JP2981247B2 - Method for producing sodium pyrophosphate - Google Patents

Method for producing sodium pyrophosphate

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Publication number
JP2981247B2
JP2981247B2 JP2028574A JP2857490A JP2981247B2 JP 2981247 B2 JP2981247 B2 JP 2981247B2 JP 2028574 A JP2028574 A JP 2028574A JP 2857490 A JP2857490 A JP 2857490A JP 2981247 B2 JP2981247 B2 JP 2981247B2
Authority
JP
Japan
Prior art keywords
sodium
sodium pyrophosphate
aqueous solution
disodium phosphate
water
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 - Fee Related
Application number
JP2028574A
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Japanese (ja)
Other versions
JPH03232712A (en
Inventor
武人 松木
秀男 釜田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsui Chemicals Inc
Original Assignee
Mitsui Chemicals Inc
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Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は水に対する溶解速度の早いピロ燐酸ナトリウ
ムの製造方法に関する。更に詳しくは、冷水に対しても
溶解速度の早いピロ燐酸ナトリウムの製造方法に関す
る。
Description: TECHNICAL FIELD The present invention relates to a method for producing sodium pyrophosphate having a high dissolution rate in water. More specifically, the present invention relates to a method for producing sodium pyrophosphate having a high dissolution rate even in cold water.

〔従来の技術〕[Conventional technology]

ピロ燐酸ナトリウムは食品添加物、清缶剤、洗浄剤等
として幅広く使用されている。中でも、食品添加物とし
て使用されているものは、水に対する溶解速度、特に冷
水に対する溶解速度の早い品質のものが要求されてい
る。
Sodium pyrophosphate is widely used as a food additive, cleaning agent, detergent and the like. Among them, those used as food additives are required to have a high dissolution rate in water, especially a high quality in cold water.

通常、ピロ燐酸ナトリウムは次のような方法で製造さ
れている。
Usually, sodium pyrophosphate is produced by the following method.

即ち、水酸化ナトリウム、炭酸ナトリウム等のナトリ
ウム化合物と燐酸水溶液とを反応させて得られた、燐酸
二ナトリウム水溶液またはスラリーを乾燥し無水塩とし
た後、300〜350℃程度の温度で焼成することにより製造
されている。
That is, sodium hydroxide such as sodium hydroxide, sodium carbonate and the like and a phosphoric acid aqueous solution are reacted, and the disodium phosphate aqueous solution or slurry is dried to form an anhydrous salt, and then calcined at a temperature of about 300 to 350 ° C. It is manufactured by.

燐酸二ナトリウムは、下記(1)式で示す反応によっ
て生成する。(但し、(1)式ではナトリウム化合物を
水酸化ナトリウムで表した)。
Disodium phosphate is produced by a reaction represented by the following formula (1). (However, the sodium compound is represented by sodium hydroxide in the formula (1)).

また、ピロ燐酸ナトリウムは、下記(2)式による脱
水反応により得ることができる。
Further, sodium pyrophosphate can be obtained by a dehydration reaction according to the following formula (2).

H3PO4+2NaOH=Na2HPO4+2H2O ……(1) 2Na2HPO4→Na4P2O7+H2O ……(2) 上記(1)式及び(2)式から明らかなように、ピロ
燐酸ナトリウムを得るためには、水酸化ナトリウム及び
/または炭酸ナトリウムと燐酸水溶液は、モル比がNa/P
として2.0の割合で反応させなければならない。
H 3 PO 4 + 2NaOH = Na 2 HPO 4 + 2H 2 O (1) 2Na 2 HPO 4 → Na 4 P 2 O 7 + H 2 O (2) It is clear from the above equations (1) and (2). Thus, in order to obtain sodium pyrophosphate, sodium hydroxide and / or sodium carbonate and a phosphoric acid aqueous solution have a molar ratio of Na / P
Must be reacted at a rate of 2.0.

〔発明が解決しようとする課題〕[Problems to be solved by the invention]

しかしながら、このようにして得られたピロ燐酸ナト
リウムは食品添加物として使用する場合、水に対する溶
解速度、特に冷水に対する溶解速度の早い品質の要求に
対処できないという問題点があった。
However, when the sodium pyrophosphate thus obtained is used as a food additive, there is a problem that it is not possible to cope with a requirement for a high dissolution rate in water, particularly a high dissolution rate in cold water.

