CN109053610A - A kind of good process for cleanly preparing of environment of high-purity cyanuric acid - Google Patents
A kind of good process for cleanly preparing of environment of high-purity cyanuric acid Download PDFInfo
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- CN109053610A CN109053610A CN201810803348.2A CN201810803348A CN109053610A CN 109053610 A CN109053610 A CN 109053610A CN 201810803348 A CN201810803348 A CN 201810803348A CN 109053610 A CN109053610 A CN 109053610A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/30—Only oxygen atoms
- C07D251/32—Cyanuric acid; Isocyanuric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/58—Ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/79—Injecting reactants
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- C—CHEMISTRY; METALLURGY
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/242—Preparation from ammonia and sulfuric acid or sulfur trioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2251/00—Reactants
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- B01D2251/506—Sulfuric acid
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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Abstract
The present invention provides a kind of good process for cleanly preparing of environment of high-purity cyanuric acid, and urea and composite catalyst are mixed, carry out reacting to obtain cyanuric acid crude product in 120~270 DEG C of temperature, under conditions of pressure -0.01~-0.2Mpa；The composite catalyst is the mixture of ammonium chloride, ammonium nitrate, sodium nitrate and potassium nitrate composition；Obtained cyanuric acid crude product is mixed with aqueous sulfuric acid after crushed, is reacted in 60-170 DEG C, cyanuric acid solid is filtered to obtain；Gained cyanuric acid solid is through washing, centrifugation, dry fine work cyanuric acid.Preparation step of the present invention is simple, the discharge in production process without pernicious gas and waste liquid, and can be realized the recycling of waste liquid, exhaust gas and waste heat, improves energy utilization rate；Cyanuric acid crude product itself content obtained is high, so that target product yield and purity are higher；Crude product cyanuric acid post-processing refining methd is simple, save the cost, conducive to the industrialized production of cyanuric acid.
Description
Technical field
The present invention relates to a kind of good process for cleanly preparing of environment of high-purity cyanuric acid, belong to chemical intermediate preparation skill
Art field.
Background technique
Cyanuric acid is white crystals, odorlessness, mildly bitter flavor；Be mainly used for synthesize chlorinated derivative, trichloroisocyanuric acid, two
Chlorine isocyanuric acid sodium or potassium, it may also be used for preparation cyanurate-formaldehyde resin, epoxy resin, antioxidant, coating, adhesive, pesticide
Herbicide, metal cyanide corrosion inhibiter, polymer modification agent etc.；Its is widely used, is the important chemical reagent of one kind, organic
The raw material of synthesis and pharmaceutical synthesis.
Currently, industrially the major way of production cyanuric acid is to heat using coal as fuel to urea, urea pyrolysis
It is condensed and cyanuric acid is made；The disadvantage is that: reaction time length, temperature are high, and with coal etc. for fuel, energy consumption is high and is unfavorable for environmental protection；
Subsequent refinement treatment is complicated, and large labor intensity is at high cost；Reacting the useless gaseous ammonia generated and waste liquid has serious pollution to environment,
Worker's production environment is severe；Gained cyanuric acid crude product content itself is lower, causes target product yield and purity low.
