JPH01203348A - Production of dihydroxyacetone - Google Patents
Production of dihydroxyacetoneInfo
- Publication number
- JPH01203348A JPH01203348A JP2573988A JP2573988A JPH01203348A JP H01203348 A JPH01203348 A JP H01203348A JP 2573988 A JP2573988 A JP 2573988A JP 2573988 A JP2573988 A JP 2573988A JP H01203348 A JPH01203348 A JP H01203348A
- Authority
- JP
- Japan
- Prior art keywords
- crystallization
- dihydroxyacetone
- solvent
- concentration
- aqueous solution
- 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
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical compound OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229940120503 dihydroxyacetone Drugs 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000002425 crystallisation Methods 0.000 claims abstract description 17
- 230000008025 crystallization Effects 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000000977 initiatory effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 9
- 239000011549 crystallization solution Substances 0.000 description 7
- 238000000855 fermentation Methods 0.000 description 7
- 230000004151 fermentation Effects 0.000 description 7
- 239000012141 concentrate Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000813 microbial effect Effects 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003957 anion exchange resin Substances 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- 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）
本発明は医薬品等の原料として有用なジヒドロキシアセ
トンの製造法に関する物である。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing dihydroxyacetone, which is useful as a raw material for pharmaceuticals and the like.
（従来の技術）
従来よシ、ジヒドロキシアセトンは種々の方法により製
造されている。例えば、微生物発酵法によって製造され
たジヒドロキシアセトン含有発酵液は、菌体を除去した
後、陽イオン交換樹脂・陰イオン交換樹脂を順次接触さ
せ、Ｌ２かる後減圧濃縮して得られたジヒドロキシアセ
トン濃縮液に溶媒を加え晶析することによシジヒドロキ
シアセトンを得ている。(Prior Art) Dihydroxyacetone has conventionally been produced by various methods. For example, a dihydroxyacetone-containing fermentation liquid produced by a microbial fermentation method is obtained by removing bacterial cells, sequentially contacting a cation exchange resin and an anion exchange resin, and concentrating under reduced pressure after L2. Sidihydroxyacetone is obtained by adding a solvent to the liquid and crystallizing it.
（発明が解決しようとする課題）
この微生物発酵法では、発酵液中のジヒドロキシアセト
ン濃度はたかだか２０ ｗｔ％であり、このような低濃
度のジヒドロキシアセトン水溶液を晶析するのに適当な
濃度まで濃縮するにはかなりの時間を要する。(Problem to be Solved by the Invention) In this microbial fermentation method, the dihydroxyacetone concentration in the fermentation liquid is at most 20 wt%, and it is necessary to concentrate the dihydroxyacetone aqueous solution with such a low concentration to an appropriate concentration for crystallization. It takes a considerable amount of time to do so.
又、晶析液から結晶を濾過・分離する際の結晶の濾過性
が極端に低下する場合がある。そのため、晶析液からの
結晶の分離に遠心分離機を使用する場合には、より高性
能な遠心分離機を必要としたシ、濾過性が悪いために得
られる結晶の品質に問題が生じたシ、濾過に長時間を要
した。Furthermore, the filterability of the crystals when filtering and separating them from the crystallization solution may be extremely reduced. Therefore, when using a centrifuge to separate crystals from the crystallization solution, a higher-performance centrifuge was required, and problems occurred with the quality of the crystals obtained due to poor filtration. However, filtration took a long time.
本発明はこのような問題点を解決するために晶析液の濾
過性を改良する仁とを目的とするものである。In order to solve these problems, the present invention aims to improve the filterability of a crystallization solution.
（課題を解決するための手段）
本発明者等は前述の濾過性について鋭意検討した結果、
意外にも、濃縮後、晶析を開始するまでの時間が、晶析
液の濾過性に大きな影響を与えていることを見いだし本
発明に至った。(Means for Solving the Problems) As a result of intensive study on the above-mentioned filterability, the present inventors found that
Surprisingly, it was discovered that the time from concentration to the start of crystallization has a great effect on the filterability of the crystallization solution, leading to the present invention.
