CN109053611B - Method for producing trichloroisocyanuric acid in high gravity field - Google Patents
Method for producing trichloroisocyanuric acid in high gravity field Download PDFInfo
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- CN109053611B CN109053611B CN201810951744.XA CN201810951744A CN109053611B CN 109053611 B CN109053611 B CN 109053611B CN 201810951744 A CN201810951744 A CN 201810951744A CN 109053611 B CN109053611 B CN 109053611B
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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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- Treatment Of Water By Oxidation Or Reduction (AREA)
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Abstract
The invention discloses a method for producing trichloroisocyanuric acid in a hypergravity field, which belongs to the technical field of heterocyclic compounds and comprises the following steps of (1) carrying out gas-liquid countercurrent reaction on excessive chlorine and a metal compound consuming hydrochloric acid in a first hypergravity field, separating hypochlorous acid mist upwards and separating a chloride solution downwards; (2) desalting the hypochlorous acid mist prepared in the step (1); (3) and (3) carrying out gas-liquid-solid three-phase reaction on the hypochlorous acid mist prepared in the step (2) and cyanuric acid slurry in a second super-gravity field to prepare trichloroisocyanuric acid. The method adopts excessive chlorine gas to generate hypochlorous acid and chloride salt as much as possible, and also enables the first high gravity field to be in an acid environment to reduce decomposition; the desalted hypochlorous acid mist is more beneficial to subsequent reaction, and the yield of trichloroisocyanuric acid is finally improved together; and cyanuric acid or trichloroisocyanuric acid does not contact with alkaline substances, thus avoiding the generation of nitrogen trichloride and environmental pollution.
Description
Technical Field
The invention belongs to the technical field of heterocyclic compounds, and particularly relates to a method for producing trichloroisocyanuric acid in a high-gravity field.
Background
Trichloroisocyanuric acid is one of chloroisocyanuric acid series products, is white crystalline powder or granular solid, and has strong chlorine stimulation smell. The effective chlorine of the fish-shaped bleaching powder is more than 90 percent and 2-3 times higher than that of bleaching powder, has high-efficiency, broad-spectrum and relatively safe disinfection effects, gradually becomes a renewal product of bleaching powder and bleaching essence, and is used for disinfection and sterilization of drinking water, industrial circulating water, swimming pools, restaurants, hotels, public places, families, hospitals, eggs, fish diseases and the like. And the three wastes generated in the production of trichloroisocyanuric acid are greatly reduced compared with bleaching extract, so the trend of replacing the bleaching extract by the three wastes in advanced countries is realized.
At present, trichloroisocyanuric acid is mainly produced by adopting a chlorine method, namely chlorine directly reacts with alkali, carbonate or isocyanate dissolved in water or other solvents, and the process has the defects that: the consumption of reactants is large, 6-9 tons of wastewater can be generated when 1 ton of products are produced, the wastewater contains a large amount of sodium chloride and trichloroisocyanuric acid or dichloroisocyanuric acid, but the value of the wastewater is not as high as the recycling cost, so that the recycling comprehensive value is low, the wastewater is basically in an outward discharge state, and serious environmental pollution is caused. In addition, in the process, because cyanuric acid is easy to generate nitrogen trichloride in an alkaline solution, a trichloroisocyanuric acid product can also be decomposed to generate nitrogen trichloride under the condition of heating or alkalinity, and the nitrogen trichloride is easy to explode in a closed reaction container of chlorination reaction, so that the safe production is influenced.
The Chinese invention patent application 200510048183.5 discloses a production method for continuously synthesizing sodium dichloroisocyanurate and co-producing trichloroisocyanuric acid by using sodium hypochlorite-chlorine gas in one step, 201010254956.6 discloses a production process for producing trichloroisocyanuric acid by using calcium carbonate as a raw material, and 201510238770.4 discloses research and application of an ecological environment-friendly zero-emission new process of cyanuric acid derivatives, which belong to the category of the traditional processes and do not get rid of the problems of the traditional processes; and the kettle reactor has high consumption, low yield, high process labor intensity and poor production continuity.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for producing trichloroisocyanuric acid in a high-gravity field, which can improve the product yield on the premise of safety and environmental protection.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for producing trichloroisocyanuric acid in a high gravity field is designed, and is characterized in that: the method comprises the following steps:
(1) preparing hypochlorous acid mist: carrying out gas-liquid countercurrent reaction on excessive chlorine and metal compounds consuming hydrochloric acid in a first hypergravity field, separating out hypochlorous acid mist upwards and chloride solution downwards;
(2) desalting: desalting the hypochlorous acid mist prepared in the step (1);
(3) preparing trichloroisocyanuric acid: and (3) carrying out gas-liquid-solid three-phase reaction on the hypochlorous acid mist treated in the step (2) and cyanuric acid slurry in a second super-gravity field to prepare trichloroisocyanuric acid, wherein the molar ratio of chlorine to cyanuric acid is 3-10: 1.
