CN102516188A - Preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid - Google Patents
Preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid Download PDFInfo
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- CN102516188A CN102516188A CN2011104107983A CN201110410798A CN102516188A CN 102516188 A CN102516188 A CN 102516188A CN 2011104107983 A CN2011104107983 A CN 2011104107983A CN 201110410798 A CN201110410798 A CN 201110410798A CN 102516188 A CN102516188 A CN 102516188A
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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 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 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 title claims abstract description 19
- 229950009390 symclosene Drugs 0.000 title claims abstract description 18
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 title abstract 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 101
- 239000000463 material Substances 0.000 claims abstract description 91
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000007670 refining Methods 0.000 claims abstract description 39
- 239000002253 acid Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000007664 blowing Methods 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- 238000010792 warming Methods 0.000 claims description 19
- 239000011343 solid material Substances 0.000 claims description 18
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 17
- 210000004916 vomit Anatomy 0.000 claims description 16
- 230000008673 vomiting Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 235000011149 sulphuric acid Nutrition 0.000 claims description 14
- 239000001117 sulphuric acid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 230000004927 fusion Effects 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 abstract description 2
- 235000011130 ammonium sulphate Nutrition 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000012043 crude product Substances 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 238000005520 cutting process Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- VEMGMDZKKZMAIQ-UHFFFAOYSA-N 7,9-dihydro-3H-purine-2,6,8-trione 2,2,2-trichloroacetonitrile Chemical compound N1C(=O)NC=2NC(=O)NC2C1=O.ClC(C#N)(Cl)Cl VEMGMDZKKZMAIQ-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 0 O=C(*CN1)NC1=O Chemical compound O=C(*CN1)NC1=O 0.000 description 2
- 241000237502 Ostreidae Species 0.000 description 2
- 150000001880 copper compounds Chemical class 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000020636 oyster Nutrition 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 1
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 238000009827 uniform distribution Methods 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid comprises the following steps of: uniformly mixing urea and a catalyst ammonium sulfate, adding the mixture into a reaction vessel, forming a uniform thin material layer on a conveyor belt when the materials reach a certain temperature, liquid viscosity is increased and the liquid is still at a liquid state, and allowing the thin material layer to pass through a tunnel type heating chamber of a tunnel type heating device for heating at high temperature such that the temperature of the materials is rapidly raised to 250-280 DEG C in a short time. As the reaction time of the materials is short and the reaction speed is fast, there are few side effects and product decomposition is low. The cyanuric acid crude product prepared in the invention has high purity and high yield. During the refining process, inorganic dilute acid is used to process the cyanuric acid crude product. After centrifugation, a cyanuric acid refined product is directly used in the synthesis of its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid without being dried. By the adoption of the method, the adhesive problem of heating surface in production preparation is solved, production speediness and continuity are realized, and industrial production efficiency is raised.
Description
Technical field
The present invention relates to a kind of preparation method of cyanuric acid; The invention still further relates to the verivate Surchlor GR 60 of cyanuric acid and the preparation method of trichloroisocyanuric acid; The preparation field that belongs to the industrial chemicals midbody, putting it briefly is the preparation method of a kind of high yield cyanuric acid and dichloro thereof, three chlorine derivatives.
