-04-10 | 2014-07-16 | 宁夏宝马化工集团有限公司 | Method for efficient synthesis of hydrogen cyanamide employing lime nitrogen |
| CN205346849U (en) * | 2015-12-07 | 2016-06-29 | 上海弗鲁克科技发展有限公司 | System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500314A (en) * | 2017-09-06 | 2017-12-22 | 山东益丰生化环保股份有限公司 | A kind of preparation method of cyanamide organic solution |
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