A7 B7 五、發明説明（1 ) 本發明係關於由紫鉚素二醇合成所得粗製紫鉚素二醇 溶液、分離乙炔、甲醛、炔丙醇等不欲成份之方法。 由紫鉚素二醇合成所得粗製紫鉚素二酵溶液，仍含有 物理上溶化之乙炔、未反應甲醛、炔丙酵，Μ及輕餾份 和重餾份。已知利用於提塔去除乙炔，然後將粗製紫鉚 素二醇溶液引進前後串聯之二真空蒸餾塔内。在第一真 空蒸餾塔內，粗製紫鉚素二醇溶液脫除甲醛和輕餾份， 而在第二真空蒸餾塔内，分離重餾份，從塔頂取出純紫 鉚素二醇溶液（參見例如化學系統公司：紫鉚素二酵/ 四氫呋喃報告，91S15號，1993年4月，第22頁，圖Ε. Β . 1 )。由粗製紫鉚素二醇溶液分離上述不欲成份有其 必要，否則乙炔和甲醛在隨後的加氫反應器內，會增加 副產品的生成，使產品品質和產率惡化，因此降低觸媒 活性。 . 本發明之目的，在於此一次分離製程分離不欲成份。 按照本發明是如此達成：即 > 利用過熱蒸汽汽提，從 粗製紫鉚素二醇溶液分離不欲成份。 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 如今利用過熱蒸汽汽提，即可在單一塔内，從粗製紫 鉚素二醇溶液分離不欲成份。如此可得許多優點。在已 知製法所用真空蒸豳中，進行甲醛分離，釋出甲醛的粗 製紫柳素二醇溶液，留在第一真空蒸餾塔底，幾乎不含 水份。粗製紫鉚素二醇溶液經煮沸，會強化重餾份的形 成。因此，有 礙加氫的重餾份之量高到如前所述，則 必須藉另一真空蒸餾塔加Μ分離。然而，紫鉚素二醇的 -3- 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ 297公釐） 經濟、部中央標準局員工消費合作社印製 A7 _B7_五、發明説明（2 ) 頂部蒸餾，若發生粗製紫鉚素二酵溶液的自然分解，將 會導致注意不到的意外危害。蒸餾塔内臨界底部之溫度 約15〇υ。在本發明製法中，粗製紫鉚素二醇溶液的含 水量保持幾乎一定。因此，不含水的紫鉚素二醇溶液， 不像現有技術中許多製法的情形那樣煮沸。因而不致於 發生自然分解。所Μ ,粗製紫鉚素二醇溶液，加上蒸汽 提塔内停留時間較短，比加熱蒸餾處理情形為佳。 本發明及其特定實施例，參見第1圖及下表詳述之。 各成份的濃度是以莫耳％表示。 (請先閱讀背面之注意事項再填寫本頁) 線路1 線路2 線路3 塔區4 C 2 Η 2 0.03 0.00 0.00 0.01 甲醛 1.54 0.00 0.50 0.46 CH 3 0Η 1.48 0.00 0.00 0.65 甲酸 0.01 0.00 0.00 0.00 乙酸 0.02 0.00 0.00 0.01 炔丙醇 0.27 0.00 0.00 0.12 Η 2 〇 82.79 100.00 85.05 98.74 1,4-丁二醇 13.45 0.00 14.00 0.01 其餘 0.43 0.00 0.44 0.00 訂 蒸汽汽提堪Κ是由線路1引進壓力1.3巴且溫度約 105^0的祖製紫鉚素二醇溶液。塔Κ再由線路2送人壓 力1 . 3巴且溫度為1 4 0 TC的過熱蒸汽。引進的蒸汽溫度 —4 — 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ知j公釐） A7 B7 五、發明説明（3 ) 可在1 Ο 5和1 4 0 t間，而壓力則在1 . 2和1 . 5巴範圍内。經 線路3所得紫鉚素二醇溶液含稍多於約0 . 5莫耳甲醛。 為調節此殘餘甲醛量，1仟克/時的粗製紫鉚素二醇需要 約1 . 5仟克/時之蒸汽。殘餘甲醛含量可藉提高蒸汽 量，而減少到甲醛檢測限度，即1 Ο Ο P P m左右。由線路5 ，從蒸汽汽提塔K之頂部取出乙炔，而經線路6則取出 甲醛、水和炔丙醇等輕餾份。從線路3取出的紫鉚素二 醇溶液，如今可直接進行後绩的加氫（圖上未示），或光 分離重餾份，再進行加氫。 總之，本發明方法與已知方法相較，至少可節省一塔 。故過熱蒸汽汽提不但兼備已知方法的汽提和第一蒸腺 製程，而且在相當於選定參數情況下，即視進行過熱蒸 汽汽提的粗製紫鉚素二醇溶液之組成份，而免除分離重 餾份之第二蒸餾製程。 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局員工消費合作社印裝 -5- 本紙張尺度逋用中國國家標準（CNS ) A4規格（210X297公釐） A7 B7 ;:ΐ·王 五、發明説明（） 圔式概述 圖1偽用於自紫嫌素二酵溶液分離不欲成份之蒸汽汽提 塔K的示s圔。 主要元件之簡單說明 1 用於輸入粗製紫_素二酵溶液之線路 2 用於輪入水蒸汽之線路 3 用於输出已分離不欲成份之紫撕素二醇的線路 4 塔區 5 用於輸出乙炔之線路 6 用於输出甲醛、水及輕臛份之線路。 K 蒸汽汽提塔 n m ί ^^^1 m* i d^i Ik ^^^1 ^^^1 ^^^1 m In - J. J i (請先閱讀背面之注意事項再填寫本頁) 經濟部中央揉準局貝工消費合作社印裝 5*1 - 本紙張尺度逋用中國國家橾準（CNS ) A4規格（210X297公釐）A7 B7 V. Description of the invention (1) The present invention relates to a method for separating crude zirindiol diol solution obtained from zirindiol and separating undesirable components such as acetylene, formaldehyde and propargyl alcohol. The crude purple rivetin secondary enzyme solution synthesized from purple rivet diol still contains physically dissolved acetylene, unreacted formaldehyde, propargyl ferment, M and light and heavy fractions. It is known to use a lifting tower to remove acetylene, and then introduce the crude stamenol glycol solution into the second vacuum distillation tower connected in series. In the first vacuum distillation tower, the crude taxol glycol solution removes formaldehyde and light fractions, while in the second vacuum distillation column, the heavy fraction is separated, and the pure taxol glycol solution is taken from the top of the tower (see For example, Chemical Systems Corporation: Zirinase / Tetrahydrofuran Report, No. 91S15, April 1993, page 22, Figure E. Β.1). It is necessary to separate the above-mentioned undesired components from the crude purpurindiol solution, otherwise acetylene and formaldehyde will increase the production of by-products in the subsequent hydrogenation reactor, deteriorating the product quality and yield, and thus reducing the catalyst activity. The purpose of the present invention is to separate undesirable components in this one-time separation process. According to the present invention, it is achieved that: > superheated steam stripping is used to separate undesirable components from the crude violagendiol solution. Printed by the Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the precautions on the back before filling in this page). Now using superheated steam stripping, you can separate undesirable components from the crude purple rylene glycol solution in a single tower. This gives many advantages. In the known vacuum distillation method, the formaldehyde is separated, and the crude syringindiol solution releasing formaldehyde is left at the bottom of the first vacuum distillation tower and contains almost no moisture. The boiling of the crude