Background technology
Cyanuric acid belongs to the midbody of Organic Chemicals; Use extremely extensive; Be mainly used in producing of cyanuric acid muriate, salt, ester class; SYNTHETIC OPTICAL WHITNER, resin, oxidation inhibitor, paint, selective herbicide and metal cyanide negative catalyst synthetic, and as the additive of nylon, fire-retardant for plastic and makeup, in organic synthesis, occupy an important position.Cyanuric acid synthetic has many methods, like cyanic acid polymerization, cyanuric chloride hydrolysis, phosgene and ammonia react, uric acid oxidation, the condensation of urea in high boiling organic solvent etc.The raw material that these methods have, technological process is poisonous or complicated, and the cost that has is high, is difficult to large-scale industrial production, and industriallization at present is a difficult problem, and cyanuric acid adopts the urea melting condensation method to produce.Adopting the urea melting condensation method to produce in the process of cyanuric acid, the physical condition of reactant from liquid, white opacity thickness state to solid-state.At first obtain low viscous relatively limpid liquid, continue to be heated to certain temperature, the liquid thickness more that becomes, when finally generating cyanuric acid, completely solidified.With regard to regard to the heating surface direct control, it is difficult avoiding the adhesion at heating surface.CN1121513A discloses a kind of cyanuric acid prepared by solvent induced pyrolysis method; It is urea in a certain amount of hydrogen peroxide and less water, be catalyzer with platinic compound or copper compound or platinum, copper compound, on family expenses microwave oven or electric furnace, heat; Make its rapid reaction, obtain cyanuric acid.Again cyanuric acid is dissolved in hot water, lets its cooling leave standstill, can contain the cyanuric acid of 2 crystal water.This method can be accomplished reaction in 2 ~ 10 minutes.CN1749251A discloses a kind of preparation method of cyanuric acid, includes preparation, hydrolysis and three operations of washing of cyanuric acid bullion.Wherein hydrolyzing process is: cyanuric acid bullion, saturated hot steam and the sulfuric acid that makes after using three pump lines with the urea reacting by heating respectively is transported at least by in two first reaction towers in the reaction tower that pipeline is communicated with continuously; Control the vitriolic flow simultaneously, sulfuric acid concentration, the flow of cyanuric acid bullion, reaction back cooling and through washing with separate cyanuric acid.CN101429169A discloses a kind of preparing white cyanuric acid, may further comprise the steps: stir down, fused urea is added in the organic solvent also feeds rare gas element simultaneously, after the condensation reaction, get hot slurry; Under the agitation condition, add quench liquid in the thermotropism slurry, after cooling, obtain cold slurry; Cold slurry is carried out solid-liquid separation, get filter cake; With filter cake, under certain temperature and mobile inert gas conditions, carry out drying, get the white pyruric acid xln.More than these technology for how solving in the product prepn at the sticking problem of heating surface and production changed rapidly, continuously, thereby improve the efficiency of suitability for industrialized production, do not provide concrete guidance program.
Summary of the invention
Technical problem to be solved by this invention is, a kind of preparation method of cyanuric acid is provided, and this preparation method can solve in the product prepn sticking problem at heating surface, and production is changed rapidly, continuously, thereby improves the efficient of suitability for industrialized production.
Technical problem to be solved by this invention also is; A kind of verivate Surchlor GR 60 of cyanuric acid, the preparation method of trichloroisocyanuric acid are provided; This preparation method can solve in the product prepn sticking problem at heating surface; And production is changed rapidly, continuously, thereby improve the efficient of suitability for industrialized production.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of preparation method of cyanuric acid; Its technical scheme is; It is to process the cyanuric acid product through following process successively: be that the mixed of 1:0.1 ~ 0.2 is even with urea and catalyst sulfuric acid ammonium according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150 ~ 190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185 ~ 190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1 ~ 3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15 ~ 20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250 ~ 280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5 ~ 2 with the ratio of the weight of inorganic diluted acid, is warming up to 95 ~ 100 ℃, is incubated 1.5 ~ 2 hours; Be cooled to 25 ~ 30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20% ~ 25% wet feed cyanuric acid elaboration; 7. the vacuum-drying of wet feed cyanuric acid elaboration is obtained the cyanuric acid product.
In the technique scheme, said step 2. in, the temperature of controlling thermal oil in the chuck of said reaction kettle is preferably 190 ℃.Above-mentioned steps 3. in; The homocline vomit pipe preferably has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals.Above-mentioned tunnel like heating unit can be the tunnel type micro wave heating unit.The length of the tunnel like heating chamber of above-mentioned tunnel like heating unit can be 20 meters.Above-mentioned steps 6. in, inorganic diluted acid can be 18% ~ 23% dilute sulphuric acid for massfraction.
A kind of preparation method of verivate Surchlor GR 60 of cyanuric acid; Its technical scheme is; It is to process the Surchlor GR 60 product through following process successively: be that the mixed of 1:0.1 ~ 0.2 is even with urea and catalyst sulfuric acid ammonium according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150 ~ 190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185 ~ 190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1 ~ 3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15 ~ 20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250 ~ 280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5 ~ 2 with the ratio of the weight of inorganic diluted acid, is warming up to 95 ~ 100 ℃, is incubated 1.5 ~ 2 hours; Be cooled to 25 ~ 30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20% ~ 25% wet feed cyanuric acid elaboration; 7. wet feed cyanuric acid elaboration does not need drying, and it is directly produced its verivate Surchlor GR 60 by ordinary method, finally obtains the Surchlor GR 60 product.
