CN103316621A - Method for preparing trichloroisocyanuric acid by using pipeline reactor - Google Patents
Method for preparing trichloroisocyanuric acid by using pipeline reactor Download PDFInfo
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- CN103316621A CN103316621A CN2013103079881A CN201310307988A CN103316621A CN 103316621 A CN103316621 A CN 103316621A CN 2013103079881 A CN2013103079881 A CN 2013103079881A CN 201310307988 A CN201310307988 A CN 201310307988A CN 103316621 A CN103316621 A CN 103316621A
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Abstract
The invention belongs to the technical field of trichloroisocyanuric acid preparation, and discloses a method for preparing a trichloroisocyanuric acid by using a pipeline reactor. The technical scheme of the invention is as follows: after water, a dry cyanuric acid product and calcium carbonate are added in a first reaction kettle in proportion, an outer circulating pump is started to circulate the obtained mixture, and chlorine gas is sucked in a pipeline reaction mechanism by using a Venturi tube, so that a slurry of the calcium carbonate, the cyanuric acid and the water carries out chlorination synthesis reaction with the chlorine gas by the pipeline reactor, and meanwhile, the reaction temperature is controlled, when the pH value reaches 2.4-3.2, the feeding of the chlorine gas is stopped; a material is fed into a cooling crystallization reaction kettle and cooled so as to obtain trichloroisocyanuric acid crystals, and then the trichloroisocyanuric acid crystals are separated through a centrifugal mechanism so as to obtain a wet trichloroisocyanuric acid product. The method for preparing a trichloroisocyanuric acid by using a pipeline reactor is high in chlorine gas absorption rate, sufficient in reaction and safe in production, and the conversion rate of the cyanuric acid is over 90%.
Description
Technical field
The invention belongs to sym-closene fabricating technology field, relate to a kind of method of utilizing the duct type reaction unit to prepare sym-closene.
Background technology
At present, it is standby that sym-closene typically uses reactor employing liquid caustic soda legal system.But when utilizing the liquid caustic soda legal system standby, utilize liquid caustic soda (NaOH) and cyanuric acid to press 3.5 by mole; 1 ratio prepares trisodium-salt solution, in trisodium-salt solution, pass into again the reaction of chlorine and water and generate hypochlorous acid, the hypochlorous acid oxidization cyanuric acid prepares sym-closene, this technique preparation cost is high, the consumption of cyanuric acid is 0.65 ton/ton, yield only has 85%, and chlorine consumption consumes 3 tons/ton of liquid caustic soda (concentration 32% NaOH) simultaneously at 1.0-1.2 ton/ton; The problem that the absorptivity that this technique exists chlorine is low, reaction is insufficient and preparation cost is high, and exist the unsafe factor of preparation.
Summary of the invention
The absorptivity that purpose of the present invention just provides a kind of chlorine is high, the duct type reaction unit of sufficient reacting, preparation sym-closene that preparation cost is low.
Another object of the present invention just provides a kind of method of utilizing the duct type reaction unit to prepare sym-closene.
The technical scheme that realizes the invention described above the first purpose is:
The preparation sym-closene the duct type reaction unit by
The discharging opening of the first reactor is communicated with the charging aperture of Venturi tube by circulating pump, the material sucking port of this Venturi tube and discharging opening are communicated with the charging aperture of chlorine pipeline and duct type reaction mechanism respectively, and the discharging opening of duct type reaction mechanism is communicated with the outer circulation reaction mechanism that consists of with the charging aperture of the first reactor; With
Consist of the crystallization centrifugal mechanism by described the first reactor and by its discharging opening by reaction mass beating pump, decrease temperature crystalline reactor and centrifugal mechanism
Consist of.
And described duct type reaction mechanism is for vertically setting up, and it highly is set to 8-10 meters.
The technical scheme that realizes the invention described above the second purpose is:
The method of utilizing the duct type reaction unit to prepare sym-closene comprises:
The reactant circulating process:
In the first reactor, the water that adds 2000 kilograms, open rabbling mechanism and the outer circulation pump of described reactor, and add therein behind 300 kilograms of 263 kilograms of the cyanuric acid dry products, calcium carbonate so that reactant liquor by circulating in circulating pump, Venturi tube, duct type reaction mechanism and the first reactor, after slurry mixes, suck chlorine by described Venturi tube and enter in the lump in the duct type reaction mechanism, the reaction temperature in described the first reactor is controlled between the 10-20 degree simultaneously; Arrive 2.4-3.2 when detecting pH value, stop chlorine and pass into; With
The Crystallization Separation operation:
Material is squeezed into the sym-closene crystallization of lowering the temperature in the decrease temperature crystalline reactor to get by beating pump, and then separate to get the wet product of sym-closene by centrifugal mechanism.
