CN109053610B - Environment-friendly clean production process of cyanuric acid - Google Patents

Environment-friendly clean production process of cyanuric acid Download PDF

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CN109053610B
CN109053610B CN201810803348.2A CN201810803348A CN109053610B CN 109053610 B CN109053610 B CN 109053610B CN 201810803348 A CN201810803348 A CN 201810803348A CN 109053610 B CN109053610 B CN 109053610B
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cyanuric acid
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cyanuric
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sulfuric acid
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CN109053610A (en
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程仁坤
杨申
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Shandong Xingda Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D251/00Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/12Heterocyclic 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
    • C07D251/26Heterocyclic 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
    • C07D251/30Only oxygen atoms
    • C07D251/32Cyanuric acid; Isocyanuric acid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/54Nitrogen compounds
    • B01D53/58Ammonia
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77Liquid phase processes
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    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • C01C1/242Preparation from ammonia and sulfuric acid or sulfur trioxide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2251/00Reactants
    • B01D2251/50Inorganic acids
    • B01D2251/506Sulfuric acid
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2258/00Sources of waste gases
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    • YGENERAL 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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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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Abstract

The invention provides an environment-friendly clean production process of high-purity cyanuric acid, which comprises the steps of mixing urea and a composite catalyst, and reacting at the temperature of 120-270 ℃ and under the pressure of-0.01-0.2 Mpa to obtain a cyanuric acid crude product; the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate, sodium nitrate and potassium nitrate; crushing the obtained cyanuric acid crude product, mixing the crushed cyanuric acid crude product with a sulfuric acid aqueous solution, reacting at 60-170 ℃, and filtering to obtain cyanuric acid solid; washing, centrifuging and drying the obtained cyanuric acid solid to obtain fine cyanuric acid. The preparation method has simple preparation steps, no harmful gas and waste liquid are discharged in the production process, the waste liquid, waste gas and waste heat can be recycled, and the energy utilization rate is improved; the obtained cyanuric acid crude product has high content, so that the yield and the purity of a target product are high; the post-treatment refining method of the crude cyanuric acid is simple, saves cost and is beneficial to the industrial production of the cyanuric acid.

Description

Environment-friendly clean production process of cyanuric acid
Technical Field
The invention relates to an environment-friendly clean production process of high-purity cyanuric acid, belonging to the technical field of chemical intermediate preparation.
Background
Cyanuric acid is white crystal, odorless and slightly bitter in taste; the method is mainly used for synthesizing chloro derivatives, trichloroisocyanuric acid and sodium or potassium dichloroisocyanurates, and can also be used for preparing cyanuric acid-formaldehyde resin, epoxy resin, antioxidant, coating, adhesive, pesticide herbicide, metal cyaniding corrosion inhibitor, polymer material modifier and the like; the application is wide, and the method is an important raw material for chemical reagents, organic synthesis and drug synthesis.
At present, the main mode for industrially producing cyanuric acid is to heat urea by taking coal as fuel, and prepare cyanuric acid by pyrolysis and condensation of urea; the disadvantages are that: the reaction time is long, the temperature is high, coal and the like are used as fuels, the energy consumption is high, and the environment is not protected; the subsequent refining treatment is complex, the labor intensity is high, and the cost is high; the waste gas ammonia and waste liquid generated by the reaction have serious pollution to the environment, and the production environment of workers is severe; the content of the obtained cyanuric acid crude product is low, so that the yield and the purity of a target product are low.
