CN101899015A - Process for producing trichloroisocyanuric acid by using calcium carbonate - Google Patents
Process for producing trichloroisocyanuric acid by using calcium carbonate Download PDFInfo
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- CN101899015A CN101899015A CN 201010254956 CN201010254956A CN101899015A CN 101899015 A CN101899015 A CN 101899015A CN 201010254956 CN201010254956 CN 201010254956 CN 201010254956 A CN201010254956 A CN 201010254956A CN 101899015 A CN101899015 A CN 101899015A
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Abstract
The invention relates to a production process for producing trichloroisocyanuric acid by using calcium carbonate as a raw material. The process is characterized in that: reactants comprise calcium carbonate, cyanuric acid, water and chlorine; and in the technical scheme, the chlorine and the water perform a hydrolysis reaction, and then the hydrolysate reacts with the calcium carbonate and the cyanuric acid to produce side products calcium chloride and trichloroisocyanuric acid respectively. Since no strong alkali substance, such as sodium hydroxide and the like, is used in the whole reaction and the reaction system is neutral or alkalescent, the chlorine and the cyanuric acid are prevented from the risk of performing derivative-damaging reaction to produce nitrogen trichloride, and the safety of the production process is greatly improved; furthermore, the cost of the calcium carbonate used in the process is obviously reduced in comparison with that of alkali liquor, the process does not have any requirement on the grain diameter of the calcium carbonate, so that the cost of the process in the invention is obviously reduced.
Description
Technical field
The present invention relates to a kind of production technique of utilizing lime carbonate for the raw material production trichloroisocyanuric acid.
Background technology
The production technique of trichloroisocyanuric acid mainly is to adopt the liquid caustic soda method to produce at present, i.e. trisodium salt is produced in liquid caustic soda (as NaOH solution) and cyanuric acid reaction, and logical again chlorine generates trichloroisocyanuric acid.The consumption of the liquid caustic soda that this technology is used is big, and price is higher than lime carbonate far away, so such production technique cost height.And cyanuric acid when under alkaline condition, meeting chlorine broken easily ring generate nitrogen trichloride, the concentration of nitrogen trichloride in gas phase reaches 5% will blast, so such process safety is poor.
Summary of the invention
Main purpose of the present invention provides a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid, and this process safety is reliable, and production cost is low.
For achieving the above object, the technical solution adopted in the present invention is: a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid, it is characterized in that: reactant is lime carbonate, cyanuric acid, water and chlorine.
When adopting technique scheme: in four kinds of reactants, at first chlorine and water generation hydrolysis reaction, hydrolysate and lime carbonate and cyanuric acid react respectively and generate by product calcium chloride and trichloroisocyanuric acid then, owing to do not use strong alkaline substances such as sodium hydroxide in the entire reaction, reaction system is neutrality or weakly alkaline, so just avoided chlorine and cyanuric acid that the risk that broken ring derivatives reaction generates nitrogen trichloride takes place, the security of production technique improves greatly, and the lime carbonate cost that uses in this technology significantly reduces than alkali lye, and the particle diameter of lime carbonate also had no requirement, so the cost of technology of the present invention significantly reduces.
Embodiment
A kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid, this technology utilization lime carbonate, cyanuric acid, water and chlorine are reactant, four reaction mechanism is: at first chlorine and water generation hydrolysis reaction, hydrolysate and lime carbonate and cyanuric acid react respectively and generate by product calcium chloride and product trichloroisocyanuric acid then.Because the chemical property of four kinds of materials itself determined that the reaction process between the material is above-mentioned order, so the order of addition(of ingredients) of this technology is not strict with, its temperature of reaction pressure also all is that normal temperature and pressure gets final product.
This processing method mainly contains three kinds of embodiments usually: a kind of is earlier lime carbonate to be joined in the cyanuric acid aqueous solution, because of water mainly plays carrier in reaction system, be used for reactant is uniformly dispersed, the amount of water reduces hardly, so the not strict demand of water consumption of reaction in other words conj.or perhaps of the concentration of cyanuric acid; Usually the concentration of the cyanuric acid aqueous solution for well, can guarantee that reactant is uniformly dispersed between 5～18%, guarantees that again reactant has enough concentration and guarantees that speed of reaction is higher.The mol ratio of cyanuric acid and lime carbonate preferably between 1: 1.5～1.7, makes reactant reaction more thorough, is convenient to follow-up separation and purification.Logical then chlorine reacts in solution, reacts under the condition that is preferably in 5～30 ℃ and carries out, when the PH of solution can be judged to be reaction end between 3.0～3.5.The judgement of this temperature of reaction and reaction end is identical with the existing technology of utilizing alkali lye to produce trichloroisocyanuric acid.Reaction finishes the first solid-liquid separation in back and goes out product, from mother liquor just recovered acid, chlorine and calcium chloride the filtrate, reclaims acid, chlorine in the mother liquor usually earlier then, reclaims calcium chloride then.
