CN1075049C - 从丁炔二醇溶液中分离不希望的组分的方法 - Google Patents

从丁炔二醇溶液中分离不希望的组分的方法

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CN1075049C
CN1075049C CN95116690A CN95116690A CN1075049C CN 1075049 C CN1075049 C CN 1075049C CN 95116690 A CN95116690 A CN 95116690A CN 95116690 A CN95116690 A CN 95116690A CN 1075049 C CN1075049 C CN 1075049C
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cymogene
solution
formaldehyde
alkyne diol
butindio
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CN1123788A (zh
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卡尔-海因茨·霍夫曼
尼科尔·舍德尔
弗兰克·维泽纳尔
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SK Corp
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C33/00—Unsaturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C33/04—Acyclic alcohols with carbon-to-carbon triple bonds
    • C07C33/042—Acyclic alcohols with carbon-to-carbon triple bonds with only one triple bond
    • C07C33/044—Alkynediols
    • C07C33/046—Butynediols
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

从由丁炔二醇合成获得的粗丁炔二醇溶液中分离不希望的组分的方法，所述不希望的组分象例如乙炔，甲醛，炔丙醇等，其中借助热蒸汽汽提从粗丁炔二醇溶液中分离出不希望的组分。在此情况下，供给热蒸汽汽提的水蒸汽所具有的温度在105和140℃之间、压力在1.2和1.5巴之间。

Description

从丁炔二醇溶液中分离不希望的组分的方法
本发明涉及从由丁炔二醇合成获得的粗丁炔二醇溶液中分离不希望的组分，象例如乙炔、甲醛、炔丙醇等的方法。
由丁炔二醇合成获得的粗丁炔二醇溶液还含有物理溶解的乙炔，不反应的甲醛，炔丙醇以及其它低沸点和高沸点组分。众所周知，借助汽提塔分离出乙炔和接着将粗丁炔二醇溶液输入两个连续设置的真空蒸馏塔。在第一真空蒸馏塔中，从粗丁炔二醇溶液中清除甲醛和低沸点组分，而在第二真空蒸馏塔中分离高沸点组分，并经顶部获得纯丁炔二醇溶液(参见例如，Chem System Inc., Butanediol/Tetrahydrofuran-Report,Nr.91S15,1993年4月，第22页，图2,B,1)。从粗丁炔二醇溶液中分离上述不希望的组分是十分重要的，否则在并联的氢化反应器中乙炔和甲醛将导致提高副产品生成并因此降低产品质量和产率。此外还会降低催化剂的活性。
本发明的目的是以一步独特的分离工艺分离这些不希望的组分。
按照本发明，如此达到该目的，即借助热蒸汽汽提从粗丁炔二醇溶液中分离出这些不希望的组分。
现已能借助热蒸汽汽提在一独特的塔中从粗丁炔二醇溶液中分离出这些不希望的组分，由此产生许多优点。在所用的已知方法中，真空蒸馏分离甲醛将导致在第一真空蒸馏塔槽中的清除甲醛的粗丁炔二醇溶液几乎不含水。通过粗丁炔二醇溶液的煮沸增加了高沸点组分的生成。由于在氢化中起干扰作用的高沸点组分的成份太高，如上面所述，而必须在另一真空蒸馏塔中分离出这些组分。然而，经顶部蒸馏丁炔二醇导致不小的事故危险，如果粗丁炔二醇出现自发的分解，那么该事故危险将发生。在这种情况下，蒸馏塔中的临界槽温度度为大约150℃。与此相反，在本发明的方法中粗丁炔二醇溶液的水含量几乎保持恒量。因此不会象现有技术中许多方法那样出现无水丁炔二醇溶液的煮沸。因此也不会出现自发分解。而且，由于在水蒸汽汽提塔中很短的停留时间，象热蒸馏那样粗丁炔二醇溶液经受精心的处理。
借助图1及下述表更进一步说明本发明及特定的实施例。在此情况下以Mol％给出各组分的浓度。
表1
    管路1    管路2  管路3  塔范围4
C2H2甲醛CH3OH甲酸乙酸炔丙醇H2O1,4-丁炔二醇其他组分     0.031.541.480.010.020.2782.7913.450.43     0.000.000.000.000.000.00100,000.000.00  0.000.500.000.000.000.0085.0514.000.44  0.010.460.650.000.010.1298.740.010.00
经管路1用1.3巴压力和约105℃温度将粗丁炔二醇溶液送入水蒸汽汽提塔K。此外，经管路2向塔K供应压力为1.3巴和温度为140℃的过热水蒸汽，供给的水蒸汽温度可为105至140℃，而压力优选在1.2和1.5巴之间的范围内。经管路3获取的丁炔二醇溶液仅含有最多约0.5Mol％甲醛。为了调整剩余甲醛量，对于1Kg/h粗丁炔二醇溶液需用约1.5Kg/h水蒸汽。可通过高蒸汽量降低剩余甲醛量至甲醛检测极限，也即大约至100ppm范围。经管路5在水蒸汽汽提塔K的顶部抽出乙炔，而经管路6抽出甲醛，水，及低沸点组分，象例如炔丙醇。经管路3获取的丁炔二醇溶液从现在起或是直接送去并联的氢化(未示出)或是先分离高沸点组分和接着送去氢化。
总而言之，可以断定用本发明的方法可以比已知方法节省至少一个塔或柱。因此，热蒸汽汽提不仅结合了已知方法的汽提工序及第一蒸馏工序，而且，在相应选择的参数或取决于进行热蒸汽汽提的粗丁炔二醇溶液的组成的情况下，可以放弃用于分离高沸点组分的第二蒸馏工序。