In the technique scheme; Said homocline vomit pipe preferably has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals; The tunnel like heating unit can be the tunnel type micro wave heating unit, and the length of the tunnel like heating chamber of above-mentioned tunnel like heating unit can be 20 meters; Above-mentioned steps 6. in, inorganic diluted acid can be 18% ~ 23% dilute sulphuric acid for massfraction.
A kind of preparation method of verivate trichloroisocyanuric acid of cyanuric acid; Its technical scheme is; It is to process the trichloroisocyanuric acid product through following process successively: be that the mixed of 1:0.1 ~ 0.2 is even with urea and catalyst sulfuric acid ammonium according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150 ~ 190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185 ~ 190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1 ~ 3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15 ~ 20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250 ~ 280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5 ~ 2 with the ratio of the weight of inorganic diluted acid, is warming up to 95 ~ 100 ℃, is incubated 1.5 ~ 2 hours; Be cooled to 25 ~ 30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20% ~ 25% wet feed cyanuric acid elaboration; 7. wet feed cyanuric acid elaboration does not need drying, and it is directly produced its verivate trichloroisocyanuric acid by ordinary method, finally obtains the trichloroisocyanuric acid product.
In the technique scheme; Said homocline vomit pipe has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals; The tunnel like heating unit can be the tunnel type micro wave heating unit, and the length of the tunnel like heating chamber of above-mentioned tunnel like heating unit can be 20 meters; Above-mentioned steps 6. in, inorganic diluted acid can be 18% ~ 23% dilute sulphuric acid for massfraction.
The present invention is after urea and catalyst sulfuric acid ammonium are mixed; Add in the reaction kettle, when material reaches certain temperature (185 ~ 190 ℃), liquid viscosity increases and still appears liquid the time; Deliver on the travelling belt; Material forms uniform material thin layer on travelling belt, the pass through tunnel tunnel like heating chamber of formula heating unit of material thin layer carries out heat, and material is warming up to 250 ~ 280 ℃ in the short period of time rapidly.Because the material reaction time is short, speed is fast, thereby side reaction is few, and product decomposes low.Prepared cyanuric acid bullion purity is high, and yield is high.In treating process, use inorganic diluted acid to handle the cyanuric acid bullion, after spinning, the cyanuric acid elaboration directly is used for the synthetic of its verivate Surchlor GR 60 and trichloroisocyanuric acid without drying.This method technology is simple, and product can the adhesive reaction still in the preparation process, and facility investment is little, and throughput is big, is suitable for suitability for industrialized production.
In sum, the present invention is corresponding suitable viscosity when the certain temperature point of reaction solution (feed liquid), makes material can be dispersed into thin layer but can arbitrarily not trickle; The material thin layer at high temperature solidifies the generation cyanuric acid; Saved the reaction times, improved reaction yield, solved in the product prepn sticking problem at heating surface; And production is changed rapidly, continuously, improved the efficient of suitability for industrialized production.
Description of drawings
Fig. 1 is the structural representation of the present invention when preparing the cyanuric acid bullion.
Embodiment
With reference to Fig. 1; The present invention's used equipment (mainly) when preparation cyanuric acid bullion has mixer 1, has reaction kettle 2, homocline vomit pipe (cloth tube) 3, tunnel like heating unit (tunnel like heating system, or perhaps tunnel like heat drying equipment) 4, cutting knife 5, the kibbler 6 of thermal oil circulation type of heating.Tunnel like heating unit 4 has a pair of transfer roller (cylinder), travelling belt 41, tunnel like heating chamber 42, (and the frame of not drawing among the figure, transport tape drive-motor etc.), and the length of said tunnel like heating chamber 42 can be 20 meters; Travelling belt is also referred to as transfer plate, can be processed by steel plate, and travelling belt is installed on a pair of transfer roller, the