CN116332863A - Multistage serial cyanuric acid purification system and process - Google Patents
Multistage serial cyanuric acid purification system and process Download PDFInfo
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- CN116332863A CN116332863A CN202310141992.9A CN202310141992A CN116332863A CN 116332863 A CN116332863 A CN 116332863A CN 202310141992 A CN202310141992 A CN 202310141992A CN 116332863 A CN116332863 A CN 116332863A
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- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000746 purification Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 116
- 239000002253 acid Substances 0.000 claims abstract description 56
- 238000005406 washing Methods 0.000 claims abstract description 54
- 238000005554 pickling Methods 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000004744 fabric Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 description 51
- 238000006243 chemical reaction Methods 0.000 description 19
- 239000000047 product Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 239000004202 carbamide Substances 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- YSKUZVBSHIWEFK-UHFFFAOYSA-N ammelide Chemical compound NC1=NC(O)=NC(O)=N1 YSKUZVBSHIWEFK-UHFFFAOYSA-N 0.000 description 4
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NGWKGSCSHDHHAJ-YPFQVHCOSA-N Liquoric acid Chemical compound C1C[C@H](O)C(C)(C)C2CC[C@@]3(C)[C@]4(C)C[C@H]5O[C@@H]([C@](C6)(C)C(O)=O)C[C@@]5(C)[C@@H]6C4=CC(=O)C3[C@]21C NGWKGSCSHDHHAJ-YPFQVHCOSA-N 0.000 description 2
- -1 beta-hydroxyethyl Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229930194542 Keto Natural products 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002587 enol group Chemical group 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000000468 ketone group Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
- B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a multistage serial cyanuric acid purification system and a multistage serial cyanuric acid purification process, wherein the purification system comprises the following steps: crushing the cyanuric acid powder crude product to obtain cyanuric acid powder; carrying out primary pickling on cyanuric acid powder by adopting sulfuric acid solution with the mass percentage of 15% -25%, wherein the mass ratio of the cyanuric acid powder to the sulfuric acid solution is 1:2-3, the primary pickling temperature is 60-80 ℃, and the time is 4-10min; carrying out secondary acid washing on cyanuric acid powder subjected to primary acid washing by adopting 25% -35% sulfuric acid solution, wherein the mass ratio of cyanuric acid powder to 25% -35% sulfuric acid solution is 1:1-1.5, the temperature of the secondary acid washing is 80-100 ℃, and the time is 4-10min; and after the secondary acid washing is finished, cleaning by adopting clear water to remove the acid liquor on the surface of cyanuric acid.
Description
Technical Field
The invention belongs to the technical field of cyanuric acid purification, and particularly relates to a multistage serial cyanuric acid purification system and process.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Cyanuric acid (Cyanuric acid) is also known as Cyanuric acid (Tricyanic acid), and has the chemical formula C 3 H 3 N 3 O 3 There are two isomers, i.e., keto and enol structures, typically as a mixture of the two isomers. White crystallization; slightly bitter in taste, basically non-toxic, can be dissolved in hot water, slightly dissolved in cold water, and its aqueous solution is acidic, and can not be dissolved in cold organic solvents of alcohol, ether and benzene, etc..
Cyanuric acid is a very important chemical synthesis raw material and is mainly used for preparing sodium dichloroisocyanurate, trichloroisocyanuric acid, tri (beta-hydroxyethyl) isocyanurate, triallyl ester, cyanuric acid-formaldehyde resin, epoxy resin, antioxidant, paint, adhesive and medical halogenated trihydroxy oxazine medicines. At present, the serial products developed by cyanuric acid at home and abroad are up to 500, wherein more than 200 products are commercially available, and the products are fine chemical products with high added value, wide application, strong competitiveness and urgent market demand.
