CN106380453A - Waste water discharge-free chlorinated isocyanuric acid industrial production method - Google Patents
Waste water discharge-free chlorinated isocyanuric acid industrial production method Download PDFInfo
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- CN106380453A CN106380453A CN201610765646.8A CN201610765646A CN106380453A CN 106380453 A CN106380453 A CN 106380453A CN 201610765646 A CN201610765646 A CN 201610765646A CN 106380453 A CN106380453 A CN 106380453A
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- acid
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- chlorated fulminuric
- isocyanuric acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/30—Only oxygen atoms
- C07D251/36—Only oxygen atoms having halogen atoms directly attached to ring nitrogen atoms
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Abstract
The invention provides a waste water discharge-free chlorinated isocyanuric acid industrial production method and belongs to the technical field of fine chemical production. The method realizes zero discharge of waste water, can eliminate environmental pollution, can greatly save energy and can reduce a cost. The method comprises diluting chlorine, carrying out a reaction process on the chlorine and sodium carbonate at a temperature of -20 to 30 DEG C for 18-22min to produce dichloroxide and solid sodium chloride, discharging the solid sodium chloride, feeding the produced dichloroxide into cyanuric acid slurry, carrying out a reaction process under control of reaction system pH to 2.6 or less from 4.1 to produce chlorinated isocyanuric acid slurry, carrying out centrifugation on the chlorinated isocyanuric acid slurry to obtain a reaction cycling mother liquid and hydrous chlorinated isocyanuric acid, dehydrating the hydrous chlorinated isocyanuric acid to obtain chlorinated isocyanuric acid filter cake, and drying the chlorinated isocyanuric acid filter cake to obtain chlorinated isocyanuric acid. The method can be used for industrial production of chlorinated isocyanuric acid.
Description
Technical field
The present invention relates to technical field of fine chemical production, more particularly, to a kind of chlorated fulminuric acid of non-wastewater discharge
Industrialized preparing process.
Background technology
Chlorated fulminuric acid product mainly includes sym-closene, dichlord isocyanurice acid, sodium dichloro cyanurate and two
At most, volume of production is also maximum for the manufacturer of symclosene potassium, wherein sym-closene and sodium dichloro cyanurate.They
It is the disinfectant of a class high-efficiency broad spectrum, have many uses.
At present, the conventional production process of chlorated fulminuric acid is to react generation cyanuric acid three using cyanuric acid, water and Caustic soda
Sodium salt solution, then generates chlorated fulminuric acid aqueous solution with chlorine reaction, in a kettle. through centrifuge dehydration, then by filter cake
It is dried, obtain chlorated fulminuric acid finished product.A large amount of waste water can be produced in this production process, specifically, often produce 1 ton of chloro isocyanide
Uric acid will produce 14 tons about of waste water, and the main component of waste water is:The sodium chloride of 7-9%, 0.4% about effective chlorine,
0.4% about cyanuric acid, partly soluble sodium dichloro cyanurate, solution ph is 2-3.These waste water are because of nitrogen content
Higher, total nitrogen content about 1600mg/L it is impossible to as salt dissolving Water circulation, and in these waste water due to containing cyanuric acid, two
The components such as symclosene sodium, organochlorine, and the content of organic carbon and ammonia nitrogen is considerably beyond discharging standards, thus nor
Directly discharge is it is necessary to be processed.Existing processing method includes the techniques such as concentration and evaporation, crystallization, decomposition, absorption, but investment
All very high with operating cost.Therefore it provides a kind of industrialized preparing process of the chlorated fulminuric acid being capable of water zero discharge will be
The important topic that this area is studied.
Content of the invention
It is an object of the invention to provide a kind of industrialized preparing process of the chlorated fulminuric acid of non-wastewater discharge, can
Make wastewater zero discharge, not only can eliminate environmental pollution, but also the energy, reduces cost can be greatlyd save.