In view of the above deficiencies, the report in terms of cyanuric acid preparation improves is also more.Such as, Chinese patent literature
CN102532045A discloses a kind of method for producing cyanuric acid as raw material using urea, includes the following steps: 1. to take urea and chlorine
Change ammonium to be uniformly mixed, obtain mixture, mixture is placed in ceramic bowl；It is obtained 2. the ceramic bowl for containing mixture is sent into condensation furnace
To cyanuric acid crude product；3. cyanuric acid crude product is crushed spare；4. adding after water, the concentrated sulfuric acid and ammonium hydrogen sulfate is added in refining kettle
Enter cyanuric acid crude product crushed material；5. controlling the vapour pressure of refining kettle, the steam valve adjusted on refining kettle rises temperature；6. keeping 108
Insulation reaction 4 hours at DEG C, it is primary every stirring in 1 hour to the material in refining kettle；7. rate-determining steps 6. reaction mass, works as object
When cyanuric acid content in material >=98.5%, refining kettle parks steam and blowing cooling, filters, and fine work cyanogen urine is obtained after dry
Acid.Although this method can improve cyanuric acid yield to a certain extent, the content of cyanuric acid in obtained cyanuric acid crude product
It is lower, therefore the yield of cyanuric acid is relatively low；Subsequent purification purification process is relatively complicated, complex for operation step, need using
The concentrated sulfuric acid and sulfuric acid cyanamide are refined, and cost and labour cost are higher；The patent is condensed furnace using coal as fuel
Interior reaction temperature is higher, and energy consumption is high, and is unfavorable for environmental protection；Also, pernicious gas generation is had, while generating a large amount of waste liquids, it is dirty
Contaminate environment.For another example, Chinese patent literature CN104961699A provides a kind of production of producing sulfuric acid and jointly cyanuric acid and its steam step
Utilize the research and application of electrification technique, comprising the following steps: urea and ammonium chloride, ammonium carbonate are uniformly mixed merging condensation furnace
In ceramic bowl in, control condensation furnace temperature be 175-195 DEG C, obtain cyanuric acid crude product and flue gas, the purified device of flue gas is net
Change and enters ammonia absorption tower；Cyanuric acid crude product crushed material and sulfuric acid solution are uniformly mixed and obtain feed liquid；Feed liquid is successively squeezed into
Multi-stage reacting kettle is reacted, and obtains solid material and acid pickle, solid material washed, be centrifuged drying after product.Although this
Invention shortens the reaction time, reduces reaction temperature to a certain extent, but reaction temperature is still higher, and energy consumption is high；Gained
To cyanuric acid crude product in cyanuric acid content it is lower, therefore the yield of cyanuric acid is relatively low；Subsequent cyanuric acid crude product and sulphur
The reaction of acid is needed by multi-stage reacting kettle, and subsequent refinement treatment is complicated, operates and prepare cumbersome, at high cost and sulfuric acid dosage
Greatly, waste liquid yield is big, is unfavorable for environmental protection；And cyanuric acid purity problem is also not directed in the patent.
Summary of the invention
In view of the deficienciess of the prior art, the present invention provides a kind of good clean manufacturing work of environment of high-purity cyanuric acid
Skill.Reaction temperature of the present invention is low, the reaction time is short, and preparation and operating procedure are simple, and process is easily controllable；The present invention is preferably with sulphur
Heat caused by sulphur Sulphuric acid is heat source, and low energy consumption, environmentally protective；Discharge in production process without pernicious gas and waste liquid,
The recycling that can be realized waste liquid exhaust gas, improves energy utilization rate；Cyanuric acid crude product itself content obtained is high, so that mesh
It marks product yield and purity is higher；Crude product cyanuric acid post-processing refining methd is simple, save the cost, conducive to the industrialization of cyanuric acid
Production.
Technical scheme is as follows:
A kind of production technology of high-purity cyanuric acid, comprising steps of
(1) urea and composite catalyst are uniformly mixed, in 120~270 DEG C of temperature, pressure -0.01~-0.2Mpa item
0.5~7h is reacted under part, obtains cyanuric acid crude product and ammonia；
The composite catalyst is the mixture of ammonium chloride, ammonium nitrate and sodium nitrate composition；
(2) the cyanuric acid crude product that step (1) obtains mixes to obtain mixed liquor with aqueous sulfuric acid after crushed, in 60-170 DEG C
Reaction 3-18 hours, filters to obtain cyanuric acid solid and sulfate liquor；
(3) cyanuric acid solid obtained by step (2) is washed to obtain wet cyanuric acid and acid pickle；Wet cyanuric acid is centrifuged, is dried
Obtain fine work cyanuric acid.
