JPS62190141A - Purification of diacetone alcohol - Google Patents
Purification of diacetone alcoholInfo
- Publication number
- JPS62190141A JPS62190141A JP3172686A JP3172686A JPS62190141A JP S62190141 A JPS62190141 A JP S62190141A JP 3172686 A JP3172686 A JP 3172686A JP 3172686 A JP3172686 A JP 3172686A JP S62190141 A JPS62190141 A JP S62190141A
- Authority
- JP
- Japan
- Prior art keywords
- diacetone alcohol
- acetone
- distillation
- distilled
- crude
- 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
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000000746 purification Methods 0.000 title description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000009835 boiling Methods 0.000 claims abstract description 28
- 238000004821 distillation Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 18
- 230000000447 dimerizing effect Effects 0.000 claims 1
- 238000004040 coloring Methods 0.000 abstract description 13
- 238000006482 condensation reaction Methods 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 abstract description 2
- 239000011541 reaction mixture Substances 0.000 abstract 2
- 239000007809 chemical reaction catalyst Substances 0.000 abstract 1
- 238000006471 dimerization reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- OZXIZRZFGJZWBF-UHFFFAOYSA-N 1,3,5-trimethyl-2-(2,4,6-trimethylphenoxy)benzene Chemical compound CC1=CC(C)=CC(C)=C1OC1=C(C)C=C(C)C=C1C OZXIZRZFGJZWBF-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- SHOJXDKTYKFBRD-UHFFFAOYSA-N mesityl oxide Natural products CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- HSJKGGMUJITCBW-UHFFFAOYSA-N 3-hydroxybutanal Chemical compound CC(O)CC=O HSJKGGMUJITCBW-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229960004106 citric acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229940116315 oxalic acid Drugs 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はジアセトンアルコールの精製法に関する。詳し
くは本発明は、アセト／を縮合反応させて得られた粗ジ
アセトンアルコールを蒸留操作の縮合せによって精製す
る方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for purifying diacetone alcohol. Specifically, the present invention relates to a method for purifying crude diacetone alcohol obtained by a condensation reaction of acetone by condensation with distillation.
ジアセトンアルコールはアセトンをｍ金融Ｗ例えばアル
カリ性物質の存在下に二址化することによシ裏造される
。祷られた反応液中にはアセトン及びジアセトンアルコ
ールの外にメシチルオキシド、水、イソホロン、ホロン
等の不純物を含んでいる。従ってかかる反応液から精製
されたジアセトンアルコールを取得する精製法としては
一般に蒸留法が採用され、該反応液から、先ず低沸分離
塔により低沸点成分を除去し、次いで高沸分離塔により
高沸点成分を除去すると同時にジアセトンアルコールを
塔頂または側流から抜き出す方法により製品ジアセトン
アルコールを取得している。また、該精製法において、
ジアセトンアルコールは熱安定性が悪く、１００℃以上
に加熱すると一部はアセトンに解離し、また一部はメシ
チルオキシドと水とに分解するので、通常、ジアセトン
アルコールの蒸留を１００℃以下で行なうか、或いはジ
アセトンアルコールを微鷲の酸の存在下に７００℃以上
の温度で蒸留すること（特公昭３１−６３６１号）等が
行なわれている。Diacetone alcohol is prepared by converting acetone, for example in the presence of an alkaline substance. The desired reaction solution contains impurities such as mesityl oxide, water, isophorone, and holone in addition to acetone and diacetone alcohol. Therefore, a distillation method is generally adopted as a purification method to obtain purified diacetone alcohol from such a reaction liquid, in which low-boiling components are first removed from the reaction liquid using a low-boiling separation column, and then high-boiling components are removed from the reaction liquid using a high-boiling separation column. Product diacetone alcohol is obtained by removing boiling point components and simultaneously extracting diacetone alcohol from the top or side stream. Furthermore, in the purification method,
Diacetone alcohol has poor thermal stability, and when heated above 100°C, part of it dissociates into acetone, and part of it decomposes into mesityl oxide and water. Therefore, diacetone alcohol is usually distilled at temperatures below 100°C. Alternatively, diacetone alcohol is distilled at a temperature of 700° C. or higher in the presence of a slight acid (Japanese Patent Publication No. 31-6361).
