CN110590688B - Method for preparing cyanuric acid - Google Patents
Method for preparing cyanuric acid Download PDFInfo
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- CN110590688B CN110590688B CN201910913121.8A CN201910913121A CN110590688B CN 110590688 B CN110590688 B CN 110590688B CN 201910913121 A CN201910913121 A CN 201910913121A CN 110590688 B CN110590688 B CN 110590688B
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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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Abstract
The invention discloses a method for preparing cyanuric acid, which comprises the following steps: and (3) wet grinding: carrying out wet grinding on the crude cyanuric acid product to obtain micron-sized coarse cyanuric acid particles; hydrolysis refining step: reacting the crude cyanuric acid particles with dilute sulfuric acid under the action of saturated steam while stirring, and then cooling to obtain refined cyanuric acid; and a water washing step, namely washing, filtering and drying the refined cyanuric acid to obtain fine cyanuric acid. The hydrolysis constant-temperature refining reaction time is short, and only 0.03 ton of steam is consumed by one ton of products; the energy consumption is lower than 0.025 ton standard coal.
Description
Technical Field
The invention relates to the field of preparation of cyanuric acid, and particularly relates to a method for preparing cyanuric acid.
Background
At present, the traditional cyanuric acid hydrolysis production process in China basically adopts the method that a cyanuric acid crude product with the content of about 75-80 percent is crushed by a Raymond mill to obtain cyanuric acid powder with the particle size diameter of about 1 millimeter. Then the qualified cyanuric acid product is prepared by pulp preparation, sulfuric acid hydrolysis refining, temperature reduction, water washing and drying. The production process has 30 years of history in China, and is mainly characterized in that the production process adopts the traditional crushing and normal pressure or pressure hydrolysis refining production, and the main problems of the process are as follows:
1) the reaction time of the normal pressure device is long, and the constant temperature time is up to 8 hours; although the time of the pressurizing device is short, the pressurizing device still needs 3 hours, and the hydrolysis constant-temperature tank has great potential safety hazard in the process of temperature rise and pressurization;
2) the heat quantity needs to be supplemented externally, which causes high steam consumption. Because the method of steam heating is adopted in the refining process of the cyanuric acid crude product sulfuric acid, the longer the reaction time is, the larger the steam consumption is;
3) because the granularity of the crude product after traditional crushing is large, the reaction time is long, the efficiency is low, the occupied area of devices with the same scale is large, and the investment is high;
4) the energy consumption is higher: because of the long reaction time, 0.5 ton of steam is needed for producing 1 ton of cyanuric acid.
Disclosure of Invention
In view of the limitations of the prior art, it is an object of the present invention to provide a process for the preparation of cyanuric acid.
A method of preparing cyanuric acid, comprising:
and (3) wet grinding: carrying out wet grinding on the crude cyanuric acid product to obtain micron-sized coarse cyanuric acid particles;
hydrolysis refining step: and (3) reacting the crude cyanuric acid particles with dilute sulfuric acid under the action of saturated steam while stirring, and then cooling to obtain refined cyanuric acid.
And a water washing step, namely washing, filtering and drying the refined cyanuric acid to obtain fine cyanuric acid.
In the above method for producing cyanuric acid, as a preferred embodiment, in the wet grinding step, the wet grinding is: grinding the crude cyanuric acid product in water to obtain crude product slurry containing micron-sized crude cyanuric acid particles; preferably, the mass ratio of the cyanuric acid crude product to water is 1:2-3, if the water amount is too small, the cyanuric acid crude product is too viscous due to high solid-liquid ratio of materials during grinding, so that a grinding cavity is blocked and cannot work; if the amount of water is too large, the polishing efficiency is lowered. Preferably, the mass ratio of the cyanuric acid crude product to water is 1:3, wherein wet grinding and a certain (for example, 1:3) solid-liquid ratio (wherein solid refers to cyanuric acid crude product) are adopted in the invention, so that the grinding time is shortened by about half compared with dry grinding; preferably, the wet grinding is carried out using zirconia beads having a diameter of 0.6 to 1.2 mm (e.g., 0.7 mm, 0.8 mm, 0.9 mm, 1.0 mm, 1.1 mm); more preferably, the zirconia beads have a diameter of 0.6 to 0.8 mm; the invention uses zirconia beads as grinding balls, and has higher cost performance than other grinding media such as diamond and the like; wherein, zirconia pearl's loading accounts for 80% -90% of grinding the chamber volume, and bulk density is higher, and extrusion energy is high, and unit volume grinds the pearl many to make grind more high-efficient, open the secondary and reunite the phenomenon and can be more thorough. Preferably, the content of the effective component in the crude cyanuric acid (i.e. C in the crude cyanuric acid)3H3N3O3Content of) above 75%, if the crude cyanuric acid isWhen the content of the effective component is less than 75%, acid consumption is increased.