It is preferred according to the present invention, in step (1) described composite catalyst, mole of ammonium chloride, ammonium nitrate and sodium nitrate
Than for 1-3:1-3:1；Preferably, in step (1) described composite catalyst, the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is
2:2:1。
Preferred according to the present invention, the quality of composite catalyst described in step (1) is the 0.5%- of urea quality
1.5%.
Preferred according to the present invention, reaction temperature described in step (1) is 150~250 DEG C, reaction pressure is -0.01~-
0.1Mpa, reaction time are 1~5h.
Preferred according to the present invention, it is 50-100 mesh powder that cyanuric acid crude product, which is ground into partial size, in step (2).
Preferred according to the present invention, the mass concentration of sulfuric acid is 15-25wt%, cyanogen urine in mixed liquor described in step (2)
The mass content of acid crude is 18-25%.
Preferred according to the present invention, gained sulfate liquor and step (3) gained acid pickle can be with mass concentrations in step (2)
The aqueous sulfuric acid in step (2) is used to prepare for the concentrated sulfuric acid mixing circulation of 90wt%-95wt%.
Preferred according to the present invention, reaction temperature described in step (2) is 80-150 DEG C, reaction time 5-15h.
Preferred according to the present invention, the water content of wet cyanuric acid described in step (3) is 17-27wt%.
It is preferred according to the present invention, the content > 98wt% of cyanuric acid in step (3) the fine work cyanuric acid, water content≤
0.5wt%.
Preferred according to the present invention, ammonia obtained in step (1) can be with the sulfate liquor system of reacting obtained in step (2)
Obtain ammonium sulfate.
Preferred according to the present invention, reaction system heats used heat source and prepares heat caused by sulfuric acid from sulphur
Amount.
Technical characterstic of the invention and the utility model has the advantages that
(1) present invention uses Negative pressure during urea reaction, and the ammonia generated can be made quickly to extract out；Locate in this way
The benefit of reason greatly improves the purity of cyanuric acid crude product, cyanuric acid first is that be conducive to the progress of positive reaction in reaction process
The content of cyanuric acid is higher in crude product, is conducive to the yield and purity that improve fine work cyanuric acid, and at the same time after enormously simplifying
The purification step of continuous cyanuric acid crude product；Second is that the timely extraction of ammonia, reduces the leakage of traditional mode of production mode ammonia, improves
The work situation of worker is conducive to environmental protection.
(2) present invention carries out catalysis reaction using composite catalyst, relative to traditional single catalyst, composite catalyst
Various components play synergistic effect, to reduce reaction temperature, accelerate reaction process and reduce side reaction in production process
Occur, to improve the purity and yield of final products cyanuric acid.
(3) Negative pressure is used simultaneously using specific composite catalyst during urea reaction due to the present invention, greatly
Ground improves the purity of cyanuric acid crude product, so urinating in the fine work cyanogen that refining stage only needs a pickling just to obtain high-purity
Acid, cumbersome, that is, the drawbacks of high-purity fine work cyanuric acid can be obtained by needing multiple pickling just for the refining stage of changing over；This hair
Bright purification step is simple, reduces labor intensity, and sulfuric acid solution used is less, and waste liquid yield is few, at low cost and environmentally friendly,
Conducive to the industrialized production of cyanuric acid.
(4) heat in reaction system of the present invention is preferably derived from heat caused by sulphur Sulphuric acid, belongs to waste heat benefit
With, change traditional mode of production using coal as origin of heat, avoid using coal heating caused by air pollution, green ring
It protects；The waste for reducing resource, improves energy utilization rate, and low energy consumption, has saved production cost.
