JPH0138111B2 - - Google Patents
Info
- Publication number
- JPH0138111B2 JPH0138111B2 JP11614681A JP11614681A JPH0138111B2 JP H0138111 B2 JPH0138111 B2 JP H0138111B2 JP 11614681 A JP11614681 A JP 11614681A JP 11614681 A JP11614681 A JP 11614681A JP H0138111 B2 JPH0138111 B2 JP H0138111B2
- Authority
- JP
- Japan
- Prior art keywords
- cyanuric acid
- water
- reaction
- sodium
- present
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 13
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 13
- -1 cyanuric acid sodium salt Chemical class 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 150000004677 hydrates Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- GLYUSNXFOHTZTE-UHFFFAOYSA-L disodium;carbonate;heptahydrate Chemical compound O.O.O.O.O.O.O.[Na+].[Na+].[O-]C([O-])=O GLYUSNXFOHTZTE-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- BWAUQTFFVCLSOS-UHFFFAOYSA-N sodiosodium hydrate Chemical compound O.[Na].[Na] BWAUQTFFVCLSOS-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Description
【発明の詳細な説明】
本発明は、工業的規模の実施に好適なシアヌル
酸ナトリウム塩の製造法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a process for producing cyanuric acid sodium salt, which is suitable for implementation on an industrial scale.
シアヌル酸ナトリウム塩はプール水中における
活性塩素の安定剤として注目されている化合物で
ある。 Cyanuric acid sodium salt is a compound that is attracting attention as a stabilizer of active chlorine in pool water.
シアヌル酸ナトリウム塩の工業的製法として
は、水媒中でシアヌル酸と苛性ソーダあるいは炭
酸ナトリウム等のアルカリ物質を加えて中和させ
る方法が知られているけれども、シアヌル酸の水
に対する溶解度が常温で１％以下と極めて少ない
のでこれを溶解するのに多量の水媒を必要とする
ため装置を大型化し且つ生成物の分離回収が煩雑
で排水処理を困難にするなど実施上多くの問題が
残されており、その工業的製法は未だ確立されて
いない。 As an industrial method for producing cyanuric acid sodium salt, a method is known in which cyanuric acid is neutralized in an aqueous medium by adding an alkaline substance such as caustic soda or sodium carbonate, but the solubility of cyanuric acid in water is 1 at room temperature. %, and a large amount of water medium is required to dissolve it, resulting in large-sized equipment, complicated separation and recovery of the product, and difficulty in wastewater treatment, leaving many problems in practice. However, its industrial manufacturing method has not yet been established.
本発明者等は、このような事情に鑑み克明な試
験研究を重ねた結果、シアヌル酸と炭酸ナトリウ
ム又は炭酸水素ナトリウムあるいは両者の混合物
を反応させるに当り、これら原料が常温で水和物
を形成しうる範囲の水を反応系に存在させ、各原
料を粉状とし且つ遊離水を生じる温度に維持しな
がら混練することによつて、シアヌル酸ナトリウ
ム塩を生産しうることを認め、本発明を完成した
ものである。 In view of these circumstances, the inventors of the present invention have carried out extensive testing and research, and have found that when reacting cyanuric acid with sodium carbonate, sodium bicarbonate, or a mixture of both, these raw materials form hydrates at room temperature. It has been recognized that cyanuric acid sodium salt can be produced by making each raw material into powder form and kneading the raw materials while maintaining the temperature at which free water is produced, in which water is present in the reaction system within the range that is possible, and the present invention has been developed. It is completed.