Another kind of operating method is exactly: earlier lime carbonate is mixed with water, the add-on of water is not strict with, and can suitably determine with reference to the water consumption of first kind of embodiment; When the solution pH value is that the feeding amount of decidable chlorine is enough between 4.4～4.6.Again cyanuric acid or cyanuric acid solution are mixed with this solution, reactant promptly can rapid reaction to terminal; Conditions such as the temperature of this reaction, pressure also are identical with prior art, promptly react under 5～30 ℃ temperature condition.The mol ratio of employed cyanuric acid and lime carbonate is preferably between 1: 1.5～1.7.
Perhaps, also can adopt lime carbonate to mix, feed chlorine reaction then, again the hypochlorous acid that generates be extracted to join in the cyanuric acid aqueous solution and react to terminal with suitable quantity of water in order to adapt to the cyanuric acid solution of different concns.The judgement of capacity is identical with second kind of embodiment to feed chlorine, and the mol ratio of employed cyanuric acid and lime carbonate is also preferably between 1: 1.5～1.7.No matter adopt which kind of embodiment because produce, reaction mechanism all is that water contacts back immediate response generation trichloroisocyanuric acid with the anti-hypochlorous acid that generates of chlorine with cyanuric acid, so after hypochlorous acid extracted with the operating method of cyanuric acid solution reaction in, concentration of active substance is the highest, and reaction efficiency is also the highest; And the concentration of cyanuric acid solution can be selected arbitrarily.
First then solid-liquid separation goes out product, reclaims by product or raw material that calcium chloride etc. has economic worth again from mother liquor.
The invention has the advantages that: the ordinary calcium carbonate that can use cheap any particle diameter, lime carbonate can lightweight also can be heavy, usually more little its surface-area of lime carbonate particle diameter is big more, speed of reaction is high more, but it is not linear, and in fact the particle diameter of lime carbonate is as long as just can reach good effect less than 1 millimeter; And the cost of such ordinary calcium carbonate significantly reduces than sodium hydroxide liquid or the particle diameter lime carbonate less than 0.1 micron.And lime carbonate replaces in the sodium hydroxide production trichloroisocyanuric acid process, it is neutral that solution is, and PH is about 6.3, so ring can not take place brokenly cyanuric acid, also can not generate nitrogen trichloride with chlorine after feeding chlorine, this has also just been avoided the danger that generates the by product nitrogen trichloride and blast.Such process safety improves greatly.
Embodiment 1
In the 5000ml container, add the 129g cyanuric acid, 150g lime carbonate adds 1620g water, introduce chlorine gas to make reaction, control reaction temperature is 5 ℃ under agitation condition, filter during pH value 3.0, wash, dry trichloroisocyanuric acid 208g, the available chlorine 90.9% of product.Meeting has chlorine 〉=90% export inspection standard.
Embodiment 2
In the 5000ml container, add the 129g cyanuric acid, 165g lime carbonate adds 1800g water, introduce chlorine gas to make reaction, control reaction temperature is 30 ℃ under agitation condition, filter during pH value 3.2, wash, dry trichloroisocyanuric acid 212g, the available chlorine 91.4% of product.Meeting has chlorine 〉=90% export inspection standard.
Embodiment 3
In the 5000ml container, add lime carbonate 160g and water 1500g, under 25 ℃ of conditions logical chlorine to solution PH 4.4, the cyanuric acid solution that adds 260 ml concns 50% then reacts, get trichloroisocyanuric acid 200.58g behind the filtering drying, effectively cyanogen 91.2%.
Embodiment 4
In the 5000ml container, add lime carbonate 150g and water 2700g, under 15 ℃ of conditions logical chlorine to solution PH 4.6, extract the cyanuric acid solution that hypochlorous acid joins 650 ml concns 20% then and react, get trichloroisocyanuric acid 232g behind the filtering drying, effectively cyanogen 91.7%.