(5) the exhaust gas ammonia and waste liquid sulfate liquor generated in cyanuric acid production process of the present invention can react and prepare sulfuric acid
Ammonium makes in production process without noxious gas emission；Generated sulfate liquor and acid pickle can also prepare sulfuric acid water with the concentrated sulfuric acid
Solution takes full advantage of waste liquid and exhaust gas for the purification of cyanuric acid crude product, realizes the recycling of waste, environmentally protective, into
One step improves energy utilization rate；It can be seen that the method that the present invention prepares cyanuric acid is a kind of environmental-friendly production method.
(6) reaction temperature of the present invention is low, the reaction time is short, and whole preparation and operating procedure are simple, and process is easily controllable, at
This is low, conducive to the industrialized production of cyanuric acid.
Specific embodiment
Below by specific embodiment, the present invention will be further described, but not limited to this.
Raw materials used in embodiment is conventional raw material, commercially available acquisition；The method is existing unless otherwise specified
Technology.
Heat source used is heated in embodiment prepares heat caused by sulfuric acid from sulphur.
Embodiment 1
A kind of good process for cleanly preparing of environment of high-purity cyanuric acid, comprising steps of
(1) 1000g urea and 5g composite catalyst are uniformly mixed heating, at 150 DEG C of temperature, the item of pressure -0.1Mpa
5h is heated under part, pyrolysis obtains cyanuric acid crude product and ammonia；The quality of the composite catalyst is the 0.5% of urea quality；Institute
State the mixture that composite catalyst is ammonium chloride, ammonium nitrate and sodium nitrate composition, the ammonium chloride, ammonium nitrate and sodium nitrate rub
You are 1:1:1；
The purity (i.e. the mass content of cyanuric acid) for being detected cyanuric acid crude product is 85.6%；
(2) cyanuric acid crude product obtained by step (1) is ground into partial size is 50 mesh powders, is added in pickling reaction kettle, adds
The aqueous sulfuric acid for entering 206g 93wt%, adding the mass concentration of sulfuric acid in water modulation mixed liquor is 16.5wt%, cyanuric acid crude product
Mass content be 18.25%；150 DEG C are heated to, reaction was cooled to 80 DEG C after 5 hours, filtered to obtain cyanuric acid solid and sulfuric acid
Mother liquor；
(3) cyanuric acid solid is washed to obtain wet cyanuric acid (water content 17wt%) and acid pickle；Wet cyanuric acid through centrifugation,
Dry fine work cyanuric acid；The purity (i.e. the mass content of cyanuric acid) for being detected fine work cyanuric acid is 98.9%, water content
0.3wt%；Fine work cyanuric acid total recovery is 85.67%；
(4) step (1) pyrolysis gained ammonia, which is reacted with part of sulfuric acid mother liquor obtained by step (2) in ammonia absorption tower, is made sulphur
Sour ammonium；Acid pickle obtained by residual sulfuric acid mother liquor and step (3) can be used for the concentrated sulfuric acid mixing circulation that mass concentration is 93wt%
Aqueous sulfuric acid in preparation step (2).
Embodiment 2
A kind of good process for cleanly preparing of environment of high-purity cyanuric acid, comprising steps of
(1) 1000g urea and 10g composite catalyst are uniformly mixed heating, at 200 DEG C of temperature, pressure -0.05Mpa's
Under the conditions of heat 2.5h, pyrolysis obtains cyanuric acid crude product and ammonia；The quality of the composite catalyst is the 1% of urea quality；
The composite catalyst is the mixture of ammonium chloride, ammonium nitrate and sodium nitrate composition, the ammonium chloride, ammonium nitrate and sodium nitrate
Molar ratio is 2:2:1；
The purity for being detected cyanuric acid crude product is 86.7%；
(2) cyanuric acid crude product obtained by step (1) is ground into partial size is 80 mesh powders, is added in pickling reaction kettle, adds
Enter acid pickle obtained by remaining sulfate liquor after reacting in embodiment 1 with ammonia, 1 step of embodiment (3), mass concentration is
The concentrated sulfuric acid of 93wt%, makes the mass concentration 20wt% of sulfuric acid in gained mixed liquor, and the mass content of cyanuric acid crude product is
20%, 120 DEG C are heated to, reaction was cooled to 50 DEG C after 10 hours, filtered to obtain cyanuric acid solid and sulfate liquor；
(3) cyanuric acid solid is washed to obtain wet cyanuric acid (water content 22wt%) and acid pickle；Wet cyanuric acid through centrifugation,
Dry fine work cyanuric acid；The purity for being detected fine work cyanuric acid is 99.1%, water content 0.2wt%；It is computed, fine work cyanogen urine
Sour total recovery is 87.36%；
(4) step (1) pyrolysis gained ammonia, which is reacted with part of sulfuric acid mother liquor obtained by step (2) in ammonia absorption tower, is made sulphur
Sour ammonium；Acid pickle obtained by residual sulfuric acid mother liquor and step (3) can be used for the concentrated sulfuric acid mixing circulation that mass concentration is 93wt%
Aqueous sulfuric acid in preparation step (2).