The invention provides a kind of industrialized preparing process of the chlorated fulminuric acid of non-wastewater discharge, walk including following
Suddenly:
Chlorine is reacted 18-22 minute with soda in -20 DEG C -30 DEG C after dilution, generates dichloroxide and solid-state chlorination
Sodium;
Discharge solid sodium chloride, and the dichloroxide of generation is passed through in the serosity of cyanuric acid is reacted, control reaction
When system pH is down to less than 2.6 by 4.1, reaction generates chlorated fulminuric acid serosity;
Described chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle mother solution and aqueous chlorated fulminuric acid, will
Described aqueous chlorated fulminuric acid carries out dehydrate and obtains chlorated fulminuric acid filter cake, and described chlorated fulminuric acid filter cake is obtained
To chlorated fulminuric acid.
Specifically, the dichloroxide of generation is passed through in the serosity of cyanuric acid and carries out reaction and be specially:
The dichloroxide generating first generates hypochlorous acid with water fast reaction in the serosity of cyanuric acid, then hypochlorous acid again with cyanogen
Uric acid reaction generates chlorated fulminuric acid serosity.
Preferably, described reaction cycle mother solution includes a small amount of cyanuric acid, hypochlorous acid and chlorated fulminuric acid.
Preferably, moisture accounts for 10%-20% in described chlorated fulminuric acid filter cake.
Preferably, using air contained water, chlorine is diluted.
Preferably, described soda has 0.3-5.2m2The specific surface area of/g.
Optionally, described chlorated fulminuric acid be tri chloroisocyanuric acid or dichloro- isocyanuric acid or the two
Compositionss.
The invention provides a kind of industrialized preparing process of the chlorated fulminuric acid of non-wastewater discharge, compared to existing side
For method, this method is using having the soda of large specific surface area as raw material so as to occur in gas solid reactor with chlorine
Reaction, generates dichloroxide and solid sodium chloride, and solid sodium chloride can return to Sodium Carbonate Plant and uses as raw material, then by generation
Dichloroxide and the slurry reaction of cyanuric acid, generate chlorated fulminuric acid.The product of the method is except obtained chloro isocyanide
Outside uric acid product, it is only the raw material of not reaction completely in remaining reaction cycle mother solution, can be back to completely in production.With
When, due to contained moisture in chlorated fulminuric acid filter cake obtained after dewatering seldom, therefore can quickly be evaporated,
The industrial policy meeting country at present reaches the requirement producing zero-emission.Additionally, in the industrial production, obtain product separating
Afterwards, system only need to be supplemented a small amount of moisture and can be up to the standard weighing apparatus, and course of reaction is more steady, exchange in little external energy
Under the premise of temperature rise not over 50 DEG C, therefore do not need big energy conversion, can greatly save the energy, reduce at least about 20%
Cost.
Specific embodiment
The enforcement it is clear that described will be clearly and completely described to the technical scheme in the embodiment of the present invention below
Example is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of not making creative work, broadly falls into the model of present invention protection
Enclose.
The embodiment of one aspect of the present invention provides a kind of industrialized production side of the chlorated fulminuric acid of non-wastewater discharge
Method, comprises the following steps:
S1:Chlorine is reacted 18-22 minute with soda in -20 DEG C -30 DEG C after dilution, generates dichloroxide and solid-state chlorine
Change sodium.
In this step, it is carried out with the chlorine after dilution first for raw material by reaction generation dichloroxide and chlorine with soda
Change sodium, in this step, the reaction temperature of the two be -20 DEG C -30 DEG C, the response time be 18-22 minute it is to be understood that
In above-mentioned reaction temperature and reaction time range, reaction all can generate the satisfactory intermediate product obtaining.It is worth mentioning
In this step, to generate the sodium chloride of the be expelled directly out reaction vessel of solid-state obtaining, rather than be dissolved in water also need into
The sodium chloride that one step is processed, solid sodium chloride not only can directly return Sodium Carbonate Plant and use as raw material it is thus also avoided that if molten
Further loaded down with trivial details process step in Xie Shui.It is understood that reaction temperature also can for -15 DEG C, -10 DEG C, -5 DEG C, 0
DEG C, 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C etc., the response time can also be 19,20,21 minutes etc., and those skilled in the art can
With reference to above-mentioned parameter, reaction condition is optimized during the course of the reaction.Also, it should be noted this method provides one kind
Industrialized production method, rather than lab scale, whole reaction system is in a homeostasis process, therefore, does not specifically limit
Determine the addition of raw material, as long as reaction raw materials are added, and carry out according to the reaction condition of defined in method, you can obtain
Required intermediate product.