The existing methods for synthesizing cyanuric acid mainly comprise urea pyrolysis method, phosgene and ammonia reaction synthesis method, cyanuric acid trimerization method, hydrocyanic acid oxidation method, cyanuric chloride hydrolysis method and the like. The current mainstream technology is urea pyrolysis, the method has a plurality of parallel side reactions, the selectivity of target products is reduced, and the products have a plurality of impurities, wherein the main impurities are biuret, cyanuric acid monoamide and the like. The reliable data show that the content of cyanuric acid in the urea pyrolysis product is only about 70%. Therefore, purification treatment is needed to reach the national first-class standard of 98.5%. However, the purity of the purified cyanuric acid is low, the purification time is long, the energy consumption is high, and the requirements are difficult to meet in many aspects.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a multistage serial cyanuric acid purification system and a multistage serial cyanuric acid purification process.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in a first aspect, the invention provides a multistage serial cyanuric acid purification process, comprising the steps of:
crushing the cyanuric acid powder crude product to obtain cyanuric acid powder;
carrying out primary pickling on cyanuric acid powder by adopting sulfuric acid solution with the mass percentage of 15% -25%, wherein the mass ratio of the cyanuric acid powder to the sulfuric acid solution is 1:2-3, the primary pickling temperature is 60-80 ℃, and the time is 4-10min;
carrying out secondary acid washing on cyanuric acid powder subjected to primary acid washing by adopting 25% -35% sulfuric acid solution, wherein the mass ratio of cyanuric acid powder to 25% -35% sulfuric acid solution is 1:1-1.5, the temperature of the secondary acid washing is 80-100 ℃, and the time is 4-10min;
and after the secondary acid washing is finished, cleaning by adopting clear water to remove the acid liquor on the surface of cyanuric acid.
The primary acid washing is carried out at a relatively low temperature at a relatively low rotation speed, and the primary acid washing aims at impurities such as cyanuric acid monoamide and the like outside the particle size.
The secondary acid washing is carried out at a higher rotating speed, because the material is pasty after the primary acid washing, the contact of the acid liquor and cyanuric acid is not facilitated, at the moment, the stirring at a higher speed has a certain breaking/sticking effect, a better breaking and demulsification effect is achieved on the pasty material, the better contact of the acid liquor and cyanuric acid is facilitated, and a small amount of biuret is converted into cyanuric acid under the effects of higher temperature and higher concentration of sulfuric acid, so that the purity of cyanuric acid is effectively improved.
The cyanuric acid monoamide is easy to be washed away, the biuret needs sulfuric acid with higher concentration to react, and the acid liquor after secondary acid washing can be used for primary acid washing, so that the recycling of the acid liquor is realized, and the cost is saved. If the primary acid washing and the secondary acid washing are carried out simultaneously, the acid concentration is insufficient to quickly react biuret in the cyanuric acid monoamide after the acid washing is finished, so that the purity of the material after the acid washing is low.
In some embodiments, the crude cyanuric acid powder has a particle size of less than 80 mesh after crushing. Cyanuric acid is usually produced through urea pyrolysis, and a pyrolyzed product is often in a big block shape, and is broken to increase the contact area of cyanuric acid and pickling solution, so that the pickling effect is improved.
In some embodiments, the mass percent of the sulfuric acid solution at the time of the primary acid wash is 17% -22%.
Preferably, the primary acid wash temperature is 65-75deg.C.
Preferably, the mass ratio of cyanuric acid powder to sulfuric acid solution is 1:2.5-3 during primary acid washing.
In some embodiments, the mass percent of the sulfuric acid solution at the time of the secondary acid wash is 25% -35%.
Preferably, the mass percentage of the sulfuric acid solution in the secondary acid washing is 27% -32%.
In some embodiments, the agitation speed at the time of the primary acid wash is 90-110r/min; the stirring speed in the secondary acid washing is 140-160r/min.
In some embodiments, when clean water is used for cleaning, acid-resistant filter cloth is paved on the conveyor belt, cyanuric acid is paved on the conveyor belt, and the cyanuric acid is sprayed and cleaned by the clean water.
In a second aspect, the invention provides a multistage serial cyanuric acid purification system, which comprises a primary pickling tank, a secondary pickling tank and a washing tank, wherein the bottom of the primary pickling tank is communicated with the top end of the secondary pickling tank through a pipeline, and the bottom end of the secondary pickling tank is communicated with the washing tank;
a conveyor belt is arranged in the washing tank, and strong acid resistant filter cloth is laid on the conveyor belt;
the conveyor belt is kept at a set distance from the bottom of the washing tank;
the top of the conveyor belt is provided with a spraying layer.