即ち、本発明はジヒドロキシアセトン水溶液を濃縮し、
濃縮液に溶媒を加えて晶析を行う際に、濃縮液中の水分
が２０ ｗｔ％以下となってから、濃縮を終了し溶媒を
添加して晶析を開始するまでの時間が５０時間を越えな
いようにする事を特徴とスルノヒドロキシアセトンの製
造法でアル。That is, the present invention concentrates a dihydroxyacetone aqueous solution,
When performing crystallization by adding a solvent to the concentrated liquid, the time from when the water content in the concentrated liquid becomes 20 wt% or less until the concentration is finished, the solvent is added, and crystallization starts is 50 hours. The method for producing sulnohydroxyacetone is characterized by the fact that it does not exceed Al.
上記時間が５０時間を超えると加速度的に晶析液の濾過
性が低下し好しくない。If the above-mentioned time exceeds 50 hours, the filterability of the crystallization solution will deteriorate at an accelerated rate, which is not preferable.
ジヒドロキシアセトン水溶液は合成法によシ得られたも
のでも発酵法によシ得られたものでもよい。The dihydroxyacetone aqueous solution may be obtained by a synthetic method or by a fermentation method.
発酵法によシ得られる該水溶液のジヒドロキシアセトン
濃度はたかだか２０ ｗｔ％であり、通常はこれを約９
０チ程度以上にまで脱水濃縮する。The dihydroxyacetone concentration of the aqueous solution obtained by the fermentation method is at most 20 wt%, and usually this is about 9% by weight.
Dehydrate and concentrate to about 0% or more.
濃縮後、溶媒を加えて通常の方法によシ晶析を行うが、
溶媒としては、イソプロｉＪ？ノール等の低級アルコー
ル、アセトン等が使用できる。After concentration, a solvent is added and crystallization is performed in the usual manner.
As a solvent, Isopro iJ? Lower alcohols such as alcohol, acetone, etc. can be used.
用いる溶媒量は、ジヒドロキシアセトン１重量部に対し
０．３−２．Ｑ重量部用いるのが好ましい。The amount of solvent used is 0.3-2.0 parts by weight of dihydroxyacetone. It is preferable to use Q parts by weight.
溶媒の使用量が少な過ぎると操作上結晶の取シ出しが困
難となシ、また、多過ぎると収率が悪くなる。If the amount of solvent used is too small, it will be difficult to remove the crystals during operation, and if it is too large, the yield will be poor.
晶析を行なう温度は特に限定しないが、好ましくは０−
３０℃である。The temperature for crystallization is not particularly limited, but is preferably 0-
The temperature is 30°C.
実施例１
微生物発酵法によってジヒドロキシアセトンを製造し、
菌体除去した発酵液を陽イオン交換樹脂（ＩＲ−１２０
８） 、陰イオン交換樹脂（ＩＲＡ−６８）、活性炭処
理して粗ジヒドロキシアセトン水溶液を得た。Example 1 Dihydroxyacetone was produced by microbial fermentation method,
The fermented liquid from which the bacterial cells have been removed is treated with cation exchange resin (IR-120).
8) An anion exchange resin (IRA-68) was treated with activated carbon to obtain a crude dihydroxyacetone aqueous solution.
この粗ジヒドロキシアセトン水溶液を、５０’Ｃの水浴
中で攪拌しながら水分２０ ｗｔ％まで約４時間かけて
減圧濃縮し、引き続き水分１０ ｗｔ％まで５０時間か
けて濃縮した。This crude dihydroxyacetone aqueous solution was concentrated under reduced pressure in a 50'C water bath with stirring to a moisture content of 20 wt% over about 4 hours, and then concentrated to a moisture content of 10 wt% over a period of 50 hours.
