CN1300119C - Process for preparing cyanuric acid - Google Patents
Process for preparing cyanuric acid Download PDFInfo
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- CN1300119C CN1300119C CNB2005100128932A CN200510012893A CN1300119C CN 1300119 C CN1300119 C CN 1300119C CN B2005100128932 A CNB2005100128932 A CN B2005100128932A CN 200510012893 A CN200510012893 A CN 200510012893A CN 1300119 C CN1300119 C CN 1300119C
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Abstract
The present invention belongs to the technical field of preparation of an intermediate body of organic chemical industry raw material. More specifically, the present invention discloses a method for preparing cyanuric acid. The preparation method comprises a preparation step of a cyanuric acid crude product, a hydrolysis step and a washing step, wherein the hydrolysis step comprises the following steps: three pump pipes are respectively used to continuously convey a cyanuric acid crude product prepared by reaction in which urea is heated, saturated heating steam and sulphuric acid into a first reaction tower in at least two reaction towers communicated with a pipeline; simultaneously, the flow quantity of the sulphuric acid, the concentration of the sulphuric acid and the flow quantity of the cyanuric acid crude products are controlled; after the reaction, the temperature is lowered, and through washing operation and separation operation, cyanuric acid is obtained. Because in the hydrolysis step for preparing the cyanuric acid, the tower type continuous hydrolysis technology is adopted, the hydrolysis step can be continuously carried out at the high temperature and under the high pressure, and the reaction speed is enhanced. Therefore, the technology has the advantages of short reaction period, simple operation, and easy control of quality of products. The preparation efficiency is improved.
Description
Technical field
The invention belongs to the preparing technical field of Organic Chemicals intermediate, relate in particular to the preparation method of cyanuric acid.
Background technology
Cyanuric acid belongs to the intermediate of Organic Chemicals, uses extremely extensive.Be mainly used in producing of cyanuric acid muriate, salt, lipid, SYNTHETIC OPTICAL WHITNER, resin, oxidation inhibitor, paint, selective herbicide and metal cyanide negative catalyst synthetic, and as the additive of nylon, fire-retardant for plastic and makeup.In organic synthesis, occupy an important position.
At present, produce the preparation, refining and wash three process that cyanuric acid technology comprises crude product.Wherein, refining step adopts is that single jar of operation of intermittent type comprises complex acid, feeds intake, heats up, is incubated and the production method of step such as cooling, and every jar of reaction times after feeding intake is between 8-10 hour.If the throughput of 10000 tons of refining cyanuric acids is produced in design per year, then must dispose at least 20 5 cubic metres reactor, and must control respectively the processing parameter of each reactor in process of production.Therefore, in the technology of preparation cyanuric acid, refining step adopts that this intermittent type operation exists the equipment complexity, the production cycle is long, usefulness is low and can not guarantee the metastable defective of quality product.
The content of invention
Purpose of the present invention just provides a kind of preparation method of with short production cycle, the metastable cyanuric acid of quality product.
Realize that the technical scheme that above-mentioned purpose of the present invention adopted is:
The preparation method of cyanuric acid includes preparation, hydrolysis and three operations of washing of cyanuric acid crude product, and wherein said hydrolyzing process is:
Cyanuric acid crude product, saturated hot steam and the dilute sulphuric acid that makes after using three pump lines with the urea reacting by heating respectively is transported to continuously at least by in two first reaction towers in the reaction tower that pipeline is communicated with; Control the flow of dilute sulphuric acid simultaneously, the sulfuric acid concentration of reaction solution is wherein kept between the 20%-30%; Control the flow of described cyanuric acid crude product, make be controlled at its reaction times in described reaction tower 0.5-2 hour; Reaction back effusive reaction solution from described reaction tower promptly makes the purified cyanuric acid after the cooling tank cooling;
Above-mentioned purified cyanuric acid is promptly got the cyanuric acid product through washing step with separating.
Its additional technical feature is:
Be fixed with stirring mechanism in described first reaction tower;
The mounting height of described first reaction tower is higher than the height of other retort;
The temperature of described saturated hot steam is 120---130 ℃;
The preparation method of cyanuric acid provided by the present invention compared with prior art, have the following advantages: because in this cyanuric acid preparation method's hydrolyzing process, adopted the technology of tower continuous hydrolysis, be about to several reaction towers and be connected in series, utilize pressure to make input raw material wherein in process of flowing, finish chemical reaction with pipeline.Owing to selected the liquid height in the sulfuric acid concentration in the reacting pipe, reaction pressure, temperature, the retort and the flow of various reactants, make hydrolyzing process under high temperature and high pressure, to carry out continuously, accelerated its speed of response (generally from the reaction times that is dosed into out product be 0.5---2 hours).Therefore, this technology has the advantage that reaction time is short, simple to operate, quality product is controlled easily, and has improved production efficiency.