Embodiment 5
In the 5000ml container, add lime carbonate 160g and water 3000g, under 22 ℃ of conditions logical chlorine to solution PH 4.5, the cyanuric acid solution that adds 260 ml concns 50% then reacts, behind the filtering drying trichloroisocyanuric acid 235g, effective cyanogen 91.4%.
Claims (6)
1. technology of utilizing lime carbonate to produce trichloroisocyanuric acid, it is characterized in that: reactant is lime carbonate, cyanuric acid, water and chlorine.
2. a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid according to claim 1, it is characterized in that: the mol ratio of described cyanuric acid and lime carbonate is 1: 1.5～1.7.
3. a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid according to claim 2 is characterized in that: earlier lime carbonate is mixed with cyanuric acid solution, the concentration of cyanuric acid solution feeds chlorine reaction to terminal then in solution between 5～18%.
4. a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid according to claim 2, it is characterized in that: earlier lime carbonate is mixed with water, in system, feed chlorine then, the solution pH value stopped feeding chlorine at 4.4～4.6 o'clock, again with its with cyanuric acid or cyanuric acid solution mixing afterreaction to terminal.
5. a kind of technology of utilizing lime carbonate to produce trichloroisocyanuric acid according to claim 2, it is characterized in that: earlier lime carbonate is mixed with water, in system, feed chlorine then, the solution pH value stopped feeding chlorine at 4.4～4.6 o'clock, the hypochlorous acid of abstraction reaction generation and cyanuric acid solution reaction are to terminal again.
6. according to claim 3 or 4 or 5 described a kind of technologies of utilizing lime carbonate to produce trichloroisocyanuric acid, it is characterized in that: described temperature of reaction is 5～30 ℃.
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| CN2010102549566A CN101899015B (en) | 2010-08-11 | 2010-08-11 | Process for producing trichloroisocyanuric acid by using calcium carbonate |
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| CN2010102549566A CN101899015B (en) | 2010-08-11 | 2010-08-11 | Process for producing trichloroisocyanuric acid by using calcium carbonate |
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Cited By (5)
| 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 |
| CN103980214A (en) * | 2013-11-01 | 2014-08-13 | 山东大明消毒科技有限公司 | Method for treating waste gas and wastewater in trichloroisocyanuric acid production process |
| CN104909388A (en) * | 2015-05-12 | 2015-09-16 | 山东兴达化工有限公司 | Research of information automation production technology for combined production of cyanuric acid and ammonium sulfate, and synthesis and research of chloro derivative |
| 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 |
| CN109053611A (en) * | 2018-08-21 | 2018-12-21 | 山东昌邑海能化学有限责任公司 | A method of sym-closene is produced in super gravity field |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380290A (en) * | 2002-03-20 | 2002-11-20 | 唐银华 | Technological process for producing chlorinated isocyanuric acid |
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2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380290A (en) * | 2002-03-20 | 2002-11-20 | 唐银华 | Technological process for producing chlorinated isocyanuric acid |
Non-Patent Citations (1)
| Title |
|---|
| 《化工生产与技术》 20011231 蒋琦等 三氯异氰尿酸合成 45-46，特别是46页左栏第8段 1-6 第8卷, 第4期 2 * |
Cited By (6)
| 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 |
| CN103980214A (en) * | 2013-11-01 | 2014-08-13 | 山东大明消毒科技有限公司 | Method for treating waste gas and wastewater in trichloroisocyanuric acid production process |
| CN104909388A (en) * | 2015-05-12 | 2015-09-16 | 山东兴达化工有限公司 | Research of information automation production technology for combined production of cyanuric acid and ammonium sulfate, and synthesis and research of chloro derivative |
| 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 |
| CN109053611A (en) * | 2018-08-21 | 2018-12-21 | 山东昌邑海能化学有限责任公司 | A method of sym-closene is produced in super gravity field |
| CN109053611B (en) * | 2018-08-21 | 2022-04-19 | 山东昌邑海能化学有限责任公司 | Method for producing trichloroisocyanuric acid in high gravity field |
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| CN101899015B (en) | 2012-05-30 |
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Effective date of registration: 20160525 Address after: Gold Hui Road Huaishang District Industrial Zone in Anhui province 233300 Mo estuary Bengbu City No. 2-1 Patentee after: Bengbu Jingxian Hongfa Chemical Co.,Ltd. Address before: 241000 201 gardeners, 2 districts, 21 buildings, Anhui, Wuhu Patentee before: Tang Yinhua |
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