JPS6152831B2 - - Google Patents
Info
- Publication number
- JPS6152831B2 JPS6152831B2 JP3240378A JP3240378A JPS6152831B2 JP S6152831 B2 JPS6152831 B2 JP S6152831B2 JP 3240378 A JP3240378 A JP 3240378A JP 3240378 A JP3240378 A JP 3240378A JP S6152831 B2 JPS6152831 B2 JP S6152831B2
- Authority
- JP
- Japan
- Prior art keywords
- melamine
- urea
- melamine cyanurate
- cyanuric acid
- heated
- 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.)
- Expired
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Description
【発明の詳細な説明】
本発明はメラミンシアヌレートを合成する新規
な方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel method for synthesizing melamine cyanurate.
メラミンシアヌレートはグリースのシツクナー
や難燃剤として需要が開拓され、その価値が高ま
りつつある化合物である。 Melamine cyanurate is a compound whose value is increasing, with demand developed as a grease thickener and flame retardant.
メラミンシアヌレートはメラミンとシアヌル酸
の１対１錯体であり、メラミンの水溶液とシアヌ
ル酸の水溶液を混合することにより定量的にメラ
ミンシアヌレートの沈殿を得ることができる。し
かしながらこの方法は、シアヌル酸とメラミンの
水に対する溶解度が小さい為に大量の水が必要で
あり、かつ原料として高価なシアヌル酸を用いる
ので、製品が高価になる欠点を有しており、工業
的製法としては好ましいものではない。 Melamine cyanurate is a one-to-one complex of melamine and cyanuric acid, and by mixing an aqueous solution of melamine and an aqueous solution of cyanuric acid, it is possible to quantitatively precipitate melamine cyanurate. However, this method requires a large amount of water due to the low solubility of cyanuric acid and melamine in water, and uses expensive cyanuric acid as a raw material, making the product expensive. This is not a preferable manufacturing method.
本発明者等は鋭意研究を続けた結果、尿素とメ
ラミンから直接メラミンシアヌレートを合成する
新規な方法を見い出し本発明に至つた。 As a result of intensive research, the present inventors discovered a new method for directly synthesizing melamine cyanurate from urea and melamine, leading to the present invention.
本発明は尿素とメラミンを混合して加熱、反応
させることによりメラミンシアヌレートを合成す
る方法である。 The present invention is a method for synthesizing melamine cyanurate by mixing urea and melamine, heating and reacting the mixture.
尿素を単独加熱すればシアヌル酸が生じること
は公知であるが尿素とメラミンの混合物を加熱し
て一挙にメラミンシアヌレートを得る方法は未だ
知られていない。 Although it is known that heating urea alone produces cyanuric acid, there is no known method to obtain melamine cyanurate all at once by heating a mixture of urea and melamine.
本発明の方法によればシアヌル酸を原料とする
ことなく尿素とメラミンから直接工業的にメラミ
ンシアヌレートを製造することができる。 According to the method of the present invention, melamine cyanurate can be industrially produced directly from urea and melamine without using cyanuric acid as a raw material.
本発明の方法に於て、尿素とメラミンはそれぞ
れ粉末のまま例えばロータリーキルンや撹拌器付
きの釜に供給し加熱してもよいし、また先す尿素
を加熱して溶解した後メラミン粉末を添加し均一
液状物にした後上記装置に供給、あるいは加熱し
てあるスチールベルトの一端に供給してもよい。 In the method of the present invention, urea and melamine may be supplied as powders to, for example, a rotary kiln or a pot equipped with a stirrer and heated, or urea may be heated and dissolved first, and then melamine powder may be added. It may be supplied to the above-mentioned apparatus after being made into a homogeneous liquid, or it may be supplied to one end of a heated steel belt.
尿素とメラミンの混合物は加熱に伴い、脱アン
モニアを起しながら自濁溶液→粘稠物→固化の状
態変化をするが、尿素を単独で加熱したときに生
ずる付着性の強固な塊りは生成しない。この付着
性の塊りを生成しないことがメラミンシアヌレー
トの製造を著しく容易なものとしている。 When a mixture of urea and melamine is heated, its state changes from a cloudy solution to a viscous substance to solidification while deammonizing, but the sticky solid lump that occurs when urea is heated alone does not form. do not. This absence of sticky lumps makes the production of melamine cyanurate significantly easier.