Preferably, the concentration of the cyanuric acid slurry in the step (3) is 20-50%.
Preferably, the salt removing operation in the step (2) is completed by a salt trap.
Preferably, the residual chlorine gas in the step (1) is returned to the first high gravity field again to prepare the hypochlorous acid mist.
Preferably, in step (1), the first high gravity field is generated by a first high gravity reactor; in the step (2), a second high gravity field is generated by a second high gravity reactor.
Preferably, the chloride salt in the chloride salt solution in step (1) is recovered and extracted.
Preferably, the metal compound consuming hydrochloric acid in step (1) is a metal oxide, metal hydroxide or/and carbonate.
Compared with the prior art, the invention has the beneficial effects that:
1. in the whole process, the cyanuric acid or trichloroisocyanuric acid is not contacted with alkaline substances, so that the generation of nitrogen trichloride is avoided, the production safety is greatly improved, and the liquid-phase chloride in the first high-gravity field is not contacted with organic substances such as cyanuric acid or trichloroisocyanuric acid, so that saline containing the organic substances is not generated, and the environmental pollution is avoided.
2. Due to the adoption of excessive chlorine, on one hand, hypochlorous acid and chloride salt are generated as much as possible, and on the other hand, the first high-gravity field is in an acid environment, so that the decomposition of the hypochlorous acid or hypochlorite is reduced; and the desalted hypochlorous acid mist is more beneficial to the subsequent reaction, so that the yield of the trichloroisocyanuric acid is finally improved together.
3. Because the reactions are carried out in a high-gravity field, the surface tension is overcome by huge shearing stress, so that the liquid is pulled up or torn into tiny liquid films, liquid threads and liquid drops, huge interphase contact area is generated, and the relative speed and mutual contact between phases are enhanced, thereby realizing efficient mass and heat transfer processes and chemical reaction processes, and further preparing the stable and gas-phase hypochlorous acid mist.
4. Because no water is added in the reaction and only water is generated in the reaction, the concentration of the hypochlorous acid mist is greatly improved, the decomposition of hypochlorous acid is avoided, the concentration of chloride is increased, and the recycling operation is facilitated.
5. The whole process is easy to control, high in efficiency, high in product yield, safe and environment-friendly, and convenient to widely popularize and apply in the industry.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Example one
The production method of trichloroisocyanuric acid comprises the following steps:
(1) preparing hypochlorous acid mist: carrying out gas-liquid countercurrent reaction on excessive chlorine and metal oxide in a high-gravity field formed by a first high-gravity reactor, separating hypochlorous acid mist upwards, separating chloride solution downwards, recovering and extracting chloride in the chloride solution, and returning the residual chlorine to the first high-gravity field after being discharged from a tail gas outlet of the first high-gravity reactor to prepare hypochlorous acid mist;
(2) desalting: desalting the hypochlorous acid mist prepared in the step (1) by using a salt catcher;
(3) preparing trichloroisocyanuric acid: and (3) carrying out gas-liquid-solid three-phase reaction on the hypochlorous acid mist treated in the step (2) and cyanuric acid slurry in a supergravity field formed by a second supergravity reactor to prepare trichloroisocyanuric acid. The cyanuric acid slurry used was prepared by mixing cyanuric acid with water at a concentration of 20% and a molar ratio of cyanuric acid to chlorine gas of 1: 3.
The metal oxide to be used may specifically be sodium oxide, calcium oxide, zinc oxide, magnesium oxide, or the like, and specific substances thereof are not particularly limited as long as hydrochloric acid generated in the reaction can be consumed.
In the process, the detection shows that the TOC content in the chloride solution generated by the first supergravity reactor is zero, the content of nitrogen trichloride in the water phase in the second supergravity reactor is zero, the discharged water can be recycled for cyanuric acid pulping, and the effective chlorine of the prepared trichloroisocyanuric acid is detected to be more than 91.2 percent, so that the prepared trichloroisocyanuric acid meets the requirement of high-grade products.
Example two
The difference between the present embodiment and the first embodiment is:
in the step (1), chlorine and metal hydroxide react in a high gravity field formed by the first high gravity reactor, wherein the metal hydroxide can be sodium hydroxide, calcium hydroxide or/and magnesium hydroxide and the like, as long as hydrochloric acid generated in the reaction can be consumed, and specific substances of the metal hydroxide are not particularly limited;
in the step (3), preparing trichloroisocyanuric acid: the concentration of the cyanuric acid slurry used was 35%, and the molar ratio of chlorine to cyanuric acid was 6: 1.
