CN101386603B - Clean production process of sodium dichloroisoyanurate - Google Patents
Clean production process of sodium dichloroisoyanurate Download PDFInfo
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- CN101386603B CN101386603B CN2008101583666A CN200810158366A CN101386603B CN 101386603 B CN101386603 B CN 101386603B CN 2008101583666 A CN2008101583666 A CN 2008101583666A CN 200810158366 A CN200810158366 A CN 200810158366A CN 101386603 B CN101386603 B CN 101386603B
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- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title 1
- 229910052708 sodium Inorganic materials 0.000 title 1
- 239000011734 sodium Substances 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 24
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 21
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000012065 filter cake Substances 0.000 claims abstract description 17
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 16
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000006298 dechlorination reaction Methods 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000007790 solid phase Substances 0.000 claims abstract description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 12
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000011229 interlayer Substances 0.000 claims description 12
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 10
- MSFGZHUJTJBYFA-UHFFFAOYSA-M sodium dichloroisocyanurate Chemical compound [Na+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O MSFGZHUJTJBYFA-UHFFFAOYSA-M 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 7
- 239000012267 brine Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 6
- 235000017550 sodium carbonate Nutrition 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000009991 scouring Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- -1 cyanuric acid disodium salt Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention disclosed a process for cleanly producing sodium dichloro isocyanurate. The process comprises the following steps: putting cyanuric acid, calcium carbonate and water which are mixed and put into a batching kettle to be stirred into slurry according to the proportion, pouring the slurry into a pre-chlorination reactor to perform pre-chlorination reaction; putting the slurry after the pre-chlorinated into a differential circulator to perform chlorination reaction, and sending the residual chlorine generated in the chlorination reaction back to the pre-chlorination reactor for reutilization; using a centrifugal machine to perform liquid-solid separation on the materials after the chlorination; performing settlement dechlorination on the separated liquid, adding hydrochloric acid to the liquid to generate cyanuric acid and chlorine after decomposition, and sending the chlorine back to the pre-chlorination reactor; washing a filter cake obtained after centrifuging with water, and sending the washing water after the washing back to the batching kettle; and using sodium carbonate to perform solid phase neutralization on the filter cake after the washing, and using airflow to dry the filter cake after the neutralization so as to obtain the sodium dichloro isocyanurate product. The process adopts continuous reaction to produce the sodium dichloro isocyanurate, so that the production efficiency is greatly improved; besides, the production process does not discharge wastewater, thus the environment is not polluted at all.
Description
Technical field
Step of the present invention and Surchlor GR 60 are a kind of process for producing sodium dichloro cyanurate.
Background technology
At present, the production technique of Surchlor GR 60 generally all adopts the liquid caustic soda method to produce, and adopts the reaction of liquid caustic soda and cyanuric acid, produces the cyanuric acid disodium salt, logical then chlorine reaction generates DICHLOROISOCYANURIC ACID, and DICHLOROISOCYANURIC ACID generates Surchlor GR 60 with the liquid caustic soda reaction again.This production is the batch production method, its deficiency mainly show following some: directly discharging after the wastewater treatment that produces in the production, cause serious environmental to pollute; Because it is low-temperature condition that reaction requires, so energy expenditure is higher; Depositing in the process product decomposes serious; Water consumption is bigger in the production process, to bigger burden of subsequent wastewater treatment increase etc.
Summary of the invention
The objective of the invention is, a kind of process for producing sodium dichloro cyanurate is provided, adopt successive reaction to produce Surchlor GR 60, reduce water consumption, realize non-wastewater discharge.