S2:Discharge solid sodium chloride, and the dichloroxide of generation is passed through in the serosity of cyanuric acid is reacted, control anti-
When answering system pH to be down to less than 2.6 by 4.1, reaction generates chlorated fulminuric acid serosity.
In this step, while discharging solid sodium chloride, the dichloroxide of generation is passed into the slurry of cyanuric acid
Reacted in liquid, generated, to react, the serosity obtaining chlorated fulminuric acid.In this step, because cyanuric acid is molten in water
Xie Du is very low, and the liquid that therefore cyanuric acid and water are formed is serosity.When the dichloroxide generating is passed through cyanuric acid, reactant
The pH of system is 4.1, and in industrialized production, in order to the chlorated fulminuric acid serosity required for obtaining, key point is to control
The pH of system processed, when pH drops to below 2.6, i.e. reaction generates required chlorated fulminuric acid serosity.As described above, it is our
Method provides a kind of industrialized production method, and whole reaction system is in a homeostasis process, therefore, in this step
In rapid, also specifically do not limit the addition of dichloroxide and cyanuric acid, after dichloro to be oxidized is passed through, only need to control reaction system
PH value, you can obtain required chlorated fulminuric acid serosity.
S3:Described chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle mother solution and aqueous chlorated fulminuric acid,
Described aqueous chlorated fulminuric acid is carried out dehydration and obtains chlorated fulminuric acid filter cake, described chlorated fulminuric acid filter cake is done
Dry, obtain chlorated fulminuric acid.
In this step, in order to obtain chlorated fulminuric acid product it is only necessary to centrifugation is carried out to chlorated fulminuric acid serosity being
Can, obtain two parts after separating, a part is reaction cycle mother solution, is back to system, another part is aqueous chloro isocyanide urine
Acid, after being dehydrated aqueous chlorated fulminuric acid, due to the moisture content less in filter cake, therefore quickly can be dried to obtain chloro
Isocyanuric acid product.It is understood that can be dried to it in the way of using pneumatic conveying drying.
Concrete reaction equation is as follows:
2CL2+2Na2CO3+H2O=CL2O+2NaHCO3+NaCL
2CL2+NaHCO3=CL2O+2CO2+H2O+NaCL
CL2O+H2O+H3C3N3O3=C3N3O3HCL2+2H2O
3CL2O+H2O+2H3C3N3O3=2C3N3O3CL3+4H2O
From above-mentioned reaction, in a preferred embodiment, chlorated fulminuric acid product may include tri chloroisocyanuric acid,
Or dichloro- isocyanuric acid or combination thing.The difference of dichloro- isocyanuric acid and tri chloroisocyanuric acid is effectively
The quantity of chlorine is different, and tri chloroisocyanuric acid further chloro on the basis of dichloro- isocyanuric acid obtains, this area
Technical staff can obtain corresponding chlorated fulminuric acid product by the node that control reaction is carried out according to actual needs.
In one embodiment, specifically illustrate the course of reaction of dichloroxide and cyanuric acid serosity, wherein aoxidize two
Chlorine first can generate hypochlorous acid with water fast reaction in the serosity of cyanuric acid, then reacts generation chloro by hypochlorous acid and cyanuric acid different
Cyanuric acid, rather than chlorated fulminuric acid is generated with cyanuric acid direct reaction by dichloroxide.
In a preferred embodiment, described reaction cycle mother solution includes a small amount of cyanuric acid, hypochlorous acid and chloro isocyanide urine
Acid.In the present embodiment, the material included in reaction cycle mother solution is unreacted completely raw material, wherein, reaction cycle
Chlorated fulminuric acid in mother solution constitutes about 1% about, and this also has after precipitation mainly due to chlorated fulminuric acid product
Remain on a small quantity so that reaction cycle mother solution can return directly to reaction system in mother solution, and without other extra places
Reason step, the industrial policy meeting country at present reaches the requirement producing zero-emission.