Wherein, in the described reactant circulating process, when the weight portion of correspondence was kilogram, the speed that described Venturi tube sucks chlorine was controlled at 350-400 cubes m/hs; In the described reactant circulating process, the granularity of described calcium carbonate is controlled at more than 300 orders.
The method of utilizing the duct type reaction unit to prepare sym-closene provided by the present invention, following advantage is compared with prior art arranged: the absorptivity of this technique chlorine is high, sufficient reacting, the characteristics that production safety and cost are low---pipeline reactor is applicable to fast reaction, heat release, inflammable and explosive reaction process, the advantage of pipeline reactor maximum is to utilize the advantage of static mixer, the gas-liquid two-phase medium fully contacts, finish mass transport process, it is than tank reactor stable reaction, the time of staying of tubular reactor material generally wants shorter, and the time of staying of tank reactor is generally longer, from removing reaction heat, it is difficult that tubular reactor is wanted, and tank reactor is easy, can establish coil pipe in still peripheral hardware chuck or still solves, the pipeline reactor of the present invention's design is the combined reactor that pipeline reactor adds reactor, be that reactor bottom outlet material enters tubular reactor by the outer circulation pump and turns back to reactor again, the outer circulation chuck is set reactor and built-in coiled pipe cooler is controlled reaction temperature, tubular reactor leading portion Venturi tube, utilize venturi principle that the chlorine air-flow is sucked wherein, the static mixer section of utilizing the pressure of circulating pump to enter tubular reactor, gas-liquid fully contacts, and carries out the chlorination synthetic reaction.Outer circulation pump continuous operation, the control ph value of reaction reaches 2.4-3.2, and reaction can be finished; Utilize the duct type reaction unit to prepare the method for sym-closene, the consumption of cyanuric acid reaches 0.6 ton/ton, and yield brings up to 90%, and chlorine consumption reduces by 10%, and the preparation cost of sym-closene is declined to a great extent, and has improved the competitiveness of product.
Description of drawings
Fig. 1: be the structural representation of duct type reaction unit of preparation sym-closene.
The specific embodiment
As shown in Figure 1, for consisting of the structural representation of the duct type reaction unit for preparing sym-closene, this device is made of outer circulation reaction mechanism and crystallization centrifugal mechanism; Namely by the first reactor 1 that carries out exothermic reaction and by its discharging opening by reaction mass circulating pump 2, be used for to suck chlorine Venturi tube 9, realize that material and chlorine carry out the outer circulation reaction mechanism that the duct type reaction mechanism 3 of abundant chemical reaction consists of, wherein the discharging opening of the first reactor is communicated with the charging aperture of Venturi tube 9 by circulating pump 2, the material sucking port of this Venturi tube 9 and discharging opening are communicated with the charging aperture of chlorine pipeline and duct type reaction mechanism 3 respectively, and the discharging opening of duct type reaction mechanism 3 is communicated with the charging aperture of the first reactor 1; Consist of the crystallization centrifugal mechanism by the first reactor 1 that carries out exothermic reaction and by its discharging opening by reaction mass beating pump 5, decrease temperature crystalline reactor 6 and centrifugal mechanism 7.
In order to promote gas-liquid fully to contact to carry out the chlorination synthetic reaction, the duct type reaction mechanism is for vertically setting up, and it highly is set between 8-10 meters.
The principle of utilizing above-mentioned duct type reaction unit to prepare sym-closene is, at first cyanuric acid, calcium carbonate, water are inserted in the first reactor in proportion, then open its discharging opening and open the Matter Transfer pump and make material by Venturi tube and suck chlorine and enter in the lump static mixer section in the duct type reaction mechanism 3, so that fully contacting, gas-liquid carries out the chlorination synthetic reaction, outer circulation pump continuous operation, the outer circulation chuck is set the first reactor and built-in coiled pipe cooler is controlled reaction temperature, and control to react when ph value of reaction reaches 2.4-3.2 and finish; To finish the material that reacts by the centrifugal crystallization of valve opening mechanism again and squeeze in the decrease temperature crystalline reactor 6, decrease temperature crystalline consists of the crystallization centrifugal mechanisms by centrifuge and centrifugal mechanism 7 afterwards.