The available chlorine of the prepared trichloroisocyanuric acid is over 91.5 percent through detection. The rest is the same as the first embodiment.
EXAMPLE III
The difference between the present embodiment and the first embodiment is:
in the step (1), chlorine and carbonate react in a high gravity field formed by the first high gravity reactor, wherein the carbonate can be sodium carbonate, calcium carbonate or/and magnesium carbonate, and the like, as long as hydrochloric acid generated in the reaction can be consumed, and specific substances of the carbonate are not particularly limited;
in the step (3), preparing trichloroisocyanuric acid: the concentration of the cyanuric acid slurry used was 50%, and the molar ratio of chlorine to cyanuric acid was 10: 1. The rest is the same as the first embodiment.
The available chlorine of the prepared trichloroisocyanuric acid is over 91.4 percent through detection. The rest is the same as the first embodiment.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (5)
1. A method for producing trichloroisocyanuric acid in a high gravity field is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing hypochlorous acid mist: carrying out gas-liquid countercurrent reaction on excessive chlorine and metal compounds consuming hydrochloric acid in a first hypergravity field, separating out hypochlorous acid mist upwards and chloride solution downwards;
(2) desalting: desalting the hypochlorous acid mist prepared in the step (1);
(3) preparing trichloroisocyanuric acid: carrying out gas-liquid-solid three-phase reaction on the hypochlorous acid mist treated in the step (2) and cyanuric acid slurry in a second super-gravity field to prepare trichloroisocyanuric acid, wherein the molar ratio of chlorine to cyanuric acid is 3-10: 1, and the concentration of the cyanuric acid slurry is 20-50%;
in the step (1), a first hypergravity field is generated by a first hypergravity reactor; in the step (3), a second high gravity field is generated by a second high gravity reactor.
2. The method for producing trichloroisocyanuric acid in a high gravity field according to claim 1, wherein the method comprises the following steps: step (2)
The desalting operation in (1) is completed by a salt catcher.
3. The process for the production of trichloroisocyanuric acid in a high gravity field according to claim 1 or 2, wherein:
and (2) returning the residual chlorine in the step (1) to the first high gravity field again to prepare the hypochlorous acid mist.
4. The method for producing trichloroisocyanuric acid in a high gravity field according to claim 3, wherein the method comprises the following steps: recovering and extracting
And (3) taking chloride in the chloride solution in the step (1).
5. The method for producing trichloroisocyanuric acid in a high gravity field according to claim 4, wherein the method comprises the following steps: step (1)
The metal compound(s) consuming hydrochloric acid in (a) is (are) a metal oxide, metal hydroxide or/and carbonate.
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| CN201810951744.XA CN109053611B (en) | 2018-08-21 | 2018-08-21 | Method for producing trichloroisocyanuric acid in high gravity field |
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| CN201810951744.XA CN109053611B (en) | 2018-08-21 | 2018-08-21 | Method for producing trichloroisocyanuric acid in high gravity field |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048513A (en) * | 1996-09-11 | 2000-04-11 | The Dow Chemical Company | Method for synthesis of hypohalous acid |
| CN101899015A (en) * | 2010-08-11 | 2010-12-01 | 唐银华 | Process for producing trichloroisocyanuric acid by using calcium carbonate |
| 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 |
| CN106268575A (en) * | 2015-06-04 | 2017-01-04 | 北京化工大学 | The hypergravity swinging bed device of a kind of simultaneous reaction and separation and application thereof |
| CN106397081A (en) * | 2015-07-14 | 2017-02-15 | 北京化工大学苏州（相城）研究院 | Halogenation reaction method |
-
2018
- 2018-08-21 CN CN201810951744.XA patent/CN109053611B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048513A (en) * | 1996-09-11 | 2000-04-11 | The Dow Chemical Company | Method for synthesis of hypohalous acid |
| CN101899015A (en) * | 2010-08-11 | 2010-12-01 | 唐银华 | Process for producing trichloroisocyanuric acid by using calcium carbonate |
| 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 |
| CN106268575A (en) * | 2015-06-04 | 2017-01-04 | 北京化工大学 | The hypergravity swinging bed device of a kind of simultaneous reaction and separation and application thereof |
| CN106397081A (en) * | 2015-07-14 | 2017-02-15 | 北京化工大学苏州（相城）研究院 | Halogenation reaction method |
Non-Patent Citations (2)
| Title |
|---|
| A guide on the industrial application of rotating packed beds;Kolja Neumann et al.;《Chemical Engineering Research and Design》;20180422;第134卷;第443-462页 * |
| 超重力技术在卤代异氰尿酸（盐）生产技术及其废水废气处理中的应用探究;王宝品;《科技与企业》;20121231(第10期);第290页 * |
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