〔課題を解決するための手段〕[Means for solving the problem]

本発明らは、水に対する溶解速度、特に冷水に対する
溶解速度の早いピロ燐酸ナトリウムを得るために種々検
討を重ねた結果、水酸化ナトリウム、炭酸ナトリウム等
のナトリウム化合物と燐酸水溶液とを特定のモル比で反
応させ、次に乾燥品の水分を3〜6%に調整した後、焼
成することによってより溶解速度の早いピロ燐酸ナトリ
ウムを得ることが可能であることを見出し、本発明を完
成するに至ったものである。
The present inventors have conducted various studies to obtain sodium pyrophosphate having a high dissolution rate in water, particularly in cold water, and as a result, a sodium compound such as sodium hydroxide and sodium carbonate and a phosphoric acid aqueous solution have a specific molar ratio. And then adjusting the water content of the dried product to 3 to 6%, followed by baking to find that it is possible to obtain sodium pyrophosphate having a higher dissolution rate, thereby completing the present invention. It is a thing.

即ち、本発明は水酸化ナトリウム及び/または炭酸ナ
トリウムと燐酸水溶液とを反応させて燐酸二ナトリウム
水溶液またはスラリーとした後、該燐酸二ナトリウム水
溶液またはスラリーを乾燥し、焼成してピロ燐酸ナトリ
ウムを得る方法において、水酸化ナトリウム及び/また
は炭酸ナトリウムと燐酸水溶液とのモル比をNa/Pとして
1.986〜1.995の範囲で反応し、該燐酸二ナトリウム水溶
液またはスラリーを乾燥し、燐酸二ナトリウムの乾燥品
中に含まれる全水分量を3〜6%に調整した後、焼成
し、食品添加物として用いることを特徴とするピロ燐酸
ナトリウムの製造方法に関する。
That is, in the present invention, sodium hydroxide and / or sodium carbonate is reacted with an aqueous solution of phosphoric acid to form an aqueous solution or slurry of disodium phosphate, and then the aqueous solution or slurry of disodium phosphate is dried and calcined to obtain sodium pyrophosphate. In the method, the molar ratio of sodium hydroxide and / or sodium carbonate to the aqueous solution of phosphoric acid is Na / P
After reacting in the range of 1.986 to 1.995, the disodium phosphate aqueous solution or slurry is dried, and the total water content in the dried product of disodium phosphate is adjusted to 3 to 6%. The present invention relates to a method for producing sodium pyrophosphate, characterized in that it is used.

本発明を更に詳細に説明する。 The present invention will be described in more detail.

本発明では、燐酸二ナトリウム乾燥品中の水分の調整
は特に重要で、該燐酸二ナトリウム中に含まれる水分含
有量は3〜6%の範囲で、更にNa/Pのモル比は1.986〜
1.995の範囲である。
In the present invention, the adjustment of the water content in the dried disodium phosphate product is particularly important. The water content in the disodium phosphate product is in the range of 3 to 6%, and the molar ratio of Na / P is 1.986 to
It is in the range of 1.995.

水酸化ナトリウム、炭酸ナトリウム等のナトリウム化
合物と燐酸水溶液との反応温度は、特に限定はなく、通
常90〜105℃の温度で実施される。得られた燐酸二ナト
リウム水溶液またはスラリーはスプレードライヤー、パ
ドルドライヤー等通常公知の乾燥機により100〜110℃の
温度で乾燥し無水塩とすることが可能である。
The reaction temperature between the sodium compound such as sodium hydroxide and sodium carbonate and the phosphoric acid aqueous solution is not particularly limited, and is usually performed at a temperature of 90 to 105 ° C. The obtained disodium phosphate aqueous solution or slurry can be dried at a temperature of 100 to 110 ° C. by a commonly known dryer such as a spray drier or a paddle drier to obtain an anhydrous salt.

しかし、該燐酸二ナトリウム水溶液またはスラリーを
上記無水塩を得る場合より若干低い温度、短い時間で乾
燥することによって、乾燥品の水分量を3〜6%に調整
することができる。また、燐酸二ナトリウムの無水塩に
水を吹き付けて水分含有量を調整してもかまわない。次
で、該乾燥品をカルサイナー等のこれも公知の方法で焼
成することにより、容易にピロ燐酸ナトリウムを得るこ
とができる。
However, the water content of the dried product can be adjusted to 3 to 6% by drying the disodium phosphate aqueous solution or slurry at a slightly lower temperature and for a shorter time than when the above-mentioned anhydrous salt is obtained. Further, water may be sprayed on the anhydrous salt of disodium phosphate to adjust the water content. Next, the dried product is calcined by a known method such as calciner, so that sodium pyrophosphate can be easily obtained.