The specific embodiment
Embodiment 1
In 5000 kilograms of enamel reaction stills 1, add 2000 kilograms of entry, opening enamel pot stirs and the outer circulation pump, and add therein circulated 15 minutes behind 300 kilograms of 263 kilograms of the cyanuric acid dry products, calcium carbonate after, after slurry mixes, by Venturi tube and suck chlorine and enter in the lump in the duct type reaction mechanism 3 400 cubes m/hs of its chlorine flowrates, open temperature-reducing coil valve in reacting kettle jacketing cooling valve and the still, the control reaction temperature is between the 15-18 degree.Detect pH value and arrive 3.0, stop chlorine and pass into; Material is squeezed in the decrease temperature crystalline reactor by beating pump, by the sym-closene crystallization of lowering the temperature to get, and then separated to get 458 kilograms of wet product of sym-closene by centrifugal mechanism 7, wet product effective chlorine 90.6% wherein, moisture 8.1%.
Embodiment 2
In 5000 kilograms of enamel reaction stills 1, add 2000 kilograms of entry, opening enamel pot stirs and the outer circulation pump, and add therein circulated 10 minutes behind 310 kilograms of 263 kilograms of the cyanuric acid dry products, calcium carbonate after, after slurry mixes, by Venturi tube and suck chlorine and enter in the lump in the duct type reaction mechanism 3 380 cubes m/hs of its chlorine flowrates, open temperature-reducing coil valve in reacting kettle jacketing cooling valve and the still, the control reaction temperature is between the 10-15 degree.Detect pH value and arrive 2.8, stop chlorine and pass into; Material is squeezed in the decrease temperature crystalline reactor by beating pump, by the sym-closene crystallization of lowering the temperature to get, and then separated to get 462 kilograms of wet product of sym-closene by centrifugal mechanism 7, wet product effective chlorine 90.8% wherein, moisture 8.5%.
Embodiment 3
In 5000 kilograms of enamel reaction stills 1, add 2000 kilograms of entry, opening enamel pot stirs and the outer circulation pump, and add therein circulated 18 minutes behind 320 kilograms of 263 kilograms of the cyanuric acid dry products, calcium carbonate after, after slurry mixes, by Venturi tube and suck chlorine and enter in the lump in the duct type reaction mechanism 3 370 cubes m/hs of its chlorine flowrates, open temperature-reducing coil valve in reacting kettle jacketing cooling valve and the still, the control reaction temperature is between the 18-20 degree.Detect pH value and arrive 2.4, stop chlorine and pass into; Material is squeezed in the decrease temperature crystalline reactor by beating pump, by the sym-closene crystallization of lowering the temperature to get, and then separated to get 462 kilograms of wet product of sym-closene by centrifugal mechanism 7, wet product effective chlorine 90.5% wherein, moisture 9.1%.
Utilize in the technical process that pipeline reactor produces sym-closene above-mentioned, the slurries of calcium carbonate, cyanuric acid, water are through pipeline reactor and chlorine generation chlorination synthetic reaction, be characterized in that chlorine can contact fully, react completely with slurries, reaction time is short, avoided side reaction to produce the danger that agene is blasted, and the conversion ratio of cyanuric acid reaches more than 90%.
Claims (5)
1. duct type reaction unit for preparing sym-closene is characterized in that: by
The discharging opening of the first reactor is communicated with the charging aperture of Venturi tube by circulating pump, the material sucking port of this Venturi tube and discharging opening are communicated with the charging aperture of chlorine pipeline and duct type reaction mechanism respectively, and the discharging opening of duct type reaction mechanism is communicated with the outer circulation reaction mechanism that consists of with the charging aperture of the first reactor; With
Consist of the crystallization centrifugal mechanism by described the first reactor and by its discharging opening by reaction mass beating pump, decrease temperature crystalline reactor and centrifugal mechanism
Consist of.
2. a kind of duct type reaction unit for preparing sym-closene as claimed in claim 1, it is characterized in that: described duct type reaction mechanism is for vertically setting up, and it highly is set to 8-10 meters.