In view of the above-mentioned disadvantages, many reports have been made on the improvement of cyanuric acid production. For example, chinese patent document CN102532045A discloses a method for producing cyanuric acid from urea, which comprises the following steps: firstly, uniformly mixing urea and ammonium chloride to obtain a mixture, and placing the mixture into a porcelain basin; secondly, sending the porcelain basin containing the mixture into a condensation furnace to obtain a cyanuric acid crude product; thirdly, crushing the cyanuric acid crude product for later use; adding water, concentrated sulfuric acid and ammonium bisulfate into the refining kettle, and then adding the crushed cyanuric acid crude product; controlling the steam pressure of the refining kettle, and adjusting a steam valve on the refining kettle to increase the temperature; maintaining the temperature at 108 deg.c for 4 hr, and stirring the material inside the refining kettle once every 1 hr; seventhly, controlling the reaction materials, and when the content of the cyanuric acid in the materials is more than or equal to 98.5 percent, placing gas in a refining kettle, discharging, cooling, filtering, and drying to obtain fine cyanuric acid. Although the method can improve the yield of the cyanuric acid to a certain extent, the content of the cyanuric acid in the obtained crude cyanuric acid is lower, so that the yield of the cyanuric acid is relatively lower; the subsequent refining and purifying process is complicated, the operation steps are complicated, concentrated sulfuric acid and cyanamide sulfate are required to be used for refining, and the cost and the labor cost are high; the patent takes coal as fuel, and the reaction temperature in the condensation furnace is higher, the energy consumption is high, and the environment is not protected; in addition, harmful gas is generated, and a large amount of waste liquid is generated to pollute the environment. For another example, chinese patent document CN104961699A provides a research and application of sulfuric acid co-production cyanuric acid production and steam cascade utilization power generation process thereof, comprising the following steps: uniformly mixing urea, ammonium chloride and ammonium carbonate, putting the mixture into a porcelain basin in a condensation furnace, controlling the temperature of the condensation furnace to be 175-195 ℃ to obtain a cyanuric acid crude product and flue gas, purifying the flue gas by a purifier, and introducing the purified flue gas into an ammonia absorption tower; uniformly mixing the crushed cyanuric acid crude product and a sulfuric acid solution to obtain a feed liquid; and (3) sequentially pumping the feed liquid into a multistage reaction kettle for reaction to obtain a solid material and a waste acid solution, and washing and centrifugally drying the solid material to obtain a product. Although the invention shortens the reaction time and reduces the reaction temperature to a certain extent, the reaction temperature is still higher and the energy consumption is high; the content of cyanuric acid in the obtained crude cyanuric acid is low, so that the yield of cyanuric acid is relatively low; the subsequent reaction of the cyanuric acid crude product and sulfuric acid needs to pass through a multi-stage reaction kettle, the subsequent refining treatment is complex, the operation and preparation are complex, the cost is high, the sulfuric acid consumption is large, the waste liquid generation amount is large, and the environmental protection is not facilitated; and the problem of cyanuric acid purity is not addressed in this patent either.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an environment-friendly clean production process of high-purity cyanuric acid. The method has the advantages of low reaction temperature, short reaction time, simple preparation and operation steps and easy control of the process; the invention preferably uses the heat generated by preparing the sulfuric acid by the sulfur as a heat source, has low energy consumption and is green and environment-friendly; no harmful gas and waste liquid are discharged in the production process, the waste liquid and the waste gas can be recycled, and the energy utilization rate is improved; the obtained cyanuric acid crude product has high content, so that the yield and the purity of a target product are high; the post-treatment refining method of the crude cyanuric acid is simple, saves cost and is beneficial to the industrial production of the cyanuric acid.
The technical scheme of the invention is as follows:
a production process of high-purity cyanuric acid comprises the following steps:
(1) uniformly mixing urea and a composite catalyst, and reacting for 0.5-7 h at the temperature of 120-270 ℃ and under the pressure of-0.01-0.2 Mpa to obtain a cyanuric acid crude product and ammonia gas;
the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate and sodium nitrate;
(2) crushing the cyanuric acid crude product obtained in the step (1), mixing the crushed cyanuric acid crude product with a sulfuric acid aqueous solution to obtain a mixed solution, reacting at the temperature of 60-170 ℃ for 3-18 hours, and filtering to obtain cyanuric acid solid and sulfuric acid mother liquor;
(3) washing the cyanuric acid solid obtained in the step (2) with water to obtain wet cyanuric acid and waste acid liquid; the wet cyanuric acid is centrifuged and dried to obtain fine cyanuric acid.
According to the invention, in the composite catalyst in the step (1), the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 1-3:1-3: 1; preferably, in the composite catalyst in the step (1), the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 2:2: 1.
Preferably according to the invention, the mass of the composite catalyst in step (1) is 0.5% to 1.5% of the mass of urea.
According to the invention, the reaction temperature in the step (1) is preferably 150-250 ℃, the reaction pressure is-0.01-0.1 Mpa, and the reaction time is preferably 1-5 h.
According to a preferred embodiment of the invention, in step (2), the crude cyanuric acid is ground to a powder having a particle size of 50 to 100 mesh.