There is no solid-liquid separation device in the middle of the primary pickling tank and the secondary pickling tank, the pickling solution and the material are all fed into the secondary pickling tank through the pipeline after pickling, strong acid resistant filter cloth is arranged between the secondary pickling tank and the washing tank, the filter cloth can realize the purpose of solid-liquid separation, and the spray is arranged above the filter cloth, so that the residual pickling solution can be washed cleanly.
In some embodiments, the spray layer covers the entire length of the conveyor belt.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
in the products of urea pyrolysis, the content of cyanuric acid is only about 70%, purification treatment is needed, the energy consumption of the currently adopted purification process is high, and the production cost of cyanuric acid is increased. The invention provides a multistage series cyanuric acid purification process, which can improve the purity of cyanuric acid from 72% to more than 99%. The whole process has high automation degree and simple and convenient operation, and the product meets the quality requirements of national superior products.
The process has no waste water and waste, is green and environment-friendly, and conforms to the national policy of zero emission.
The process provides a high-efficiency process of multi-stage pickling, the acid concentration, stirring speed and temperature of each stage of pickling are different, the pickling time is greatly shortened, the productivity under the same scale is improved, the energy consumption is reduced, and the national policy of carbon reduction and carbon reduction is complied with.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a flow chart of an acid wash process of an embodiment of the present invention;
FIG. 2 is an arrangement of a strong acid resistant filter cloth according to an embodiment of the present invention;
FIG. 3 is a graph comparing the pre-and post-pickling process of an embodiment of the invention.
In the figure, a: a primary pickling tank; b: a secondary pickling tank; c: a washing tank: (1) the method comprises the following steps A powder crude product inlet; (2) the method comprises the following steps A pickling solution inlet; (3) the method comprises the following steps A stirrer; (4) the method comprises the following steps A connecting pipeline between the primary pickling tank and the secondary pickling tank; (5) the method comprises the following steps A secondary tank discharge port; (6) the method comprises the following steps Strong acid resistant filter cloth; (7) the method comprises the following steps Spraying layer: (8) the method comprises the following steps A washing liquid discharge port; (9) the method comprises the following steps A blow-off valve; the material after washing.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The invention is further illustrated below with reference to examples.
Example 1
After the cyanuric acid powder crude product is crushed, the cyanuric acid powder crude product enters a primary pickling tank A through a powder crude product inlet (1), meanwhile, prepared pickling solution (the ratio of the pickling solution and the adding ratio are described below) enters through a pickling solution inlet (2), the residence time of the mixture in the primary pickling tank A is 5min, the residence time is controlled by controlling the adding amount, the stirring rate in the primary pickling tank A is 100r/min, the primary pickling tank A and the secondary pickling tank B are connected through a pipeline (4), the mixture enters a secondary pickling tank B, the residence time of the mixture in the secondary pickling tank B is 5min, and the stirring rate is 150r/min.
After the mixed material is washed twice, the mixed material falls into a strong acid resistant filter cloth (6) in a washing tank C (the arrangement mode of the strong acid resistant filter cloth is shown as figure 2), and as the conveyor belt rotates forwards, the material enters into a water tank after being sprayed by process water, wherein residual acid liquor is washed, the residual solid falls into a drying container, the compound in the water tank is mainly ammonium sulfate, and crystals can be sold as agricultural fertilizers after being discharged.
The primary washing tank uses 20% sulfuric acid solution, and crude cyanuric acid: the mass ratio of the sulfuric acid solution is 1:2.7, the reaction temperature is 70 ℃, the rotating speed is 100r/min, and the residence time is 5min; the concentration of sulfuric acid solution in the secondary tank is 30%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 90 ℃, rotation speed 150r/min, residence time 5min.
Example 2
The primary washing tank uses 20% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 70 ℃, rotation speed 100r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 30%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 90 ℃, rotation speed 150r/min, residence time 5min.
Example 3
The primary washing tank uses 20% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 70 ℃, rotation speed 150r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 30%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 90 ℃, rotational speed 100r/min, residence time 5min.
Example 4
The primary washing tank uses 30% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 70 ℃, rotation speed 100r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 20%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 90 ℃, rotation speed 150r/min, residence time 5min.
Example 5
The primary washing tank uses 30% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 90 ℃, rotation speed 150r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 20%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 70 ℃, rotational speed 100r/min, residence time 5min.
