JP5966230B1

JP5966230B1 - Production method of cyclic polymerization L-lactic acid.

Info

Publication number: JP5966230B1
Application number: JP2015139187A
Authority: JP
Inventors: 中村　等; 等中村; 進杉木
Original assignee: SCRUM CO. LTD.
Current assignee: SCRUM CO. LTD.
Priority date: 2015-06-25
Filing date: 2015-06-25
Publication date: 2016-08-10
Anticipated expiration: 2035-06-25
Also published as: JP2017008279A

Abstract

【課題】本発明は、Ｌ−乳酸ｐＨ＝１の強酸を縮合重合により環状重合Ｌ−乳酸ｐＨ＝７の分子構造に生成させる。【解決手段】Ｌ−乳酸液体を容器に投入し加熱と減圧と圧力の条件下において窒素ガスを注入しＬ−乳酸の分子内脱水反応を行い発生した化合物、水素、酸素、炭素、窒素、を排出させる事により環状重合Ｌ−乳酸液を生じる。【選択図】図１The present invention generates a strong acid having L-lactic acid pH = 1 into a molecular structure having cyclic polymerization L-lactic acid pH = 7 by condensation polymerization. An L-lactic acid liquid is charged into a container, and nitrogen gas is injected under conditions of heating, decompression, and pressure, and an intramolecular dehydration reaction of L-lactic acid is performed. Hydrogen, oxygen, carbon, and nitrogen are generated. By discharging, a cyclic polymerization L-lactic acid solution is produced. [Selection] Figure 1

Description

本発明は、Ｌ−乳酸を環状重合Ｌ−乳酸に生成させる。 In the present invention, L-lactic acid is produced into cyclic polymerized L-lactic acid.

通常のＬ−乳酸は強酸ｐＨ１であり脱水重合を行なう事で分子構造の変化により環状重合Ｌ−乳酸ｐＨ７に生成させる。 Ordinary L-lactic acid has a strong acid pH of 1 and is formed into cyclic polymerized L-lactic acid pH 7 by dehydrating polymerization to change the molecular structure.

特開２００４−１５５６７０号JP 2004-155670 A

Ｌ−乳酸液を環状重合Ｌ−乳酸に生成する。 An L-lactic acid solution is produced into cyclic polymerized L-lactic acid.

Ｌ−乳酸液を加熱、（減圧と圧力）を交互に使い脱水縮合を繰返し発生した化合物を窒素ガスで排出させ、縮合で得られた低分子の環状重合Ｌ−乳酸である。 A low molecular weight cyclic polymerized L-lactic acid obtained by condensation by heating an L-lactic acid solution and exhausting a compound in which dehydration and condensation are repeatedly generated by alternately using (depressurization and pressure) with nitrogen gas.

環状重合Ｌ−乳酸製造装置の正面図を示す。The front view of a cyclic polymerization L-lactic acid manufacturing apparatus is shown. 同装置の平面図を示す。The top view of the apparatus is shown. 同装置の左側面図を示す。The left view of the apparatus is shown.

１球形容器本体
２マントルヒーター
３Ｌ−乳酸挿入口
４温度計挿入口
５窒素ガス直噴ノズル挿入口
６環状重合Ｌ−乳酸取出口
７排気口
８排気口
９蒸留水貯留部
１０蒸留水取出口
１１蒸留塔
１２冷却水入口
１３冷却水出口
１４吸出口DESCRIPTION OF SYMBOLS 1 Spherical container body 2 Mantle heater 3 L-lactic acid insertion port 4 Thermometer insertion port 5 Nitrogen gas direct injection nozzle insertion port 6 Cyclic polymerization L-lactic acid outlet 7 Exhaust port 8 Exhaust port 9 Distilled water storage part 10 Distilled water outlet 11 Distillation tower 12 Cooling water inlet 13 Cooling water outlet 14 Suction outlet

