CN103732582A - Method for preparing melamine cyanurate - Google Patents
Method for preparing melamine cyanurate Download PDFInfo
- Publication number
- CN103732582A CN103732582A CN201280033642.0A CN201280033642A CN103732582A CN 103732582 A CN103732582 A CN 103732582A CN 201280033642 A CN201280033642 A CN 201280033642A CN 103732582 A CN103732582 A CN 103732582A
- Authority
- CN
- China
- Prior art keywords
- melamine cyanurate
- reaction zone
- temperature
- water
- reagent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C07D251/34—Cyanuric or isocyanuric esters
-
- 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
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
-
- 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
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/70—Other substituted melamines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention relates to organic chemistry, specifically to an improved method for preparing melamine cyanurate, which is used in various compositions as a fire retardant. When reacting cyanuric acid and melamine in a molar ratio in the presence of 2-30% water based on the mass of dry reagents at a temperature of from 10 to 100 DEG C in air counterflows at 2-10 kp/cm2, melamine cyanurate with a high percentage yield of end product is produced and with a reduced consumption of energy. A further advantage of the proposed method consists in the possibility of implementing said method in the continuous mode.
Description
Invention field
The present invention relates to organic chemistry, particularly prepare improving one's methods of melamine cyanurate, melamine cyanurate is used for multiple combination thing as fire retardant.
Background of invention
In known aqueous medium (with respect to the 20-2000wt% of mixture total weight amount) in circular double leaf agitator, by make trimeric cyanamide (M) with cyanuric acid (CA) with the component ratio of 1:9 to 9:1 (wt), react at 0-250 ℃ the method (being published in the patent JP54055587 on May 2nd, 1979) of preparing melamine cyanurate for 5 minutes to 5 hours.The disadvantage of the method is to reclaim end product difficulty, needs to filter, is dried, grinds melamine cyanurate.
Knownly be included in the situation that does not have aqueous medium, in the method for preparing melamine cyanurate (being published in the patent US5493023 on February 20th, 1996) of the dry powder mixture of 250-500 ℃ of heating M and CA.The ratio of M and CA be 1:0.5 to 1:20 (mole), be preferably 1:0.9 to 1:1.1.The method preferably should for example, at rare gas element medium (N
2) in carry out.Component is in advance in mixed at room temperature.The method is in fact by making component react and carry out under molten state.Because the difference of M and CA sublimation temperature, the method is accompanied by reagent loss.In addition, need expensive equipment (autoclave), and the method is accompanied by high-energy cost, and needs long-time (several hours) maintain high temperature.
The method approaching the most with the present invention comprise with M:CA=1:1 (mole) ratio trimeric cyanamide is reacted with cyanuric acid, then mixture (water-content is 50-500wt%) is heated, is vacuumized.For promoting to mix, use through efflorescence the initial component (being published in the patent JP55147266 on November 17th, 1980) to particle dia≤100 μ m.
By the then dry recovery of carrying out end product of decompression water distillation.The disadvantage of the method is that the heterogeneous character of the method needs high-energy cost, and need to be by initial product efflorescence and decompression.Desciccate, except cost of energy (warm air conveying), is also accompanied by end product and is ejected into the height loss in atmosphere, causes thus environmental pollution and needs to install heavy and expensive waste disposal facilities.
Summary of the invention
The problem that technical scheme of the present invention solves is to propose a kind of method that obtains high yield end product, without high water and cost of energy, can implement continuously.
Described problem is by providing a kind of method of preparing melamine cyanurate to be resolved, described method comprises the mixture of the water that comprises trimeric cyanamide that mol ratio is 1:1 and cyanuric acid and be 2-30% based on dry reagent quality meter content, at pressure, is 2-10kp/cm
2air inversion in, the temperature of 10-100 ℃, be delivered to reaction zone.
If do not meet the condition of implementing the inventive method, the quality of end product and yield reduce, and cost of energy raises.
As adopting the result of technical scheme of the present invention, can obtain the end product yield of high per-cent, by the amount of institute's water in reduction method, reduce cost of energy, do not use dry, grind, screening step.The further benefit of the method is that it can carry out with continuous mode.