Claims (2)

1、从由丁炔二醇合成获得的粗丁炔二醇溶液中分离不希望的组分的方法，其特征在于，借助温度在105和140℃之间、压力在1.2和1.5巴之间热蒸汽汽提，从粗丁炔二醇溶液中分离出不希望的组分。
2、如权利要求1所述的方法，其特征在于，所述的不希望的组分包括乙炔、甲醛、炔丙醇中的一种或多种。
CN95116690A 1994-08-24 1995-08-24 从丁炔二醇溶液中分离不希望的组分的方法 Expired - Fee Related CN1075049C (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4430057A DE4430057C2 (de) 1994-08-24 1994-08-24 Verfahren zum Abtrennen unerwünschter Bestandteile aus einer Butindiollösung
DEP4430057.3 1994-08-24

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CN1123788A CN1123788A (zh) 1996-06-05
CN1075049C true CN1075049C (zh) 2001-11-21

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DE102005042185A1 (de) * 2005-09-06 2007-03-08 Basf Ag Verfahren zur Abtrennung von polymeren Nebenprodukten aus 1,4-Butindiol

Citations (1)

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US3154589A (en) * 1960-06-27 1964-10-27 Allied Chem Process for butynediol

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US4371723A (en) * 1980-04-16 1983-02-01 Gaf Corporation Process of producing a distilled butanediol product of high quality in high yield
DE3114153A1 (de) * 1981-04-08 1982-10-28 Gaf-Hüls Chemie GmbH, 4370 Marl Verfhren zur gefahrlosen destillation von zur spontanen zersetzung neigenden verbindungen
DE3732955A1 (de) * 1987-09-30 1989-04-13 Basf Ag Verfahren zur entfernung von formaldehyd aus waessrigen loesungen von 2-butindiol-1,4
DE4120446A1 (de) * 1991-06-20 1992-12-24 Linde Ag Verfahren und vorrichtung zur synthese von butindiol

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
US3154589A (en) * 1960-06-27 1964-10-27 Allied Chem Process for butynediol

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TW303355B (zh) 1997-04-21
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KR100368736B1 (ko) 2003-05-23
CN1123788A (zh) 1996-06-05
DE4430057A1 (de) 1996-02-29

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