In the above method for producing cyanuric acid, as a preferred embodiment, the micron-sized crude cyanuric acid particles have a particle size of 0.1 to 10 μm.
In the above method for producing cyanuric acid, as a preferred embodiment, in the hydrolysis purification step, the mass ratio of the crude cyanuric acid to the dilute sulfuric acid is 1:1 to 1.5 (e.g., 1: 1.1, 1:1.2,1:1.3,1: 1.4); preferably, the mass ratio of the cyanuric acid crude product to the dilute sulfuric acid is 1: 1.2; preferably, the mass ratio of the cyanuric acid crude product to the saturated steam is 1: 0.02-0.04; more preferably, the mass ratio of the cyanuric acid crude product to the saturated steam is 1: 0.03; proper saturated steam can ensure the reaction temperature and pressure in the hydrolysis refining reaction process and can participate in the hydrolysis reaction, so that monoamide and diamide in crude cyanuric acid can be hydrolyzed to produce fine cyanuric acid. The concentration of the dilute sulfuric acid is 16-18% (mass fraction); the micron-sized material can be in full contact with acid molecules, the reaction is thorough, and the reaction time is reduced, so that the acid consumption is correspondingly reduced.
In the above method for producing cyanuric acid, as a preferred embodiment, in the hydrolysis purification step, the pressure of the saturated steam is 0.3 to 0.4MPa (i.e., the pressure of the steam line), and the temperature is 170-; because the reaction kettle is made of enamel materials, the higher the pressure is, the lower the safety coefficient is, and therefore, the steam pressure of 0.3-0.4MPa is adopted in the invention.
In the above method for producing cyanuric acid, as a preferred embodiment, in the hydrolysis purification step, the stirring speed is 150-.
In the above method for producing cyanuric acid, as a preferred embodiment, in the hydrolysis purification step, the reaction time is 15 to 30 minutes (e.g., 16 minutes, 18 minutes, 20 minutes, 22 minutes, 24 minutes, 26 minutes, 28 minutes).
In the above method for producing cyanuric acid, as a preferred embodiment, in the hydrolysis purification step, the temperature is decreased to 40 ℃ or lower.
In the above method for producing cyanuric acid, as a preferred embodiment, in the washing step, washing is performed until the PH is 3.8 or more, preferably until the PH is 4.0 or more, and the number of washing times is controlled reasonably, so as to ensure not only that the material is qualified but also that no water is wasted.
In the above method for preparing cyanuric acid, as a preferred embodiment, in the water washing step, the vacuum filtration is performed until the water content is below 30% (qualified), wherein the vacuum filtration negative pressure is controlled to be 0.06-0.07 Mpa; preferably, the vacuum filtration is carried out to a moisture content of 26-30%.
In the above method for producing cyanuric acid, as a preferred embodiment, the drying is carried out to a moisture content of 0.3 to 0.5%.
In the above method for producing cyanuric acid, as a preferred embodiment, the wet grinding is performed using a pin-and-rod type nano sand mill; the grinding rod in the sand mill hits a point of the grinding bead in the grinding process, the relative kinetic energy is higher, the movement speed is higher, the linear velocity is high, and the impact force is larger. Preferably, the discharge mesh of the sand mill has a size of 0.1 to 0.3 square mm, which prevents leakage of the grinding beads.
Compared with the prior art, the invention has the following beneficial effects:
1) the rod pin type high-efficiency nano sand mill is adopted, and the advanced grinding technology is adopted to carry out wet superfine grinding on the cyanuric acid crude product, so that the method has the characteristics of high grinding efficiency, high yield and low energy consumption; and the crude cyanuric acid particles with the particle size of 0.1-10 microns can be obtained by grinding under the grinding process condition of the invention. In addition, in the wet grinding process, cyanuric acid and water are fully mixed, and compared with the prior art in which cyanuric acid slurry is additionally prepared after dry grinding, the method disclosed by the invention is more beneficial to the reaction of the subsequent hydrolysis refining step.
