CN205346849U - System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide - Google Patents

System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide Download PDF

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Publication number
CN205346849U
CN205346849U CN201521010265.6U CN201521010265U CN205346849U CN 205346849 U CN205346849 U CN 205346849U CN 201521010265 U CN201521010265 U CN 201521010265U CN 205346849 U CN205346849 U CN 205346849U
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China
Prior art keywords
organic solvent
reactor
storage tank
low boiling
pipeline
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Expired - Fee Related
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CN201521010265.6U
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Chinese (zh)
Inventor
张金利
周鸣亮
杨超
李韡
韩优
付雁
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SHANGHAI FLUKO TECHNOLOGY DEVELOPMENT Co Ltd
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SHANGHAI FLUKO TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN201521010265.6U priority Critical patent/CN205346849U/en
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Publication of CN205346849U publication Critical patent/CN205346849U/en
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Abstract

The utility model discloses a system for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide, including reactor (1), characterized by the reactor passes through the pipeline and is connected with filter (2), phase splitter (3), single cyandiamide solution storage tank (4) in proper order, phase splitter (3) are connected with organic solvent storage tank (5), reactor (1) through the pipeline in proper order, the reactor passes through the pipeline and is connected with condenser (6), organic solvent storage tank (5) in proper order, be provided with carbon dioxide gas inlet port, lime nitrogen inlet port and water inlet port on reactor (1), filter (2) are provided with the waste residue discharge port, organic solvent storage tank (5) are provided with organic solvent inlet port. The utility model discloses a system utilizes the direct reaction liberated heat that absorbs of low boiling organic solvent boiling, the interior temperature gradient of elimination reaction ware, and the controlled reaction temperature has reduced the formation of dicyandiamide below 60 DEG C, do not need the cooling water, avoided indirect cooling's equipment scale deposit problem, saved energy consumption and water resource.

