JPS6351350A - Production of sodium salt of chlorinated lower fatty acid - Google Patents

Production of sodium salt of chlorinated lower fatty acid

Info

Publication number
JPS6351350A
JPS6351350A JP19556986A JP19556986A JPS6351350A JP S6351350 A JPS6351350 A JP S6351350A JP 19556986 A JP19556986 A JP 19556986A JP 19556986 A JP19556986 A JP 19556986A JP S6351350 A JPS6351350 A JP S6351350A
Authority
JP
Japan
Prior art keywords
lower fatty
fatty acid
chlorinated lower
chlorinated
anhydrous
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.)
Granted
Application number
JP19556986A
Other languages
Japanese (ja)
Other versions
JPH0717559B2 (en
Inventor
Zenzo Fujino
藤野 善蔵
Etsuo Takahashi
悦雄 高橋
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.)
Daicel Corp
Original Assignee
Daicel Chemical Industries Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Daicel Chemical Industries Ltd filed Critical Daicel Chemical Industries Ltd
Priority to JP19556986A priority Critical patent/JPH0717559B2/en
Publication of JPS6351350A publication Critical patent/JPS6351350A/en
Publication of JPH0717559B2 publication Critical patent/JPH0717559B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PURPOSE:To obtain high-quality sodium salt of chlorinated lower fatty acid having low salt content in a short time and efficiently, by using a chlorinated lower fatty acid and anhydrous sodium carbonate containing specific particles as raw materials, drying at a specific temperature and reacting. CONSTITUTION:A chlorinated lower fatty acid ester such as monochloroacetic acid, etc., and anhydrous sodium carbonate powder containing >=70% particles with 100-200 meshes in an amount of 20-25kg unit and in a feed ratio of equimolar amount are fed to an agitated blender type reactor, dried and reacted at 45-65 deg.C, preferably 50-55 deg.C to give the aimed compound such as sodium monochloroacetate, etc. By this method, production ability per device is improved and the method is industrially advantageous.

Description

【発明の詳細な説明】 (産業上の第1]用分野) 本発明は、モノクロル酢酸の様なりロル化低級脂肪酸と
無水炭酸ソーダを用いてクロル化低級脂肪酸ソーダを製
造する方法に関する。
DETAILED DESCRIPTION OF THE INVENTION (First Industrial Field) The present invention relates to a method for producing chlorinated lower fatty acid soda using a chlorinated lower fatty acid such as monochloroacetic acid and anhydrous soda carbonate.

(従来技術) クロル化低級脂肪酸、例えば、七ノクロル酢酸ソーダは
、一般に結晶状またはフレーク状の固体モノクロル酢酸
と粉末状の固体無水炭酸ソーダを、攪拌混合型の反応機
に入れて製造できることが知られている。
(Prior Art) It is known that chlorinated lower fatty acids, such as sodium heptanochloroacetate, can generally be produced by placing crystalline or flaky solid monochloroacetic acid and powdered solid anhydrous sodium carbonate in a stirring-mixing reactor. It is being

この場合、下式に示すように反応生成水が約8%発生す
る。
In this case, about 8% of reaction product water is generated as shown in the formula below.

2CtCH2C00H+Na2Co3→2CtCH2C
OONa 十CO□+H20 このため含水量の少いモノクロル酢酸ソーダを得るため
には加熱乾燥が必要であるが、そのために温度を高くす
ると生成したモノクロル酢酸ソーダの加水分解が進みグ
リコール酸と食塩が生成し逆にモノクロル酢酸ソーダの
純度が低下する。
2CtCH2C00H+Na2Co3→2CtCH2C
OONa 10CO□+H20 For this reason, heat drying is necessary to obtain sodium monochloroacetate with a low water content, but when the temperature is raised for this purpose, the hydrolysis of the produced sodium monochloroacetate progresses to produce glycolic acid and salt. Conversely, the purity of monochlorosodium acetate decreases.

従ってなるべく低い温度で反応及び乾燥を行なう必要が
あるが、この場合には反応速度及び乾燥時間が遅くなる
ため製造時間が長くなり、結局、食塩の生成量も多くな
ってしまう。この様な問題点を解決するための詳細な後
文ばこれまでのところ殆んど見られない。
Therefore, it is necessary to carry out the reaction and drying at as low a temperature as possible, but in this case, the reaction rate and drying time are slowed down, resulting in a longer production time and, ultimately, an increase in the amount of salt produced. So far, there has been little detailed support for solving these problems.

(発明が解決しようとする問題点) 本発明は上記の問題点を解決し、高品質のモノクロル酢
酸ソーダ、ひいてはクロル化低級脂肪酸ソーダを短時間
で製造することを特徴とする特許である。
(Problems to be Solved by the Invention) The present invention is a patent that solves the above-mentioned problems and is characterized by producing high-quality sodium monochloroacetate and, by extension, chlorinated lower fatty acid soda in a short time.