According to the invention, the mass concentration of the sulfuric acid in the mixed solution in the step (2) is 15-25 wt%, and the mass content of the cyanuric acid crude product is 18-25%.
According to the invention, preferably, the sulfuric acid mother liquor obtained in the step (2) and the waste acid liquor obtained in the step (3) can be mixed with concentrated sulfuric acid with the mass concentration of 90-95 wt% for recycling to prepare the sulfuric acid aqueous solution in the step (2).
According to the invention, the reaction temperature in the step (2) is preferably 80-150 ℃ and the reaction time is preferably 5-15 h.
Preferably, according to the invention, the moisture content of the wet cyanuric acid in step (3) is 17 to 27 wt.%.
According to the invention, the content of cyanuric acid in the refined cyanuric acid in the step (3) is more than 98 wt%, and the water content is less than or equal to 0.5 wt%.
Preferably, according to the invention, the ammonia gas obtained in step (1) can react with the sulfuric acid mother liquor obtained in step (2) to prepare ammonium sulfate.
According to the invention, the heat source for heating the reaction system is derived from the heat generated by the preparation of sulfuric acid from sulfur.
The invention has the technical characteristics and beneficial effects that:
(1) according to the invention, negative pressure treatment is adopted in the urea reaction process, so that the generated ammonia gas can be rapidly extracted; the treatment has the advantages that the positive reaction in the reaction process is favorably carried out, the purity of the crude cyanuric acid is greatly improved, the content of the cyanuric acid in the crude cyanuric acid is higher, the yield and the purity of fine cyanuric acid are favorably improved, and the subsequent refining step of the crude cyanuric acid is greatly simplified; secondly, the ammonia gas is timely pumped out, thereby reducing the leakage of the ammonia gas in the traditional production mode, improving the labor environment of workers and being beneficial to environmental protection.
(2) The invention adopts the composite catalyst to carry out catalytic reaction, and compared with the traditional single catalyst, various components of the composite catalyst play a synergistic role, thereby reducing the reaction temperature, accelerating the reaction process and reducing the occurrence of side reactions in the production process, and further improving the purity and the yield of the final product cyanuric acid.
(3) Because the invention adopts the specific composite catalyst and the negative pressure treatment in the urea reaction process, the purity of the cyanuric acid crude product is greatly improved, so the high-purity fine cyanuric acid can be obtained only by one-time acid washing in the refining stage, and the defect that the high-purity fine cyanuric acid can be obtained only by multiple acid washing in the refining stage in the past is overcome; the method has the advantages of simple refining steps, labor intensity reduction, less sulfuric acid solution, less waste liquid generation, low cost, environmental protection and contribution to industrial production of cyanuric acid.
(4) The heat in the reaction system is preferably derived from the heat generated by preparing sulfuric acid from sulfur, belongs to waste heat utilization, changes the traditional production that coal is used as a heat source, avoids air pollution caused by heating coal, and is green and environment-friendly; the waste of resources is reduced, the energy utilization rate is improved, the energy consumption is low, and the production cost is saved.
(5) The waste gas ammonia gas generated in the production process of cyanuric acid and the waste liquid sulfuric acid mother liquor can react to prepare ammonium sulfate, so that no harmful gas is discharged in the production process; the generated sulfuric acid mother liquor and the waste acid liquor can also be used for preparing a sulfuric acid aqueous solution with concentrated sulfuric acid for refining a crude product of cyanuric acid, so that the waste liquor and the waste gas are fully utilized, the waste is recycled, the environment is protected, and the energy utilization rate is further improved; therefore, the method for preparing cyanuric acid is an environment-friendly production mode.
(6) The method has the advantages of low reaction temperature, short reaction time, simple integral preparation and operation steps, easy control of the process and low cost, and is beneficial to the industrial production of cyanuric acid.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following specific examples.
The raw materials used in the examples are conventional raw materials and can be obtained commercially; the methods are known in the art unless otherwise specified.
In the embodiment, the heat source for heating is the heat generated by preparing sulfuric acid from sulfur.
