CN100361981C - Method and device for refining cyanuric acid under normal temperature - Google Patents
Method and device for refining cyanuric acid under normal temperature Download PDFInfo
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- CN100361981C CN100361981C CNB2006100075840A CN200610007584A CN100361981C CN 100361981 C CN100361981 C CN 100361981C CN B2006100075840 A CNB2006100075840 A CN B2006100075840A CN 200610007584 A CN200610007584 A CN 200610007584A CN 100361981 C CN100361981 C CN 100361981C
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Abstract
The present invention relates to a method and a device for refining cyanuric acid under normal temperature, which belongs to the technical field of chemical engineering. In the method for refining cyanuric acid, first of all, sulphuric acid or hydrochloric acid is arranged in a reaction vessel, crude cyanuric acid is added under a stirring condition, and then ultrasonic waves are exerted on the reactants in the reaction vessel for reacting for certain time. In the device for refining cyanuric acid, ultrasonic generators are arranged in the reaction vessel and uniformly distributed along the circumference of the inner wall of the reaction vessel, and the ultrasonic generators are driven by a power supply outside the reaction vessel. A stirring paddle is arranged at the bottom of the reaction vessel and driven by a motor outside the reaction vessel. A discharge valve is arranged at the bottom of the reaction vessel, and the ultrasonic generators can be also arranged on the outer wall of the bottom of the reaction vessel. The method and the device of the present invention have the advantages of shortening the time of refining cyanuric acid, reducing corrosion on equipment and prolonging the service life of the equipment. The present invention also has the advantages of simple whole production processes, safety, reliability, energy saving, high productive efficiency and favorable economic and social benefit.
Description
Technical field
The present invention relates to a kind of method and device thereof of refining cyanuric acid under normal temperature, belong to chemical technology field.
Background technology
From thanked in 1776 rein in invention by the urea synthesis cyanuric acid since, now developed into important fine-chemical intermediate.Cyanuric acid has triazine structure, reactions such as addition, replacement, condensation easily take place, being a kind of important chemical product, is that raw material has been developed nearly 500 kinds of cyanuric acid derived product with it, is widely used in chemical industry, light industry, machinery, electrical equipment, weaving, agricultural, field such as daily.China has more than 20 tame factories now, about 10.0 ten thousand tons of annual production.
At present, domestic main employing solid phase method is produced the acid of cyanogen urea, be about to urea (or adding catalyzer ammonium chloride) and become the acid of crude product cyanogen urea 250～300 ℃ of following condensation reactions, its cyanogen urea acid content is generally 60～80%, impurity is urea, biuret, the triuret that contracts, acyl ammonium etc., cyanogen urea acid product content requirement is more than 98%, and this just need make with extra care the acid of crude product cyanogen urea, to reach specification of quality.
Cyanogen urea acid treating technology mainly is to utilize sulfuric acid or hydrochloric acid that the acyl ammonium in the crude product is converted into cyanuric acid again, and other impurity is removed.
U.S. Pat 2768167 is pointed out, when producing trimeric cyanamide, the by product cyanuramide of producing is difficult to separate with cyanurodiamide and trimeric cyanamide, therefore just their mixture is focused on, in acidic aqueous solution, heat, when temperature reaches more than 165 ℃, just can obtain the transformation efficiency more than 90%, generate cyanuric acid.Used acid is sulfuric acid preferably, hydrochloric acid also can, but the use of hydrochloric acid will bring more serious equipment corrosion problem.The vitriolic consumption is: three substituting groups of trimeric cyanamide all are amino, and every mole of material needs 3/2 mol sulfuric acid; Cyanurodiamide contains two amino, and every mole of material needs 1 mol sulfuric acid; Cyanuramide contains an amino, and every mole of material needs 1/2 mol sulfuric acid.The concentration of free acid has directly been controlled speed of response, is 5%～20% o'clock at sulfuric acid concentration, and speed of response is relatively more suitable.Temperature of reaction is minimum also to be wanted more than 150 ℃, and the heating of this moment must guarantee pressure, otherwise moisture will volatilize; When temperature of reaction is lower than 165 ℃, it is slower that speed of response increases, when being higher than this temperature, speed of response speeds rapidly, when reaching 175 ℃～180 ℃, just very attractive from the technical scale consideration, best speed of response appears at 200 ℃, will bring increasing rapidly of cost but temperature is too high.