The present invention is achieved through the following technical solutions for achieving the above object: a kind of process for producing sodium dichloro cyanurate may further comprise the steps:
1. insert after cyanuric acid, lime carbonate and water being proportioned in the batching still and stir into slurries, the weight ratio of cyanuric acid and lime carbonate is 1: 0.7-0.8, water are 7-16 times of cyanuric acid weight;
2. slurries are squeezed into and carried out the prechlorination reaction in the prechlorination reactor;
3. enter after slurries react through prechlorination again and carry out chlorination reaction in the differential hydrokineter, feed chlorine from differential hydrokineter bottom simultaneously, temperature of reaction is 10 ℃-30 ℃;
4. the recycling of prechlorination reactor is sent in the chlorine residue that produces in the chlorination reaction back to;
5. adopt whizzer to carry out liquid-solid separation to the material after the chlorination reaction;
6. the liquid after 5. step being separated carries out the sedimentation dechlorination, adds hydrochloric acid in liquid, and the weight that adds hydrochloric acid is the 0.1%-0.3% of liquid weight, and decomposing the back is cyanuric acid and chlorine, and chlorine is sent back in the prechlorination reactor;
7. to step 6. in the liquid of sedimentation dechlorination filter, the cyanuric acid filter cake that obtains after the filtration is sent into the batching still;
8. add the milk of lime neutralization through the dechlorination filtrate filtered, milk of lime is the suspension liquid that contains calcium hydroxide 20%-30%, and the milk of lime weight of adding is the 5%-10% of filtrate weight;
9. the liquid after the neutralization is through the pressure filter press filtration, and filter residue is unreacted Wingdale, utilizes again after the taking-up, and filtrate enters evaporization process, is condensed into sheet after the filtrate evaporation, and drying obtains the calcium chloride byproduct, and the distilled water after the evaporation enters the prechlorination reactor;
10. the filter cake that step is obtained after 5. centrifugal washes with water, and washing after scouring water is admitted to the batching still;
Described a kind of process for producing sodium dichloro cyanurate, the differential hydrokineter of step described in 3. has an annular reaction pipe, reaction tubes both sides outer wall is provided with first interlayer cover and the second interlayer cover respectively, first interlayer cover bottom is provided with the first salt water inlet, top is provided with first brine outlet, second interlayer cover bottom is provided with the second salt water inlet, top is provided with second brine outlet, annular reaction pipe top is provided with the pre-reactor Link Port, the bottom is provided with inlet mouth and drain hole respectively, cyanuric acid and the import of lime carbonate mixed solution are offered in annular reaction pipe top, and chlorine inlet is offered in annular reaction pipe bottom.The annular reaction pipe is the oval ring pipe.
The invention has the advantages that: adopt successive reaction production, production efficiency is had a more substantial increase; Reduced water consumption, made solid-to-liquid ratio higher; The consumption of chlorine has bigger reduction; Production technique non-wastewater discharge of the present invention without any pollution, can be decomposed into chlorine with the DICHLOROISOCYANURIC ACID in the waste water and cyanuric acid is recovered utilization to environment, thereby reduce consumption of raw materials etc.
Description of drawings
Accompanying drawing 1 is a process flow sheet of the present invention; Accompanying drawing 2 is structural representations of differential hydrokineter in the accompanying drawing 1.
Embodiment
Production technique of the present invention may further comprise the steps:
1. insert after cyanuric acid, lime carbonate and water being proportioned in the batching still and stir into slurries, the weight ratio of cyanuric acid and lime carbonate is 1: 0.7-0.8, water are 7-16 times of cyanuric acid weight, and the arbitrary value in described numerical range all can;
2. slurries are squeezed into and carried out the prechlorination reaction in the prechlorination reactor;
3. enter after slurries react through prechlorination again and carry out chlorination reaction in the differential hydrokineter, feed chlorine from differential hydrokineter bottom simultaneously, temperature of reaction is 10 ℃-30 ℃;
4. the recycling of prechlorination reactor is sent in the chlorine residue that produces in the chlorination reaction back to;
5. adopt whizzer to carry out liquid-solid separation to the material after the chlorination reaction;
6. the liquid after 5. step being separated carries out the sedimentation dechlorination, adds hydrochloric acid in liquid, and the weight that adds hydrochloric acid is the 0.1%-0.3% of liquid weight, and decomposing the back is cyanuric acid and chlorine, and chlorine is sent back in the prechlorination reactor;
7. to step 6. in the liquid of sedimentation dechlorination filter, the cyanuric acid filter cake that obtains after the filtration is sent into the batching still;
8. add the milk of lime neutralization through the dechlorination filtrate filtered, milk of lime is the suspension liquid that contains calcium hydroxide 20%-30%, and the milk of lime weight of adding is the 5%-10% of filtrate weight;
9. the liquid after the neutralization is through the pressure filter press filtration, and filter residue is unreacted Wingdale, utilizes again after the taking-up, and filtrate enters evaporization process, is condensed into sheet after the filtrate evaporation, and drying obtains the calcium chloride byproduct, and the distilled water after the evaporation enters the prechlorination reactor;
10. the filter cake that step is obtained after 5. centrifugal washes with water, and washing after scouring water is admitted to the batching still;
The structure of the differential hydrokineter of processing step of the present invention described in 3. is that an annular reaction pipe 1 is arranged, annular reaction pipe 1 both sides outer wall is provided with first interlayer cover, 3 and second interlayer cover 6 respectively, first interlayer overlaps 3 bottoms the first salt water inlet 2 is set, top is provided with first brine outlet 4, second interlayer overlaps 6 bottoms the second salt water inlet 7 is set, top is provided with second brine outlet 5, annular reaction pipe 1 top is provided with pre-reactor Link Port 11, the bottom is provided with inlet mouth 8 and drain hole 9 respectively, cyanuric acid and lime carbonate mixed solution import 12 are offered in annular reaction pipe 1 top, and chlorine inlet 13 is offered in annular reaction pipe 1 bottom.This structure can realize successive reaction in this technology, sufficient reacting increases output, and salt solution is circulated by the salt solution entrance and exit, is the cooling of differential hydrokineter, makes it keep temperature of reaction below 30 ℃; Annular reaction pipe 1 of the present invention is the oval ring pipe, and this shape is convenient to liquid-flow, and is convenient to cooling.The lime carbonate of production craft step of the present invention described in 1. is meal.Step in the production technique of the present invention
Described filter cake is about 20% through washing back water content, uses light ash to mix post neutralization with it again, and the purity of soda ash is more than 92%, and the mass ratio of filter cake and soda ash is generally 1: about 0.24-0.29, the back pH value is that 5.8-6.5 is as the criterion to neutralize.The present invention not detailed description is a known technology.10 is spare interface among the figure.