In a preferred embodiment, moisture in described chlorated fulminuric acid filter cake accounts for 10%-20%.At this
In embodiment, the moisture in aqueous chlorated fulminuric acid filter cake obtained after dewatering is little, about only 10%-
20% about, the content of this water taken away from system after also implying that reaction seldom so that system only need to supplement a small amount of
Moisture can be up to the standard weighing apparatus, because without big energy conversion, thus the energy, reduces cost can be greatlyd save.Additionally, by
Moisture content less in filter cake, so additionally aids the rapid draing of product, thus can quickly process that product is obtained, it is to avoid middle
Increase extra redundancy step.
In a preferred embodiment, using air contained water, chlorine is diluted.In the present embodiment, from air contained water
Chlorine is diluted be not suitable for directly being diluted with water mainly due to chlorine, such chlorine can produce time chlorine with water reaction
Acid, thus larger corrosivity can be produced reaction vessel.It is understood that the water content of in the air is little, using sky
Moisture in gas carrys out diluted chlorine gas, so contributes to causing the generation of gas-solid reaction between chlorine and soda.
In a preferred embodiment, described soda has 0.3-5.2m2The specific surface area of/g.In the present embodiment, made
Raw material soda has larger specific surface area, and specific surface area is more big more to contribute to being combined the efficient gas-solid of generation with chlorine anti-
Should.It is understood that the soda specific surface area in above range is all conducive to the generation reacted to prepare required chlorine
For isocyanuric acid, its specific surface area can be also 0.5m2/g、1m2/g、1.5m2/g、2m2/g、2.5m2/g、3m2/g、3.5m2/g、
4m2/g、4.5m2/g、5m2/ g etc., those skilled in the art can be carried out from suitable within the above range according to real reaction condition
The soda of specific surface area.
In order to become apparent from the work of the chlorated fulminuric acid introducing the non-wastewater discharge that the embodiment of the present invention is provided in detail
Industry production method, is described in detail below in conjunction with specific embodiment.
Embodiment 1
Chlorine is reacted 22 minutes in -20 DEG C with soda after Dilution air, generates dichloroxide and solid sodium chloride;Row
Go out solid sodium chloride, the dichloroxide of generation is passed through in the serosity of cyanuric acid and is reacted, control reaction system pH to be dropped by 4.1
During to less than 2.6, reaction generates chlorated fulminuric acid serosity;Chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle
Mother solution and aqueous chlorated fulminuric acid, reaction cycle mother solution is back in cyanuric acid serosity via pipeline, will be different for aqueous chloro
Cyanuric acid carries out dehydration and obtains chlorated fulminuric acid filter cake, and described chlorated fulminuric acid filtration cakes torrefaction obtains chloro isocyanide urine
Acid 1.In this chlorated fulminuric acid 1, the content of effective chlorine is 90.3%, and the pH value of its 1% aqueous solution is 2.71.
Embodiment 2
Chlorine is reacted 20 minutes in 15 DEG C with soda after Dilution air, generates dichloroxide and solid sodium chloride;Row
Go out solid sodium chloride, the dichloroxide of generation is passed through in the serosity of cyanuric acid and is reacted, control reaction system pH to be dropped by 4.1
During to less than 2.6, reaction generates chlorated fulminuric acid serosity;Chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle
Mother solution and aqueous chlorated fulminuric acid, reaction cycle mother solution is back in cyanuric acid serosity via pipeline, will be different for aqueous chloro
Cyanuric acid carries out dehydration and obtains chlorated fulminuric acid filter cake, and described chlorated fulminuric acid filtration cakes torrefaction obtains chloro isocyanide urine
Acid 2.In this chlorated fulminuric acid 2, the content of effective chlorine is 90.7%, and the pH value of its 1% aqueous solution is 2.70.
Embodiment 3
Chlorine is reacted 18 minutes in 30 DEG C with soda after Dilution air, generates dichloroxide and solid sodium chloride;Row
Go out solid sodium chloride, the dichloroxide of generation is passed through in the serosity of cyanuric acid and is reacted, control reaction system pH to be dropped by 4.1
During to less than 2.6, reaction generates chlorated fulminuric acid serosity;Chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle
Mother solution and aqueous chlorated fulminuric acid, reaction cycle mother solution is back in cyanuric acid serosity via pipeline, will be different for aqueous chloro
Cyanuric acid carries out dehydration and obtains chlorated fulminuric acid filter cake, and described chlorated fulminuric acid filtration cakes torrefaction obtains chloro isocyanide urine
Acid 3.In this chlorated fulminuric acid 3, the content of effective chlorine is 89.8%, and the pH value of its 1% aqueous solution is 2.78.