3. the method for utilizing a kind of duct type reaction unit claimed in claim 1 to prepare sym-closene comprises:
The reactant circulating process:
In the first reactor, the water that adds 2000 kilograms, open rabbling mechanism and the outer circulation pump of described reactor, and add therein behind 300 kilograms of 263 kilograms of the cyanuric acid dry products, calcium carbonate so that reactant liquor by circulating in circulating pump, Venturi tube, duct type reaction mechanism and the first reactor, after slurry mixes, suck chlorine by described Venturi tube and enter in the lump in the duct type reaction mechanism, the reaction temperature in described the first reactor is controlled between the 10-20 degree simultaneously; Arrive 2.4-3.2 when detecting pH value, stop chlorine and pass into; With
The Crystallization Separation operation:
Material is squeezed into the sym-closene crystallization of lowering the temperature in the decrease temperature crystalline reactor to get by beating pump, and then separate to get the wet product of sym-closene by centrifugal mechanism.
4. the method for preparing sym-closene according to claim 3 is characterized in that: in the described reactant circulating process, when the weight portion of correspondence was kilogram, the speed that described Venturi tube sucks chlorine was controlled at 350-400 cubes m/hs.
5. the method for preparing sym-closene according to claim 3, it is characterized in that: in the described reactant circulating process, the granularity of described calcium carbonate is controlled at more than 300 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103079881A CN103316621A (en) | 2013-07-22 | 2013-07-22 | Method for preparing trichloroisocyanuric acid by using pipeline reactor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103079881A CN103316621A (en) | 2013-07-22 | 2013-07-22 | Method for preparing trichloroisocyanuric acid by using pipeline reactor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104478697A (en) * | 2014-11-21 | 2015-04-01 | 河北科技大学 | Method for preparing chloroacetic acid by using intermittent chlorination process |
| CN105037286A (en) * | 2015-05-12 | 2015-11-11 | 山东兴达化工有限公司 | Researching and application of cyanuric acid derivative ecological environment-friendly zero-emission new process |
| CN108722338A (en) * | 2018-06-08 | 2018-11-02 | 湖北可赛化工有限公司 | A kind of tubular reactor system and method being used to prepare TCCA |
Citations (5)
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| EP1693357A1 (en) * | 2005-02-22 | 2006-08-23 | Miltitz Aromatics GmbH | Process and apparatus for carying out a ring opening cross-metathesis reaction between cyclic and acyclic olefins |
| CN201572636U (en) * | 2009-11-13 | 2010-09-08 | 广州市道明化学有限公司 | Continuous circulation production device for pearlescent slurry |
| CN102329275A (en) * | 2011-07-19 | 2012-01-25 | 鄄城康泰化工有限公司 | Preparation methods of trichloroisocyanuric acid and sodium dichloro isocyanurate |
| CN102335573A (en) * | 2010-07-23 | 2012-02-01 | 中国石油化工股份有限公司 | Caprolactam causticization device |
| CN203346310U (en) * | 2013-07-22 | 2013-12-18 | 河北冀衡化学股份有限公司 | Pipeline-type reaction device for preparing trichloroisocyanuric acid |
-
2013
- 2013-07-22 CN CN2013103079881A patent/CN103316621A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1693357A1 (en) * | 2005-02-22 | 2006-08-23 | Miltitz Aromatics GmbH | Process and apparatus for carying out a ring opening cross-metathesis reaction between cyclic and acyclic olefins |
| WO2006089675A1 (en) * | 2005-02-22 | 2006-08-31 | Miltitz Aromatics Gmbh | Method and plant for carrying out a ring-opening crossed metathesis reaction between cyclic and acyclic olefins |
| CN201572636U (en) * | 2009-11-13 | 2010-09-08 | 广州市道明化学有限公司 | Continuous circulation production device for pearlescent slurry |
| CN102335573A (en) * | 2010-07-23 | 2012-02-01 | 中国石油化工股份有限公司 | Caprolactam causticization device |
| CN102329275A (en) * | 2011-07-19 | 2012-01-25 | 鄄城康泰化工有限公司 | Preparation methods of trichloroisocyanuric acid and sodium dichloro isocyanurate |
| CN203346310U (en) * | 2013-07-22 | 2013-12-18 | 河北冀衡化学股份有限公司 | Pipeline-type reaction device for preparing trichloroisocyanuric acid |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104478697A (en) * | 2014-11-21 | 2015-04-01 | 河北科技大学 | Method for preparing chloroacetic acid by using intermittent chlorination process |
| CN105037286A (en) * | 2015-05-12 | 2015-11-11 | 山东兴达化工有限公司 | Researching and application of cyanuric acid derivative ecological environment-friendly zero-emission new process |
| CN108722338A (en) * | 2018-06-08 | 2018-11-02 | 湖北可赛化工有限公司 | A kind of tubular reactor system and method being used to prepare TCCA |
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Application publication date: 20130925 |