travelling belt 41 formula heating chamber 42 that passes through tunnel.4 of tunnel like heating units can be the tunnel type micro wave heating unit as prior art, and it comprises tunnel like heating chamber (chamber) and microwave generator, and several microwave heating box are formed tunnel type micro wave heating chamber (chamber).Certainly, the tunnel like heating unit can also be the tunnel like tubing heating system.The drain hole of mixer 1 is connected with the opening for feed of reaction kettle 2, and the autoclave body bottom of reaction kettle 2 is provided with blowing bottom valve (being tapping hole), and Reference numeral 21 is a heat conductive oil inlet, and Reference numeral 22 is the thermal oil outlet.Homocline vomit pipe 3 has to be connected with the blowing bottom valve of reaction kettle and (is connected; Can be to be threaded) pipeline 31, the horizontal pipeline 32 that is connected with this pipeline 31, a plurality of laterals 33 that are connected with this horizontal pipeline 32, be fixed in the scraper plate 34 on the horizontal pipeline 32; Said horizontal pipeline 32 is along width (or perhaps the fore-and-aft direction of travelling belt of travelling belt 41; Be edge and the vertical direction of the traffic direction of travelling belt 41; The traffic direction of travelling belt 41 upper ends is for from left to right) stretch, said a plurality of laterals 33 are (side by side) uniform distribution at the width of horizontal pipeline 32 upper edge travelling belts 41.The width of the total width of said a plurality of lateral 33 and travelling belt 41 is suitable; Scraper plate 34 is positioned at the back (being right-hand member or right side) of said a plurality of lateral 33; Scraper plate 34 is compared with said a plurality of laterals in other words conj.or perhaps; It is positioned at the front of the traffic direction of travelling belt 41; Said a plurality of lateral 33, scraper plate 34 are positioned at the travelling belt top of feeding mouth one end of tunnel like heating unit; Said a plurality of lateral 33 can be 10 ~ 20mm with the distance of travelling belt (material-dropping face of upper end), and scraper plate 34 is 1 ~ 3mm with the distance of travelling belt (material-dropping face of upper end), and scraper plate 34 shakeouts said a plurality of lateral 33 effusive materials that are positioned on the travelling belt 41.Above-mentioned pipeline 31, horizontal pipeline 32, a plurality of lateral 33 can be processed by stainless-steel pipe, and its mode of connection can be welding or be threaded; Scraper plate can be processed by stainless-steel sheet, and it can be welding with horizontal pipeline 32 or be threaded, and can regulate the relative position of scraper plate and horizontal pipeline if adopt to be threaded, and then regulates the distance of the material-dropping face of scraper plate and travelling belt upper end.Above-mentioned cutting knife 5 can be processed by stainless-steel sheet, and cutting knife 5 can be by frame (perhaps base) support limit (location), cutting knife 5 be inclined to set (tilting with the higher form of the lower and the other end of an end); The edge of a knife of cutting knife (knife edge) end higher (its width quite perhaps equates with the length of transfer roller); The transfer roller place that is positioned at discharge port one end of above-mentioned tunnel like heating unit (is positioned at the outside of transfer roller, a little less than 3 ~ 5 millimeters on the top of the outer circumference surface of this transfer roller, can contact with this transfer roller; The edge of a knife of cutting knife and the horizontal throw of this transfer roller can be 0.5 ~ 1 millimeter; Certainly, the edge of a knife of cutting knife also can contact with the outer circumference surface of transfer roller, and the edge of a knife of cutting knife and the outer circumference surface of transfer roller form combining site); Like this solid materials thin slice herein (being said combining site) be cut off (be sliding trackle or shovel broken; Accomplish section, section is promptly cut off), and the other end of cutting knife is connected with the feeding mouth of kibbler 6; Cut solid materials thin slice gets into kibbler pulverizing (obtaining the cyanuric acid bullion) along the cutter hub (landing voluntarily) of cutting knife; Kibbler 6 can be enterprising material formula, also can be feed type (present embodiment adopts feed type down) down, and 6 in kibbler is as prior art.