即ち、焼成してピロ燐酸ナトリウムを得る場合に無水
の燐酸二ナトリウムを焼成するより、3〜6%の水分を
含んだ燐酸二ナトリウムを焼成した方が冷水に対する溶
解速度は早くなる。その理由は定かではないが燐酸二ナ
トリウムの水分が触媒として作用し、ピロ燐酸ナトリウ
ムの性状が変化し水に対する分散・溶解速度を改善する
ための推定される。
That is, in the case of obtaining sodium pyrophosphate by firing, the dissolution rate in cold water is faster when firing disodium phosphate containing 3 to 6% water than when firing anhydrous disodium phosphate. Although the reason is not clear, it is presumed that the water content of disodium phosphate acts as a catalyst and the properties of sodium pyrophosphate change to improve the dispersing / dissolving rate in water.

本発明では、水酸化ナトリウム及び/または炭酸ナト
リウムと燐酸水溶液のモル比は特に重要で、Na/Pとして
1.986〜1.995の範囲である。Na/Pのモル比が1.995より
高くなると、本発明で問題とする溶解速度が悪化するの
で不都合である。逆に、Na/Pのモル比が1.986を下廻る
と、トリポリ燐酸ナトリウムの生成量の増加によりピロ
燐酸ナトリウムの純度低下を招き、食添規格を維持出来
ない。
In the present invention, the molar ratio between sodium hydroxide and / or sodium carbonate and the aqueous solution of phosphoric acid is particularly important.
It is in the range of 1.986 to 1.995. When the molar ratio of Na / P is higher than 1.995, the dissolution rate, which is a problem in the present invention, is disadvantageously deteriorated. Conversely, when the molar ratio of Na / P is less than 1.986, the purity of sodium pyrophosphate is reduced due to an increase in the amount of sodium tripolyphosphate produced, and the food specification cannot be maintained.

また、モル比を上記範囲に調整するのはピロ燐酸ナト
リウム中にわずかにトリポリ燐酸ナトリウムを生成させ
ることにより、ピロ燐酸ナトリウムの分散・溶解速度が
改善するためと推定される。しかしながら、必要以上に
トリポリ燐酸ナトリウムを生成させると、厚生省が定め
る食品添加物等の規格基準(以下、食添規格と略記す
る。)の示す純度97%以上の数値を満足させることがで
きなくなるので好ましくない。
Further, it is presumed that the molar ratio is adjusted to the above range because the dispersing / dissolving speed of sodium pyrophosphate is improved by slightly forming sodium tripolyphosphate in sodium pyrophosphate. However, if sodium tripolyphosphate is produced more than necessary, it is not possible to satisfy the value of purity of 97% or more indicated by the standard for food additives and the like specified by the Ministry of Health and Welfare (hereinafter abbreviated as food additive standard). Not preferred.

本発明のピロ燐酸ナトリウムの製造方法は、以上に述
べたように、水酸化ナトリウム、炭酸ナトリウム等のナ
トリウム化合物と燐酸水溶液とを反応させる時、モル比
(Na/P)を1.986〜1.995という特定の範囲に調整し、次
に乾燥品の水分が3〜6%になるように乾燥した後、焼
成する。このようにして得られたピロ燐酸ナトリウムは
極めて水に対する、特に冷水に対する溶解速度が早いの
で食品添加物として好適に使用し得る。
As described above, in the method for producing sodium pyrophosphate of the present invention, when a sodium compound such as sodium hydroxide or sodium carbonate is reacted with a phosphoric acid aqueous solution, the molar ratio (Na / P) is specified to be 1.986 to 1.995. , And then dried so that the moisture content of the dried product becomes 3 to 6%, followed by firing. The sodium pyrophosphate thus obtained has a very high dissolution rate in water, particularly in cold water, and can be suitably used as a food additive.

以下、実施例により具体的に説明する。 Hereinafter, specific examples will be described.