本発明方法によれば、反応容器内にシアヌル酸
を水和物として投入するかあるいは原料シアヌル
酸を反反応に存在する水と反応させて水和物を形
成し、炭酸ナトリウムあるいは炭酸水素ナトリウ
ムとの混合を粉状として極めて均一に行なうこと
ができ、次いで反応系をシアヌル酸水和物の転移
が起る約58℃以上の温度に加熱して遊離水を放出
させ、これにアルカリ物質が溶解して中和反応が
起り、更に中和によつて生じた水によつて反応は
連鎖的に進行し、且つ反応系における水は炭酸ナ
トリウム、炭酸水素ナトリウムの反応によつて生
じる炭酸ガスに同伴して気化逸散し、反応容器内
をほぼ粉体状態のまま混練することによつて定量
的に所期の目的物を得ることができ、通常その乾
燥工程を省略して差し支えない。 According to the method of the present invention, cyanuric acid is introduced into a reaction vessel as a hydrate, or cyanuric acid as a raw material is reacted with water present in the reaction to form a hydrate, and the cyanuric acid is reacted with sodium carbonate or sodium hydrogen carbonate. can be mixed extremely uniformly in powder form, and then the reaction system is heated to a temperature of approximately 58°C or higher, at which the transformation of cyanuric acid hydrate occurs, to release free water, and the alkali substance is dissolved in this. A neutralization reaction occurs, and the reaction proceeds in a chain reaction due to the water produced by the neutralization, and the water in the reaction system is entrained in the carbon dioxide gas produced by the reaction of sodium carbonate and sodium hydrogen carbonate. The desired target product can be quantitatively obtained by vaporizing and dissipating and kneading the powder in a substantially powder state inside the reaction vessel, and the drying step can usually be omitted.
本発明の実施に際しては、シアヌル酸及び炭酸
ナトリウムあるいは炭酸水素ナトリウムのいずれ
も水和物を形成しうるので、反応系を粉体状態で
均一に混練するために、シアヌル酸に対して約50
％以内の水を存在させることができ、反応を進行
させるためには、60〜100℃、好ましくは60〜80
℃の温度に加熱すべきである。 In carrying out the present invention, cyanuric acid and sodium carbonate or sodium bicarbonate can both form hydrates, so in order to uniformly knead the reaction system in powder form, approximately 50%
% of water can be present, and in order for the reaction to proceed, the temperature is 60-100℃, preferably 60-80℃.
It should be heated to a temperature of °C.
本発明方法によつて得られたシアヌル酸ナトリ
ウム塩は、流動性に富み全くケーキングを伴なわ
ないので、粉体のまま用いることができ水に対す
る溶解速度が著しく大きいものとする。 The cyanuric acid sodium salt obtained by the method of the present invention has excellent fluidity and does not cause caking at all, so it can be used as a powder and has a significantly high dissolution rate in water.
以下実施例によつて本発明を具体的に説明す
る。 The present invention will be specifically explained below using Examples.
実施例 １
加熱ジヤケツトを備えた200のリボンブレン
ダーに水分16.5％を含むシアヌル酸水和物100Kg
を仕込み、50rpmの速度で撹拌し乍ら34Kgの無水
炭酸ナトリウムを投入した。Example 1 100Kg of cyanuric acid hydrate containing 16.5% moisture in a 200 ribbon blender equipped with a heating jacket
was charged, and 34 kg of anhydrous sodium carbonate was added while stirring at a speed of 50 rpm.
徐々に反応を進み、温度は28℃から42℃に上昇
したが、このままでは反応は完結しなかつた。更
にジヤケツトに蒸気を通し、60〜70℃の温度で２
時間混練を続け、流動性のよい粉状のシアヌル酸
ナトリウム塩111.4Kgを得た。 The reaction progressed gradually, and the temperature rose from 28°C to 42°C, but the reaction was not completed at this rate. Furthermore, pass steam through the jacket and heat it at a temperature of 60 to 70℃.
Kneading was continued for hours to obtain 111.4 kg of cyanuric acid sodium salt in powder form with good fluidity.
遊離水分は1.8％であり、もはや乾燥する必要
のないものであつた。 The free moisture content was 1.8% and there was no need to dry it any longer.
本品は、赤外線吸収スペクトル分析の結果、シ
アヌル酸モノナトリウム塩の１水和物であること
が確認された。 As a result of infrared absorption spectrum analysis, this product was confirmed to be a monohydrate of cyanuric acid monosodium salt.