2) The wet grinding reduces the particle size of the raw material, thereby improving the reaction speed (the reaction speed can be increased by 20 times) in the hydrolysis refining process so as to achieve the purposes of reducing the reaction device, reducing the investment and improving the safety coefficient of the device.
The reaction equation involved in the hydrolysis refining step of the invention is as follows:
wherein, the main purpose of the hydrolysis reaction of the invention is to remove C in the cyanuric acid crude product3H2N3O2NH2，C3H2N3O(NH2)2Conversion to C3H3N3O3(wherein, C3H2N3O2NH2，C3H2N3O(NH2)2、C3H3N3O3The mixture of the three substances is referred to as crude cyanuric acid).
3) The method has the advantages that the reaction speed is greatly improved, the devices adopted in the preparation process are greatly reduced, the safety coefficient is greatly improved, and the labor intensity of personnel operation is greatly reduced; and the supporting equipment is few, and the occupied area and the test cost can be reduced. In addition, the hydrolysis refining step of the invention does not need to adopt high pressure condition, and only needs 0.3-0.4Mpa, thus greatly reducing the safety of operation.
4) The hydrolysis constant-temperature refining reaction time is short, only 15-30 minutes are needed, and only 0.03 ton of steam is needed for one ton of products; the energy consumption is lower than 0.025 ton of standard coal; the concentration of the sulfuric acid is reduced to 16-18% from the original 25-28%, and the consumption of the sulfuric acid is reduced by 3-6%.
5) In the hydrolysis reaction process, the materials react fully, uniformly and thoroughly, and each index of the refined product can reach the high-quality standard, wherein the content of the refined product cyanuric acid is not less than 99%, the mass content of sulfate radicals is reduced from 0.15% to 0.1%, and the pH value is increased from 3.8 to 4.0. The quality completely reaches the standard of superior products. There may be a move from supplying disinfectants to supplying seeks and the like. The selling price will be greatly increased.
6) The comprehensive energy consumption is lower than that of the original traditional production device by 50 percent, and the equipment continuously runs for 72 hours without blockage; wherein, the small granularity of the grinded particles greatly shortens the reaction time and correspondingly greatly reduces the energy consumption. The material inlet and outlet quantity can be adjusted by speed regulation, and the reaction temperature, the steam addition quantity, the sulfuric acid addition quantity and the acid concentration can be freely adjusted.
Detailed Description
In order that the present invention may be more readily and clearly understood, there now follows a more detailed description of the invention, taken in conjunction with the accompanying detailed description of specific embodiments of the invention. The specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
By simulating and researching the cyanuric acid hydrolysis process, the invention refines the reaction mechanism, selects proper reaction time, temperature and acid concentration, and reduces the generation of waste acid and byproducts; short reaction time is selected, and great energy conservation and consumption reduction are realized; under the same scale as the prior art, the adopted equipment is miniaturized, so that the device is safer and cleaner, the equipment is operated under normal pressure (steam is introduced into the reaction equipment and then is reduced to the normal pressure, and the hydrolysis reaction is carried out under the normal pressure), the operation intensity of workers is reduced, the working environment is improved, the operation process is optimized, the organic unification of human, machine, material, method and ring is realized, the technology is a successful technical change, the success of the project is bound to become a demonstration project of the industry, and the method has great popularization value for the hydrolysis refining production of cyanuric acid.
The preparation process of the invention comprises the following steps: prepared crude slurry → wet grinding → slurry finished by grinding (namely slurry containing micron-sized crude cyanuric acid particles) → ramming material → hydrolytic refining under acidic condition → cooling → material washing → suction filtration → transportation → drying.
The preparation process is completed by adopting the following equipment, wherein the equipment is commercially available equipment, namely a slurry storage tank → a pin-type nano sand mill → a slurry storage tank after grinding → a centrifugal pump (material beating) → an atmospheric pressure hydrolysis reaction tank → a temperature reduction tank (temperature reduction of materials after reaction) → a water washing tank (material washing) → a suction filtration device → conveying (bagging) → a drying system (drying moisture). Each device and its connection relationship are described below.
A device for preparing cyanuric acid, comprising: a slurry storage device for storing a mixed feed liquid (mixed slurry) of the cyanuric acid crude product and water; the pin type nanometer sand mill is used for grinding the mixed feed liquid containing the cyanuric acid crude product; the hydrolysis reactor is used for carrying out hydrolysis refining reaction; one end of the rod pin type nanometer sand mill is connected with the slurry storage tank, and the other end of the rod pin type nanometer sand mill is connected with the hydrolysis reaction tank.
