CN103102318A - Preparation method of cyanuric acid - Google Patents
Preparation method of cyanuric acid Download PDFInfo
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- CN103102318A CN103102318A CN2013100626970A CN201310062697A CN103102318A CN 103102318 A CN103102318 A CN 103102318A CN 2013100626970 A CN2013100626970 A CN 2013100626970A CN 201310062697 A CN201310062697 A CN 201310062697A CN 103102318 A CN103102318 A CN 103102318A
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Abstract
The invention provides a preparation method of cyanuric acid. The preparation method comprises the steps ofsoaking urea in a prepared inorganic acid composite solution for 3-8h, adding the urea in a heat conducting oil cyclical heating reaction kettle with a stirring device; rapidly increasing the temperature to 260 DEG C; reacting urea for 0.5-1h in the reaction kettle to obtain a cyanuric acid crude product; and finally refining, thereby obtaining the cyanuric acid product. As the urea is soaked in the inorganic acid composite solution before being added in the reaction kettle and the reaction kettle is internally provided with the fixed stirring device, a wall adhesion phenomenon is avoided, the heat transfer rate is accelerated, the purity of the prepared cyanuric acid crude product is high, the concentration of inorganic acid (generally dilute sulfuric acid solution) used in acid washing during the follow-up refining process is lowered to 5%-8% from 20%-25% of the inorganic acid used in a traditional solid phase method, meanwhile the number of times of water washing is reduced to 2-3, the cost is saved and simultaneously the production efficiency is improved. The cyanuric acid crude product is fine powder without grinding and the labor force is reduced greatly. Therefore, the technology has the advantages of short reaction period, simple operation, high product purity, high production efficiency and the like, and can realize continuous production.
Description
Technical field
The present invention relates to a kind of preparation method of cyanuric acid, belong to the preparing technical field of Organic Chemicals intermediate.
Background technology
Cyanuric acid (cyanuric acid, CA) has another name called tricyanic acid, is a kind of important organic intermediate of the exploitation eighties in 20th century, uses very extensive.It is mainly used in water quality stabilizer, selective herbicide, mollusc agrochemical, be to produce high-effective disinfecting sterilizing and algae-removing agent---the main raw material of Surchlor GR 60 (potassium) and trichloroisocyanuric acid, can be used as in addition the aspects such as additive of nylon, fire-retardant for plastic and makeup.
At present, the industrial process of cyanuric acid has solid phase method and liquid phase method.Solid phase method refers to solid urea in industry kiln, stove or direct heating to 200 ℃～290 ℃ of melting pyrolysis in the reaction unit of agitator, form cyanuric acid crude product (contain cyanuric acid approximately 60%～70%), then obtain content and be about 98% product after fragmentation, pickling, separation and drying.Solvent method refers to urea is suspended in the high boiling solvents such as tetramethylene sulfone, dimethyl sulfoxide (DMSO), o-isopropyl phenol, after heated polymerizable, sloughs solvent in reactor, and then washing, obtain high purity product after drying.
According to the literature (Zhou Xinlong. the synthesis technique of cyanuric acid and applied research thereof. Institutes Of Technology Of Nanjing, 2006.), liquid phase method can cause environmental pollution, and brings the problems such as solvent recuperation and product color be not good, so the feasibility of suitability for industrialized production is lower.Although also there are problems in solid phase method, mostly can solve by concrete approach, therefore have larger development space.Solid phase method is divided into again scorification, returning charge method, fused salt pyrolysis method, molten metal pyrolysis method and other method.Scorification easily adheres to, raw material availability is low, reaction purity is not high and can only batch production; Although the returning charge method has been improved the sticking wall problem in producing, can realize serialization production, improve labour intensity, but structure of reactor is very complicated; Fused salt pyrolysis method production operation condition is more easy to control, be suitable for intermittently and serialization production, but technical process is complicated, energy consumption is excessive, conversion rate of urea is low, and equipment corrosion is serious; Molten metal pyrolysis method cost is low, and technique is simple, easy control of reaction system, but yield is very low.