しかしながら、上記の精製法で得られた高純度ジアセト
ンアルコールは、精製直後には無色透明であるが、該製
品を長期間貯蔵中に着色が徐々に進行して製品の品質が
低下する。この現象はその詳細は明らかではないが、ジ
アセトンアルコール中の微量不純物の作用によって製品
の着色が促進されるためと考えられる。However, although the high-purity diacetone alcohol obtained by the above-mentioned purification method is colorless and transparent immediately after purification, coloring gradually progresses during long-term storage of the product, degrading the quality of the product. Although the details of this phenomenon are not clear, it is thought that the coloring of the product is promoted by the action of trace impurities in diacetone alcohol.
この製品の着色を促進させるジアセトンアルコール中の
微量不純物についてはその詳細が明らかではないが、本
発明者等の研究によれば上記の精製法では精留効率を上
げても製品の着色を促進させる不純物を除去するのが難
しいことが判明した。The details of the trace impurities in diacetone alcohol that promote the coloring of this product are not clear, but according to research by the present inventors, the above purification method promotes the coloring of the product even if the rectification efficiency is increased. It has proven difficult to remove the impurities that cause
本発明者等は上記の問題点を解決すべく、ジアセトンア
ルコールの効果的な蒸留精製法につキ鋭意検討した結果
、粗ジアセトンアルコールの蒸留方法の変更により、得
られるジアセトンアルコール製品の着色が著しく抑制さ
れることを見出して本発明を完成した。In order to solve the above-mentioned problems, the present inventors have made extensive studies on an effective distillation purification method for diacetone alcohol. By changing the distillation method of crude diacetone alcohol, the resulting diacetone alcohol product can be improved. The present invention was completed by discovering that coloring was significantly suppressed.
即ち、本発明の狭旨は、アセトンを縮合触媒の存在下に
二証化することによυ得られた粗ジアセトンアルコール
を蒸留によってＭＷ Ｈするに尚り、該粗ジアセトンア
ルコールから予め島沸点物の実質的全量を蒸留分離した
のち、精留することを特徴とするジアセトンアルコール
の精製法、に存する。That is, the narrow gist of the present invention is that when the crude diacetone alcohol obtained by converting acetone in the presence of a condensation catalyst is subjected to MWH by distillation, The present invention relates to a method for purifying diacetone alcohol, which comprises separating substantially all of the boiling point by distillation and then rectifying it.
以下本発明につき更に詳細に説明する。The present invention will be explained in more detail below.
本発明はアセトンを縮合触媒の存在下に二型化すること
により得られた粗ジアセトンアルコールに適用される。The invention applies to crude diacetone alcohol obtained by dimorphizing acetone in the presence of a condensation catalyst.
縮合触媒としては、通常、アルカリ金属またはアルカリ
土類全組の水酸化物を主体として、これに各種の結合剤
を結合した固体触媒やアニオン交換樹脂触媒等が主とし
て用いられる。アセトンの縮合反応は上記の触媒を用い
て常法に従って行なわれる。例えば、流通式反応管に上
記触媒を充填し、これに低温上トンアルコールの平衡は
高温はどアセトンの方に移行するので、反応は低温で行
なうのが望ましい。かくして得られる反応液中には１０
〜２０％のジアセトンアルコール及びｒＯ〜りＯチのア
セトンの外にメシチルオキシド、水、インホロン、ホロ
ン、高沸点物等の不純物を含んでいる。As the condensation catalyst, a solid catalyst or an anion exchange resin catalyst, which is mainly composed of alkali metal or alkaline earth hydroxides combined with various binders, is mainly used. The condensation reaction of acetone is carried out using the above-mentioned catalyst according to a conventional method. For example, it is desirable to fill a flow-through reaction tube with the above catalyst and carry out the reaction at a low temperature, since the equilibrium of alcohol shifts toward acetone at high temperatures. The reaction solution thus obtained contained 10
Contains impurities such as mesityl oxide, water, inholone, holone, and high boiling point substances in addition to ~20% diacetone alcohol and rO~riO2 acetone.
本発明は上記の反応液に直接適用することも可能である
が、該反応液から未反応アセトンを分離回収し、ジアセ
トンアルコールを濃縮した濃縮液に適用するのが望まし
い。Although the present invention can be applied directly to the above reaction liquid, it is preferable to separate and recover unreacted acetone from the reaction liquid and apply it to a concentrated liquid obtained by concentrating diacetone alcohol.