From embodiment 1-3, the available chlorine content of obtained chlorated fulminuric acid is all higher than 89.5%, its 1% water
The pH value of solution, all between 2.6-3.3 scope, all meets industry standard.As can be seen here, the side that the embodiment of the present invention is provided
Method can be effectively used in the industrialized production of chlorated fulminuric acid.
Claims (7)
1. a kind of industrialized preparing process of the chlorated fulminuric acid of non-wastewater discharge is it is characterised in that comprise the following steps:
Chlorine is reacted 18-22 minute with soda in -20 DEG C -30 DEG C after dilution, generates dichloroxide and solid sodium chloride;
Discharge solid sodium chloride, and the dichloroxide of generation is passed through in the serosity of cyanuric acid is reacted, control reaction system
When pH is down to less than 2.6 by 4.1, reaction generates chlorated fulminuric acid serosity;
Described chlorated fulminuric acid serosity is centrifuged, obtains reaction cycle mother solution and aqueous chlorated fulminuric acid, will be described
Aqueous chlorated fulminuric acid carries out dehydration and obtains chlorated fulminuric acid filter cake, and described chlorated fulminuric acid filtration cakes torrefaction obtains
Chlorated fulminuric acid.
2. industrialized preparing process according to claim 1 is it is characterised in that be passed through cyanuric acid by the dichloroxide of generation
Serosity in carry out reaction and be specially:
The dichloroxide generating first generates hypochlorous acid with water fast reaction in the serosity of cyanuric acid, then hypochlorous acid again with cyanuric acid
Reaction generates chlorated fulminuric acid serosity.
3. industrialized preparing process according to claim 2 it is characterised in that described reaction cycle mother solution include a small amount of
Cyanuric acid, hypochlorous acid and chlorated fulminuric acid.
4. industrialized preparing process according to claim 1 is it is characterised in that moisture in described chlorated fulminuric acid filter cake
Content accounts for 10%-20%.
5. industrialized preparing process according to claim 1 it is characterised in that carried out dilute using air contained water to chlorine
Release.
6. industrialized preparing process according to claim 1 is it is characterised in that described soda has 0.3-5.2m2The ratio of/g
Surface area.
7. the industrialized preparing process according to any one of claim 1-6 is it is characterised in that described chlorated fulminuric acid is
Tri chloroisocyanuric acid or dichloro- isocyanuric acid or combination thing.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106957276A (en) * | 2017-04-06 | 2017-07-18 | 河北冀衡集团有限公司 | The preparation method of dichlord isocyanurice acid |
CN107141263A (en) * | 2017-04-06 | 2017-09-08 | 河北冀衡集团有限公司 | The preparation method of sym-closene |
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US3988336A (en) * | 1975-06-30 | 1976-10-26 | Olin Corporation | Preparation of dihaloisocyanuric acid salts |
CN1380290A (en) * | 2002-03-20 | 2002-11-20 | 唐银华 | Technological process for producing chlorinated isocyanuric acid |
CN105175350A (en) * | 2015-09-11 | 2015-12-23 | 鄄城康泰化工有限公司 | Preparation method of dihydrate sodium dichloroisocyanate |
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2016
- 2016-08-30 CN CN201610765646.8A patent/CN106380453A/en active Pending
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Publication number | Priority date | Publication date | Assignee | Title |
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US3988336A (en) * | 1975-06-30 | 1976-10-26 | Olin Corporation | Preparation of dihaloisocyanuric acid salts |
CN1380290A (en) * | 2002-03-20 | 2002-11-20 | 唐银华 | Technological process for producing chlorinated isocyanuric acid |
CN105175350A (en) * | 2015-09-11 | 2015-12-23 | 鄄城康泰化工有限公司 | Preparation method of dihydrate sodium dichloroisocyanate |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106957276A (en) * | 2017-04-06 | 2017-07-18 | 河北冀衡集团有限公司 | The preparation method of dichlord isocyanurice acid |
CN107141263A (en) * | 2017-04-06 | 2017-09-08 | 河北冀衡集团有限公司 | The preparation method of sym-closene |
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Application publication date: 20170208 |