Claims

（１）〜（３）の工程による環状重合Ｌ−乳酸の製造方法。
（１）第１工程：球形容器本体にＬ‐乳酸液を加熱させ、温度８０℃から１３０℃まで上昇させ気圧７６０ｍｍＨｇから気圧−６７５ｍｍＨｇまで減圧し、窒素ガスを球形容器内Ｌ‐乳酸液中に注入撹拌しながら気圧を調整し、Ｌ‐乳酸に含まれている副生化合物を除去しながら加熱と減圧及び窒素ガスで排出させる。
（２）第２工程：球形容器内Ｌ‐乳酸液を加熱させ温度１３０℃から１６０℃の間で窒素ガスの注入量を調整し、気圧を上下させ気圧−６７５ｍｍＨｇから気圧−２２５ｍｍＨｇに上げて重合反応させ球形容器内Ｌ‐乳酸の脱水縮合を行ない、発生する副生化合物を窒素ガスで排出させ、球形容器内Ｌ‐乳酸液を加熱させ温度１３０℃から１６０℃まで上昇させながら気圧を上下数回繰り返しＬ‐乳酸の重合反応を行う。
（３）第３工程：球形容器内Ｌ‐乳酸液を加熱しながら温度１６０℃から１９０℃の間で窒素ガスの注入量を調整し気圧‐９７５ｍｍＨｇピーク時まで減圧し、窒素ガスを球形容器内Ｌ‐乳酸液中に注入しながら加熱と減圧でＬ‐乳酸の脱水縮合を行ない、発生する化合物を窒素ガスで排出させながら温度１９０℃ピーク時を保ち窒素ガスの注入量を調整し気圧−２２５ｍｍＨｇに上げ重合反応を行い環状重合体の構造を安定、生成させる。(1) The manufacturing method of cyclic polymerization L-lactic acid by the process of (3).
(1) First step: The L-lactic acid solution is heated in the spherical container body, the temperature is increased from 80 ° C. to 130 ° C., the pressure is reduced from 760 mmHg to -675 mmHg, and nitrogen gas is introduced into the L-lactic acid solution in the spherical container. The pressure is adjusted while stirring with injection, and the mixture is discharged with heating, reduced pressure and nitrogen gas while removing by-product compounds contained in L-lactic acid.
(2) Second step: The L-lactic acid solution in the spherical container is heated to adjust the injection amount of nitrogen gas between 130 ° C. and 160 ° C., and the pressure is raised and lowered to raise the pressure from −675 mmHg to atmospheric pressure −225 mmHg. The reaction is carried out to dehydrate and condense L-lactic acid in the spherical container, the generated by-product compound is discharged with nitrogen gas, and the L-lactic acid solution in the spherical container is heated to raise the temperature from 130 ° C. to 160 ° C. The polymerization reaction of L-lactic acid is repeated repeatedly.
(3) Third step: While heating the L-lactic acid solution in the spherical container, the injection amount of nitrogen gas is adjusted between 160 ° C. and 190 ° C., and the pressure is reduced to the atmospheric pressure-975 mmHg peak, and nitrogen gas is stored in the spherical container. While dehydrating and condensing L-lactic acid by heating and decompression while injecting into L-lactic acid solution, adjusting the injection amount of nitrogen gas while keeping the temperature at 190 ° C peak while discharging the generated compound with nitrogen gas, and adjusting the injection pressure of nitrogen gas The structure of the cyclic polymer is stabilized and formed by conducting a polymerization reaction.

球形容器内Ｌ‐乳酸液中に窒素ガスを注入しＬ‐乳酸の沸点１１８℃〜１２２℃を超える温度で加熱、減圧と気圧を交互に使い脱水縮合を繰返し連続して行い、最高温度１９０℃ピーク時まで上昇、気圧７６０ｍｍＨｇから気圧−９７５ｍｍＨｇピーク時減圧調整しつつ分子内脱水縮合の反応で合成する製造方法。 Nitrogen gas is injected into the L-lactic acid solution in the spherical container and heated at a temperature exceeding the boiling point of 118-122 ° C of L-lactic acid. A production method in which the pressure is increased up to the peak, and the pressure is adjusted at a pressure of 760 mmHg to a pressure of -975 mmHg, and the pressure is adjusted at the peak to adjust the dehydration condensation within the molecule.