JPS60139641A - Purification of monochloroacetic acid - Google Patents
Purification of monochloroacetic acidInfo
- Publication number
- JPS60139641A JPS60139641A JP24489883A JP24489883A JPS60139641A JP S60139641 A JPS60139641 A JP S60139641A JP 24489883 A JP24489883 A JP 24489883A JP 24489883 A JP24489883 A JP 24489883A JP S60139641 A JPS60139641 A JP S60139641A
- Authority
- JP
- Japan
- Prior art keywords
- monochloroacetic acid
- hydrogen peroxide
- quality
- mca
- acid
- 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
Links
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000746 purification Methods 0.000 title description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 238000007796 conventional method Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 229960005215 dichloroacetic acid Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
本発明はモノクロル酢酸（以下、ＭＣＡと略す。）の精
製方法に関する。更に、詳しくは、処理すべきＭＣＡ中
に過酸化水、素を添加することによって、より優れた高
品質のＭＣＡを得る方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for purifying monochloroacetic acid (hereinafter abbreviated as MCA). More specifically, the present invention relates to a method of obtaining MCA of better quality by adding water peroxide and hydrogen into the MCA to be treated.
ＭＣＡの製法として、一般に酢酸を塩素化することによ
ってＴ業的に製造される。この際、常に副生成物として
、多かれ少かれ、ジクロ／し酢酸等が生成し、現在、例
えば蒸溜、晶析或いは水素添加等によって精製され、工
業用ＩＶＩ ＣＡが必要とする品質必要条件に応じてい
る。しかし、これ等精製方法等によっても、なお、正体
が未だ充分に解明されない微量の不純物が含まれ１おり
、さらに高品質のＭＣＡの取得問題が残っている。MCA is generally produced commercially by chlorinating acetic acid. In this process, more or less by-products such as dichloro/dichloroacetic acid are produced, which are currently purified by, for example, distillation, crystallization, or hydrogenation, to meet the quality requirements required by industrial IVI CA. ing. However, even with these purification methods, there are still trace amounts of impurities whose true nature has not been fully elucidated1, and there remains the problem of obtaining high-quality MCA.
近年、業界では例えば食品関連等の特殊な用途に関し、
微妙な色相及び加熱（溶解）時、その緑変等と従来にな
かった高品質を有するＭＣＡが要求される様になって来
た。In recent years, the industry has been focusing on special applications such as food-related applications.
There is a growing demand for MCAs that have a delicate hue and a green discoloration when heated (melted), and have unprecedented high quality.
本発゛明者らは高品質のＭＣＡを得る方法につ□いて検
討を重□ねた結果、従来法とは全く訳る本発明即ち、モ
ノクロル酢酸法過酸化水素で処理することにより、さら
に高品質のモレクロル酢酸を得ることを特徴とするモノ
クロル酢酸の精製 法を見い出したものである。The inventors of the present invention have repeatedly investigated methods for obtaining high-quality MCA, and as a result, the present invention, which is completely different from the conventional method, has been developed, namely, the monochloroacetic acid method. We have discovered a method for purifying monochloroacetic acid that is characterized by obtaining high-quality molechloroacetic acid.
この場合、特定の品質−微妙な色相及び加熱買溶解）時
、壬の緑変一番悪化させていた微ｉ社の不純物は恐らく
、過１雲化水素により酸化分解され、良質なものに％化
するも”あと推定へれる。In this case, the impurities that were most aggravating the green discoloration of the bottle during the specific quality (subtle hue and hot melting) were probably oxidized and decomposed by the hydrogen peroxide, resulting in % of good quality. ``It will be estimated later.''
本発明において処理される対象液は原則的には贈造工□
程中、とめ段階のモノクロル酢酸にも適用できる。しか
し、反応工程より得らノＬる粗ＭＣＡ等、不純物の多い
ＭＣＡに直接適用する場合過酸゛化水素の添加量が多く
なり、必ずしも、有利でない。粗ＭＣＡを従来法で精製
して得られた精ＭＣＡ等、容易に取除ける不純物と分離
した純度、約９７チ以上のＭＣＡに適用する方が一層効
果的である。In principle, the target liquid to be treated in the present invention is
It can also be applied to monochloroacetic acid at the intermediate and final stages. However, when directly applied to MCA containing many impurities, such as crude MCA obtained from a reaction process, the amount of hydrogen peroxide added becomes large, which is not necessarily advantageous. It is more effective to apply the method to purified MCA obtained by refining crude MCA by a conventional method, which has a purity of about 97% or higher, which is separated from impurities that can be easily removed.
本発明において、用いる過酸化水素は通常、２０〜５０
％の水溶液として市販されるものでよい。過酸化水素の
添加量（純分）はＭＣＡ基準として、約０．０５〜１．
０重量％である。In the present invention, the hydrogen peroxide used is usually 20 to 50%
% aqueous solution may be used. The amount of hydrogen peroxide added (purity) is approximately 0.05 to 1.0% based on MCA standards.
It is 0% by weight.
なお、これは実用的には処理すべきＭＣＡ中の特定の品
質等に悪影響を及ぼすと考えられる不純物の含有量に見
合う数値で充分であるが、実験により適宜、決めること
が必要である。Note that, in practical terms, it is sufficient to set this value to a value commensurate with the content of impurities that are considered to have an adverse effect on specific quality, etc. in the MCA to be treated, but it is necessary to determine it appropriately through experiments.
本発明における処理温度はＭＣＡの融点以上。The processing temperature in the present invention is higher than the melting point of MCA.
約７０〜１２０℃から選ばれる。通常、処理時間は必要
ならば蒸溜時間も含め、約１〜５時間、程度である。Selected from about 70 to 120°C. Usually, the processing time is about 1 to 5 hours, including distillation time if necessary.