加熱温度は尿素の融点以上であればよいが、約
140℃ないし約350℃更に好ましくは約160℃ない
し約300℃の範囲で反応させるのがよい。140℃未
満では反応が必常に遅く、350゜をこえると生成
物のメラミンシアヌレートの急速な分解がおこ
る。加熱時間は約５ないし約12時間好ましくは約
10分ないし約２時間の範囲が用いられる。 The heating temperature should be above the melting point of urea, but about
The reaction is preferably carried out at a temperature ranging from 140°C to about 350°C, more preferably from about 160°C to about 300°C. Below 140°C the reaction is necessarily slow and above 350° rapid decomposition of the product melamine cyanurate occurs. The heating time is about 5 to about 12 hours, preferably about
A range of 10 minutes to about 2 hours is used.
原料の尿素とメラミンの割合は、メラミンの量
に対応するシアヌル酸を生成するのに十分な尿素
があればよい。メラミン１モルに対し尿素約３モ
ルないし約10モル好ましくは約４モルないし約６
モルの範囲が用いられる。この割合より尿素が少
ないとメラミンが未反応で残り、多いとシアヌル
酸が過剰に生成する。 The ratio of urea and melamine in the raw materials may be such that there is sufficient urea to produce cyanuric acid corresponding to the amount of melamine. About 3 moles to about 10 moles of urea per mole of melamine, preferably about 4 moles to about 6 moles.
Molar ranges are used. If urea is less than this ratio, melamine remains unreacted, and if it is higher than this ratio, cyanuric acid is produced in excess.
こうして加熱により得られた固体粉末は純度約
92％ないし約97％のメラミンシアヌレートであ
る。不純物はシアヌル酸、ビウレツトおよび尿素
が主であり、これらの不純物は水洗すれば除去で
きる。水洗に必要な水量は生成物に対し重量比で
約１ないし約200の範囲である。こうして精製し
たメラミンシアヌレートは99.5％以上の純度を持
つ。 The solid powder obtained by heating in this way has a purity of approximately
It is 92% to about 97% melamine cyanurate. The main impurities are cyanuric acid, biuret, and urea, and these impurities can be removed by washing with water. The amount of water required for washing ranges from about 1 to about 200 parts by weight of product. Melamine cyanurate purified in this way has a purity of over 99.5%.
本発明の方法によれば、尿素とメラミンから直
接メラミンシアヌレートが合成でき、従来法に比
べて極めて安価にメラミンシアヌレートを製造す
ることができる。またその工程中に、強固な付着
性の粘稠物を生じないので反応操作が容易であ
る。 According to the method of the present invention, melamine cyanurate can be directly synthesized from urea and melamine, and melamine cyanurate can be produced at a much lower cost than conventional methods. In addition, since no strongly adhesive viscous material is produced during the process, the reaction operation is easy.
次に本発明の方法を実施例によつて更に具体的
に説明する。 Next, the method of the present invention will be explained in more detail with reference to Examples.
実施例 １
500mlのガラス製セパラフルフラスコに粒状尿
素90ｇ（1.5モル）メラミン45ｇ（0.36モル）を
付込み、撹拌器で撹拌しながらヒーターで加熱し
た。140℃になると混合物は白濁溶液となり、200
℃までこの状態が続いた。200℃を越えると急速
に粘稠になるが、器壁に付着することはないし、
撹拌も可能である。加熱をさらに続けると固化し
粉末となつた。140℃から30分かゝつて徐々に温
度を上げ最終的に300℃まで加熱した。製品収量
は94ｇであり、メラミンシアヌレート97％、シア
ヌル酸1.5％、尿素0.2％、その他、1.3％であつ
た。この全量を100℃の水100mlに投入し熱時ろ過
したところ不溶分は91.5ｇであり、そのメラミン
シアヌレートの純度は99.5％であつた。Example 1 90 g (1.5 mol) of granular urea and 45 g (0.36 mol) of melamine were added to a 500 ml glass Separate flask, and heated with a heater while stirring with a stirrer. At 140°C, the mixture becomes a cloudy solution and 200°C
This situation continued until the temperature reached ℃. When the temperature exceeds 200℃, it quickly becomes viscous, but it does not stick to the vessel wall.