実施例1 容積300反応槽(攪拌機、冷却用ジャケット付き)7
5.0%燐酸水溶液150kgを仕込み、これに濃度48.5%の市
販の水酸化ナトリウム水溶液188.4kgを徐々に加えて反
応させて、Na/Pのモル比1.990に調整した。この水溶液
を約70kg/hの流量でパドルドライヤーに供給し、熱風を
熱源にしてパドルドライヤー出口排風温度を約95℃で脱
水反応を行ない乾燥した。この乾燥品の水分を測定した
ところ4.5%であった。
Example 1 300-volume reaction tank (with stirrer and cooling jacket) 7
150 kg of a 5.0% phosphoric acid aqueous solution was charged, and 188.4 kg of a commercially available aqueous sodium hydroxide solution having a concentration of 48.5% was gradually added thereto and reacted to adjust the molar ratio of Na / P to 1.990. This aqueous solution was supplied to a paddle dryer at a flow rate of about 70 kg / h, and a dehydration reaction was performed at a paddle dryer outlet exhaust temperature of about 95 ° C. using hot air as a heat source to dry. The water content of the dried product was measured and found to be 4.5%.

次いで、該乾燥品をカルサイナーに供給し、熱風を熱
源にしてカルサイナー出口温度約310℃にて焼成を行
い、ピロ燐酸ナトリウムを約150kg得た。得られたピロ
燐酸ナトリウムの物性を第1表に示す。
Next, the dried product was supplied to a calsiner, and calcined at a calciner outlet temperature of about 310 ° C. using hot air as a heat source to obtain about 150 kg of sodium pyrophosphate. Table 1 shows the physical properties of the obtained sodium pyrophosphate.

実施例2 水酸化ナトリウム水溶液の添加量を188.7kg(Na/Pモ
ル比1.993)に変更、乾燥品の水分が5.3%になった以外
は、実施例1と全く同様にしてピロ燐酸ナトリウムを約
150kg得た。得られたピロ燐酸ナトリウムの物性を第1
表に示す。
Example 2 The same procedure as in Example 1 was repeated except that the amount of the aqueous sodium hydroxide solution was changed to 188.7 kg (Na / P molar ratio: 1.993), and the water content of the dried product was reduced to 5.3%.
150 kg was obtained. The physical properties of the obtained sodium pyrophosphate are
It is shown in the table.

比較例1 水酸化ナトリウム水溶液の添加量を189.4kg(Na/Pモ
ル比2.000)パドルドライヤー出口排風温度を約105℃に
変更、乾燥品の水分が0.1%になった以外は実施例1と
全く同様にしてピロ燐酸ナトリウムを約150kg得た。得
られたピロ燐酸ナトリウムの物性を第1表に示す。
Comparative Example 1 The same procedure as in Example 1 was carried out except that the amount of the aqueous sodium hydroxide solution added was 189.4 kg (Na / P molar ratio: 2.000), and the outlet air temperature at the paddle dryer outlet was changed to about 105 ° C., and the water content of the dried product became 0.1%. Approximately 150 kg of sodium pyrophosphate was obtained in exactly the same way. Table 1 shows the physical properties of the obtained sodium pyrophosphate.

(註)−1 第1表に示す溶解速度は下記の方法によっ
て測定した。
(Note) -1 The dissolution rates shown in Table 1 were measured by the following methods.

1)溶解速度(1) 100mlの広口ビーカーに温度25℃の水を100ml入れ、中
央部の水位迄の水量が75mlになる様な強度にマグネチッ
クスターラーで攪拌し、これにピロ燐酸ナトリウム5gを
添加し、完溶する迄の時間で表した。
1) Dissolution rate (1) 100 ml of water at a temperature of 25 ° C is put into a 100 ml wide-mouth beaker, and the mixture is stirred with a magnetic stirrer so that the amount of water up to the center water level becomes 75 ml, and 5 g of sodium pyrophosphate is added thereto. It was expressed as the time until addition and complete dissolution.

2)溶解速度(2) 水温を5℃、ピロ燐酸ナトリウムの添加量を1gとした
以外は、溶解速度(1)と同一の方法で測定し、ピロ燐
酸ナトリウムの完溶する迄の時間で表した。
2) Dissolution rate (2) Measured in the same manner as dissolution rate (1) except that the water temperature was 5 ° C and the amount of sodium pyrophosphate added was 1 g, and expressed as the time until sodium pyrophosphate was completely dissolved. did.

(註)−2 第1表に示すピロ燐酸ナトリウムの純度は
食品添加物公定書に定める定量法(HCl)による中和滴
定法により測定した。従って、滴定時不純物として含ま
れるトリポリ燐酸ナトリウムもHClを消費するので、そ
の分ピロ燐酸ナトリウムの純度は実際の純度より高い値
を示す。また、トリポリ燐酸ナトリウムの含有量の測定
は樹脂分離法によった。このため、ピロ燐酸ナトリウム
の純度とトリポリ燐酸ナトリウムの含有量の合計量が10
0%以上となる数値を示した。
(Note) -2 The purity of sodium pyrophosphate shown in Table 1 was measured by a neutralization titration method using a quantitative method (HCl) specified in the official standard of food additives. Therefore, sodium tripolyphosphate included as an impurity during titration also consumes HCl, and the purity of sodium pyrophosphate is higher than the actual purity. The content of sodium tripolyphosphate was measured by a resin separation method. For this reason, the total amount of the purity of sodium pyrophosphate and the content of sodium tripolyphosphate is 10%.
The numerical value which becomes 0% or more was shown.

