CN1253443C - Prepn of high-purity melamine cyanuric acid - Google Patents
Prepn of high-purity melamine cyanuric acid Download PDFInfo
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- CN1253443C CN1253443C CN 02128011 CN02128011A CN1253443C CN 1253443 C CN1253443 C CN 1253443C CN 02128011 CN02128011 CN 02128011 CN 02128011 A CN02128011 A CN 02128011A CN 1253443 C CN1253443 C CN 1253443C
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- cyanuric acid
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- trimeric cyanamide
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- ammonia
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Abstract
The present invention provides a preparation method of melamine cyanuric acid. The method uses melamine and cyanuric acid as raw materials and uses ammonia water solution with the concentration of 2 to 14% as solvent to react under the conditions that the temperature is from 100 to 200 DEG C and the pressure is from 0.05-1.5MPa to prepare the melamine cyanuric acid product with 5 to 55 mum of grain size and 99.9 % or more than 99.9 % of purity.
Description
The present invention relates to a kind of production method of high-purity melamine cyanuric acid.
(english abbreviation: MCA) be a kind of nylon combustion inhibitor special, it has characteristics nontoxic, efficient, environmental protection to melamine cyanurate.In recent years, MCA also is used as the fire retardant of urethane, PS, PE, PET, PBT and organosilicon etc.; Also can be used as the rubber lubricant, in rubber, add this product and can disperse filler fast, reduce sizing material and give birth to heat.Water as solvent is generally adopted in the production of existing melamine cyanurate, and trimeric cyanamide and cyanuric acid are made raw material, and reaction generates under normal pressure.This method technological process of production is long, must carry out powder particle diameter after the melamine cyanurate drying of generation and just can reach below the 55um; The melamine cyanurate product purity that generates is low, and flame retardant properties is poor, is to improve flame retardant rating, has only its addition of raising, has so not only increased cost but also has influenced the mechanical property of flame retardant products.For this reason, US5493023 has announced a kind of under 300-380 ℃ of temperature condition, the employing particle diameter is that trimeric cyanamide and the cyanuric acid thorough mixing of 100um reacted 2-4 hour, generate purity and be the production method of 99.9% MCA, this method long reaction time, the temperature height, the energy consumption height, the reactor product yield only has 90%.
The object of the present invention is to provide a kind of melamine cyanurate production method, overcome many shortcomings of above background technology, improve the product quality of melamine cyanurate, production cost has fallen at the end.
Unreacted cyanuric acid, trimeric cyanamide and other impurity can influence the purity of the product of melamine cyanurate, the present invention has adopted the solution that can dissolve unreacted cyanuric acid, trimeric cyanamide and other impurity to make reaction medium, the method of reaction mother liquor recycle applications after centrifugation, solved the problem that remains cyanuric acid, trimeric cyanamide and other impurity in the melamine cyanurate preferably, improve the product quality of melamine cyanurate, its yield is up to 99% simultaneously.
Production method of the present invention is as follows:
A. trimeric cyanamide and cyanuric acid are in the ratio metering of 1: 1.10~1.15 (mol ratios), 2~14% ammonia soln is pressed 5~10 times of meterings of trimeric cyanamide and cyanuric acid total amount (weight), or taking by weighing 5~10 times water of trimeric cyanamide and cyanuric acid total amount (weight) and Xiang Shuizhong, to feed ammonia to the concentration of ammonia be 2~14% standby.
B. above-mentioned material being added in the reactor, stir, is 100-200 ℃ in temperature, and pressure is between 0.05-1.5Mpa, and constant temperature, constant voltage are reacted 30-45min.
C. above-mentioned reacted material is sent in the airtight separator and separated, the filter cake after the separation is sent in the moisture eliminator dry, and obtaining particle diameter is 5-55um, the product of purity 〉=99.9%; Mother liquor is returned circulating reaction in the reactor, accumulates when a certain amount of when impurity, can be recycled again after filtration is separated out in cooling.
Preferably, the concentration of ammonia soln is 13-14%, and temperature of reaction is at 120-150 ℃, and reaction pressure is 0.2-1.0Mpa.
The present invention has been owing to adopted ammonia soln to make solvent, solved in the melamine cyanurate unreacted about 0.3% remaining tricyanic acid and cyanuric acid well, through the remaining trimeric cyanamide of stratographic analysis and tricyanic acid all below 0.02%.Simultaneously, the reaction times shortens to 30-45min by generally speaking 2-4 hour under the effect of ammonia soln.The melamine cyanurate particle diameter that generates need not pulverized and can use saving of work and time between 5-55um.Generate melamine cyanurate purity 〉=99.9%, improved product quality.
Embodiment one
The reactor that embodiment adopts is that volume is the steam heating reactor of 1.6Mpa for the 1m3 design pressure.