purple diol solution will enhance the formation of heavy fractions. Therefore, the amount of heavy fractions that hinder the hydrogenation is as high as mentioned above, and it must be separated by another vacuum distillation column. However, the standard of this paper for purple rivetdiol -3- is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ 297 mm). The A7 _B7_ printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs and the Ministry of Invention (2) Top distillation, if the natural decomposition of the crude purple rivastrin solution, will lead to unexpected hazards. The temperature at the critical bottom of the distillation tower is about 15 °. In the production method of the present invention, the water content of the crude purple pigment solution is kept almost constant. Therefore, the non-aqueous solution of rhizomatindiol is not boiled as in the case of many preparation methods in the prior art. Therefore, natural decomposition does not occur. As a result, the crude violacetin diol solution plus the residence time in the steam stripper is shorter, which is better than the heating distillation treatment. The present invention and its specific embodiments are described in detail in Figure 1 and the following table. The concentration of each component is expressed in mol%. (Please read the precautions on the back before filling this page) Line 1 Line 2 Line 3 Tower Area 4 C 2 Η 2 0.03 0.00 0.00 0.01 Formaldehyde 1.54 0.00 0.50 0.46 CH 3 0Η 1.48 0.00 0.00 0.65 Formic acid 0.01 0.00 0.00 0.00 Acetic acid 0.02 0.00 0.00 0.01 propargyl alcohol 0.27 0.00 0.00 0.12 Η 2 〇82.79 100.00 85.05 98.74 1,4-butanediol 13.45 0.00 14.00 0.01 remaining 0.43 0.00 0.44 0.00 ^ 0 ancestral purple rivetin diol solution. Tower K is then fed by line 2 with superheated steam at a pressure of 1.3 bar and a temperature of 140 TC. Introduced steam temperature — 4 — This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ Known j mm) A7 B7 5. Invention description (3) can be between 1 Ο 5 and 1 4 0 t, and the pressure is In the range of 1.2 and 1.5 bar. The solution of viologendiol obtained via line 3 contains slightly more than about 0.5 mole formaldehyde. To adjust the amount of residual formaldehyde, 1 mg / h of crude violagendiol requires about 1.5 mg / h of steam. The residual formaldehyde content can be reduced to the detection limit of formaldehyde by increasing the amount of steam, which is about 1 Ο Ο P P m. From line 5, acetylene is taken from the top of the steam stripper K, and light fractions such as formaldehyde, water, and propargyl alcohol are taken out through line 6. The purple diol solution taken out from line 3 can now be directly hydrogenated afterwards (not shown in the figure), or the heavy fraction can be optically separated and then hydrogenated. In short, compared with the known method, the method of the present invention can save at least one tower. Therefore, superheated steam stripping not only has the known method of stripping and the first steam gland process, but also is equivalent to the selected parameters, that is, depending on the composition of the crude purple rivetin diol solution that is superheated steam stripped Second distillation process to separate heavy fractions. (Please read the precautions on the back before filling out this page) Printed by the Employees ’Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs -5- This paper uses the Chinese National Standard (CNS) A4 specification (210X297 mm) A7 B7;: l · Wang Wu. Description of the invention () 圔 式 Overview Figure 1 shows the pseudo-sequence of the steam stripping tower K used to separate undesirable components from the purple yeast solution. Brief description of the main components 1 Line for input of crude violet-sugar fermentation solution 2 Line for steam incorporation 3 Line for output of violactin diol with separated undesired components 4 Tower area 5 for output Acetylene line 6 is used to output formaldehyde, water and light components. K steam stripper nm ί ^^^ 1 m * id ^ i Ik ^^^ 1 ^^^ 1 ^^^ 1 m In-J. J i (please read the precautions on the back before filling this page) Economy 5 * 1 printed by Beigong Consumer Cooperative of the Central Bureau of Standardization of the Ministry-This paper uses the Chinese National Standard (CNS) A4 (210X297mm)