Description

Low boiling point organic solvent direct heat transfer is utilized to produce the system of cyanamide
Technical field
This utility model relates to a kind of system utilizing low boiling point organic solvent direct heat transfer to produce cyanamide.
Background technology
Cyanamide is widely used in pesticide and medical material industry as the raw material of industry, is used as epoxy curing agent, dye fixing agent, flocculant etc..Crystal cyanamide is mainly used in the synthesis of medicine, health promoting product, the synthesis of feed additive and pesticide intermediate, and cyanamide aqueous solution can make the defoliant of fruit fruit tree, nontoxic insecticide.Cyanamide is also the intermediate product in synthesis dicyandiamide technique.Dicyandiamide, has another name called cyanamid dimerization, and abridge DICY or DCD, chemical formula C2H4N4.White crystalline powder, is the dimer of cyanamide, is also the cyano derivative of guanidine, and in water, dissolubility is 4.13g/100g (298.15K).Dicyandiamide is typically used as the raw materials for production of tripolycyanamide and medical and dyestuff intermediate, is a kind of very important fine chemical material.In medical industry, it is used for producing Guanidine nitrate (1:1) and sulfa drugs etc..Can also be used for producing guanidine, thiourea, celluloid stabilizer, steel surface sclerosing agent, thiofide, printing and dyeing color fixing agent, artificial leather filler and binding agent etc..Existing production cyanamide and dicyandiamide technology are to be hydrolyzed the cyanogen ammonia hydrogen calcium suspension of gained by nitrolim (having another name called lime nitrogen), calcium hydroxide filtering residue is removed through filtration under diminished pressure, pass into carbon dioxide to filtrate again to be precipitated out as calcium carbonate by calcium, obtain cyanamide aqueous solution.Make it be polymerized in the basic conditions, then through filtration, crystallisation by cooling, separation, dry, obtain dicyandiamide.Its equation is as follows:
2CaCN2+2H2O→Ca(HCN2)2+Ca(OH)2
Ca(HCN2)2+CO2+H2O→2NH2CN+CaCO3
2NH2CN→(NH2CN)2
Lime nitrogen hydrolysis decalcification can release amount of heat, owing to cyanamide is unstable, temperature is too high can be polymerized, easily form dicyandiamide, so, what temperature obtained when controlling bad is cyanamide and dicyandiamide mixture, due in now mixed liquor containing waste residue, therefore the dicyandiamide that this step produces can only be got rid of with waste residue.Therefore, at present by additional cooling water control temperature, it is thus achieved that highly purified cyanamide.In existing technique, adopt dividing wall type heat exchanger cooling, cause and in reactor, there is very big thermograde, it is impossible to avoid reactor hot(test)-spot temperature to generate dicyandiamide more than 60 DEG C, heat transmission equipment fouling can be caused simultaneously, cause that heat transfer effect reduces.
Utility model content
The purpose of this utility model is the deficiency that the high energy consumption overcoming prior art to exist is inefficient, it is provided that the low boiling point organic solvent direct heat transfer that utilizes that a kind of flow process is simple, operating cost is low, energy-conservation produces the system of cyanamide.
The technical solution of the utility model is summarized as follows:
Low boiling point organic solvent direct heat transfer is utilized to produce the system of cyanamide, including reactor 1, reactor is connected with filter 2, phase separator 3, cyanamide solution storage tank 4 successively by pipeline, and described phase separator 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 filter 2 is provided with waste residue outlet;Described organic solvent storage tank 5 is provided with organic solvent and adds entrance.
System of the present utility model can utilize the low boiling point organic solvent direct absorption reaction liberated heat of boiling, eliminates the thermograde in reactor, it is possible to controlling reaction temperature preferably, equal control reaction temperature, below 60 DEG C, decreases the generation of dicyandiamide;Water need not be cooled down, it is to avoid the equipment scaling problem of indirect cooling, save energy consumption and water resource.
Accompanying drawing explanation
Fig. 1 is the system schematic utilizing low boiling point organic solvent direct heat transfer to produce cyanamide.
Detailed description of the invention
Below in conjunction with specific embodiment and Figure of description, this utility model is further described.Embodiment of the present utility model is to enable those skilled in the art to be more fully understood that this utility model, but this utility model is not imposed any restrictions.
Low boiling point organic solvent direct heat transfer is utilized to produce the system of cyanamide, including reactor 1, reactor is connected with filter 2, phase separator 3, cyanamide solution storage tank 4 successively by pipeline, and described phase separator 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 filter 2 is provided with waste residue outlet;Described organic solvent storage tank 5 is provided with organic solvent and adds entrance.
Embodiment 1
The method utilizing said system to utilize low boiling point organic solvent direct heat transfer Batch Process cyanamide, comprises the steps:
Lime nitrogen by the pulverizing of 1.5kg nitrogen content 20wt%, 3L water, 2L pentane and carbon dioxide pass in reactor 1 and are uniformly dispersed, control the temperature in reactor below 60 DEG C, the flow controlling carbon dioxide is 6L/min, utilization utilizes the vaporization of low boiling point organic solvent pentane directly to absorb and generates cyanamide reaction liberated heat, reaction is terminated as the pH=9 of reactant liquor, what pentane heat absorption was formed pentane steam recycles by returning organic solvent storage tank 5 after condenser 6 condensation, product removes filtering residue 2.1kg at filter 2 inner filtration, after filtrate divides phase processor in phase separator 3, obtain cyanamide aqueous solution and pentane that mass fraction is 24.5%, cyanamide aqueous solution passes into cyanamide solution storage tank 4, pentane passes into organic solvent storage tank circulation 5 use.
It is demonstrated experimentally that instruction terminates reaction, other same the present embodiment, it is possible to obtain the cyanamide aqueous solution that mass fraction is 22.5% as pH=10.
The flow of carbon dioxide can control within the scope of 5-10L/min, and the big reaction of flow is fast, and the little reaction of flow is slow.
It is demonstrated experimentally that substitute the pentane of the present embodiment with isopentane, neopentane, petroleum ether, ether, dichloromethane, acetone or 1,1-dichloroethanes, other same the present embodiment, it is possible to obtain mass fraction cyanamide aqueous solution within the scope of 10%-30%.
Embodiment 2
Utilize said system to utilize the method that low boiling point organic solvent direct heat transfer produces cyanamide continuously, comprise the steps:
By in the 15kg/h continuous input reactor 1 of lime nitrogen, 30L/h water, 20L/h pentane and carbon dioxide that nitrogen content 20wt% is pulverized, control the temperature in reactor below 60 DEG C, utilize the vaporization of low boiling point organic solvent pentane directly to absorb and generate cyanamide reaction liberated heat, control the amount of carbon dioxide within the scope of 5-10L/min, make reaction system at pH=9-10;What pentane heat absorption was formed steam recycles by returning organic solvent storage tank 5 after condenser 6 condensation, the product discharged from reactor is filtered to remove waste calcium carbonate by filter 2, after filtrate carries out point phase processor in phase separator 3, obtain cyanamide aqueous solution and pentane that mass fraction is 21.17%, cyanamide aqueous solution passes into cyanamide solution storage tank 4, and pentane passes into organic solvent storage tank 5 and recycles.
It is demonstrated experimentally that substitute the pentane of the present embodiment with isopentane, neopentane, petroleum ether, ether, dichloromethane or acetone, other same the present embodiment, it is possible to obtain mass fraction cyanamide aqueous solution within the scope of 10%-30%.

Claims (1)

1. utilize low boiling point organic solvent direct heat transfer to produce the system of cyanamide, including reactor (1), it is characterized in that described reactor is connected with filter (2), phase separator (3), cyanamide solution storage tank (4) successively by pipeline, described phase separator (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 filter (2) is provided with waste residue outlet;Described organic solvent storage tank (5) is provided with organic solvent and adds entrance.
CN201521010265.6U 2015-12-07 2015-12-07 System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide Expired - Fee Related CN205346849U (en)

Priority Applications (1)

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CN201521010265.6U CN205346849U (en) 2015-12-07 2015-12-07 System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide

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Application Number Priority Date Filing Date Title
CN201521010265.6U CN205346849U (en) 2015-12-07 2015-12-07 System for utilize low boiling organic solvent direct heat transfer manufacture order cyandiamide

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105523572A (en) * 2015-12-07 2016-04-27 上海弗鲁克科技发展有限公司 System for direct-heat-exchange production of cyanamide by utilization of low-boiling-point organic solvent and method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105523572A (en) * 2015-12-07 2016-04-27 上海弗鲁克科技发展有限公司 System for direct-heat-exchange production of cyanamide by utilization of low-boiling-point organic solvent and method thereof

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CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160629

Termination date: 20191207