By product when also the direct pyrolysis of urea generates cyanuric acid just such as trimeric cyanamide, cyanuramide and cyanurodiamide, they have constituted crude product cyanuric acid purified raw material with the urea of complete reaction not, biuret etc.The crude product cyanuric acid is exactly common with the sulfuric acid digestion and the supporting process for purification of cyanuric acid is produced in the direct pyrolysis of solid phase method urea.
It all is periodical operation that reaction is boiled in acid, and representational reaction formula is:
C
3N
3NH
2(OH)
2+H
2O → (HCNO)
3+NH
3
C
3N
3(NH
2)
2OH+2H
2O→(HCNO)
3+2NH
3
C
3N
3(NH
2)
3+3H
2O → (HCNO)
3+3NH
3
2NH
3+H
2SO
4→ (NH
4)
2SO
4
Be heated under the certain temperature condition, acid amides is converted into cyanuric acid, ammonia that produces and sulfuric acid reaction generate ammonium sulfate, broken the balance of conversion reaction, conversion reaction is carried out towards positive dirction, and under the situation of sulfuric acid q.s, conversion reaction is carried out fully, acid amides all becomes cyanuric acid, reaches refining effect.
It all is to carry out under normal pressure that reaction is boiled in acid the earliest, and under certain acid concentration, maximum heating temperature can only reach 105 ℃, and temperature is high again, and moisture will evaporate in a large number, so the reaction times is all long, all want 3～4hr generally speaking.European patent EP A0124710 has carried out high-temperature acid and has boiled experiment, and when Heating temperature reached 160 ℃, reaction needed was carried out 90min; When Heating temperature reached 170 ℃, reaction needed was carried out 40min; When Heating temperature reached 180 ℃, reaction needed was carried out 20min; When Heating temperature reached 200 ℃, reaction needed was carried out 5～8min.And along with Heating temperature raises, the working pressure of system also progressively increases.
The process for refining that extensively adopts is at present: crude cyanuric acid is pulverized (about 60 orders), place enamel still and sulfuric acid to be made into 20%～30% slurry, refining 4～8hr under the condition of boiling is after the refined liquid cooling, after filtration, can get purity after the washing, drying greater than 98% cyanuric acid.
Above-mentioned technology can be divided into normal pressure and high-pressure process.The high-pressure process reaction times is short, is easy to realize serialization production, but because its temperature of reaction is higher, and equipment material is difficult to satisfy that corrosion requires or investment is bigger, and domestic do not have industrial applications as yet; Normal pressure technology is the domestic technology that generally adopts, its subject matter is that temperature is higher, about 105 ℃, make equipment corrosion serious, even enamel reaction still, also have only work-ing life about 1 year, and long reaction time, the acid of cyanogen urea is easily decomposed, and product yield is reduced, therefore production efficiency of equipment is low, and energy consumption is higher.
Summary of the invention
The objective of the invention is to propose a kind of method and device thereof of refining cyanuric acid under normal temperature, ultrasonic wave is used for the acid treating of cyanogen urea, to shorten the reaction times, to reduce temperature of reaction, reach that production process is simple, safety, efficient, purpose of energy saving.
The method of the refining cyanuric acid under normal temperature that the present invention proposes comprises following each step:
(1) be that 15～25% sulfuric acid or concentration are that 4～10% hydrochloric acid places in the reactor with concentration, add the acid of crude product cyanogen urea under agitation condition, the weight ratio of adding is: the acid of crude product cyanogen urea: sulphuric acid soln or hydrochloric acid soln=and 1: 1.5～1: 2.5;
(2) reactant in the reactor is applied ultrasonic wave, ultrasonic frequency is 20～80KHz, the ultrasonic wave sound intensity 0.2～10W/cm
2, the reaction times is 30～120 minutes.