(問題点を解決するための手段) 本発明者等は、上記目的を達成するために、製造条件あ
るいは原料について種々検討を加えた結果、特定の原料
を用いかつ特定の温度で反応乾燥する事により高品質の
モノクロル酢酸ソーダを短時間に製造できることを見い
出し本発明に到達した。即ち本発明は、クロル化低級脂
肪酸と無水炭酸ソーダを混合して、クロル化低級脂肪酸
ソーダを製造する際に、反応温度45〜65℃で、10
0〜200メツシュの粒子を70%以上含有する無水炭
酸ソーダを用いることを特徴とするクロル化低級脂肪酸
ソーダの製造方法である。
(Means for Solving the Problems) In order to achieve the above object, the inventors of the present invention have conducted various studies on manufacturing conditions and raw materials, and have found that a specific raw material is used and reaction drying is performed at a specific temperature. The inventors have discovered that high-quality sodium monochloroacetate can be produced in a short period of time and have arrived at the present invention. That is, in the present invention, when mixing chlorinated lower fatty acids and anhydrous sodium carbonate to produce chlorinated lower fatty acid soda, the reaction temperature is 45 to 65°C, and 10
This is a method for producing chlorinated lower fatty acid soda, characterized by using anhydrous soda carbonate containing 70% or more of particles of 0 to 200 mesh.

本発明に使用するクロル化低級脂肪酸とは例えばモノク
ロル酢酸、ジクロル酢酸、トリクロル酢酸、モノクロル
プロピオン酸、ジクロルプロピオン酸等がある。
Examples of the chlorinated lower fatty acids used in the present invention include monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monochloropropionic acid, and dichloropropionic acid.

本発明に使用する無水炭酸ソーダは粒子径100〜20
0メソシュ好しくは100〜150メツシュのものを7
0%以上含む粉末である。なお70(X未満では本発明
の効果が十分に達成されない。
The anhydrous soda carbonate used in the present invention has a particle size of 100 to 20
0 meshes, preferably 100-150 meshes 7
It is a powder containing 0% or more. Note that if it is less than 70 (X), the effects of the present invention will not be fully achieved.

無水炭酸ソーダの粒子径は、200メソシユより細かい
と排気ダクトへの飛散が激しくなるため好ましくない。
If the particle size of the anhydrous soda carbonate is smaller than 200 mesos, it is not preferable because it will scatter into the exhaust duct.

又、粒子径が100メツシュより太きいものが多いと、
反応が遅くなり、反応が完結するまで水分の生成が続き
、結果的に乾燥時間が長くなるので好しくない。
Also, if there are many particles with a diameter larger than 100 mesh,
This is undesirable because the reaction slows down and moisture continues to be produced until the reaction is completed, resulting in a longer drying time.

反応及び乾燥温度は、45〜65℃好ましくは50〜5
5℃であるが、70 ’Cを越えると食塩の生成が顕著
に早くなり、また45℃を下根ると反応速度及び乾燥が
遅くなるため製造時間が長くなり、結局食塩の生成も多
くなるので好しくない。
The reaction and drying temperature is 45-65°C, preferably 50-55°C.
The temperature is 5°C, but if it exceeds 70'C, the production of salt will be significantly faster, and if the temperature is lower than 45°C, the reaction rate and drying will slow down, resulting in a longer production time, and eventually more salt will be produced. So I don't like it.

なお本発明を工業的に実施するにあたっては、モノクロ
ル酢酸等のクロル化低級脂肪酸と前述した無水炭酸ソー
ダを所定温度の攪拌混合型反応器に例えば20〜25k
li+単位で又互におよそ当モル量の仕込比で仕込めば
よい。
In carrying out the present invention industrially, chlorinated lower fatty acids such as monochloroacetic acid and the above-mentioned anhydrous soda are placed in a stirring-mixing reactor at a predetermined temperature, for example, at a temperature of 20 to 25 kg.
They may be charged in units of li+ at a charging ratio of about equimolar amounts to each other.

(発明の効果) 本発明の方法により例えばモノクロル酢酸と無水炭酸ソ
ーダよりモノクロル酢酸ソーダを製造する場合、 1)食塩含量の少い高品質のモノクロル酢酸ソーダを 2)短時間に効率よく 得ることができる。従って装置あたりの製造能力も向上
し工業的にも極めて有利である。
(Effects of the Invention) When producing sodium monochloroacetate from, for example, monochloroacetic acid and anhydrous sodium carbonate by the method of the present invention, 1) high-quality sodium monochloroacetate with a low salt content can be obtained efficiently in a short time. can. Therefore, the manufacturing capacity per device is improved, which is extremely advantageous from an industrial perspective.