Embodiment 1: the preparation method of (high yield) cyanuric acid processes (referring to the following reaction formula) of cyanuric acid product successively through following process:
1. be that the ratio of 1:0.1 mixes in mixer that (urea should be even with mixing of catalyst sulfuric acid ammonium with 1500 kg urea and 150 kg catalyst ammonium sulfate according to its weight ratio; Side reaction to reduce urea takes place); It is joined in (2000 liters) reaction kettle that has thermal oil circulation type of heating, open and stir.2. the temperature of controlling thermal oil in the chuck of said reaction kettle is 190 ℃, opens the chuck valve, feeds deep fat, and intensification material, material melt (90 ℃ time become paste liquid) gradually in the time of 80 ~ 90 ℃.Material becomes limpid liquid (clarified liq) when being warmed up to 110 ~ 130 ℃ (present embodiment is 120 ℃).3. after the complete fusion of material, continue to heat up, when being warmed up to 180 ℃, it is muddy that material begins to become, and presents oyster white.(present embodiment is 185 ℃ to continue to be warming up to 185 ~ 190 ℃; This moment, said liquid was creamy white); Open the blowing bottom valve of reaction kettle,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle.4. regulate dispensing speed; The control material is formed the material thin layer (laminated layer that thickness is 1 ~ 3mm (present embodiment is 2mm) on travelling belt; Thin slice); Said material thin layer on the travelling belt passes the tunnel like heating chamber of (promptly through or through) above-mentioned tunnel like heating unit through 15 ~ 20 minutes motion times spent (present embodiment is 20 minutes) of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250 ~ 280 ℃ (present embodiment is 270 ℃), and obtains white solid material thin slice.5. with the solid materials thin slice through section, pulverize, obtain the cyanuric acid bullion, get into refining step (pack into deliver to refining step with the cyanuric acid bullion in the enamel waggon) then.6. at refining step, in refining kettle, add inorganic diluted acid, inorganic diluted acid can be 18% ~ 23% dilute sulphuric acid (massfraction of present embodiment dilute sulphuric acid is 20%) or Hydrogen chloride for massfraction; Again the cyanuric acid bullion is dropped into (conveying) in refining kettle, promptly in refining kettle, add 1500 kilograms of (massfraction is 20%) dilute sulphuric acids, drop into 1000 kilograms of cyanuric acid bullions; The ratio of the weight of cyanuric acid bullion and dilute sulphuric acid (inorganic diluted acid) is 1:1.5; Open steam, be warming up to 95 ~ 100 ℃ (present embodiment is 100 ℃), be incubated 1.5 ~ 2 hours (present embodiment is 2 hours); Steam off; ON cycle water is cooled to 25 ~ 30 ℃ (present embodiment is 25 ℃), is discharged to whizzer through the blowing bottom valve of refining kettle; Centrifuge dripping (isolating solid with whizzer) obtains water cut and is 1300 kilograms of the wet feed cyanuric acid elaboration of 20% (weight percent).7. 60 ℃ of vacuum-dryings of wet feed cyanuric acid elaboration are obtained cyanuric acid product (finished product), content 99%, molar yield: 96%.
Embodiment 2: the preparation method of (high yield) cyanuric acid processes the cyanuric acid product through following process successively:
1. 1500 kg urea and 300 kilograms of (perhaps 200 kilograms) catalyst sulfuric acid ammoniums are mixed in mixer that (urea should be even with mixing of catalyst sulfuric acid ammonium; Side reaction to reduce urea takes place); It is joined in (2000 liters) reaction kettle that has thermal oil circulation type of heating, open and stir.2. the temperature of controlling thermal oil in the chuck of said reaction kettle is 150 ℃ (perhaps 175 ℃), opens the chuck valve, feeds deep fat, and intensification material, material melt (90 ℃ time become paste liquid) gradually in the time of 80 ~ 90 ℃.Material becomes limpid liquid (clarified liq) when being warmed up to 110 ~ 130 ℃ (present embodiment is 125 ℃).3. after the complete fusion of material, continue to heat up, when being warmed up to 180 ℃, it is muddy that material begins to become, and presents oyster white.(present embodiment is 190 ℃ to continue to be warming up to 185 ~ 190 ℃; This moment, said liquid was creamy white); Open the blowing bottom valve of reaction kettle,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle.4. regulate dispensing speed; The control material is formed the material thin layer (laminated layer that thickness is 1 ~ 3mm (present embodiment is 3mm) on travelling belt; Thin slice); Said material thin layer on the travelling belt passes the tunnel like heating chamber of (promptly through or through) above-mentioned tunnel like heating unit through 15 ~ 20 minutes motion times spent (present embodiment is 15 minutes) of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250 ~ 280 ℃ (present embodiment is 260 ℃ or is 280 ℃), and obtains white solid material thin slice.5. with the solid materials thin slice through section, pulverize, obtain the cyanuric acid bullion, get into refining step (pack into deliver to refining step with the cyanuric acid bullion in the enamel waggon) then.6. at refining step, in refining kettle, add inorganic diluted acid, inorganic diluted acid can be 18% ~ 23% dilute sulphuric acid (massfraction of present embodiment dilute sulphuric acid is 23%) or Hydrogen chloride for massfraction; Again the cyanuric acid bullion is dropped into (conveying) in refining kettle, promptly in refining kettle, add 1500 kilograms of (massfraction is 20%) dilute sulphuric acids, drop into 750 kilograms of cyanuric acid bullions; The ratio of the weight of cyanuric acid bullion and dilute sulphuric acid (inorganic diluted acid) is 1:2; Open steam, be warming up to 95 ~ 100 ℃ (present embodiment is 98 ℃), be incubated 1.5 ~ 2 hours (present embodiment is 1.5 hours); Steam off; ON cycle water is cooled to 25 ~ 30 ℃ (present embodiment is 30 ℃), is discharged to whizzer through the blowing bottom valve of refining kettle; Centrifuge dripping (isolating solid with whizzer), obtaining water cut is the wet feed cyanuric acid elaboration of 22% (weight percent).7. 60 ℃ of vacuum-dryings of wet feed cyanuric acid elaboration are obtained cyanuric acid product (finished product), content 99%, molar yield: 96%.