Stirring is also possible. When heating was continued, it solidified into a powder. The temperature was gradually increased from 140°C over 30 minutes and finally heated to 300°C. The product yield was 94g, containing 97% melamine cyanurate, 1.5% cyanuric acid, 0.2% urea, and 1.3% others. When this whole amount was poured into 100 ml of water at 100°C and filtered while hot, the insoluble matter was 91.5 g, and the purity of the melamine cyanurate was 99.5%.
実施例 ２
500mlのガラス製セパラブルフラスコに粒状尿
素90ｇを仕込み、ヒーターで加熱し、140℃に保
ち溶融状態にした。撹拌をしながらメラミン45ｇ
を加えた。その後の加熱の実施例１と同様に行な
い、製品98ｇを得た。メラミンシアヌレート93
％、シアヌル酸3.7％、ビウレツト0.7％、その他
0.2％であつた。実施例１と同様に熱ろ過したと
ころ不溶分は91ｇであり、これは純度99.7％のメ
ラミンシアヌレートであつた。Example 2 90 g of granular urea was placed in a 500 ml glass separable flask, heated with a heater, and kept at 140° C. to a molten state. Melamine 45g while stirring
added. Subsequent heating was carried out in the same manner as in Example 1 to obtain 98 g of product. Melamine cyanurate 93
%, cyanuric acid 3.7%, biuret 0.7%, others
It was 0.2%. When it was hot-filtered in the same manner as in Example 1, the amount of insoluble matter was 91 g, which was melamine cyanurate with a purity of 99.7%.
実施例 ３
容積３のステンレス製フラスコに粒状尿素
1.4Kgを仕込み、ヒーターで加熱して溶解させ
た。これを、250℃に加熱した内容積６のニー
ダーの槽に全量注いだ。続いて撹拌しながらメラ
ミン690ｇを加えた。１時間加熱撹拌したところ
反応物は完全に粉末となつていた。収量は1490ｇ
であつた。この全量を100℃の水1.5に投入し、
熱ろ過したところ、不溶分は1400ｇであり、その
メラミンシアヌレートの純度は99.1％であつた。Example 3 Granular urea in a stainless steel flask with a volume of 3
1.4 kg was charged and heated with a heater to dissolve it. The entire amount was poured into a kneader tank having an internal volume of 6 and heated to 250°C. Subsequently, 690 g of melamine was added while stirring. After heating and stirring for 1 hour, the reaction product had completely become a powder. Yield is 1490g
It was hot. Pour this entire amount into 1.5 liters of water at 100℃,
When filtered under heat, the amount of insoluble matter was 1400 g, and the purity of the melamine cyanurate was 99.1%.
Claims (1)
ヌレートを製造することを特徴とするメラミンシ
アヌレートの製造方法。 ２ メラミンに対する尿素のモル比が３ないし10
である特許請求の範囲第１項記載の方法。 ３ 加熱温度が140℃ないし350℃の範囲である特
許請求の範囲第１項記載の方法。[Claims] 1. A method for producing melamine cyanurate, which comprises producing melamine cyanurate by mixing and heating urea and melamine. 2 Molar ratio of urea to melamine is 3 to 10
The method according to claim 1. 3. The method according to claim 1, wherein the heating temperature is in the range of 140°C to 350°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3240378A JPS54125690A (en) | 1978-03-23 | 1978-03-23 | Preparation of melamine cyanurate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3240378A JPS54125690A (en) | 1978-03-23 | 1978-03-23 | Preparation of melamine cyanurate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS54125690A JPS54125690A (en) | 1979-09-29 |
| JPS6152831B2 true JPS6152831B2 (en) | 1986-11-14 |
Family
ID=12357981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3240378A Granted JPS54125690A (en) | 1978-03-23 | 1978-03-23 | Preparation of melamine cyanurate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS54125690A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5493023A (en) * | 1992-12-09 | 1996-02-20 | Mitsui Toatsu Chemicals, Inc. | Granular melamine cyanurate and preparation process thereof |
| JP3988895B2 (en) * | 1996-03-22 | 2007-10-10 | 協同油脂株式会社 | Grease composition for constant velocity joints |
| CN101899354B (en) * | 2010-07-29 | 2012-12-05 | 济南泰星精细化工有限公司 | Method for producing high-purity flame-resistant lubricant by improved powder method |
-
1978
- 1978-03-23 JP JP3240378A patent/JPS54125690A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS54125690A (en) | 1979-09-29 |
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