本発明方法においては、上記の反応液または濃縮液（以
下、両者を併せて粗ジアセトンアルコールと称す。）か
ら、先ずジアセトンアルコールよりも高沸点の成分の実
質的全量を蒸留分離した後、蒸留精製して低沸点成分を
分離除去することにより、精製ジアセトンアルコールを
取得する。粗ジアセトンアルコールからの高沸点成分の
分離は理論段数５段以上の蒸留塔を用いて、通常減圧又
は常圧下に、好ましくは１０〜３００ ｍｍＨｇ の圧
力下に、塔底温度が通常６０〜／ １０℃好ましくはｔ
ｏｏ〜ｔ３Ｏ℃の温度条件下で蒸留して、ジアセトンア
ルコールよりも高沸点の成分を缶出させて分離し、一方
ジアセトンアルコール及び低沸点成分を塔頂または側流
よシ留出させて抜き出す。該理論段数が上記未満では熱
分解によシ着色原因物質に変化する高沸点物を分離除去
することが難しい。In the method of the present invention, first, substantially the entire amount of components having a higher boiling point than diacetone alcohol is separated by distillation from the above reaction solution or concentrate (hereinafter, both are collectively referred to as crude diacetone alcohol), and then, Purified diacetone alcohol is obtained by distillation and purification to separate and remove low-boiling components. The separation of high-boiling components from crude diacetone alcohol is carried out using a distillation column with 5 or more theoretical plates, usually under reduced pressure or normal pressure, preferably under a pressure of 10 to 300 mmHg, and at a bottom temperature of 60 to 60 mmHg. 10℃ preferably t
Distillation is carried out under a temperature condition of oo to 30°C, and components with a higher boiling point than diacetone alcohol are distilled out and separated, while diacetone alcohol and lower boiling components are distilled off from the top of the column or through a side stream. Pull it out. If the number of theoretical plates is less than the above, it is difficult to separate and remove high-boiling substances that turn into color-causing substances by thermal decomposition.
該留出液を次いで理論段数１段以上、好ましくはｊ段以
上の精留塔に供給し、通゛常減圧又は常圧下、好ましく
は！Ｏ〜７６０ ｍｍＨｇ の圧力下に塔底温度が通常
ｔｏ−ｉｊｏ℃の温度条件下で蒸留して低沸点成分（ア
セトン、水及びメシチルオキシド及び着色原因物質等）
を留去し、ジアセトンアルコールを塔頂または側流より
抜き出して取得する。該理論段数が上記未満では着色原
因物質を分離除去することが難しい。これらの蒸留操作
は回分式または連続式のいずれＣｈｆｘ″″８１６・ト
また、本発明方法においては、ジアセトンアルコールの
蒸留系内に微量、例えば、ｔ−１０００重ｆｋ ｐｐｍ
ＣＤ酸を存在させてジアセトンアルコールの分解を抑
制しつつ蒸留するのが好ましい。The distillate is then fed to a rectification column having one or more theoretical plates, preferably j or more theoretical plates, usually under reduced pressure or normal pressure, preferably! It is distilled under a pressure of 0 to 760 mmHg and a bottom temperature of usually 0 to 10℃ to remove low boiling point components (acetone, water, mesityl oxide, coloring substances, etc.)
is distilled off, and diacetone alcohol is extracted from the top or side stream. If the number of theoretical plates is less than the above, it is difficult to separate and remove coloring substances. These distillation operations may be carried out either batchwise or continuously.In addition, in the method of the present invention, a trace amount, e.g.
It is preferable to carry out distillation while suppressing the decomposition of diacetone alcohol in the presence of CD acid.
蒸留系内に存在させる酸としては、例えばマレイン酸、
フタル酸、吉草酸、クエン酸、シュウ酸、アスコルビン
酸寺の有機酸および硫酸、リン酸等の無機酸が皐げられ
る。Examples of the acid present in the distillation system include maleic acid,
Organic acids such as phthalic acid, valeric acid, citric acid, oxalic acid, ascorbic acid, and inorganic acids such as sulfuric acid and phosphoric acid are used.
