CN113461601B - 3-甲基吡啶废液的处理方法 - Google Patents

3-甲基吡啶废液的处理方法 Download PDF

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CN113461601B
CN113461601B CN202110705691.5A CN202110705691A CN113461601B CN 113461601 B CN113461601 B CN 113461601B CN 202110705691 A CN202110705691 A CN 202110705691A CN 113461601 B CN113461601 B CN 113461601B
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evaporator
methylpyridine
waste liquid
tower
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CN113461601A (zh
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陈建伟
邵峰
梁倩
张群辉
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Xingke High Purity Solvents Shanghai Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D213/00Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D213/00Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/06Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
    • C07D213/127Preparation from compounds containing pyridine rings

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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
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Abstract

本发明涉及3‑甲基吡啶废液的处理方法,依次经过以下步骤处理:进入蒸发器蒸发分离,蒸发器的操作条件为:压力10‑101kPa,温度70‑170℃,蒸发器蒸出的蒸汽进入第一精馏塔精馏,第一精馏塔的操作条件为压力10‑101kPa,塔顶温度10‑50℃,塔釜温度50‑150℃,第一精馏塔的塔釜物料进入第二精馏塔精馏,第二精馏塔的操作条件为压力20‑101kPa,塔顶温度40‑85℃,塔釜温度90‑150℃。本发明的处理方法能够从制药工业的含有3‑甲基吡啶的废液中分离提纯得到高纯度的3‑甲基吡啶产品,处理过程中不会产生腐蚀性高沸物对于后续设备造成腐蚀和堵塞,具有处理效果好,产品纯度高的优点。

Description

3-甲基吡啶废液的处理方法
技术领域
本发明涉及3-甲基吡啶废液的处理方法。
背景技术
在制药工业中产生的3-甲基吡啶废液中,含有较多的3-甲基吡啶,以及含有高沸物、乙腈、二氯甲烷和水等杂质,3-甲基吡啶是重要的中间体,需要对于废液中的3-甲基吡啶进行回收。
发明内容
本发明的主要目的在于从3-甲基吡啶废液中处理回收3-甲基吡啶产品。
为了实现上述目的,本发明提供一种3-甲基吡啶废液的处理方法,依次经过以下步骤处理:
进入蒸发器蒸发分离,蒸发器的操作条件为:压力10-101kPa,温度70-170℃,
蒸发器蒸出的蒸汽进入第一精馏塔精馏,第一精馏塔的操作条件为压力10-101kPa,塔顶温度10-50℃,塔釜温度50-150℃,
第一精馏塔的塔釜物料进入第二精馏塔精馏,第二精馏塔的操作条件为压力20-101kPa,塔顶温度40-85℃,塔釜温度90-150℃。
在一些实施例中,蒸发器蒸出的蒸汽进入除沫器中除沫后,再进入所述的第一精馏塔。
在一些实施例中,所述的除沫器中设置有挡板、丝网、填料中的一种或多种。
在一些实施例中,所述的蒸发器采用夹套蒸发器、外置蒸发器、膜式蒸发器中的一种或多种。
在一些实施例中,所述的膜式蒸发器采用刮膜式蒸发器。
在一些实施例中,所述的高沸物包括高粘度有机物和腐蚀性盐中的一种或两种。
本发明的处理方法能够从制药工业的含有3-甲基吡啶的废液中分离提纯得到高纯度的3-甲基吡啶产品,处理过程中不会产生腐蚀性高沸物对于后续设备造成腐蚀和堵塞,具有处理效果好,产品纯度高的优点。
附图说明
图1为3-甲基吡啶提纯的流程示意图。
具体实施方式
本发明对于3-甲基吡啶废液的处理方法,依次经过以下步骤处理:
进入蒸发器蒸发分离,蒸发器的操作条件为:压力10-101kPa,温度70-170℃,通过该步骤能够先将废液中存在的高粘度物质、具有腐蚀性的磺酸钠、氯化钠等盐分形成蒸残,从而在蒸发器中得到去除,
蒸发器蒸出的蒸汽进入第一精馏塔精馏,第一精馏塔的操作条件为压力10-101kPa,塔顶温度10-50℃,塔釜温度50-150℃,第一精馏塔在该操作条件下,能够初步的去除废液中的二氯甲烷,以及初步去除乙腈和水。
第一精馏塔的塔釜物料进入第二精馏塔精馏,第二精馏塔的操作条件为压力20-101kPa,塔顶温度40-85℃,塔釜温度90-150℃。第二精馏塔在该操作条件下,能够进一步去除废液中的已经和水,从而得到3-甲基吡啶产品。
下面结合附图与实施例对本发明作进一步说明。本实施例中的含量除非特别标注,均为重量百分比含量。
本实施例所处理的3-甲基吡啶废水中具有占总重量61.4%的3-甲基吡啶、8.8%的乙腈、0.8%的水26.3%的二氯甲烷和2.7%的高沸物,高沸物中包括了腐蚀性盐和高粘性有机物,腐蚀性盐包括了如磺酸钠、氯化钠等盐分。
将3-甲基吡啶废液送入蒸发器中进行蒸发,3-甲基吡啶废液的流量为2000kg/h,蒸发器的操作温度为常压,160℃,在蒸发器的顶部,蒸出的废液蒸汽中含有61.0%的3-甲基吡啶、9.8%的乙腈、0.9%的水以及28.3%的二氯甲烷,流量为1847kg/h,,蒸发器的蒸残中含有66.5%的3-甲基吡啶、1.8%的乙腈、0.13%的水、2.0%的二氯甲烷以及29.57%的高沸物,流量为153kg/h,蒸残可排出作为危废处理。蒸发器可选夹套式、外置式及膜式蒸发器,优选膜式,特别是刮膜式蒸发器。蒸发器优选选用钛材、锆材。
废液蒸汽先通过除沫器进行除没,以防止高沸物夹带至废液蒸汽中。除沫器中可以配置挡板、死亡或填料增加除沫效果,除沫器可选择管道除沫器。其中采用的填料优选规整填料M252、M152。
废液蒸汽经过除沫器除沫后进入第一精馏塔中进行初步的精馏分离,第一精馏塔的操作条件为:常压、塔顶温度38℃、塔釜温度121℃,塔顶出料中含有0.26%的乙腈、2.74%的水和97.0%的二氯甲烷,流量为536kg/h,塔釜出料中含有86.7%的3-甲基吡啶、13.1%的乙腈和0.2%的水,流量为1311kg/h。
第一精馏塔的塔釜出料进入第二精馏塔中进行3-甲基吡啶的精制,塔顶出料为98.5%的乙腈和1.49%的水,流量为177kg/h,塔釜出料为含量大于99.8%的3-甲基吡啶和小于0.2%的乙腈,流量为1134kg/h。第二精馏塔的塔釜出料可直接作为3-甲基吡啶的产品。
在上述第一精馏塔和第二精馏塔的精馏过程中,第一精馏塔和第二精馏塔的塔顶出料均可被用作除沫器的回流,用于与废液蒸汽逆向接触进行除沫,图1为第一精馏塔塔顶出料部分回流至除沫器的情形,在一些实施例中,也可采用第二精馏塔塔顶出料用作除沫器回流,或者同时采用部分第一精馏塔和第二精馏塔的塔顶出料作为除沫器回流。
蒸发器产生的蒸汽经过配置挡板、丝网或填料等除沫器管线之后,在冷凝器中进行冷凝。部分冷凝液作为管线除沫器回流,部分冷凝液作为产品,可以通过已知工艺分离回收乙腈、甲基吡啶,回收设备材质选用常规304等不锈钢。管线中除沫装置优选规整填料M252、M152,材质优先316L。
本发明中的实施例仅用于对本发明进行说明,并不构成对权利要求范围的限制,本领域内技术人员可以想到的其他实质上等同的替代,均在本发明保护范围内。