Description of drawings
Accompanying drawing is the schematic flow sheet of the production technique of cyanuric acid provided by the invention.
Embodiment
Below in conjunction with accompanying drawing the production technique of cyanuric acid provided by the present invention and the principle of work of equipment thereof are described in further detail.
As shown be the flow process and the unit construction principle synoptic diagram of the production technique of cyanuric acid provided by the invention.
Urea generates the cyanuric acid crude product after pyrolysis, it is made slurries, with pump line 1 it is carried in first reaction tower 2 continuously by flow velocity of setting then, and the saturated hot steam that simultaneously 27% dilute sulphuric acid and temperature is 125 ℃ was delivered in this reaction tower continuously by 3,4 whiles of pipe pump.When carrying cyanuric acid crude product and dilute sulphuric acid, regulate its flow, make the sulfuric acid concentration of its reaction solution remain on 20%---in 30% the scope, if design is produced per year when being the throughput of 1.5 ten thousand tons of refining cyanuric acids:
Embodiment 1:
The flow of cyanuric acid crude product is 3 tons/hour, the flow of 27% dilute sulphuric acid is 7 cubic metres/hour, the temperature of importing saturated hot steam remains on 125 ℃, the pressure of saturated hot steam be adjusted at 0.75Mpa, make reaction solution after pipeline flows into second reaction tower, remain on 1 hour in the effusive time from entering first reaction tower;
The intact liquid of effusive reaction that then will be from second reaction tower is delivered in the cooling tower lowers the temperature, get final product the purified cyanuric acid.Through washing with separate baking operation and get the cyanuric acid product.
Embodiment 2:
The flow of cyanuric acid crude product is 4 tons/hour, the flow of 25% dilute sulphuric acid is 7 cubic metres/hour, the temperature of importing saturated hot steam remains on 120 ℃, the pressure of saturated hot steam be adjusted at 0.6Mpa, make reaction solution after pipeline flows into second reaction tower, remain on 0.75 hour in the effusive time from entering first reaction tower;
Cooling, washing and to separate baking operation the same.
Embodiment 3:
The flow of cyanuric acid crude product is 5 tons/hour, the flow of 28% dilute sulphuric acid is 7.5 cubic metres/hour, the temperature of importing saturated hot steam remains on 130 ℃, the pressure of saturated hot steam be adjusted at 0.14Mpa, make reaction solution after pipeline flows into second reaction tower, remain on 0.5 hour in the effusive time from entering first reaction tower;
Cooling, washing and to separate baking operation the same.
Embodiment 4:
The flow of cyanuric acid crude product is 3.5 tons/hour, the flow of 20% dilute sulphuric acid is 8 cubic metres/hour, the temperature of importing saturated hot steam remains on 120 ℃, the pressure of saturated hot steam be adjusted at 0.7Mpa, make reaction solution after pipeline flows into second reaction tower, remain on 1.5 hours in the effusive time from entering first reaction tower;
Cooling, washing and to separate baking operation the same.
Embodiment 5:
The flow of cyanuric acid crude product is 4.5 tons/hour, the flow of 30% dilute sulphuric acid is 7 cubic metres/hour, the temperature of importing saturated hot steam remains on 125 ℃, the pressure of saturated hot steam be adjusted at 0.6Mpa, make reaction solution after pipeline flows into second reaction tower, remain on 2 hours in the effusive time from entering first reaction tower;
Cooling, washing and to separate baking operation the same.
In above-mentioned conversion unit, can improve the pressure of liquid stream by the mounting height (being the height of liquid level in the tower) of increasing first reaction tower, reduce the pressure of hot steam, so that improve the safety coefficient of equipment.
In addition,, enhance productivity, in first reaction tower, be fixed with stirring mechanism, make the raw material that continuously flows in the tower also to react by thorough mixing, also can improve speed of response, increase output in order to improve the speed of response of reaction solution in the reaction tower.
In this reaction, it is high more that it imports saturated hot steam temperature, and pressure is also big more, and required reaction tower is just few more.But it is high more that required reaction tower withstand voltage just requires, and its safety coefficient will reduce.In order to improve the safety performance of reaction tower, reaction tower is increased to 3---4, the flow process of increase reaction solution, lengthening reaction times.