In selecting the rod pin type nano sand mill, the following problems should be noted: the sand mill includes the grinding chamber, the (mixing) shaft is installed at the center in grinding chamber, and is hollow be equipped with the separator in the (mixing) shaft, be favorable to improving grinding and dispersion efficiency, install stirring rotor on the (mixing) shaft, preferably, stirring rotor is jumbo size round pin stick hollow rotor, has overcome traditional sand mill grinding medium uneven distribution's shortcoming and single too little difficult problem of batching, reaches output, the big effect of batch. The rod pin type nanometer sand mill adopts a closed grinding structure design, a short/thick grinding cavity design element and a length/diameter/linear velocity coefficient ratio of a golden section ratio of 16:10 are better, so that materials are fully ground in the cavity, the production efficiency of the high-energy density high-speed bead mill is 5 times that of a common sand mill, and the rod pin type nanometer sand mill is used for continuously or circularly and ultra-finely grinding solid suspended particle materials dispersed in liquid in a large flow.
A centrifugal pump is arranged between the rod pin type nanometer sand mill and the hydrolysis reactor, wherein the slurry ground by the sand mill is placed in a storage tank and then is pumped into the hydrolysis reactor through the centrifugal pump; in an embodiment of the present invention, the hydrolysis reactor is an atmospheric hydrolysis reactor tank.
The device for preparing cyanuric acid further comprises a cooling tank, a water washing tank, a suction filtration device and a drying system.
The material of the rod pin type nanometer sand mill contacted with the crude cyanuric acid is ceramic, which can completely ensure the product quality; the inner surface of the rod pin type nanometer sand mill is acid-resistant stainless steel.
The following is an example of a process for preparing cyanuric acid according to the present invention. The cyanuric acid mass content of the crude cyanuric acid used in the following examples and comparative examples (i.e., cyanuric acid active ingredient C)3H3N3O3Content) of about 78%.
Example 1
A method of preparing cyanuric acid, comprising:
(1) mixing the cyanuric acid crude product and water in a ratio of 1:3, mixing the raw materials according to the mass ratio to prepare mixed feed liquid;
(2) conveying the mixed liquid into a pin-type nanometer sand mill and carrying out nanometer wet sand milling (wherein the wet grinding adopts zirconia beads with the diameter of 0.6-1.2 mm, and the zirconia beads account for about 85% of the volume of a grinding cavity), so as to obtain crude slurry containing 0.1-10 microns of crude cyanuric acid particles;
(3) reacting the crude slurry containing crude cyanuric acid particles with dilute sulfuric acid (17%) under the action of saturated steam (0.35MPa,175 ℃) for 25 minutes while stirring (the stirring speed is 160 revolutions per minute), and then cooling to below 40 ℃;
(4) and (3) washing and filtering the cooled material, sampling, testing the PH value (the PH value is 4.0) to be qualified and testing the moisture to be qualified (the moisture is 30%). Packing into big bags, and sending to a flip-chip storehouse to obtain wet cyanuric acid. Then, the mixture is sent to a drying station and dried until the water content is 0.5 percent to obtain fine cyanuric acid. (wherein, the mass ratio of the cyanuric acid crude product to the dilute sulphuric acid to the steam is 1:1.2:0.03)
In this example, for 1 ton of crude cyanuric acid, 0.03 ton of steam is consumed; the energy consumption is lower than 0.025 ton of standard coal; the concentration of sulfuric acid is reduced to 16-18% from the original 25-28%, and the consumption of sulfuric acid is reduced by 3-6%. The content of cyanuric acid in the refined cyanuric acid is not less than 99 percent, wherein the mass content of sulfate radical is 0.1 percent, and the PH value is 4.0.
The economic benefits which can be realized in the invention year are as follows according to the calculation of 3.5 ten thousand tons per year of cyanuric acid:
1) the cost of per ton of product is reduced by 90 yuan, and the benefit can be increased by 315 ten thousand yuan;
2) the standard coal can be saved by 1100 tons every year;
3) 6 people can be reduced and the management cost is reduced nearly: 30 ten thousand yuan (5 ten thousand yuan per person per year).