Embodiment 3
A kind of good process for cleanly preparing of environment of high-purity cyanuric acid, comprising steps of
(1) 1000g urea and 15g composite catalyst are uniformly mixed heating, at 250 DEG C of temperature, pressure -0.01Mpa's
Under the conditions of heat 1h, pyrolysis obtains cyanuric acid crude product and ammonia；The quality of the composite catalyst is the 1.5% of urea quality；
The composite catalyst is the mixture of ammonium chloride, ammonium nitrate and sodium nitrate composition, the ammonium chloride, ammonium nitrate and sodium nitrate
Mole be 3:3:1；
The purity for being detected cyanuric acid crude product is 86.5%；
(2) cyanuric acid crude product obtained by step (1) is ground into partial size is 100 mesh powders, is added in pickling reaction kettle, adds
Enter and reacts acid pickle obtained by remaining sulfate liquor, 1 step of embodiment (3), mass concentration 93wt% in embodiment 1 with ammonia
The concentrated sulfuric acid, make the mass concentration 25wt% of sulfuric acid in gained mixed liquor, the mass content of cyanuric acid crude product is 25%, is heated
To 150 DEG C, reaction was cooled to 80 DEG C after 15 hours, filtered to obtain cyanuric acid solid and sulfate liquor；
(3) cyanuric acid solid is washed to obtain wet cyanuric acid (water content 27wt%) and acid pickle；Wet cyanuric acid through centrifugation,
Dry fine work cyanuric acid；The purity for being detected fine work cyanuric acid is 99.0%, water content 0.3wt%；It is computed, fine work cyanogen urine
Sour total recovery is 85.96%；
(4) step (1) pyrolysis gained ammonia, which is reacted with part of sulfuric acid mother liquor obtained by step (2) in ammonia absorption tower, is made sulphur
Sour ammonium；Acid pickle obtained by residual sulfuric acid mother liquor and step (3) can be used for the concentrated sulfuric acid mixing circulation that mass concentration is 93wt%
Aqueous sulfuric acid in preparation step (2).
Comparative example 1
A kind of embodiment 1 one in the production technology of cyanuric acid, preparation step and Chinese patent literature CN102532045A
It causes, specific as follows:
1. 300kg urea and 6kg ammonium chloride is taken to be uniformly mixed, mixture is obtained, mixture is placed in ceramic bowl；
2. 1. ceramic bowl that step is contained to mixture is sent into condensation furnace, control condensation furnace temperature is 250 DEG C, heat condensation
Time is 5 hours, obtains cyanuric acid crude product；Through detecting, the purity of cyanuric acid crude product is 75.2%；
3. it is spare that the cyanuric acid crude product of step 2. is crushed to 60-80 mesh；
4. 400L water, the 100kg 98wt% concentrated sulfuric acid and 20kg ammonium hydrogen sulfate is added after mixing in refining kettle, add
Enter step 3. in cyanuric acid crude product crushed material；
5. controlling the vapour pressure of refining kettle between 0.25MPa-0.3MPa, after control refining kettle is warming up to 85 DEG C, essence is adjusted
Steam valve on kettle processed makes temperature be raised slowly to 108 DEG C；
6. keeping at 108 DEG C insulation reaction 4 hours, the material in refining kettle was stirred 20 minutes every 1 hour；
7. rate-determining steps 6. reaction mass, when the cyanuric acid content in material >=98.5%, refining kettle parks steam simultaneously
Blowing cooling, filters, and obtains fine work cyanuric acid after dry.Through detecting, the purity of fine work cyanuric acid is 98.6%, and yield is
81.40%.