Summary of the invention
But the object of the present invention is to provide the preparation method of a kind of energy-saving and emission-reduction, low-cost high-efficiency quantity-produced cyanuric acid.
Realize that the technical scheme that above-mentioned purpose of the present invention adopts is: urea is immersed in for some time in the mineral acid composite solution for preparing in advance, after question response is complete, urea is hung out with filter bag, join in the reactor with thermal oil circulating-heating mode, be rapidly heated, make it namely get the cyanuric acid crude product at described reaction kettle for reaction 0.5～1h, boil, namely get the cyanuric acid product after washing, centrifugal, drying finally by acid.
The concrete implementation step of the present invention is as follows:
1. the preparation of mineral acid composite solution: two or more mineral acid is added water, and to be mixed with concentration be 5%～10% mineral acid composite solution;
2. cyanuric acid crude product preparation: urea is immersed in 3～8h in the mineral acid composite solution, hang out with filter bag, join in the reactor with thermal oil circulating-heating mode, be warming up to～260 ℃, make it after described reaction kettle for reaction 0.5～1h, namely get the cyanuric acid crude product;
3. refining: pouring the cyanuric acid crude product into concentration is after in 5%～8% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely gets the cyanuric acid product after drying.
Its additional technical feature is:
Be fixed with whipping appts in described reactor.
Cyanuric acid preparation method provided by the present invention compared with prior art has the following advantages:
1. the material state in production process is less demanding, generally gets final product;
2. install simple to operationly, technical process is simple;
3. owing to having adopted the thermal oil circulating-heating, make the interior urea of reactor be heated evenly, reduced energy consumption, (reaction times is 0.5～1h) to have accelerated its speed of response;
4. because urea soaks through the mineral acid composite solution before dropping into reactor, and fixedly whipping appts has been installed in reactor, solved wall sticking phenomenon, accelerated heat transfer rate, prepared cyanuric acid crude product (content is more than 90%), and need not to pulverize, raw material availability greatly improved, reduce the labor force, can realize serialization production;
5. because the prepared cyanuric acid content in crude product of this method is higher, therefore, in follow-up treating process, pickling mineral acid (being generally dilution heat of sulfuric acid) concentration used 20%～25% is down to 5%～8% by what conventional solid-state method used, also washing times is reduced to 2～3 times simultaneously, has also improved production efficiency when having saved cost;
6. product color and luster after centrifugal, drying is good, and content reaches 99.9%.
In the present invention, described percentage is mass percent.
Embodiment
Embodiment one
1. two or more mineral acid being added water, to be mixed with concentration be 5% mineral acid composite solution;
2. urea is immersed in 8h in the mineral acid composite solution, hangs out with filter bag, join in the thermal oil circulating-heating reactor with whipping appts, be rapidly heated to～260 ℃, make it after described reaction kettle for reaction 0.5h, obtain the cyanuric acid crude product;
3. the cyanuric acid crude product is poured into concentration and be after in 5% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely get content after drying and be 99.9% cyanuric acid product.
Embodiment two
1. two or more mineral acid being added water, to be mixed with concentration be 5% mineral acid composite solution;
2. urea is immersed in 5h in the mineral acid composite solution, hangs out with filter bag, join in the thermal oil circulating-heating reactor with whipping appts, be rapidly heated to～260 ℃, make it after described reaction kettle for reaction 0.8h, obtain the cyanuric acid crude product;
3. the cyanuric acid crude product is poured into concentration and be after in 5% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely get content after drying and be 99.9% cyanuric acid product.
Embodiment three
1. two or more mineral acid being added water, to be mixed with concentration be 5% mineral acid composite solution;
2. urea is immersed in 3h in the mineral acid composite solution, hangs out with filter bag, join in the thermal oil circulating-heating reactor with whipping appts, be rapidly heated to～260 ℃, make it after described reaction kettle for reaction 1h, obtain the cyanuric acid crude product;
3. the cyanuric acid crude product is poured into concentration and be after in 5% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely get content after drying and be 99.9% cyanuric acid product.