本発明における特徴を挙げると次の通りである。The features of the present invention are as follows.
イ）過酸化水素は処理後水となり、特定品質に影響を与
えない。b) Hydrogen peroxide becomes water after treatment and does not affect specific quality.
口）過酸化水素は、工業的規模で容易入手することがで
きる。) Hydrogen peroxide can be easily obtained on an industrial scale.
ハ）処理方法が極めて簡単である。c) The processing method is extremely simple.
この様にして本発明によれば、ＭＣＡに過酸化水素を添
加することによって、イ）１口）、ハ）の特徴が発揮さ
れかつ微妙な色相及び加熱（溶解）時、その緑変のない
高品質のＭＣＡを得ることができる。In this way, according to the present invention, by adding hydrogen peroxide to MCA, the characteristics of a) 1 mouth) and c) are exhibited, and the hue is subtle and there is no greening when heated (dissolved). High quality MCA can be obtained.
以下、実施例により１本発明を更に詳しく説明する。Hereinafter, the present invention will be explained in more detail with reference to Examples.
なお、品質（色相）の評価は、８０％モノクロル酢酸の
水溶液における波長４００ ｎ ｍの透過率及び熱緑変
（７０℃×５Ｈ）のそれで実施した。The quality (hue) was evaluated based on transmittance at a wavelength of 400 nm and thermal greening (70°C x 5H) in an aqueous solution of 80% monochloroacetic acid.
実施例−１，２
処理液：水素添加後のＭＣＡを蒸溜して得られたもの（
低品質のもの）
撹拌機及び還流器を備えた三角フラスコに、処理液を投
入、さらに、過酸化水素（純度３０％）をＭＣＡ基準と
して純分換算（１，０５重１％（実施例−１斤参び（１
、１重量％（実施例−２）添加し７０℃で５時間処理し
た。結果を表−１に示す。Examples 1 and 2 Treatment liquid: one obtained by distilling MCA after hydrogenation (
Pour the treated solution into an Erlenmeyer flask equipped with a stirrer and a reflux device, and add hydrogen peroxide (purity 30%) to the pure fraction (1.05 wt 1% (Example - 1 catty visit (1
, 1% by weight (Example-2) was added and treated at 70°C for 5 hours. The results are shown in Table-1.
表 １
実施例 −３及び比較例
処理液：粗製ＭＣＡを水素添加して得られたもの
処理液、上記及び処理時間ＩＨを変えた以外は実施例
−１と同様に処理した。Table 1 Example-3 and Comparative Examples Treatment liquid: obtained by hydrogenating crude MCA Treatment liquid, Examples except for the above and treatment time IH were changed.
-1 was treated in the same manner.
継いで、得られた処理液は減圧下、連続蒸溜（オルグー
ショ塔、１０段）によって、後精製した。結果を表−２
に示す。Subsequently, the obtained treated liquid was post-purified by continuous distillation (Orgucho column, 10 stages) under reduced pressure. Table 2 of the results
Shown below.
表−２Table-2
Claims (1)
らに高品質のモノクロル酢酸ぎ得ること全特徴とするモ
ノクロル酢酸の精製 法A method for purifying monochloroacetic acid that is characterized by the fact that even higher quality monochloroacetic acid can be obtained by treating monochloroacetic acid with hydrogen peroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24489883A JPS60139641A (en) | 1983-12-27 | 1983-12-27 | Purification of monochloroacetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24489883A JPS60139641A (en) | 1983-12-27 | 1983-12-27 | Purification of monochloroacetic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60139641A true JPS60139641A (en) | 1985-07-24 |
| JPH0410461B2 JPH0410461B2 (en) | 1992-02-25 |
Family
ID=17125616
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24489883A Granted JPS60139641A (en) | 1983-12-27 | 1983-12-27 | Purification of monochloroacetic acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60139641A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5387713A (en) * | 1991-01-05 | 1995-02-07 | Bp Chemicals Limited | Process for purification of carboxylic acids |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1201260A (en) * | 1966-12-12 | 1970-08-05 | Union Carbide Corp | Purification of formic acid |
| JPS5031130A (en) * | 1973-07-23 | 1975-03-27 | ||
| JPS5428870A (en) * | 1977-08-08 | 1979-03-03 | Yamasa Shoyu Kk | Production of sweetener extract |
| JPS5640640A (en) * | 1979-09-10 | 1981-04-16 | Toray Ind Inc | Purification of terephthalic acid |
| JPS5899108A (en) * | 1981-11-23 | 1983-06-13 | モ−ビル オイル コ−ポレ−ション | Method of removing residual organic matter and color from phosphoric acid refined |
-
1983
- 1983-12-27 JP JP24489883A patent/JPS60139641A/en active Granted
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1201260A (en) * | 1966-12-12 | 1970-08-05 | Union Carbide Corp | Purification of formic acid |
| JPS5031130A (en) * | 1973-07-23 | 1975-03-27 | ||
| JPS5428870A (en) * | 1977-08-08 | 1979-03-03 | Yamasa Shoyu Kk | Production of sweetener extract |
| JPS5640640A (en) * | 1979-09-10 | 1981-04-16 | Toray Ind Inc | Purification of terephthalic acid |
| JPS5899108A (en) * | 1981-11-23 | 1983-06-13 | モ−ビル オイル コ−ポレ−ション | Method of removing residual organic matter and color from phosphoric acid refined |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5387713A (en) * | 1991-01-05 | 1995-02-07 | Bp Chemicals Limited | Process for purification of carboxylic acids |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0410461B2 (en) | 1992-02-25 |
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