Embodiment 3: the preparation method of the verivate Surchlor GR 60 of cyanuric acid processes (referring to the following reaction formula) of Surchlor GR 60 product successively through following process:
Step 1., 2., 3., 4., 5., 6. with embodiment 1.7. step is that wet feed cyanuric acid elaboration does not need drying, directly produces its verivate Surchlor GR 60 by ordinary method, finally obtains Surchlor GR 60 product (finished product).Specifically be in 5000 liters reaction kettle, to add 1000 kilograms of the wet feed cyanuric acid elaboration that embodiment 1 or present embodiment obtain, pure 6.2kmol.The adding weight percent concentration is 30% 1800 kilograms of NaOH solution (pure 12.4kmol), stirs and is warming up to 40 ℃, and material all dissolves, and obtains little yellow transparent solution.Be cooled to-5 ℃ with the cryosel bath, begin to feed chlorine, controlled temperature is between-5 ~ 0 ℃ in the feeding process, and the final pH value reaches at 2.6 ~ 2.4 o'clock and stops to feed chlorine.Be cooled to-10 ℃, suction filtration, with 500 liters of frozen water washings once.60 ℃ of vacuum-dryings.Get 1260 kilograms of two chloroethene NaDCCs, content 98%, molar yield: 95%.
Embodiment 4: the preparation method of the verivate trichloroisocyanuric acid of cyanuric acid processes (referring to the following reaction formula) of trichloroisocyanuric acid product successively through following process:
Step 1., 2., 3., 4., 5., 6. with embodiment 1.7. step is that wet feed cyanuric acid elaboration does not need drying, and it is directly produced its verivate Trichloroacetonitrile uric acid by ordinary method, finally obtains Trichloroacetonitrile uric acid product (finished product).Specifically be in 5000 liters reaction kettle, to add 1000 kilograms of the wet feed cyanuric acid elaboration that embodiment 1 or present embodiment obtain, pure 6.2kmol.The adding weight percent concentration is 30% 2480 kilograms of NaOH solution (pure 18.6kmol), stirs and is warming up to 40 ℃, and material all dissolves, and obtains little yellow transparent solution.Be cooled to-5 ℃ with the cryosel bath, begin to feed chlorine, controlled temperature is between-5 ~ 0 ℃ in the feeding process, and the final pH value reaches at 3 ~ 4 o'clock and stops to feed chlorine.Be cooled to-10 ℃, suction filtration, with 500 liters of frozen water washings once.60 ℃ of vacuum-dryings.Get 1400 kilograms of trichloroisocyanuric acids, content 99%, molar yield: 96%.
Above embodiment is used to further specify the present invention, but does not limit the present invention in any form.
Claims (10)
1. the preparation method of a cyanuric acid; It is characterized in that it is to process the cyanuric acid product through following process successively: be that the mixed of 1:0.1～0.2 is even according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating with urea and catalyst sulfuric acid ammonium; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150～190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185～190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1～3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15～20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250～280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5～2 with the ratio of the weight of inorganic diluted acid, is warming up to 95～100 ℃, is incubated 1.5～2 hours; Be cooled to 25～30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20%～25% wet feed cyanuric acid elaboration; 7. the vacuum-drying of wet feed cyanuric acid elaboration is obtained the cyanuric acid product.
2. the preparation method of cyanuric acid according to claim 1 is characterized in that above-mentioned steps 2., and the temperature of controlling thermal oil in the chuck of said reaction kettle is 190 ℃.
3. the preparation method of cyanuric acid according to claim 1; In it is characterized in that above-mentioned steps 3.; The homocline vomit pipe has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals.
4. the preparation method of cyanuric acid according to claim 1 is characterized in that above-mentioned tunnel like heating unit is the tunnel type micro wave heating unit.
5. the preparation method of cyanuric acid according to claim 1, the length that it is characterized in that the tunnel like heating chamber of above-mentioned tunnel like heating unit is 20 meters.