By implementing the method with continuous mode, in order to prepare the product of multiple dispersity and in order to stop its adhesion and coalescent, further to add the static inhibitor of the leakage semi-period with static charge≤10 to the original mixture of reagent.As static inhibitor, can use with the form of 2-5% solution or emulsion and use tensio-active agent, the alcohol (for example methyl alcohol or ethanol) of the amount that accounts for water yield 0.1-5% is introduced when material is treated, or used their mixture.In addition installation period agitator on some devices and strainer.
Embodiment
By following examples, essence of the present invention is described.
embodiment 1
To be comprised of 1.9 trimeric cyanamides, 1.93 cyanuric acids (the two mol ratio is 1:1) and 0.97 water (dry reagent quality 25%) reaction mixture of (unit is kg), be 2atm (kp/cm at pressure
2) air inversion in, the temperature of 100 ℃ and be 150nm
3the volumetric velocity of/h, with 40 seconds, to be delivered to volume be 80cm
3reaction zone.
In the outlet of reaction zone, the amount that makes melamine cyanurate is 3.84kg, and its matrix content is approximately 96%, and humidity is 0.3%, and granularity is 75-130 μ m.Reagent is～0.001 second in the residence time of reaction zone.
embodiment 2
To be formed by 2.5 trimeric cyanamides, 2.6 cyanuric acids and 0.8 water (dry reagent quality 16%) reaction mixture of (unit is kg), in pressure is the air inversion of 6atm (kp/cm2), the temperature of 55 ℃ and be 225nm
3the volumetric velocity of/h, with 45 seconds, to be delivered to volume be 80cm
3reaction zone.
In the outlet of reaction zone, the amount that makes melamine cyanurate is 5.12kg, and its matrix content is approximately 95%, and humidity is 0.4%, and granularity is 50-100 μ m.Reagent is～0.0005 second in the residence time of reaction zone.
embodiment 3
To be formed by 1.26 trimeric cyanamides, 1.3 cyanuric acids and 0.05 water (dry reagent quality 2%) reaction mixture of (unit is kg), as embodiment 1 and 2, at 10atm (kp/cm
2) pressure, 10 ℃ temperature and be 300nm
3the volumetric velocity of/h, with 20 seconds, to be delivered to volume be 80cm
3reaction zone.
In the outlet of reaction zone, the amount that makes melamine cyanurate is 2.57kg, and its matrix content is approximately 95%, and humidity is 0.45%, and granularity is 20-50 μ m.Reagent is～0.0005 second in the residence time of reaction zone.
embodiment 4
The reaction mixture that will be comprised of 1.9kg trimeric cyanamide, 1.93kg cyanuric acid and 1.16kg water (dry reagent quality 30%) is 2atm (kp/cm at pressure
2) air inversion in, the temperature of 100 ℃ and be 150nm
3the volumetric velocity of/h, with 40 seconds, to be delivered to volume be 80cm
3reaction zone.
In the outlet of reaction zone, the amount that makes melamine cyanurate is 3.81kg, and its matrix content is approximately 95%, and humidity is 0.5%.Granularity is 75-130 μ m.Reagent is～0.001 second in the residence time of reaction zone.
embodiment 5
Trimeric cyanamide take certain mol proportion and cyanuric acid and amount are delivered to temperature as the mixing tank of 20 ℃ continuously for 5% water of dry reagent quality, then at pressure are～air inversion of 10atm neutralizes and is 200nm
3it is 80cm that the volumetric velocity of/h is delivered to volume
3reaction zone.
In the outlet of reaction zone, product, through dust moisture separation system, arrives collector, with sack or bag, is packing.With a certain amount of melamine cyanurate that makes, its matrix content is approximately 95%, and humidity is 0.45%, and granularity is 20-50 μ m.