本発明方法により、粗ジアセトンアルコールから精製ジ
アセトンアルコールを取得する方法の好ましい実施態様
の一例につき添付の第１図に基づき説明する。粗ジアセ
トンアルコールにＰＲ定量の酸を添加し、これを導管（
１）を経て蒸留塔（２）に導入する。ジアセトンアルコ
ールよシモ高沸点の成分はその実質的全量を塔底から導
管（４）を経て排出させ、一方ジアセトンアルコールは
低沸点成分と共に塔頂または側流（図示せず）から留出
させ、導管（３）を経て蒸留塔（５）に導入する。ジア
セトンアルコールは原料供給段よシ下方でかつ塔底よシ
上方の位置よυ側流で抜き出し導管（７）を経て取得さ
れる。また、低沸点成分は塔頂から留出させ、導管（６
）を経て排出され、一方塔底液は４管（８）を経て蒸留
塔（１）に循環される。An example of a preferred embodiment of the method of obtaining purified diacetone alcohol from crude diacetone alcohol according to the method of the present invention will be explained based on the attached FIG. 1. Add a PR amount of acid to the crude diacetone alcohol, and add this to the conduit (
1) and then introduced into the distillation column (2). The high-boiling components, such as diacetone alcohol, are discharged in substantially their entirety from the bottom of the column via conduit (4), while the diacetone alcohol is distilled off together with the low-boiling components from the top of the column or from a side stream (not shown). , into the distillation column (5) via the conduit (3). Diacetone alcohol is obtained in a side stream below the feed stage and above the bottom of the column via the withdrawal conduit (7). In addition, low-boiling components are distilled out from the top of the column, and the conduit (6
), while the bottom liquid is recycled to the distillation column (1) via four pipes (8).
本発明方法により、得られるジアセトンアルコールの着
色が抑制される埋山は未だ充分明らかではないが、恐ら
く上記粗ジアセトンアルコールからあらかじめ高沸点物
の実質的全量を蒸留分離することにより、蒸留塔内で熱
分解を生起し着色原因物質に変化する高沸点物（アセト
ンの縮合反応で副生ずる高沸点物）が除去され、原因物
質が低沸点成分と共に分離除去されるためではないかと
推定される。Although it is not yet fully clear how the method of the present invention suppresses the coloring of the diacetone alcohol obtained, it is probably possible to remove substantially all of the high-boiling substances from the crude diacetone alcohol by distillation in advance. It is presumed that this is because high boiling point substances (high boiling point substances produced as by-products in the condensation reaction of acetone) that undergo thermal decomposition inside the tank and turn into coloring substances are removed, and the causative substances are separated and removed along with low boiling point components. .
次に本発明の具体的態様を実施例によってさらに詳細に
説明するが、本発明は、その要旨を越えない限り、以下
の実施例によって限定されるものではない。Next, specific embodiments of the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to the following Examples unless the gist thereof is exceeded.
実施例１ アセトン（ＡＴ）のアルドール綜合反応後。Example 1 After aldol synthesis reaction of acetone (AT).
未反応のＡＴを大部分除去した粗ジアセトンアルコール
（ＤＡＡ）を用いて以下の精製操作を実施した。The following purification operation was carried out using crude diacetone alcohol (DAA) from which most of the unreacted AT had been removed.
粗ＤＡＡＪ／ｋｙ（ＤＡ人含有量り０％）を実段数ＩＯ
段の蒸留塔に仕込み、／ ｊ ＯｍｍＨｇ の圧力及
び１３１℃（バス塩）の温度で蒸留分離し％ Ｉｊｋｊ
ＩのＤＡＡを得た。このＤＡＡを更に同じ条件で蒸留し
て軽沸分を追い出し、／、ｊｋｇの梢ＤＡＡを得た。Crude DAAJ/ky (DA person content 0%) to actual plate number IO
It is charged into a column distillation column and separated by distillation at a pressure of /j OmmHg and a temperature of 131°C (bath salt).
Obtained DAA of I. This DAA was further distilled under the same conditions to remove light boiling components, and 1,000 kg of treetop DAA was obtained.
これを軟ｖＡ製の容器に入れ、３０℃で保存して着色の
経時変化を観察した。結果を第１表に示す。This was placed in a soft VA container and stored at 30°C to observe changes in coloring over time. The results are shown in Table 1.