Example 1
An environmentally friendly clean production process of high-purity cyanuric acid, comprising the steps of:
(1) mixing 1000g of urea and 5g of composite catalyst uniformly, heating for 5 hours at the temperature of 150 ℃ and under the pressure of-0.1 Mpa, and pyrolyzing to obtain a cyanuric acid crude product and ammonia gas; the mass of the composite catalyst is 0.5 percent of the mass of the urea; the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate and sodium nitrate, and the mol ratio of the ammonium chloride to the ammonium nitrate to the sodium nitrate is 1:1: 1;
the purity of the cyanuric acid crude product (namely the mass content of the cyanuric acid) is 85.6 percent through detection;
(2) crushing the cyanuric acid crude product obtained in the step (1) into powder with the particle size of 50 meshes, adding the powder into an acid washing reaction kettle, adding 206g of 93 wt% sulfuric acid aqueous solution, adding water to adjust the mass concentration of sulfuric acid in the mixed solution to be 16.5 wt%, and adjusting the mass content of the cyanuric acid crude product to be 18.25%; heating to 150 ℃, reacting for 5 hours, cooling to 80 ℃, and filtering to obtain cyanuric acid solid and sulfuric acid mother liquor;
(3) washing cyanuric acid solid with water to obtain wet cyanuric acid (water content is 17 wt%) and waste acid solution; centrifuging and drying the wet cyanuric acid to obtain fine cyanuric acid; the purity (namely the mass content of the cyanuric acid) of the fine cyanuric acid is 98.9 percent and the water content is 0.3 percent by weight; the total yield of the fine cyanuric acid is 85.67 percent;
(4) reacting ammonia gas obtained by pyrolysis in the step (1) with part of sulfuric acid mother liquor obtained in the step (2) in an ammonia gas absorption tower to prepare ammonium sulfate; the residual sulfuric acid mother liquor and the waste acid liquor obtained in the step (3) can be mixed with concentrated sulfuric acid with the mass concentration of 93 wt% for recycling to prepare the sulfuric acid aqueous solution in the step (2).
Example 2
An environmentally friendly clean production process of high-purity cyanuric acid, comprising the steps of:
(1) mixing 1000g of urea and 10g of composite catalyst uniformly, heating for 2.5h at the temperature of 200 ℃ and under the pressure of-0.05 Mpa, and pyrolyzing to obtain a cyanuric acid crude product and ammonia gas; the mass of the composite catalyst is 1% of the mass of the urea; the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate and sodium nitrate, and the molar ratio of the ammonium chloride to the ammonium nitrate to the sodium nitrate is 2:2: 1;
the purity of the cyanuric acid crude product is 86.7 percent through detection;
(2) crushing the cyanuric acid crude product obtained in the step (1) into powder with the particle size of 80 meshes, adding the powder into an acid washing reaction kettle, adding the sulfuric acid mother liquor remaining after the reaction with ammonia in the example 1, the waste acid liquor obtained in the step (3) in the example 1 and concentrated sulfuric acid with the mass concentration of 93 wt%, heating the mixed liquor to 120 ℃, cooling the mixed liquor to 50 ℃ after reacting for 10 hours, and filtering to obtain cyanuric acid solid and sulfuric acid mother liquor;
(3) washing cyanuric acid solid with water to obtain wet cyanuric acid (water content is 22 wt%) and waste acid solution; centrifuging and drying the wet cyanuric acid to obtain fine cyanuric acid; the purity of the fine cyanuric acid is 99.1 percent and the water content is 0.2 percent by weight; the total yield of the fine cyanuric acid is 87.36 percent by calculation;
(4) reacting ammonia gas obtained by pyrolysis in the step (1) with part of sulfuric acid mother liquor obtained in the step (2) in an ammonia gas absorption tower to prepare ammonium sulfate; the residual sulfuric acid mother liquor and the waste acid liquor obtained in the step (3) can be mixed with concentrated sulfuric acid with the mass concentration of 93 wt% for recycling to prepare the sulfuric acid aqueous solution in the step (2).