Example 2
A method of preparing cyanuric acid, comprising:
(1) mixing the cyanuric acid crude product and water in a ratio of 1:3, mixing the raw materials according to the mass ratio to prepare mixed feed liquid;
(2) conveying the mixed liquid into a pin-type nanometer sand mill and carrying out nanometer wet sand milling (wherein the wet grinding adopts zirconia beads with the diameter of 0.6-1.2 mm, and the zirconia beads account for about 85% of the volume of a grinding cavity), so as to obtain crude slurry containing 0.1-10 microns of crude cyanuric acid particles;
(3) reacting the crude slurry containing the crude cyanuric acid particles with dilute sulfuric acid (20%) under the action of saturated steam (0.4MPa,180 ℃) for 15 minutes while stirring (the stirring speed is 170 rpm), and then cooling to below 40 ℃;
(4) and (3) washing and filtering the cooled material, sampling, testing the PH value (the PH value is 4.0) to be qualified and testing the moisture to be qualified (the moisture is 30%). Packing into big bags, and sending to a flip-chip storehouse to obtain wet cyanuric acid. Then, the mixture is sent to a drying station and dried until the water content is 0.5 percent to obtain fine cyanuric acid. (wherein, the mass ratio of the cyanuric acid crude product to the dilute sulphuric acid to the steam is 1:1.2:0.02)
In this example, for 1 ton of crude cyanuric acid, 0.02 ton of steam is consumed; the energy consumption is lower than 0.025 ton of standard coal; the concentration of sulfuric acid is reduced to 20% from the original 25% -28%, and the consumption of sulfuric acid is reduced by 3%. The content of cyanuric acid in the refined cyanuric acid is not less than 99 percent, wherein the mass content of sulfate radical is 0.1 percent, and the PH value is 4.0.
The economic benefits which can be realized in the invention year are as follows according to the calculation of 3.5 ten thousand tons per year of cyanuric acid:
1. the cost of the product per ton is reduced by 100 yuan, and the benefit can be increased by 350 ten thousand yuan;
2. 1220 tons of standard coal can be saved in a year;
3. 6 people can be reduced and the management cost is reduced nearly: 30 ten thousand yuan (5 ten thousand yuan per person per year).
Example 3
A method of preparing cyanuric acid, comprising:
(1) mixing the cyanuric acid crude product and water in a ratio of 1:3, mixing the raw materials according to the mass ratio to prepare mixed feed liquid;
(2) conveying the mixed liquid into a pin-type nanometer sand mill, and carrying out micron wet sand milling (wherein the wet grinding adopts zirconia beads with the diameter of 1.6-2 mm, and the zirconia beads account for about 85% of the volume of a grinding cavity), so as to obtain crude slurry containing crude cyanuric acid particles with the particle size of more than 10 microns, wherein the particle size of the crude cyanuric acid particles is 10-20 microns;
(3) reacting the crude slurry containing crude cyanuric acid particles with dilute sulfuric acid (24%) under the action of saturated steam (0.4MPa,180 ℃) for 3 hours while stirring (the stirring speed is 170 rpm), and then cooling to below 40 ℃;
(4) and (3) washing, filtering, sampling, testing the PH value (the PH value is 3.8) and the moisture (the moisture is 30%) of the cooled material, and determining the qualified PH value and the qualified moisture. Packing into big bags, and sending to a flip-chip storehouse to obtain wet cyanuric acid. Then, the mixture is sent to a drying station and dried until the water content is 0.5 percent to obtain fine cyanuric acid; (wherein, the mass ratio of the cyanuric acid crude product to the dilute sulfuric acid to the steam is 1:1.4: 0.36).
In this example, for 1 ton of crude cyanuric acid, 0.36 ton of steam is consumed; the energy consumption is 0.04 ton of standard coal; and sulfuric acid is concentrated by 24 percent. The content of cyanuric acid in the refined cyanuric acid is 98 percent, wherein the mass content of sulfate radical is 0.15 percent, and the PH value is 3.8.
By comparison of the above analyses, there would be no cost advantage to milling particle sizes above 10 microns.
Comparative example
Crushing the cyanuric acid crude product by a Raymond mill to obtain cyanuric acid powder with the particle size diameter of about 1 mm;
then mixing the cyanuric acid powder and water according to the mass ratio of 1:3 to prepare slurry;
adding a dilute sulfuric acid solution (26%) into the slurry, reacting for 8 hours under the action of saturated steam (0.4MPa,180 ℃) while stirring (the stirring speed is 170 rpm), and then cooling to below 40 ℃ (wherein the mass ratio of the cyanuric acid crude product to the dilute sulfuric acid to the steam is 1:1.5: 0.5);
the treatment was carried out according to the washing, suction filtration and drying steps of example 3.