比較例１ 実施例１と同じ粗ＤＡＡ２．／に１ｔを実段数ｉ。Comparative example 1 Crude DAA2. same as Example 1. / is 1t and the actual number of stages is i.
段の蒸留塔に仕込み、／ ３０ ｍｍＨｑ のポカ及び
１３ｊ℃（バス塩）の温度で蒸留して軽沸分を追いだし
、／、７に９のＤＡＡを得、ついでこのＤＡＡを同じ条
件で蒸留して、／、１ｋｇの精ＤＡＤを得た。実施例１
と同様に５０℃で保存して着色の経時変化を観察した。It was charged into a distillation column in a stage, and distilled at a temperature of /30 mmHq and 13J℃ (bath salt) to drive out the light boiling components to obtain DAA of /, 7 and 9, and then this DAA was distilled under the same conditions. As a result, 1 kg of purified DAD was obtained. Example 1
Similarly, the samples were stored at 50°C and changes in coloration over time were observed.
結果を第１ｐに示す。The results are shown in the 1st page.
第１表 ＋ｌ： 着色度はＡ Ｐ ＨＡＡで表示した。Table 1 +l: The degree of coloring was expressed as AP HAA.
本発明方法により着色度の著しく抑制された精製ジアセ
トンアルコールを得ることができる。By the method of the present invention, purified diacetone alcohol with a significantly suppressed degree of coloration can be obtained.
第１図は本発明方法で使用される蒸留系の例を模式的に
示す流れ図である。
ｌ：粗ジアセトンアルコール導入管、
２：高沸分離塔、 ｊ：精留塔、FIG. 1 is a flowchart schematically showing an example of a distillation system used in the method of the present invention. l: crude diacetone alcohol introduction pipe, 2: high boiling separation column, j: rectification column,
Claims (1)
より得られた粗ジアセトンアルコールを蒸留によつて精
製するに当り、該粗ジアセトンアルコールから予め高沸
点物の実質的全量を蒸留分離したのち、精留することを
特徴とするジアセトンアルコールの精製法。(1) When purifying the crude diacetone alcohol obtained by dimerizing acetone in the presence of a condensation catalyst by distillation, substantially the entire amount of high-boiling substances is distilled off from the crude diacetone alcohol in advance. A method for purifying diacetone alcohol, which is then subjected to rectification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61031726A JPH062703B2 (en) | 1986-02-15 | 1986-02-15 | Purification method of diacetone alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61031726A JPH062703B2 (en) | 1986-02-15 | 1986-02-15 | Purification method of diacetone alcohol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62190141A true JPS62190141A (en) | 1987-08-20 |
| JPH062703B2 JPH062703B2 (en) | 1994-01-12 |
Family
ID=12339042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61031726A Expired - Fee Related JPH062703B2 (en) | 1986-02-15 | 1986-02-15 | Purification method of diacetone alcohol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH062703B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016052307A1 (en) * | 2014-10-03 | 2016-04-07 | 富士フイルム株式会社 | Siloxane resin composition, transparent cured product using said composition, transparent pixel, microlens, and solid-state imaging element |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4852715A (en) * | 1971-10-29 | 1973-07-24 | ||
| JPS5745127A (en) * | 1980-05-27 | 1982-03-13 | Bp Chem Int Ltd | Recovery of pure acetone from cumene hydroperoxide decomposition products |
-
1986
- 1986-02-15 JP JP61031726A patent/JPH062703B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4852715A (en) * | 1971-10-29 | 1973-07-24 | ||
| JPS5745127A (en) * | 1980-05-27 | 1982-03-13 | Bp Chem Int Ltd | Recovery of pure acetone from cumene hydroperoxide decomposition products |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016052307A1 (en) * | 2014-10-03 | 2016-04-07 | 富士フイルム株式会社 | Siloxane resin composition, transparent cured product using said composition, transparent pixel, microlens, and solid-state imaging element |
| JP2016074797A (en) * | 2014-10-03 | 2016-05-12 | 富士フイルム株式会社 | Siloxane resin composition, transparent cured product using the same, transparent pixel, microlens, and solid-state imaging device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH062703B2 (en) | 1994-01-12 |
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