(実施例) 実施例1および比較例1゛ フレーク状モノクロル酢酸1323.9と粒子径50−
100メツシュの無水炭酸ソーダ742Iを約31の攪
拌混合型反応器に少しづつ又互に約10分間で仕込んだ
。ジャケットは予め60〜65℃の温水を通しておいた
。攪拌混合を続け、1時間毎に分析して反応速度、食塩
の生成等を調べた。
(Example) Example 1 and Comparative Example 1 "Flake-like monochloroacetic acid 1323.9 and particle size 50-
100 mesh of anhydrous soda carbonate 742I was charged little by little into about 31 stirred mixer reactors over about 10 minutes each. The jacket was previously run through hot water at 60-65°C. Stirring and mixing were continued, and analysis was performed every hour to check the reaction rate, salt production, etc.

別に同一条件で、粒子径100〜150メノンユの無水
炭酸ンーダ乞用いて反応させた。
Separately, under the same conditions, anhydrous carbonate powder having a particle size of 100 to 150 mm was used for reaction.

結果は次表に示す。The results are shown in the table below.

実施例2゛および比較例2 反応、乾燥温度を45°〜50℃とした以外は、実施例
1および比較例1と同様の火“験を行った。
Example 2 and Comparative Example 2 Fire experiments were carried out in the same manner as in Example 1 and Comparative Example 1, except that the reaction and drying temperatures were 45° to 50°C.

結果を次表に示す。The results are shown in the table below.

実施例3および比較例3 フレーク状モノクロル酢酸875 kg及び100メツ
シュバス76%(A)と61%(B)の2種類の無水炭
酸ソーダ各々491 kgを攪拌混合型反応機に仕込み
、50〜55℃の温水で加温しながら反応、乾燥し、実
施例1と同様の測定を行った。
Example 3 and Comparative Example 3 875 kg of flaked monochloroacetic acid and 491 kg each of two types of anhydrous soda carbonate of 76% (A) and 61% (B) of 100 mesh baths were charged into a stirring mixing reactor, and the mixture was heated at 50 to 55°C. The mixture was reacted and dried while being heated with warm water, and the same measurements as in Example 1 were performed.

結果シエ次表に示す。The results are shown in the table below.

(使用した無水炭酸ソーダの粒度分布)上表に示した通
り100〜200メツシュの粒径な有する無水炭酸ソー
ダを(A)は72%、(B)は59%含んでいる。
(Particle size distribution of anhydrous soda carbonate used) As shown in the above table, (A) contains 72% and (B) 59% of anhydrous soda carbonate having a particle size of 100 to 200 mesh.

(反応結果)(Reaction result)

Claims (1)

【特許請求の範囲】[Claims] クロル化低級脂肪酸と無水炭酸ソーダを混合して、クロ
ル化低級脂肪酸ソーダを製造するに際して、反応温度4
5〜65℃で、100〜200メッシュの粒子を70%
以上含有する無水炭酸ソーダを用いることを特徴とする
クロル化低級脂肪酸ソーダの製造方法
When mixing chlorinated lower fatty acids and anhydrous soda carbonate to produce chlorinated lower fatty acid soda, the reaction temperature is 4.
70% particles of 100-200 mesh at 5-65℃
A method for producing chlorinated lower fatty acid soda characterized by using anhydrous carbonate soda containing the above
JP19556986A 1986-08-22 1986-08-22 Method for producing chlorinated lower fatty acid soda Expired - Lifetime JPH0717559B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP19556986A JPH0717559B2 (en) 1986-08-22 1986-08-22 Method for producing chlorinated lower fatty acid soda

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP19556986A JPH0717559B2 (en) 1986-08-22 1986-08-22 Method for producing chlorinated lower fatty acid soda

Publications (2)

Publication Number Publication Date
JPS6351350A true JPS6351350A (en) 1988-03-04
JPH0717559B2 JPH0717559B2 (en) 1995-03-01

Family

ID=16343304

Family Applications (1)

Application Number Title Priority Date Filing Date
JP19556986A Expired - Lifetime JPH0717559B2 (en) 1986-08-22 1986-08-22 Method for producing chlorinated lower fatty acid soda

Country Status (1)

Country Link
JP (1) JPH0717559B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106397179A (en) * 2016-09-19 2017-02-15 禹城禹圳生物科技有限公司 Method for preparing sodium chloroacetate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106397179A (en) * 2016-09-19 2017-02-15 禹城禹圳生物科技有限公司 Method for preparing sodium chloroacetate

Also Published As

Publication number Publication date
JPH0717559B2 (en) 1995-03-01

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