実施例 ２
実施例１と同じ装置を用い、乾燥シアヌル酸
83.5Kgと炭酸水素ナトリウム54.3Kgを仕込み、撹
拌し乍ら12Kgの水を加え、次いで75℃の温度に加
温し150分間混練を続行し、シアヌル酸ナトリウ
ム塩115.6Kgを得た。Example 2 Using the same equipment as in Example 1, dry cyanuric acid
83.5 kg and 54.3 kg of sodium hydrogen carbonate were charged, 12 kg of water was added while stirring, and then the mixture was heated to 75°C and kneading was continued for 150 minutes to obtain 115.6 kg of cyanuric acid sodium salt.
本品は、赤外線吸収スペクトル分析の結果、シ
アヌル酸モノナトリウム１水和物であり、約３％
の遊離水分が認められたが流動性もよく、ケーキ
ング現象は全く認められなかつた。 As a result of infrared absorption spectrum analysis, this product is monosodium cyanurate monohydrate, approximately 3%
Although some free water was observed, the fluidity was good and no caking phenomenon was observed.
実施例 ３
実施例１で用いた装置に83.0Kgの乾燥シアヌル
酸83.0Kgと無水原料ナトリウム34Kg及び炭酸ナト
リウム７水和物74.6Kgを入れて混合し、次いで
100℃の温度で３時間反応を行なつて、シアヌル
酸ナトリウム塩125Kgを得た。Example 3 83.0Kg of dry cyanuric acid, 34Kg of anhydrous raw material sodium, and 74.6Kg of sodium carbonate heptahydrate were put into the equipment used in Example 1, and then mixed.
The reaction was carried out at a temperature of 100° C. for 3 hours to obtain 125 kg of cyanuric acid sodium salt.
赤外線吸収スペクトル分析の結果、本品はシア
ヌル酸２ナトリウム１水塩であり、遊離水1.7％
を含むものであつた。 As a result of infrared absorption spectrum analysis, this product is cyanuric acid disodium monohydrate and contains 1.7% free water.
It included:
参考例
実施例１、２及び３で得た各シアヌル酸ナトリ
ウム塩について、溶解性を測定したところ
150rpmで回転する撹拌翼を備えた60の水槽3.5
ｇの試料を投入し、経時的に採水し飽和メラミン
水溶液を加えて生ずる不溶性メラミンシアヌレー
トの濁度から溶解速度を測定した結果では、いず
れも５分以内に完全に溶解するものであつた。Reference Example The solubility of each cyanuric acid sodium salt obtained in Examples 1, 2, and 3 was measured.
60 water tanks 3.5 with stirring blades rotating at 150 rpm
The results of measuring the dissolution rate from the turbidity of insoluble melamine cyanurate produced by adding a saturated aqueous melamine solution to the water taken over time after adding a sample of .
Claims (1)
トリウムあるいは両者の混合物を反応させるに当
りこれら原料が常温で水和物を形成しうる範囲の
水を反応系に存在させ、各原料を粉状とし、且つ
遊離水を生じる温度に維持しながら混練すること
を特徴とするシアヌル酸ナトリウム塩の製造法。1. When reacting cyanuric acid with sodium carbonate, sodium hydrogen carbonate, or a mixture of both, water is present in the reaction system in an amount that allows these raw materials to form hydrates at room temperature, each raw material is powdered, and free A method for producing cyanuric acid sodium salt, which comprises kneading while maintaining the temperature at which water is produced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11614681A JPS5818370A (en) | 1981-07-23 | 1981-07-23 | Preparation of sodium cyanurate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11614681A JPS5818370A (en) | 1981-07-23 | 1981-07-23 | Preparation of sodium cyanurate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5818370A JPS5818370A (en) | 1983-02-02 |
| JPH0138111B2 true JPH0138111B2 (en) | 1989-08-11 |
Family
ID=14679877
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11614681A Granted JPS5818370A (en) | 1981-07-23 | 1981-07-23 | Preparation of sodium cyanurate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5818370A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7212757B2 (en) * | 2018-08-01 | 2023-01-25 | 中国科学院福建物質結構研究所 | Alkali metal monohydrogen cyanurate compound, its crystal, its production method and its application |
-
1981
- 1981-07-23 JP JP11614681A patent/JPS5818370A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5818370A (en) | 1983-02-02 |
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