Claims (1)
1. prepare the method for melamine cyanurate for one kind, the method comprises that making mol ratio is cyanuric acid and the trimeric cyanamide reaction under water exists of 1:1, being characterised in that, is 2-30% based on dry reagent quality meter water-content, by the mixture of reagent the temperature of 10-100 ℃, at 2-10kp/cm
2air inversion in introduce reaction zone.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU2011128117 | 2011-07-07 | ||
| RU2011128117/04A RU2471788C1 (en) | 2011-07-07 | 2011-07-07 | Method of producing melamine cyanurate |
| PCT/RU2012/000525 WO2013006092A1 (en) | 2011-07-07 | 2012-07-02 | Method for preparing melamine cyanurate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103732582A true CN103732582A (en) | 2014-04-16 |
Family
ID=47437275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280033642.0A Pending CN103732582A (en) | 2011-07-07 | 2012-07-02 | Method for preparing melamine cyanurate |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN103732582A (en) |
| RU (1) | RU2471788C1 (en) |
| WO (1) | WO2013006092A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2758252C1 (en) * | 2021-03-15 | 2021-10-27 | Федеральное государственное автономное образовательное учреждение высшего образования «Национальный исследовательский Томский государственный университет» | Method for obtaining melamine cyanurate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601542A1 (en) * | 1992-12-09 | 1994-06-15 | MITSUI TOATSU CHEMICALS, Inc. | Granular melamine cyanurate and preparation process thereof |
| JPH07149739A (en) * | 1993-11-26 | 1995-06-13 | Nissan Chem Ind Ltd | Melamine cyanurate granule and its production |
| CN1364858A (en) * | 2002-02-07 | 2002-08-21 | 合肥精汇化工研究所 | Process for preparing flame-retarding lubricant MCA |
| CN101774974A (en) * | 2005-03-07 | 2010-07-14 | 溴化合物有限公司 | A process for the preparation of melamine cyanurate |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1712320A1 (en) * | 1989-12-04 | 1992-02-15 | Дзержинский филиал Государственного научно-исследовательского и проектного института азотной промышленности и продуктов органического синтеза | Method for utilization of s-triazine aminooxo-derivatives |
| JPH11292861A (en) * | 1998-04-09 | 1999-10-26 | Mitsubishi Chemical Corp | Melamine cyanurate and its production |
| NL1014232C2 (en) * | 2000-01-31 | 2001-08-01 | Dsm Nv | Salt of a melamine condensation product and a phosphorus-containing acid. |
| ATE551331T1 (en) * | 2004-10-15 | 2012-04-15 | Basf Se | METHOD FOR PRODUCING MELAMINE CYANURATE IN CRYSTALLINE FORM |
| RU2292341C1 (en) * | 2005-05-05 | 2007-01-27 | Институт синтетических полимерных материалов (ИСПМ) им. Н.С. Ениколопова РАН | Method for preparing melamine adduct with acid |
-
2011
- 2011-07-07 RU RU2011128117/04A patent/RU2471788C1/en active
-
2012
- 2012-07-02 CN CN201280033642.0A patent/CN103732582A/en active Pending
- 2012-07-02 WO PCT/RU2012/000525 patent/WO2013006092A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601542A1 (en) * | 1992-12-09 | 1994-06-15 | MITSUI TOATSU CHEMICALS, Inc. | Granular melamine cyanurate and preparation process thereof |
| JPH07149739A (en) * | 1993-11-26 | 1995-06-13 | Nissan Chem Ind Ltd | Melamine cyanurate granule and its production |
| CN1364858A (en) * | 2002-02-07 | 2002-08-21 | 合肥精汇化工研究所 | Process for preparing flame-retarding lubricant MCA |
| CN101774974A (en) * | 2005-03-07 | 2010-07-14 | 溴化合物有限公司 | A process for the preparation of melamine cyanurate |
Non-Patent Citations (1)
| Title |
|---|
| 董妍妍，等: "阻燃剂三聚氰胺氰尿酸盐的生产与应用研究进展", 《化工进展》, vol. 30, 1 January 2011 (2011-01-01), pages 298 - 301 * |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2013006092A1 (en) | 2013-01-10 |
| RU2471788C1 (en) | 2013-01-10 |
| WO2013006092A8 (en) | 2014-02-13 |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140416 |