Crude product cyanogen urea acid in the aforesaid method, the content of its cyanogen urea acid is 60～95%.
The device of the refining cyanuric acid under normal temperature that the present invention proposes comprises reactor, ultrasonic generator, power supply, discharge valve, motor and stirring rake.Ultrasonic generator places in the reactor, and along the inwall circumference uniform distribution of reactor, ultrasonic generator is by the power drives of reactor outside.Stirring rake places the bottom of reactor, and stirring rake is by the electric motor driving of reactor outside.Discharge valve places the reactor bottom.
The another kind of structure of the device of the refining cyanuric acid under normal temperature that the present invention proposes comprises reactor, ultrasonic generator, power supply, discharge valve; Described ultrasonic generator places the reactor bottom outer wall, and uniform along the bottom of reactor, ultrasonic generator is by power drives; Described discharge valve places reactor bottom.
The method and the device thereof of the refining cyanuric acid under normal temperature that the present invention proposes, its advantage is to shorten the refining time of cyanogen urea acid, reacts at normal temperatures, can reduce the corrosion to equipment significantly, therefore can prolong equipment life greatly.And normal-temperature reaction do not need steam heating, but save energy.This device is applicable to the treating process of cyanogen urea acid, and whole process of production is simple, safe and reliable, save energy, production efficiency height, has good economic benefit and social benefit.
Description of drawings
Fig. 1 is the structural representation of the refining plant that proposes of the present invention.
Fig. 2 is the synoptic diagram of the another kind of structure of apparatus of the present invention.
Among Fig. 1 and Fig. 2, the 1st, reactor, the 2nd, ultrasonic generator, the 3rd, power supply, the 4th, discharge valve, the 5th, motor, the 6th, stirring rake, the 7th, reactor.
Embodiment
The method of the refining cyanuric acid under normal temperature that the present invention proposes, at first be that 15～25% sulfuric acid or concentration are that 4～10% hydrochloric acid places in the reactor with concentration, add the acid of crude product cyanogen urea under agitation condition, the weight ratio of adding is: the acid of crude product cyanogen urea: sulphuric acid soln or hydrochloric acid soln=and 1: 1.5～1: 2.5; Then the reactant in the reactor is applied ultrasonic wave, ultrasonic frequency is 20～80KHz, the ultrasonic wave sound intensity 0.2～10W/cm
2, the reaction times is 30～120 minutes.
Crude product cyanogen urea acid in the aforesaid method, the content of its cyanogen urea acid is 60～95%.
The device of the refining cyanuric acid under normal temperature that the present invention proposes, its structure comprises reactor 1, ultrasonic generator 2, power supply 3, discharge valve 4, motor 5 and stirring rake 6 as shown in Figure 1.Ultrasonic generator 2 places in the reactor 1, and along the inwall circumference uniform distribution of reactor, ultrasonic generator 2 is driven by the power supply 3 of reactor outside.Stirring rake 6 places the bottom of reactor 1, and stirring rake 6 is driven by the motor 5 of reactor outside.Discharge valve 4 places the bottom of reactor 1.
The another kind of structure of the device of the refining cyanuric acid under normal temperature that the present invention proposes as shown in Figure 2, comprises reactor 7, ultrasonic generator 2, power supply 3 and discharge valve 4.Ultrasonic generator 2 places the bottom outer wall of reactor 7, and is uniform along the bottom of reactor, and ultrasonic generator 2 is driven by power supply 3.Discharge valve 4 places the bottom of reactor 7.