Example 3
An environmentally friendly clean production process of high-purity cyanuric acid, comprising the steps of:
(1) mixing 1000g of urea and 15g of composite catalyst uniformly, heating for 1h at 250 ℃ and under the pressure of-0.01 Mpa, and pyrolyzing to obtain a cyanuric acid crude product and ammonia gas; the mass of the composite catalyst is 1.5 percent of the mass of the urea; the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate and sodium nitrate, and the mol ratio of the ammonium chloride to the ammonium nitrate to the sodium nitrate is 3:3: 1;
the purity of the cyanuric acid crude product is 86.5 percent through detection;
(2) crushing the cyanuric acid crude product obtained in the step (1) into powder with the particle size of 100 meshes, adding the powder into an acid washing reaction kettle, adding sulfuric acid mother liquor remaining after the reaction with ammonia in the example 1, the waste acid liquor obtained in the step (3) in the example 1 and concentrated sulfuric acid with the mass concentration of 93 wt%, heating the mixed liquor to 150 ℃ and cooling the mixed liquor to 80 ℃ after reacting for 15 hours, and filtering to obtain cyanuric acid solid and sulfuric acid mother liquor;
(3) washing cyanuric acid solid with water to obtain wet cyanuric acid (water content is 27 wt%) and waste acid solution; centrifuging and drying the wet cyanuric acid to obtain fine cyanuric acid; the purity of the refined cyanuric acid is 99.0 percent and the water content is 0.3 percent by weight; the total yield of the fine cyanuric acid is 85.96 percent by calculation;
(4) reacting ammonia gas obtained by pyrolysis in the step (1) with part of sulfuric acid mother liquor obtained in the step (2) in an ammonia gas absorption tower to prepare ammonium sulfate; the residual sulfuric acid mother liquor and the waste acid liquor obtained in the step (3) can be mixed with concentrated sulfuric acid with the mass concentration of 93 wt% for recycling to prepare the sulfuric acid aqueous solution in the step (2).
Comparative example 1
The preparation process of cyanuric acid is consistent with the preparation steps of example 1 in Chinese patent document CN102532045A, and comprises the following steps:
uniformly mixing 300kg of urea and 6kg of ammonium chloride to obtain a mixture, and placing the mixture into a porcelain basin;
secondly, feeding the porcelain basin containing the mixture in the step I into a condensation furnace, controlling the temperature of the condensation furnace to be 250 ℃, and heating the condensation furnace for 5 hours to obtain a cyanuric acid crude product; through detection, the purity of the cyanuric acid crude product is 75.2%;
thirdly, crushing the cyanuric acid crude product obtained in the second step to 60-80 meshes for later use;
adding 400L of water, 100kg of 98 wt% concentrated sulfuric acid and 20kg of ammonium bisulfate into a refining kettle, uniformly mixing, and adding the crushed cyanuric acid crude product in the step (III);
controlling the steam pressure of the refining kettle to be between 0.25MPa and 0.3MPa, controlling the temperature of the refining kettle to rise to 85 ℃, and adjusting a steam valve on the refining kettle to slowly rise the temperature to 108 ℃;
maintaining the temperature at 108 deg.c for 4 hr, and stirring the material inside the refining kettle for 20 min every 1 hr;
seventhly, controlling the reaction materials, and when the content of the cyanuric acid in the materials is more than or equal to 98.5 percent, placing gas in a refining kettle, discharging, cooling, filtering, and drying to obtain fine cyanuric acid. The purity of the fine cyanuric acid is 98.6% and the yield is 81.40% through detection.
Compared with the invention, the purity of the cyanuric acid crude product obtained in the comparative example is only 75.2 percent, the purity is lower, the high purity and the high yield of the fine cyanuric acid are not facilitated, and the refining stage, namely the pickling stage in the comparative example adopts a very complicated pickling means; the purity of the crude cyanuric acid obtained by the method is high, the high purity and the high yield of fine cyanuric acid are facilitated, the subsequent refining stage, namely the pickling stage is simple, green and environment-friendly, the cost is low, and the industrial production of cyanuric acid is facilitated; the purity of the crude cyanuric acid in the comparative example is low, namely the content of the cyanuric acid in the crude cyanuric acid is low, so that the yield of the final fine cyanuric acid is low, and the purity of the fine cyanuric acid in the comparative example can reach the higher purity of the invention only through a complex process.
Comparative example 2
A process for the production of cyanuric acid, the preparation process being as described in example 1, except that: the reaction pressure in step (1) was 0MPa, and the other steps and conditions were the same as those in example 1.
The purity of the prepared cyanuric acid crude product is 74.7%;
the purity of the prepared refined cyanuric acid is 94.7 percent; the total yield of the fine cyanuric acid is 73.26%.
As can be seen from the comparative example, the negative pressure reaction conditions have important influence on the yield and purity of the final product, and are favorable for obtaining high-purity and high-yield fine cyanuric acid.