As comparing with the present invention it is found that the purity of cyanuric acid crude product obtained by this comparative example is only 75.2%, purity is lower,
It is unfavorable for the high-purity and high yield of fine work cyanuric acid, and uses the refining stage i.e. pickling stages in comparative example very
Complicated pickling means；And the purity of present invention gained cyanuric acid crude product is higher, conducive to the high-purity and high receipts of fine work cyanuric acid
Rate, and make subsequent refining stage i.e. pickling stages simple, it is environmentally protective, it is at low cost, conducive to the industrialized production of cyanuric acid；
Since the purity of this comparative example crude product cyanuric acid is lower, i.e., the content of cyanuric acid is lower in crude product cyanuric acid, leads to final fine work
The yield of cyanuric acid is lower, and in comparative example the purity of fine work cyanuric acid need to can be only achieved by complicated technique the present invention compared with
High purity.
Comparative example 2
A kind of production technology of cyanuric acid, preparation step is as described in Example 1, except that: the reaction in step (1)
Pressure 0Mpa, other steps and condition and embodiment 1 are consistent.
The purity of prepared cyanuric acid crude product is 74.7%；
The purity of prepared fine work cyanuric acid is 94.7%；The total recovery of fine work cyanuric acid is 73.26%.
By this comparative example it is found that negative reaction condition has important influence to the yield and purity of final product, it is conducive to
Obtain the fine work cyanuric acid of high-purity and high yield.
Comparative example 3
A kind of production technology of cyanuric acid, preparation step is as described in Example 1, except that: it is compound in step (1) to urge
Agent replaces with the ammonium chloride of phase homogenous quantities, other steps and condition and embodiment 1 is consistent.
The purity of prepared cyanuric acid crude product is 72.1%；
The purity of prepared fine work cyanuric acid is 93.7%；The total recovery of fine work cyanuric acid is 71.31%.
Comparative example 4
A kind of production technology of cyanuric acid, preparation step is as described in Example 1, except that: it is compound in step (1) to urge
Agent replaces with the ammonium nitrate of phase homogenous quantities, other steps and condition and embodiment 1 is consistent.
The purity of prepared cyanuric acid crude product is 70.6%；
The purity of prepared fine work cyanuric acid is 93.1%；The total recovery of fine work cyanuric acid is 67.96%.
Comparative example 5
A kind of production technology of cyanuric acid, preparation step is as described in Example 1, except that: it is compound in step (1) to urge
Agent replaces with the sodium nitrate of phase homogenous quantities, other steps and condition and embodiment 1 is consistent.
The purity of prepared cyanuric acid crude product is 68.2%；
The purity of prepared fine work cyanuric acid is 92.8%；Cyanuric acid yield is 66.56%.
It is each in composite catalyst by above-mentioned comparative example 3-5 and present invention comparison it is found that the specific composite catalyst of the present invention
A component plays mutually synergistic effect, so that the yield of final product of the present invention and purity are higher.