In above-mentioned preparation cyanuric acid elaboration reaction, the flow of control cyanuric acid crude product and dilute sulphuric acid is crucial, makes the pH value of its reaction solution be adjusted at 4---between 5, can realize the purpose that cyanuric acid elaboration of the present invention prepares successive reaction, enhances productivity.
Claims (4)
1, the preparation method of cyanuric acid includes preparation, hydrolysis and three operations of washing of cyanuric acid crude product, it is characterized in that described hydrolyzing process is:
Cyanuric acid crude product, saturated hot steam and the sulfuric acid that makes after using three pump lines with the urea reacting by heating respectively is transported to continuously at least by in two first reaction towers in the reaction tower that pipeline is communicated with; Control the vitriolic flow simultaneously, the sulfuric acid concentration of reaction solution is wherein kept between the 20%-30%; Control the flow of described cyanuric acid crude product, make be controlled at its reaction times in described reaction tower 0.5-2 hour; Reaction back effusive reaction solution from described reaction tower promptly makes the purified cyanuric acid after the cooling tank cooling;
Above-mentioned purified cyanuric acid is promptly got the cyanuric acid product through washing step with separating.
2, the preparation method of cyanuric acid according to claim 1 is characterized in that: be fixed with stirring mechanism in described first reaction tower.
3, the preparation method of cyanuric acid according to claim 1 is characterized in that: the mounting height of described first reaction tower is higher than the height of other retort.
4, the preparation method of cyanuric acid according to claim 1 is characterized in that: the temperature of described saturated hot steam is 120---130 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100128932A CN1300119C (en) | 2005-10-11 | 2005-10-11 | Process for preparing cyanuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100128932A CN1300119C (en) | 2005-10-11 | 2005-10-11 | Process for preparing cyanuric acid |
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| Publication Number | Publication Date |
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| CN1749251A CN1749251A (en) | 2006-03-22 |
| CN1300119C true CN1300119C (en) | 2007-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100128932A Active CN1300119C (en) | 2005-10-11 | 2005-10-11 | Process for preparing cyanuric acid |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516188B (en) * | 2011-12-12 | 2014-04-16 | 河北安海化工有限公司 | Preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid |
| CN102633735B (en) * | 2012-04-17 | 2013-11-06 | 四川金象赛瑞化工股份有限公司 | Novel technology for producing cyanuric acid |
| CN106316971A (en) * | 2016-08-19 | 2017-01-11 | 鄄城康泰化工有限公司 | Preparation method of cyanuric acid |
| CN108047150A (en) * | 2018-01-24 | 2018-05-18 | 诸城市良丰化学有限公司 | A kind of cyanuric acid produces process for purification |
| CN116332863B (en) * | 2023-02-17 | 2025-02-14 | 国能(山东)能源环境有限公司 | A multi-stage series cyanuric acid purification system and process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181801A (en) * | 1977-05-09 | 1980-01-01 | Stamicarbon, B.V. | Process for preparing cyanuric acid |
| SU835407A1 (en) * | 1978-04-03 | 1981-06-07 | Предприятие П/Я Г-4302 | Method of obtaining nitrogen-phosphorus food addition for animals |
| CN1030076C (en) * | 1991-08-21 | 1995-10-18 | Y·诺夫达德斯专利公司 | Device and method for manufacturing cyanuric acid |
| CN2545198Y (en) * | 2002-04-19 | 2003-04-16 | 叶龙声 | Device for producing raw cyanuric acid by direct heating in tube |
-
2005
- 2005-10-11 CN CNB2005100128932A patent/CN1300119C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181801A (en) * | 1977-05-09 | 1980-01-01 | Stamicarbon, B.V. | Process for preparing cyanuric acid |
| SU835407A1 (en) * | 1978-04-03 | 1981-06-07 | Предприятие П/Я Г-4302 | Method of obtaining nitrogen-phosphorus food addition for animals |
| CN1030076C (en) * | 1991-08-21 | 1995-10-18 | Y·诺夫达德斯专利公司 | Device and method for manufacturing cyanuric acid |
| CN2545198Y (en) * | 2002-04-19 | 2003-04-16 | 叶龙声 | Device for producing raw cyanuric acid by direct heating in tube |
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| CN1749251A (en) | 2006-03-22 |
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Address after: 053400 Wuyi County in Hengshui province Hebei City Industrial Zone No. 8 Ji Heng Lu Patentee after: Hebei Jiheng Chemical Co., Ltd. Address before: 053000 No. 125 Zhonghua North Street, Hebei, Hengshui Patentee before: Hebei Jiheng Chemical Co., Ltd. |