Comparative example 3
A process for the production of cyanuric acid, the preparation process being as described in example 1, except that: the composite catalyst in step (1) was replaced with ammonium chloride of the same mass, and the other steps and conditions were the same as in example 1.
The purity of the prepared cyanuric acid crude product is 72.1 percent;
the purity of the prepared refined cyanuric acid is 93.7 percent; the total yield of the fine cyanuric acid is 71.31%.
Comparative example 4
A process for the production of cyanuric acid, the preparation process being as described in example 1, except that: the composite catalyst in step (1) was replaced with ammonium nitrate of the same mass, and the other steps and conditions were the same as in example 1.
The purity of the prepared cyanuric acid crude product is 70.6 percent;
the purity of the prepared refined cyanuric acid is 93.1 percent; the total yield of the fine cyanuric acid is 67.96%.
Comparative example 5
A process for the production of cyanuric acid, the preparation process being as described in example 1, except that: the composite catalyst in step (1) was replaced with sodium nitrate of the same mass, and the other steps and conditions were the same as those in example 1.
The purity of the prepared cyanuric acid crude product is 68.2 percent;
the purity of the prepared refined cyanuric acid is 92.8 percent; the yield of cyanuric acid was 66.56%.
As can be seen from the comparison of the above comparative examples 3-5 with the present invention, the specific composite catalyst of the present invention has the synergistic effect of the components in the composite catalyst, so that the final product of the present invention has high yield and purity.

Claims (9)

1. A production process of cyanuric acid comprises the following steps:
(1) uniformly mixing urea and a composite catalyst, and reacting for 1-5 hours at the temperature of 150 ℃ and under the pressure of-0.01 to-0.1 Mpa to obtain a cyanuric acid crude product and ammonia gas;
the composite catalyst is a mixture consisting of ammonium chloride, ammonium nitrate and sodium nitrate; in the composite catalyst, the mol ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 1-3:1-3: 1; the mass of the composite catalyst is 0.5-1.5% of the mass of the urea;
(2) crushing the cyanuric acid crude product obtained in the step (1), mixing the crushed cyanuric acid crude product with a sulfuric acid aqueous solution to obtain a mixed solution, reacting at the temperature of 60-170 ℃ for 3-18 hours, and filtering to obtain cyanuric acid solid and sulfuric acid mother liquor;
(3) washing the cyanuric acid solid obtained in the step (2) with water to obtain wet cyanuric acid and waste acid liquid; the wet cyanuric acid is centrifuged and dried to obtain fine cyanuric acid.
2. The process for producing cyanuric acid according to claim 1, wherein in the composite catalyst of step (1), the molar ratio of ammonium chloride, ammonium nitrate and sodium nitrate is 2:2: 1.
3. The process for producing cyanuric acid according to claim 1, wherein in step (2), the crude cyanuric acid is pulverized into powder having a particle size of 50-100 mesh.
4. The process for producing cyanuric acid according to claim 1, wherein the mass concentration of sulfuric acid in the mixed solution in step (2) is 15-25 wt%, and the mass content of the crude cyanuric acid is 18-25%.
5. The process for producing cyanuric acid according to claim 1, wherein the sulfuric acid mother liquor obtained in step (2) and the spent acid liquor obtained in step (3) are mixed with concentrated sulfuric acid having a mass concentration of 90 wt% to 95 wt% and recycled for use in preparing the aqueous sulfuric acid solution in step (2).
6. The process for producing cyanuric acid according to claim 1, wherein the reaction temperature in step (2) is 80 to 150 ℃ and the reaction time is 5 to 15 hours.
7. The process for producing cyanuric acid according to claim 1, wherein the moisture content of the wet cyanuric acid in step (3) is 17-27 wt%; in the refined cyanuric acid in the step (3), the content of cyanuric acid is more than 98 wt%, and the water content is less than or equal to 0.5 wt%.
8. The process for producing cyanuric acid according to claim 1, wherein the ammonia gas obtained in step (1) is reacted with the sulfuric acid mother liquor obtained in step (2) to produce ammonium sulfate.
9. The process for producing cyanuric acid according to claim 1, wherein the heat source for heating the reaction system is derived from the heat generated in the production of sulfuric acid from sulfur.
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