Claims (2)
1. process for producing sodium dichloro cyanurate is characterized in that: may further comprise the steps:
1. insert after cyanuric acid, lime carbonate and water being proportioned in the batching still and stir into slurries, the weight ratio of cyanuric acid and lime carbonate is 1: 0.7-0.8, water are 7-16 times of cyanuric acid weight;
2. slurries are squeezed into and carried out the prechlorination reaction in the prechlorination reactor;
3. enter after slurries react through prechlorination again and carry out chlorination reaction in the differential hydrokineter, feed chlorine from differential hydrokineter bottom simultaneously, temperature of reaction is 10 ℃-30 ℃;
4. the recycling of prechlorination reactor is sent in the chlorine residue that produces in the chlorination reaction back to;
5. adopt whizzer to carry out liquid-solid separation to the material after the chlorination reaction;
6. the liquid after 5. step being separated carries out the sedimentation dechlorination, adds hydrochloric acid in liquid, and the weight that adds hydrochloric acid is the 0.1%-0.3% of liquid weight, and decomposing the back is cyanuric acid and chlorine, and chlorine is sent back in the prechlorination reactor;
7. to step 6. in the liquid of sedimentation dechlorination filter, the cyanuric acid filter cake that obtains after the filtration is sent into the batching still;
8. add the milk of lime neutralization through the dechlorination filtrate filtered, milk of lime is the suspension liquid that contains calcium hydroxide 20%-30%, and the milk of lime weight of adding is the 5%-10% of filtrate weight;
9. the liquid after the neutralization is through the pressure filter press filtration, and filter residue is unreacted Wingdale, utilizes again after the taking-up, and filtrate enters evaporization process, is condensed into sheet after the filtrate evaporation, and drying obtains the calcium chloride byproduct, and the distilled water after the evaporation enters the prechlorination reactor;
10. the filter cake that step is obtained after 5. centrifugal washes with water, and washing after scouring water is admitted to the batching still;
The differential hydrokineter of step described in 3. has an annular reaction pipe (1), annular reaction pipe (1) both sides outer wall is provided with the first interlayer cover (3) and the second interlayer cover (6) respectively, the first interlayer cover (3) bottom is provided with the first salt water inlet (2), top is provided with first brine outlet (4), the second interlayer cover (6) bottom is provided with the second salt water inlet (7), top is provided with second brine outlet (5), annular reaction pipe (1) top is provided with pre-reactor Link Port (11), the bottom is provided with inlet mouth (8) and drain hole (9) respectively, cyanuric acid and lime carbonate mixed solution import (12) are offered in annular reaction pipe (1) top, and chlorine inlet (13) is offered in annular reaction pipe (1) bottom.
2. a kind of process for producing sodium dichloro cyanurate according to claim 1 is characterized in that: annular reaction pipe (1) is the oval ring pipe.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101583666A CN101386603B (en) | 2008-10-31 | 2008-10-31 | Clean production process of sodium dichloroisoyanurate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101583666A CN101386603B (en) | 2008-10-31 | 2008-10-31 | Clean production process of sodium dichloroisoyanurate |
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| CN101386603A CN101386603A (en) | 2009-03-18 |
| CN101386603B true CN101386603B (en) | 2010-10-06 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206192B (en) * | 2011-04-09 | 2013-08-28 | 河北冀衡化学股份有限公司 | Method for continuously synthesizing sodium dichloro isocyanurate dihydrate by wet process |
| CN102206193B (en) * | 2011-04-19 | 2013-07-10 | 菏泽华意化工有限公司 | Preparation method for trichloroisocyanuric acid |
| CN102329275B (en) * | 2011-07-19 | 2014-06-18 | 鄄城康泰化工有限公司 | Preparation methods of trichloroisocyanuric acid and 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 |
| CN110437169B (en) * | 2019-07-31 | 2022-06-24 | 青岛职业技术学院 | Preparation method of sodium dichloroisocyanurate |
| CN114436982A (en) * | 2022-01-24 | 2022-05-06 | 河北六合化工有限公司 | Method for recovering waste water from sodium dichloroisocyanurate production |
| CN114736167A (en) * | 2022-04-21 | 2022-07-12 | 河北六合化工有限公司 | Continuous production method of sodium dichloroisocyanurate |
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