The principle of work of the inventive method is: on the cyanogen urea acid treating process nature is the acid-base reaction process, and acid-base reaction can be finished under normal temperature, normal pressure fast, but normal pressure treating process speed is very slow, illustrates that its reaction process is mass transfer control.Ultrasonic wave is the sound wave of frequency greater than 20kHz, be used for cyanogen urea acid treating process its mainly to act on be mechanical effect and cavatition.Ultrasonic wave causes the alternate compression and the extension of medium particle in the medium communication process.Though vibration displacement, the velocity variations of particle are little, its acceleration quite big (10
4M/s
2).So big acceleration can increase the perviousness that acid solution enters crude product cyanogen urea granulates significantly, strengthens mass transfer process, thereby has strengthened reaction process.Yet the main reason of ultrasound-enhanced refining reaction is because the cavitation effect that ultrasonic wave produces.Ultrasonic cavitation is meant that the small complex in the solution is activated, and shows as a series of dynamic processes such as vibration, growth, contraction and even collapse of complex under acoustic wave action.According to different performances, cavitation can have stable cavitation and two kinds of forms of transient cavitation.Stable cavitation is created under the lower sound intensity effect, cavitation bubble vibrates several cycles in medium with nonlinear form, in oscillatory process, the miniflow around the cavitation bubble produces bigger tangential force to other particle in the solution, helps acid accumulator penetration to crude product cyanogen urea granulates inside.Low intensity ultrasound forms miniflow around not only can making crude product cyanogen urea granulates particle, also can make crude product cyanogen urea granulates produce intragranular circulation, thereby improve the particulate permeability.Ultrasonication need not also can strengthen mass transfer process by improving medium temperature, and this is the dominant mechanism of ultrasound-enhanced refining reaction.Transient cavitation occurs under the stronger sound intensity effect, and gas (vapour) bubble generates rapidly in the cycle, grows up, compresses, collapses at a sound wave.Studies show that can form up to the hot localised points more than the 5000K during transient cavitation collapse, pressure can reach hundreds of and even thousands of normal atmosphere.Along with highly compressed discharges, will in solution, form powerful shockwave (homogeneous phase) or high-speed jet (heterogeneous).In refining reaction, this powerful impingement flow can reduce effectively, eliminate the block layer between particle and the acid solution, thereby has strengthened rate of mass transfer.Simultaneously, impingement flow produces a kind of physics shearing force to crude product cyanogen urea granulates, makes it distortion, breaks, and discharge inclusion, and this has quickened reaction process greatly.
Below be the embodiment of the inventive method:
Embodiment 1
Selecting content for use is 65% crude product cyanogen urea acid, is that 20% sulfuric acid mixes with the acid of crude product cyanogen urea and concentration, and its ratio of components is 1: 2, is that 30KHz, the sound intensity are 0.5W/cm in ultrasonic frequency
2, temperature is under the situation of room temperature refining 40 minutes, filter, washing, dry back cyanogen urea acid product content be greater than 98%.
Embodiment 2
Selecting content for use is 75% crude product cyanogen urea acid, is that 25% sulfuric acid mixes with the acid of crude product cyanogen urea and concentration, and its ratio of components is 1: 1.7, is that 50KHz, the sound intensity are 2W/cm in ultrasonic frequency
2, temperature is under the situation of room temperature refining 30 minutes, filter, washing, dry back cyanogen urea acid product content be greater than 98%.
Embodiment 3
Selecting content for use is 85% crude product cyanogen urea acid, is that 5% hydrochloric acid mixes with the acid of crude product cyanogen urea and concentration, and its ratio of components is 1: 2, is that 80KHz, the sound intensity are 5W/cm in ultrasonic frequency
2, temperature is under the situation of room temperature refining 50 minutes, filter, washing, dry back cyanogen urea acid product content be greater than 98%.
Embodiment 4
Selecting content for use is 70% crude product cyanogen urea acid, is that 8% hydrochloric acid mixes with the acid of crude product cyanogen urea and concentration, and its ratio of components is 1: 2.3, is that 20KHz, the sound intensity are 0.2W/cm in ultrasonic frequency
2, temperature is under the situation of room temperature refining 70 minutes, filter, washing, dry back cyanogen urea acid product content be greater than 98%.