(発明の効果) Na/Pのモル比を1.995より高くして製造したピロ燐酸
ナトリウムは水に対する溶解速度、特に冷水に対する溶
解速度が著しく悪い。
(Effect of the Invention) Sodium pyrophosphate produced with a molar ratio of Na / P higher than 1.995 has a remarkably poor dissolution rate in water, particularly in cold water.

しかしながら、Na/Pのモル比を本発明で特定する範囲
(1.986〜1.995)で、水酸化ナトリウム、炭酸ナトリウ
ム等のナトリウム化合物と燐酸水溶液とを反応させて得
られた燐酸二ナトリウム水溶液またはスラリーを乾燥し
て乾燥品中に含まれる全水分量を一旦3〜6%に調整し
た後焼成して製造したピロ燐酸ナトリウムは実施例1及
び2が示すように、水に対する溶解速度、特に冷水に対
する溶解速度が早く、しかも食添規格に定める純度(97
%以上)も維持することができる。
However, the disodium phosphate aqueous solution or slurry obtained by reacting a sodium compound such as sodium hydroxide and sodium carbonate with a phosphoric acid aqueous solution within a range in which the molar ratio of Na / P is specified in the present invention (1.986 to 1.995) is used. As shown in Examples 1 and 2, the sodium pyrophosphate produced by drying and adjusting the total amount of water contained in the dried product to 3 to 6% once and then calcining, as shown in Examples 1 and 2, dissolves in water, especially in cold water. The speed is fast and the purity specified in the food standard (97
% Or more) can be maintained.

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】水酸化ナトリウム及び/または炭酸ナトリ
ウムと燐酸水溶液とを反応させて燐酸二ナトリウム水溶
液またはスラリーとした後、該燐酸二ナトリウム水溶液
またはスラリーを乾燥し、焼成してピロ燐酸ナトリウム
を得る方法において、水酸化ナトリウム及び/または炭
酸ナトリウムと燐酸水溶液とのモル比をNa/Pとして1.98
6〜1.995の範囲で反応し、該燐酸二ナトリウム水溶液ま
たはスラリーを乾燥し、燐酸二ナトリウムの乾燥品中に
含まれる全水分量を3〜6%に調整した後、焼成し、食
品添加物として用いることを特徴とするピロ燐酸ナトリ
ウムの製造方法。
An aqueous solution or slurry of disodium phosphate by reacting sodium hydroxide and / or sodium carbonate with an aqueous solution of phosphoric acid. The aqueous solution or slurry of disodium phosphate is dried and calcined to obtain sodium pyrophosphate. In the method, the molar ratio of sodium hydroxide and / or sodium carbonate to the aqueous solution of phosphoric acid is 1.98 as Na / P.
After reacting in the range of 6 to 1.995, the disodium phosphate aqueous solution or slurry is dried, and the total water content in the dried product of disodium phosphate is adjusted to 3 to 6%. A method for producing sodium pyrophosphate, which is used.
JP2028574A 1990-02-09 1990-02-09 Method for producing sodium pyrophosphate Expired - Fee Related JP2981247B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2028574A JP2981247B2 (en) 1990-02-09 1990-02-09 Method for producing sodium pyrophosphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2028574A JP2981247B2 (en) 1990-02-09 1990-02-09 Method for producing sodium pyrophosphate

Publications (2)

Publication Number Publication Date
JPH03232712A JPH03232712A (en) 1991-10-16
JP2981247B2 true JP2981247B2 (en) 1999-11-22

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Country Status (1)

Country Link
JP (1) JP2981247B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
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CN100528744C (en) * 2007-07-30 2009-08-19 四川宏达股份有限公司 Technique for preparing sodium pyrophosphate from wet method phosphoric acid

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Publication number Priority date Publication date Assignee Title
CN100528744C (en) * 2007-07-30 2009-08-19 四川宏达股份有限公司 Technique for preparing sodium pyrophosphate from wet method phosphoric acid

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