6. the preparation method of cyanuric acid according to claim 1 is characterized in that above-mentioned steps 6., and inorganic diluted acid is that massfraction is 18%～23% dilute sulphuric acid.
7. the preparation method of the verivate Surchlor GR 60 of a cyanuric acid; It is characterized in that it is to process the Surchlor GR 60 product through following process successively: be that the mixed of 1:0.1～0.2 is even according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating with urea and catalyst sulfuric acid ammonium; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150～190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185～190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1～3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15～20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250～280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5～2 with the ratio of the weight of inorganic diluted acid, is warming up to 95～100 ℃, is incubated 1.5～2 hours; Be cooled to 25～30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20%～25% wet feed cyanuric acid elaboration; 7. wet feed cyanuric acid elaboration does not need drying, and it is directly produced its verivate Surchlor GR 60 by ordinary method, finally obtains the Surchlor GR 60 product.
8. the preparation method of the verivate Surchlor GR 60 of cyanuric acid according to claim 7; In it is characterized in that above-mentioned steps 3.; The homocline vomit pipe has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals; The tunnel like heating unit is the tunnel type micro wave heating unit, and the length of the tunnel like heating chamber of above-mentioned tunnel like heating unit is 20 meters; Above-mentioned steps 6. in, inorganic diluted acid is that massfraction is 18%～23% dilute sulphuric acid.
9. the preparation method of the verivate trichloroisocyanuric acid of a cyanuric acid; It is characterized in that it is to process the trichloroisocyanuric acid product through following process successively: be that the mixed of 1:0.1～0.2 is even according to its weight ratio 1., it is joined in the reaction kettle that has thermal oil circulation type of heating with urea and catalyst sulfuric acid ammonium; 2. the temperature of controlling thermal oil in the chuck of said reaction kettle heats up and stirs material between 150～190 ℃, and material melts gradually, along with the intensification material becomes liquid; 3. after the complete fusion of material, continue to be warming up to 185～190 ℃,, material evenly is discharged to through the homocline vomit pipe on the travelling belt of feeding mouth one end of tunnel like heating unit through the blowing bottom valve blowing of reaction kettle; 4. regulate dispensing speed; The control material is formed the material thin layer that thickness is 1～3mm on travelling belt; Said material thin layer on the travelling belt passes the tunnel like heating chamber of above-mentioned tunnel like heating unit through 15～20 minutes motion times spent of travelling belt; Discharge port one end at above-mentioned tunnel like heating unit is the exit of said tunnel like heating chamber, and the material coating temperature is 250～280 ℃, and obtains the solid materials thin slice; 5. the solid materials thin slice is passed through section, pulverizes, obtain the cyanuric acid bullion, get into refining step then; 6. at refining step, in refining kettle, add inorganic diluted acid, again the cyanuric acid bullion is put in the refining kettle; The cyanuric acid bullion is 1:1.5～2 with the ratio of the weight of inorganic diluted acid, is warming up to 95～100 ℃, is incubated 1.5～2 hours; Be cooled to 25～30 ℃; Be discharged to whizzer, centrifuge dripping obtains water cut and is 20%～25% wet feed cyanuric acid elaboration; 7. wet feed cyanuric acid elaboration does not need drying, and it is directly produced its verivate trichloroisocyanuric acid by ordinary method, finally obtains the trichloroisocyanuric acid product.
10. the preparation method of the verivate trichloroisocyanuric acid of cyanuric acid according to claim 9; It is characterized in that above-mentioned homocline vomit pipe has the pipeline that is connected with the blowing bottom valve of reaction kettle, the horizontal pipeline that is connected with this pipeline, a plurality of laterals that are connected with this horizontal pipeline, is fixed in the scraper plate on the horizontal pipeline; Said horizontal pipeline stretches along the width of travelling belt; The width of said a plurality of lateral travelling belt in the horizontal pipeline upper edge is evenly distributed, and said scraper plate is positioned at the back of said a plurality of laterals; The tunnel like heating unit is the tunnel type micro wave heating unit, and the length of the tunnel like heating chamber of above-mentioned tunnel like heating unit is 20 meters; Above-mentioned steps 6. in, inorganic diluted acid is that massfraction is 18%～23% dilute sulphuric acid.