Example 6
The primary washing tank uses 30% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 90 ℃, rotation speed 100r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 20%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 70 ℃, rotation speed 150r/min, residence time 5min.
Example 7
The primary washing tank uses 15% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 40 ℃, rotation speed 80r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 25%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 60 ℃, rotation speed 120r/min, residence time 5min.
Example 8
The primary washing tank uses 25% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 60 ℃, rotation speed 120r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 15%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 40 ℃, rotation speed 80r/min, residence time 5min.
Example 9
The primary washing tank uses 20% sulfuric acid solution, and crude cyanuric acid: sulfuric acid solution=1:2.7, reaction temperature 70 ℃, rotation speed 100r/min, residence time 5min; the concentration of sulfuric acid solution in the secondary tank is 25%, and the crude cyanuric acid is: sulfuric acid solution=1:1.5, reaction temperature 90 ℃, rotation speed 150r/min, residence time 5min.
The purity of cyanuric acid after pickling in each example is shown in Table 1.
TABLE 1
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A multistage serial cyanuric acid purification process is characterized in that: the method comprises the following steps:
crushing the cyanuric acid powder crude product to obtain cyanuric acid powder;
carrying out primary pickling on cyanuric acid powder by adopting sulfuric acid solution with the mass percentage of 15% -25%, wherein the mass ratio of the cyanuric acid powder to the sulfuric acid solution is 1:2-3, the primary pickling temperature is 60-80 ℃, and the time is 4-10min;
carrying out secondary acid washing on cyanuric acid powder subjected to primary acid washing by adopting 25-35% sulfuric acid solution, wherein the mass ratio of cyanuric acid powder to 25-35% sulfuric acid solution is 1:1-1.5, the temperature of the secondary acid washing is 80-100 ℃, and the time is 4-10min;
and after the secondary acid washing is finished, cleaning by adopting clear water to remove the acid liquor on the surface of cyanuric acid.
2. The multistage tandem cyanuric acid purification process of claim 1, wherein: the grain diameter of the cyanuric acid powder crude product after being crushed is smaller than 80 meshes.
3. The multistage tandem cyanuric acid purification process of claim 1, wherein: the mass percentage of the sulfuric acid solution during primary acid washing is 17% -22%; the temperature of the primary acid washing is 65-75 ℃.
4. A multistage tandem cyanuric acid purification process as claimed in claim 3, wherein: when in primary acid washing, the mass ratio of cyanuric acid powder to sulfuric acid solution is 1:2.5-3.
5. The multistage tandem cyanuric acid purification process of claim 1, wherein: the mass percentage of the sulfuric acid solution in the secondary acid washing is 25% -35%.
6. The process for purifying cyanuric acid in series of claim 5, further comprising: the mass percentage of the sulfuric acid solution in the secondary acid washing is 27% -32%.
7. The process for purifying cyanuric acid in series of claim 6, wherein: the stirring speed during primary acid washing is 90-110r/min; the stirring speed in the secondary acid washing is 140-160r/min.
8. The multistage tandem cyanuric acid purification process of claim 1, wherein: when clean water is adopted for cleaning, acid-resistant filter cloth is paved on the conveyor belt, cyanuric acid is paved on the conveyor belt, and clean water is adopted for spraying and cleaning the cyanuric acid.
9. A multistage tandem cyanuric acid purification system is characterized in that: the device comprises a primary pickling tank, a secondary pickling tank and a washing tank, wherein the bottom of the primary pickling tank is communicated with the top end of the secondary pickling tank through a pipeline, and the bottom end of the secondary pickling tank is communicated with the washing tank;
a conveyor belt is arranged in the washing tank, and strong acid resistant filter cloth is laid on the conveyor belt;
the conveyor belt is kept at a set distance from the bottom of the washing tank;
the top of the conveyor belt is provided with a spraying layer.
10. The multi-stage serial cyanuric acid purification system of claim 9, wherein: the spraying layer covers the whole length direction of the conveyor belt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310141992.9A CN116332863A (en) | 2023-02-17 | 2023-02-17 | Multistage serial cyanuric acid purification system and process |
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| CN202310141992.9A CN116332863A (en) | 2023-02-17 | 2023-02-17 | Multistage serial cyanuric acid purification system and process |
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