A. taking by weighing purity and be 98.5% cyanuric acid 90kg and purity and be 99.0% trimeric cyanamide 110.kg puts in the reactor;
B. the ammoniacal liquor that with 800kg concentration is 13-14% adds in the reactor, starts agitator, opens steam valve heat temperature raising to 180 ℃.At this moment, the pressure in the reactor is about 1.2Mpa.Constant temperature, constant voltage are reacted half an hour;
C. reaction slurry is delivered to and carried out the feed liquid separation in the airtight separator, reaction mother liquor is delivered in the reactor standby, and filter cake send the moisture eliminator drying.Directly obtaining particle diameter after the drying is the melamine cyanurate product of 5-55um.
Melamine cyanurate product weight after drying is 180kg, and the yield of resultant of reaction is 99.0%.20 ℃ of saturated solution pH values are 5.2.Product is carried out stratographic analysis obtains a result as follows:
Melamine cyanurate 99.9%
Residue tricyanic acid 0.015%
Residue cyanuric acid 0.075%
The about 80ppm of other impurity
Water 0.02%
Embodiment two
Adopt the identical equipment of embodiment 1, the purity of trimeric cyanamide is 99.9%, and add-on is 90 kilograms.The purity of cyanuric acid is 97.5%, and add-on is 125kg.Temperature of reaction is controlled at 120 ℃, and pressure-controlling is under 0.3Mpa, and the reaction times is 40min.With slip through embodiment 1 identical step separate, drying obtains finished product melamine cyanurate 180.5kg.Reaction yield is 99.2%.Product cut size is between 5 ~ 55um.20 ℃ of saturated solution pH values are 5.8.Product is as follows through the stratographic analysis result:
Melamine cyanurate 99.9%
Residue tricyanic acid 0.033%
Residue cyanuric acid 0.035%
Other impurity 0.012%
Water 0.02%
Comparative Examples
The enforcement of Comparative Examples such as embodiment 1, wherein temperature of reaction is about 100 ℃, is reflected under the normal pressure and carries out, the reaction times is 3hr.The separation of slip is adopted the method identical with embodiment 1 with dry.Exsiccant finished product melamine cyanurate 181.0kg, product yield is 99.5%, particle diameter is 120um.Product is as follows through the stratographic analysis result:
Melamine cyanurate 98.7%
Residue tricyanic acid 0.56%
Residue cyanuric acid 0.65%
Other impurity 0.07%
Moisture content 0.02%
20 ℃ of saturated solution pH values 5.5
Claims (4)
1. the production method of a melamine cyanurate, carry out according to the following steps:
A. the ratio of trimeric cyanamide and cyanuric acid 1: 1.10 in molar ratio~1.15 metering, 2~14% ammonia soln is pressed 5~10 times of meterings of trimeric cyanamide and cyanuric acid gross weight, or taking by weighing 5~10 times water of trimeric cyanamide and cyanuric acid gross weight and Xiang Shuizhong, to feed ammonia to the concentration of ammonia be 2~14% standby;
B. above-mentioned material being added in the reactor, stir, is 100~200 ℃ in temperature, and pressure is between 0.05~1.5Mpa, and constant temperature, constant voltage are reacted 30~45min;
C. above-mentioned reacted material is sent in the airtight separator and separated, the filter cake after the separation is sent in the moisture eliminator dry, and obtaining particle diameter is 5~55um, the product of purity 〉=99.9%; Mother liquor is returned circulating reaction in the reactor, accumulates when a certain amount of when impurity, can be recycled again after filtration is separated out in cooling.
2. method according to claim 1, the concentration that it is characterized in that ammonia soln is 13~14%.
3. method according to claim 1 is characterized in that temperature of reaction is at 120~150 ℃.
4. method according to claim 1 is characterized in that reaction pressure is 0.2~1.0Mpa.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN 02128011 CN1253443C (en) | 2002-12-12 | 2002-12-12 | Prepn of high-purity melamine cyanuric acid |
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CN 02128011 CN1253443C (en) | 2002-12-12 | 2002-12-12 | Prepn of high-purity melamine cyanuric acid |
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CN1506356A CN1506356A (en) | 2004-06-23 |
CN1253443C true CN1253443C (en) | 2006-04-26 |
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CN 02128011 Expired - Fee Related CN1253443C (en) | 2002-12-12 | 2002-12-12 | Prepn of high-purity melamine cyanuric acid |
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Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1856064A4 (en) * | 2005-03-07 | 2010-08-04 | Bromine Compounds Ltd | A process for the preparation of melamine cyanurate |
CN102093300B (en) * | 2010-12-31 | 2012-08-08 | 普塞呋(清远)磷化学有限公司 | Preparation method of high-flowing property high-purity crystallization flaky melamine cyanurate |
CN102898389A (en) * | 2012-10-16 | 2013-01-30 | 郑州大学 | Method for recycling melamine waste residue |
CN102936365A (en) * | 2012-11-23 | 2013-02-20 | 杨荣 | Halogen-free flame-retardant modified plastic |
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 |
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