Claims (10)
1. a kind of production technology of high-purity cyanuric acid, comprising steps of
(1) urea and composite catalyst are uniformly mixed, in 120~270 DEG C of temperature, under conditions of pressure -0.01~-0.2Mpa
0.5~7h is reacted, cyanuric acid crude product and ammonia are obtained；
The composite catalyst is the mixture of ammonium chloride, ammonium nitrate and sodium nitrate composition；
(2) the cyanuric acid crude product that step (1) obtains mixes to obtain mixed liquor with aqueous sulfuric acid after crushed, reacts in 60-170 DEG C
3-18 hours, filter to obtain cyanuric acid solid and sulfate liquor；
(3) cyanuric acid solid obtained by step (2) is washed to obtain wet cyanuric acid and acid pickle；Wet cyanuric acid is centrifuged, dries smart
Product cyanuric acid.
2. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that step (1) is described compound to urge
In agent, the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 1-3:1-3:1；Preferably, step (1) composite catalyst
In, the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 2:2:1.
3. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that compound described in step (1)
The quality of catalyst is the 0.5%-1.5% of urea quality.
4. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that reacted described in step (1)
Temperature is 150~250 DEG C, and reaction pressure is -0.01~-0.1Mpa, and the reaction time is 1~5h.
5. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that by cyanuric acid in step (2)
It is 50-100 mesh powder that crude product, which is ground into partial size,.
6. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that mixed described in step (2)
The mass concentration of sulfuric acid is 15-25wt% in liquid, and the mass content of cyanuric acid crude product is 18-25%.
7. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that gained sulfuric acid in step (2)
Acid pickle obtained by mother liquor and step (3) can be used to prepare step with the concentrated sulfuric acid mixing circulation that mass concentration is 90wt%-95wt%
Suddenly the aqueous sulfuric acid in (2).
8. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that reacted described in step (2)
Temperature is 80-150 DEG C, reaction time 5-15h.
9. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that wet cyanogen described in step (3)
The water content of uric acid is 17-27wt%；
The content > 98wt% of cyanuric acid, water content≤0.5wt% in step (3) the fine work cyanuric acid.
10. the production technology of high-purity cyanuric acid according to claim 1, which is characterized in that ammonia obtained in step (1)
Gas can be reacted with sulfate liquor obtained in step (2) is made ammonium sulfate；
Preferably, reaction system heats used heat source and prepares heat caused by sulfuric acid from sulphur.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810803348.2A CN109053610B (en) | 2018-07-20 | 2018-07-20 | Environment-friendly clean production process of cyanuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810803348.2A CN109053610B (en) | 2018-07-20 | 2018-07-20 | Environment-friendly clean production process of cyanuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109053610A true CN109053610A (en) | 2018-12-21 |
| CN109053610B CN109053610B (en) | 2020-11-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110590688A (en) * | 2019-09-25 | 2019-12-20 | 河北冀衡集团有限公司 | Method for preparing cyanuric acid |
| CN111925337A (en) * | 2020-07-29 | 2020-11-13 | 郑州大学 | Preparation method of cyanuric acid |
| CN112409277A (en) * | 2020-11-26 | 2021-02-26 | 济宁键邦化工有限公司 | Preparation method of cyanuric acid |
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| CN104961699A (en) * | 2015-05-12 | 2015-10-07 | 山东兴达化工有限公司 | Research and application of sulfuric acid combined production cyanuric acid production and steam step electricity utilization generation technology |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590688A (en) * | 2019-09-25 | 2019-12-20 | 河北冀衡集团有限公司 | Method for preparing cyanuric acid |
| CN110590688B (en) * | 2019-09-25 | 2021-11-09 | 河北冀衡集团有限公司 | Method for preparing cyanuric acid |
| CN111925337A (en) * | 2020-07-29 | 2020-11-13 | 郑州大学 | Preparation method of cyanuric acid |
| CN111925337B (en) * | 2020-07-29 | 2023-03-31 | 郑州大学 | Preparation method of cyanuric acid |
| CN112409277A (en) * | 2020-11-26 | 2021-02-26 | 济宁键邦化工有限公司 | Preparation method of cyanuric acid |
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