Embodiment four
1. two or more mineral acid being added water, to be mixed with concentration be 8% mineral acid composite solution;
2. urea is immersed in 5h in the mineral acid composite solution, hangs out with filter bag, join in the thermal oil circulating-heating reactor with whipping appts, be rapidly heated to～260 ℃, make it after described reaction kettle for reaction 0.5h, obtain the cyanuric acid crude product;
3. the cyanuric acid crude product is poured into concentration and be after in 8% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely get content after drying and be 99.9% cyanuric acid product.
Embodiment five
1. two or more mineral acid being added water, to be mixed with concentration be 10% mineral acid composite solution;
2. urea is immersed in 3h in the mineral acid composite solution, hangs out with filter bag, join in the thermal oil circulating-heating reactor with whipping appts, be rapidly heated to～260 ℃, make it after described reaction kettle for reaction 1h, obtain the cyanuric acid crude product;
3. the cyanuric acid crude product is poured into concentration and be after in 8% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely get content after drying and be 99.9% cyanuric acid product.
Claims (5)
1. the preparation method of a cyanuric acid is characterized in that following steps:
1) preparation of mineral acid composite solution: the mineral acid more than three kinds or three kinds is added water, and to be mixed with concentration be 5%～10% mineral acid composite solution;
2) cyanuric acid crude product preparation: urea is immersed in 3～8h in the mineral acid composite solution, hang out with filter bag, join in the reactor with thermal oil circulating-heating mode, be warming up to～260 ℃, make it after described reaction kettle for reaction 0.5～1h, namely get the cyanuric acid crude product;
3) refining: pouring the cyanuric acid crude product into concentration is after in 5%～8% dilution heat of sulfuric acid, 1h is boiled in acid, centrifugal through washing 2～3 times, namely gets the cyanuric acid product after drying.
2. according to claim 1 preparation method, is characterized in that step 2) described in reactor in be fixed with whipping appts.
3. according to claim 1 preparation method, is characterized in that step 2) described in the cyanuric acid content in crude product reach more than 90%.
4. according to claim 1 preparation method, is characterized in that step 3) described in the cyanuric acid crude product need not to pulverize and be fines.
5. according to claim 1 preparation method, is characterized in that step 3) described in the cyanuric acid product content reach 99.9%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100626970A CN103102318A (en) | 2013-02-28 | 2013-02-28 | Preparation method of cyanuric acid |
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| CN2013100626970A CN103102318A (en) | 2013-02-28 | 2013-02-28 | Preparation method of cyanuric acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910088A (en) * | 2015-05-12 | 2015-09-16 | 山东兴达化工有限公司 | Research and application of energy saving, emission reduction and energy system optimization technology for producing cyanuric acid from urea |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4109089A (en) * | 1976-09-23 | 1978-08-22 | Stamicarbon, B.V. | Method of preparing cyanuric acid |
| CN1121513A (en) * | 1995-04-11 | 1996-05-01 | 中国科学院福建物质结构研究所 | Cyanuric acid prepared by solvent induced pyrolysis method |
-
2013
- 2013-02-28 CN CN2013100626970A patent/CN103102318A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4109089A (en) * | 1976-09-23 | 1978-08-22 | Stamicarbon, B.V. | Method of preparing cyanuric acid |
| CN1121513A (en) * | 1995-04-11 | 1996-05-01 | 中国科学院福建物质结构研究所 | Cyanuric acid prepared by solvent induced pyrolysis method |
Non-Patent Citations (2)
| Title |
|---|
| 周心龙: "《中国硕士学位论文》", 15 January 2007, 工程科技 * |
| 张伟伟，等: "以邻硝基甲苯为溶剂合成氰尿酸", 《广州化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910088A (en) * | 2015-05-12 | 2015-09-16 | 山东兴达化工有限公司 | Research and application of energy saving, emission reduction and energy system optimization technology for producing cyanuric acid from urea |
| 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 |
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