In this comparative example, 0.5 ton of steam was consumed for 1 ton of crude cyanuric acid; the energy consumption is 0.05 ton of standard coal. The content of cyanuric acid in the refined cyanuric acid is 98.5 percent, wherein the mass content of sulfate radical is 0.15 percent, and the PH value is 3.8.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (12)
1. A method of preparing cyanuric acid, comprising:
and (3) wet grinding: carrying out wet grinding on the crude cyanuric acid to obtain micron-sized coarse cyanuric acid particles, wherein the particle size of the micron-sized coarse cyanuric acid particles is 0.1-10 microns; the wet grinding comprises the following steps: grinding the cyanuric acid crude product in water to obtain crude product slurry containing micron-sized crude cyanuric acid particles, wherein the mass ratio of the cyanuric acid crude product to the water is 1: 2-3; the wet grinding adopts zirconia beads with the diameter of 0.6-1.2 mm for grinding, and the filling amount of the zirconia beads accounts for 80-90% of the volume of the grinding cavity;
hydrolysis refining step: reacting the crude product slurry containing the micron-sized crude cyanuric acid particles with dilute sulfuric acid under the action of saturated steam under stirring, and then cooling to obtain refined cyanuric acid, wherein the pressure of the saturated steam is 0.3-0.4MPa, the temperature is 170-180 ℃, and the reaction time is 15-30 minutes; the mass ratio of the cyanuric acid crude product to the dilute sulfuric acid is 1:1-1.5, and the concentration of the dilute sulfuric acid is 16% -18%;
and a water washing step, namely washing, filtering and drying the refined cyanuric acid to obtain fine cyanuric acid.
2. The method as claimed in claim 1, wherein the mass ratio of the crude cyanuric acid to water is 1: 3.
3. The method of claim 1, wherein C is in the crude cyanuric acid3H3N3O3The content of (A) is more than 75%.
4. The method as claimed in claim 1, wherein the mass ratio of the crude cyanuric acid to the dilute sulfuric acid is 1: 1.2.
5. The method as set forth in claim 1, wherein the stirring speed in the hydrolysis refining step is 150-180 rpm.
6. The method of claim 1, wherein the temperature is reduced to below 40 ℃.
7. The method according to claim 1, wherein in the water washing step, the washing is carried out to a pH of 3.8 or more.
8. The method of claim 7, wherein the washing is carried out with water to a pH of 4.0 or higher.
9. The method according to claim 1, wherein in the water washing step, the suction filtration is vacuum filtration, the vacuum filtration negative pressure is controlled to be 0.06-0.07Mpa, and the vacuum filtration is performed until the moisture is below 30%.
10. The method according to claim 9, wherein the vacuum filtration is carried out to a moisture of 26-30%.
11. The method of claim 1, wherein said drying is to a moisture content of 0.3-0.5%.
12. The method of claim 1, wherein the wet grinding is performed using a pin and rod nano-sand mill.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07188193A (en) * | 1993-12-27 | 1995-07-25 | Mitsui Toatsu Chem Inc | Production of melamine cyanurate |
| CN101830859A (en) * | 2010-05-14 | 2010-09-15 | 菏泽沃蓝化工有限公司 | Production method of isocyanuric acid |
| CN102532045A (en) * | 2011-12-14 | 2012-07-04 | 山东大明消毒科技有限公司 | Method for producing cyanuric acid from urea used as raw material |
| CN109053610A (en) * | 2018-07-20 | 2018-12-21 | 山东兴达化工有限公司 | A kind of good process for cleanly preparing of environment of high-purity cyanuric acid |
-
2019
- 2019-09-25 CN CN201910913121.8A patent/CN110590688B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07188193A (en) * | 1993-12-27 | 1995-07-25 | Mitsui Toatsu Chem Inc | Production of melamine cyanurate |
| CN101830859A (en) * | 2010-05-14 | 2010-09-15 | 菏泽沃蓝化工有限公司 | Production method of isocyanuric acid |
| CN102532045A (en) * | 2011-12-14 | 2012-07-04 | 山东大明消毒科技有限公司 | Method for producing cyanuric acid from urea used as raw material |
| CN109053610A (en) * | 2018-07-20 | 2018-12-21 | 山东兴达化工有限公司 | A kind of good process for cleanly preparing of environment of high-purity cyanuric acid |
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