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| CN103086990A (en) * | 2013-01-30 | 2013-05-08 | 福建省邵武市榕丰化工有限公司 | Method for producing cyanuric acid by utilizing industrial waste heat and tunnel type cracking furnace device |
| CN103772306A (en) * | 2014-01-24 | 2014-05-07 | 安徽中元化工集团有限公司 | Production method of sodium dichloro isocyanurate |
| CN103965126A (en) * | 2013-11-01 | 2014-08-06 | 山东大明消毒科技有限公司 | Preparation method for co-production of trichloroisocyanuric acid and dichloroisocyanurate |
| CN106316971A (en) * | 2016-08-19 | 2017-01-11 | 鄄城康泰化工有限公司 | Preparation method of cyanuric acid |
| CN106699679A (en) * | 2016-12-02 | 2017-05-24 | 广西洋荣科技有限公司 | Preparation method of high-yield trichloroisocyanuric acid |
| CN108047150A (en) * | 2018-01-24 | 2018-05-18 | 诸城市良丰化学有限公司 | A kind of cyanuric acid produces process for purification |
| CN112409277A (en) * | 2020-11-26 | 2021-02-26 | 济宁键邦化工有限公司 | Preparation method of cyanuric acid |
| CN112898212A (en) * | 2021-01-28 | 2021-06-04 | 山东大明消毒科技有限公司 | Method for preparing cyanuric acid by using ionic liquid |
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| CN103086990A (en) * | 2013-01-30 | 2013-05-08 | 福建省邵武市榕丰化工有限公司 | Method for producing cyanuric acid by utilizing industrial waste heat and tunnel type cracking furnace device |
| CN103086990B (en) * | 2013-01-30 | 2015-04-29 | 福建省邵武市榕丰化工有限公司 | Method for producing cyanuric acid by utilizing industrial waste heat and tunnel type cracking furnace device |
| CN103965126A (en) * | 2013-11-01 | 2014-08-06 | 山东大明消毒科技有限公司 | Preparation method for co-production of trichloroisocyanuric acid and dichloroisocyanurate |
| CN103772306A (en) * | 2014-01-24 | 2014-05-07 | 安徽中元化工集团有限公司 | Production method of sodium dichloro isocyanurate |
| CN103772306B (en) * | 2014-01-24 | 2015-10-14 | 安徽中元化工集团有限公司 | A kind of production method of Surchlor GR 60 |
| CN106316971A (en) * | 2016-08-19 | 2017-01-11 | 鄄城康泰化工有限公司 | Preparation method of cyanuric acid |
| CN106699679A (en) * | 2016-12-02 | 2017-05-24 | 广西洋荣科技有限公司 | Preparation method of high-yield trichloroisocyanuric acid |
| CN108047150A (en) * | 2018-01-24 | 2018-05-18 | 诸城市良丰化学有限公司 | A kind of cyanuric acid produces process for purification |
| CN112409277A (en) * | 2020-11-26 | 2021-02-26 | 济宁键邦化工有限公司 | Preparation method of cyanuric acid |
| CN112898212A (en) * | 2021-01-28 | 2021-06-04 | 山东大明消毒科技有限公司 | Method for preparing cyanuric acid by using ionic liquid |
| CN112898212B (en) * | 2021-01-28 | 2022-09-09 | 山东大明消毒科技有限公司 | Method for preparing cyanuric acid by using ionic liquid |
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Address after: 051530 biological industry park, Zhaoxian County Industrial Park, Shijiazhuang, Hebei Patentee after: HEBEI KEEPER CHEMICAL INDUSTRIES Co.,Ltd. Address before: 051530 biological industry park, Zhaoxian County Industrial Park, Shijiazhuang, Hebei Patentee before: HEBEI ANHAI CHEMICAL INDUSTRIES Co.,Ltd. |
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Effective date of registration: 20180119 Address after: 055150 Xingtai, Hebei province Renxian County Jianshe Road west side Peace Street south side Patentee after: HEBEI TIANJIALI BIOTECHNOLOGY CO.,LTD. Address before: 051530 biological industry park, Zhaoxian County Industrial Park, Shijiazhuang, Hebei Patentee before: Hebei Keeper Chemical Industries Co.,Ltd. |
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Effective date of registration: 20240307 Address after: No.6 Xingwang Road, Biological Industry Park, Nanbaishe Town Industrial Park, Zhao County, Shijiazhuang City, Hebei Province 051530 Patentee after: Hebei Kerr Biotechnology Co.,Ltd. Country or region after: China Address before: 055150 west of Jianshe Road south of Heping Street, Ren county, Xingtai City, Hebei Province Patentee before: HEBEI TIANJIALI BIOTECHNOLOGY CO.,LTD. Country or region before: China |