Claims (2)
1. the method for a refining cyanuric acid under normal temperature is characterized in that this method comprises following each step:
(1) be that 15～25% sulfuric acid or concentration are that 4～10% hydrochloric acid places in the reactor with concentration, under agitation condition, add the acid of crude product cyanogen urea, the weight ratio that adds is: the acid of crude product cyanogen urea: sulphuric acid soln or hydrochloric acid soln=and 1: 1.5～1: 2.5, in the acid of described crude product cyanogen urea, the content of cyanogen urea acid is 60～95%;
(2) reactant in the reactor is applied ultrasonic wave, ultrasonic frequency is 20～80KHz, the ultrasonic wave sound intensity 0.2～10W/cm
2, the reaction times is 30～120 minutes.
2. the device of a refining cyanuric acid under normal temperature is characterized in that this device comprises reactor, ultrasonic generator, power supply, discharge valve; Described ultrasonic generator places the reactor bottom outer wall, and uniform along the bottom of reactor, ultrasonic generator is by power drives; Described discharge valve places reactor bottom.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100075840A CN100361981C (en) | 2006-02-17 | 2006-02-17 | Method and device for refining cyanuric acid under normal temperature |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100075840A CN100361981C (en) | 2006-02-17 | 2006-02-17 | Method and device for refining cyanuric acid under normal temperature |
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| Publication Number | Publication Date |
|---|---|
| CN1807420A CN1807420A (en) | 2006-07-26 |
| CN100361981C true CN100361981C (en) | 2008-01-16 |
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| CN102321037A (en) * | 2011-06-02 | 2012-01-18 | 郑州大学 | Melamine ornithine aminotransferase (OAT) waste residue resource utilization method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2768167A (en) * | 1956-10-23 | Cyanuric acid preparation | ||
| US2943088A (en) * | 1959-06-22 | 1960-06-28 | Westfall Richard Howard | Production of cyanuric acid from urea |
| US3325493A (en) * | 1963-08-13 | 1967-06-13 | Showa Denko Kk | Process for producing cyanuric acid from melamine purification waste mother liquor |
| EP0124710A1 (en) * | 1983-05-09 | 1984-11-14 | Chemie Linz Aktiengesellschaft | Process for the preparation of pure cyanuric acid |
-
2006
- 2006-02-17 CN CNB2006100075840A patent/CN100361981C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2768167A (en) * | 1956-10-23 | Cyanuric acid preparation | ||
| US2943088A (en) * | 1959-06-22 | 1960-06-28 | Westfall Richard Howard | Production of cyanuric acid from urea |
| US3325493A (en) * | 1963-08-13 | 1967-06-13 | Showa Denko Kk | Process for producing cyanuric acid from melamine purification waste mother liquor |
| EP0124710A1 (en) * | 1983-05-09 | 1984-11-14 | Chemie Linz Aktiengesellschaft | Process for the preparation of pure cyanuric acid |
Non-Patent Citations (5)
| Title |
|---|
| 三聚氰酸的制备及其应用. 安徽省化工研究所有机合成研究室.安徽化工，第2期. 1976 * |
| 微波常压法制备三聚氰酸. 张竞清等.合成化学，第10卷. 2002 * |
| 由尿素合成三聚氰酸. 彭德厚.化学工程师，第3期. 1994 * |
| 超声波应用于有机合成的最新进展. 刘永等.广东化工，第2期. 2002 * |
| 超声辐射在有机合成中的应用. 曾爱群等.广西化工，第28卷第2期. 1999 * |
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Assignee: JIANGSU HUAER CHEMICAL CO., LTD. Assignor: Jiangsu Yabang Dyestuffs Co., Ltd. Contract record no.: 2012320000578 Denomination of invention: Method and device for refining cyanuric acid under normal temperature Granted publication date: 20080116 License type: Exclusive License Open date: 20060726 Record date: 20120504 |