Claims (8)

1.一种3-甲基吡啶废液的处理方法,其特征在于依次经过以下步骤处理:
进入蒸发器蒸发分离,蒸发器的操作条件为:压力10-101kPa,温度70-170℃,通过该步骤能够先将废液中存在的高粘度物质、具有腐蚀性的磺酸钠、氯化钠形成蒸残,从而在蒸发器中得到去除,
蒸发器蒸出的蒸汽进入第一精馏塔精馏,第一精馏塔的操作条件为压力10-101kPa,塔顶温度10-50℃,塔釜温度50-150℃,第一精馏塔在该操作条件下,能够初步的去除废液中的二氯甲烷,以及初步去除乙腈和水,
第一精馏塔的塔釜物料进入第二精馏塔精馏,第二精馏塔的操作条件为压力20-101kPa,塔顶温度40-85℃,塔釜温度90-150℃,第二精馏塔在该操作条件下,能够进一步去除废液中的乙腈 和水,从而得到3-甲基吡啶产品。
2.如权利要求1所述的3-甲基吡啶废液的处理方法,其特征在于蒸发器蒸出的蒸汽进入除沫器中除沫后,再进入所述的第一精馏塔。
3.如权利要求2所述的3-甲基吡啶废液的处理方法,其特征在于所述的除沫器中设置有挡板、丝网、填料中的一种或多种。
4.如权利要求1所述的3-甲基吡啶废液的处理方法,其特征在于所述的蒸发器采用夹套蒸发器、外置蒸发器、膜式蒸发器中的一种或多种。
5.如权利要求4所述的3-甲基吡啶废液的处理方法,其特征在于所述的膜式蒸发器采用刮膜式蒸发器。
6.如权利要求1所述的3-甲基吡啶废液的处理方法,其特征在于蒸发器的操作条件为:常压,160℃。
7.如权利要求1所述的3-甲基吡啶废液的处理方法,其特征在于第一精馏塔的操作条件为:常压,塔顶温度38℃,塔釜温度121℃。
8.如权利要求1所述的3-甲基吡啶废液的处理方法,其特征在于第二精馏塔的操作条件为:常压,塔顶温度82℃,塔釜温度145℃。
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