こうして得ら、れたジヒドロキシアセトン濃縮液２００
ｙ−に対しただちにインプロパツールを１６０？加えて
２０℃にて３２時間攪拌しながら晶析した。晶析液を３
０ｃＩＩＬ２の濾過面積を有する濾過装置で吸引濾過し
たところ、約１ｏ分間で濾過した。Thus obtained dihydroxyacetone concentrate 200
Immediately use Improper Tools 160 for y-? In addition, crystallization was performed at 20° C. with stirring for 32 hours. 3 of the crystallization solution
When suction filtration was carried out using a filtration device having a filtration area of 0cIIL2, the filtration took about 10 minutes.
比較例１
実施例１と同じ方法で粗ジヒドロキシアセトン水溶液を
得た。Comparative Example 1 A crude dihydroxyacetone aqueous solution was obtained in the same manner as in Example 1.
この粗ジヒドロキシアセトン水溶液を、５０℃の水浴中
で攪拌しながら水分２０ ｗｔ％まで約４時間かけて減
圧濃縮し、引き続き水分１０ ｗｔ％まで７０時間かけ
て濃縮した。This crude dihydroxyacetone aqueous solution was concentrated under reduced pressure in a 50° C. water bath with stirring to a moisture content of 20 wt% over about 4 hours, and then concentrated to a moisture content of 10 wt% over a period of 70 hours.
こうして得られたジヒドロキシアセトン濃縮液２００ｉ
Ｐに対しただちにイングロ・平ノールを１６０？加えて
２０℃にて３２時間攪拌しながら晶析した。晶析液を３
０ｃＩＩＬ２の濾過面積を有する濾過装置で吸引濾過し
たところ、約５０分間で濾過した。Dihydroxyacetone concentrate 200i obtained in this way
Immediately 160 Inglo/Hiranoru against P? In addition, crystallization was performed at 20° C. with stirring for 32 hours. 3 of the crystallization solution
When suction filtration was performed using a filtration device having a filtration area of 0cIIL2, the filtration took about 50 minutes.
実施例１および比較例１と同様の方法によ）、水分２０
ｗｔ％から１０ ｗｔ％への濃縮時間を変化させた結果
を次に示す。(by the same method as in Example 1 and Comparative Example 1), moisture 20
The results of changing the concentration time from wt% to 10 wt% are shown below.
（発明の効果）
本発明の方法によシ、濃縮時間をコントロールするだけ
で濾過性の優れた晶析液が得られ、効率的にジヒドロキ
シアセトンを製造することが可能になった。(Effects of the Invention) According to the method of the present invention, a crystallized liquid with excellent filterability can be obtained simply by controlling the concentration time, making it possible to efficiently produce dihydroxyacetone.
Claims (1)
媒を加えて晶析を行う際に、濃縮液中の水分が２０ｗｔ
％以下となってから、濃縮を終了し溶媒を添加して晶析
を開始するまでの時間が５０時間を越えないようにする
事を特徴とするジヒドロキシアセトンの製造法。1. When concentrating a dihydroxyacetone aqueous solution and adding a solvent to the concentrated liquid to perform crystallization, the water content in the concentrated liquid is 20wt.
A method for producing dihydroxyacetone, characterized in that the time from when the concentration is reduced to below 50 hours until the end of concentration, addition of a solvent, and initiation of crystallization is not exceeded.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2573988A JPH082829B2 (en) | 1988-02-08 | 1988-02-08 | Method for producing dihydroxyacetone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2573988A JPH082829B2 (en) | 1988-02-08 | 1988-02-08 | Method for producing dihydroxyacetone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01203348A true JPH01203348A (en) | 1989-08-16 |
| JPH082829B2 JPH082829B2 (en) | 1996-01-17 |
Family
ID=12174190
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2573988A Expired - Fee Related JPH082829B2 (en) | 1988-02-08 | 1988-02-08 | Method for producing dihydroxyacetone |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH082829B2 (en) |
-
1988
- 1988-02-08 JP JP2573988A patent/JPH082829B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH082829B2 (en) | 1996-01-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |