CN108083979B - 一种乙醇生产方法及装置 - Google Patents
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 238000004519 manufacturing process Methods 0.000 title claims description 18
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 45
- 239000000463 material Substances 0.000 claims description 21
- 238000000605 extraction Methods 0.000 claims description 17
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 14
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 13
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 10
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017816 Cu—Co Inorganic materials 0.000 description 1
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Abstract
发明涉及合成气制备乙醇中采用精馏‑膜设备进行脱水的新工艺。该工艺过程由精馏塔和蒸汽渗透透水膜组成,主要包括以下步骤:(1)合成气经过多步反应获得含乙醇和水的反应产物,在进入蒸汽渗透透水膜前,反应产物在精馏塔进行分离,最后一个精馏塔塔顶或侧线采出含水0.1~30%的乙醇蒸汽;(2)含水的乙醇蒸汽过热或经过热泵后进入膜装备,经过膜组件分离,膜出口(正压侧)为含水0.01~1的乙醇成品。
Description
技术领域
本发明涉及一种乙醇生产方法及装置,特别涉及一种合成气制备乙醇的脱水工艺和装置。
背景技术
乙醇在国防化工、医疗卫生、食品工业、工农业生产中都有广泛的用途。乙醇生产方法有生物发酵法和化学合成法。其中化学合成法中合成气制备乙醇生产技术已成熟,生产成本显著低于粮食路线,具有较强的竞争力和广阔发展前景。合成气生产乙醇有三种,一是合成气直接制乙醇;二是合成气生物法制乙醇;三是合成气经醋酸加氢制乙醇。无论哪种乙醇生产方法,均得到含水的乙醇。由于乙醇和水存在共沸点,传统方法无法直接得到无水乙醇。目前工业无水乙醇的生产主要采取恒沸精馏、萃取精馏和吸附分离等方法,这些传统的乙醇脱水方式都存在过程复杂、能耗高和污染严重等问题。
膜脱水技术利用被分离液体混合物中各组分在膜中溶解(吸附)与扩散速率不同而实现分离,是一种新型分离技术,具有高效节能、过程易于控制、操作方便、便于放大和产业化的优点。其突出的优点是分离过程不受组分气液平衡的限制,能够以低能耗实现精馏等传统方法难以完成的任务,如共沸、近沸混合物的分离。
发明内容
本发明的目的是提供一种合成气制备乙醇的脱水工艺,采用精馏-蒸汽渗透透水膜设备耦合技术,将传统工艺与新型分离技术耦合,不受共沸限制,不需添加第三组分,是一种高效节能环保的分离技术。
一种乙醇生产方法,包括如下步骤:
第1步,通过合成气生产出含有乙醇的反应物料;
第2步,将第1步中得到的反应物料进行精馏分离,在最后一个精馏塔的塔顶或侧线采出含有乙醇的蒸汽;
第3步,将第2步得到的含有乙醇的蒸汽送入蒸汽渗透膜中进行脱水,得到乙醇产品。
在一个实施方式中,所述的第2步中,含有乙醇的蒸汽中含水0.1~30wt%。
在一个实施方式中,所述的第3步中,乙醇产品中含水0.01~1wt%。
在一个实施方式中,所述的第3步中,蒸汽渗透膜的料液侧的操作压力为100~600kPa,操作温度为进料的饱和蒸汽压对应的温度过热10~20℃。
在一个实施方式中,所述的第3步中,蒸汽渗透膜的选自分子筛膜、二氧化硅膜或PVA膜,优选分子筛膜。
在一个实施方式中,所述的第1步,通过合成气生产出含有乙醇的反应物料选自合成气直接制乙醇、合成气生物法制乙醇、合成气经醋酸加氢制乙醇、合成气经醋酸酯加氢制乙醇中的一种。
一种乙醇生产装置,包括:
精馏塔,用于对通过合成气生产出含有乙醇的反应物料进行精馏分离;
塔顶冷凝器,连接于精馏塔的侧线或者塔顶,对于对采出的蒸汽进行部分冷凝回流至精馏塔的塔顶;
蒸汽渗透透水膜设备,连接于塔顶冷凝器的蒸汽出料口,用于对蒸汽物料进行脱水;
蒸汽渗透透水膜设备和塔顶冷凝器之间通过过热器和/或热泵连接;
蒸汽渗透透水膜设备的物料侧的出口与精馏塔的物料进口之间通过第一换热器进行换热连接;
精馏塔的塔底物料出口与精馏塔的物料进口之间通过第二换热器进行换热连接;
精馏塔的塔底还设置再沸器。
所述的蒸汽渗透透水膜设备中的蒸汽渗透膜的选自分子筛膜、二氧化硅膜或PVA膜,优选分子筛膜。
还包括加盐萃取精馏塔,加盐萃取精馏塔的塔顶出口连接至精馏塔的原料进口,用于去除原料中的乙酸甲酯。
有益效果
1、本发明采用精馏-蒸汽渗透透水膜设备耦合技术进行脱水,不受共沸限制,不需添加第三组分,是一种高效环保的分离技术。2、本发明精馏塔塔顶或侧线气相直接进入膜设备,与传统工艺相比,节能20%以上。
附图说明
图1是实施例1中采用的合成气制备乙醇的脱水工艺的流程示意图。
图2是实施例2中采用的合成气制备乙醇的脱水工艺的流程示意图;图3是实施例4中采用的合成气制备乙醇的脱水工艺的流程示意图。
其中,1、第一换热器;2、第一换热器;3、精馏塔;4、再沸器;5、塔顶冷凝器;6、过热器; 7、蒸汽渗透透水膜设备;8、热泵;9、加盐萃取精馏塔。
实施方式
实施例
如图1所示,以合成气(含65wt%H2、30wt%CO)在Cu-Co催化剂体系下直接合成乙醇,反应产物经过不凝气分离后,得到含有62wt%乙醇、20wt%甲醇、13wt%水的蒸汽,送入精馏塔中进行精馏,精馏塔内压力300kPa,塔底温度86℃,塔顶温度74℃,从塔顶采出甲醇,从侧线采出乙醇(含水8wt%),将侧线采出的物料经热交换、过热之后,送入蒸汽渗透膜中进行脱水,蒸汽渗透膜采用的是NaA分子筛膜,料液侧温度114℃,料液侧绝压120kPa,渗透侧绝压1000Pa,蒸汽渗透膜平均水通量0.98kg/m2·h,渗透侧得到含水0.5wt%的乙醇产品。
实施例
如图2所示,以合成气(含65wt% H2、30wt%CO)中的CO作为碳源,采用发酵法制乙醇(CN105755058A),发酵液经过滤除菌体后,送入精馏塔中进行精馏,精馏塔内压力300kPa,塔底温度88℃,塔顶温度78℃,从塔顶采出乙醇(含水16wt%),将侧线采出的物料经热交换、过热之后,送入蒸汽渗透膜中进行脱水,蒸汽渗透膜采用的是NaA分子筛膜,料液侧温度110℃,料液侧绝压150kPa,渗透侧绝压1500Pa,蒸汽渗透膜平均水通量0.98kg/m2·h,渗透侧得到含水0.8wt%的乙醇产品。
实施例
如图2所示,以合成气(含65wt% H2、30wt%CO)反应生成二甲醚(CH3OCH3),二甲醚羰基化生成乙酸甲酯,乙酸甲酯在催化剂的作用下加氢制得甲醇和乙醇(CN104710282A),含有54wt%甲醇、34wt%乙醇、9wt%乙酸甲酯的产物送入精馏塔中进行精馏,精馏塔内压力350kPa,塔底温度88℃,塔顶温度76℃,从塔顶采出甲醇,从侧线采出乙醇(含水1.2wt%),将侧线采出的物料经热交换、过热之后,送入蒸汽渗透膜中进行脱水,蒸汽渗透膜采用的是NaA分子筛膜,料液侧温度105℃,料液侧绝压80kPa,渗透侧绝压500Pa,蒸汽渗透膜平均水通量0.93kg/m2·h,渗透侧得到含水0.08wt%的乙醇产品。
实施例
如图3所示,以合成气(含65wt% H2、30wt%CO)反应生成二甲醚(CH3OCH3),二甲醚羰基化生成乙酸甲酯,乙酸甲酯在催化剂的作用下加氢制得甲醇和乙醇(CN104710282A),含有54wt%甲醇、34wt%乙醇、9wt%乙酸甲酯的产物采用加盐萃取精馏方法分离乙酸甲酯,将上述的反应产物送入加盐萃取精馏塔9中,加盐萃取精馏塔9塔顶设有回流口,回流的萃取剂为含有0.1g/ml的醋酸钾的水反应产物与萃取剂的采的进料质量比为1:1,加盐萃取精馏塔内为常压,塔底温度87℃,塔顶温度73℃,塔顶蒸汽采出口经过冷凝器后与精馏塔3的进口连接,从加盐萃取精馏塔9塔顶蒸汽中获得含55wt%甲醇、32wt%乙醇、11wt%水的除酯后的醇类产物,再将醇类产物送入精馏塔3中进行精馏,精馏塔内压力350kPa,塔底温度88℃,塔顶温度76℃,从塔顶采出甲醇,从侧线采出乙醇(含水1.6wt%),将侧线采出的物料经热交换、过热之后,送入蒸汽渗透膜中进行脱水,蒸汽渗透膜采用的是NaA分子筛膜,料液侧温度105℃,料液侧绝压80kPa,渗透侧绝压500Pa,蒸汽渗透膜平均水通量1.06kg/m2·h,渗透侧得到含水0.08wt%的乙醇产品。本实施例中,采用了加盐萃取精馏分离出甲醇和乙醇中的乙酸甲酯,而将夹带出的萃取剂放在甲醇、乙醇的精馏过程中进行同步分离,实现了通过精馏同时去除产物中夹带的萃取剂,同时又实现了精馏过程中的甲醇与乙醇的分离,再通过蒸汽渗透膜对含水乙醇进行脱水,也提高了蒸汽渗透过程的水通量。
Claims (4)
1.一种乙醇生产方法,其特征在于,采用如下所示的乙醇生产装置:
精馏塔(3),用于对通过合成气生产出含有乙醇的反应物料进行精馏分离;
塔顶冷凝器(5),连接于精馏塔(3)的侧线或者塔顶,用于对采出的蒸汽进行部分冷凝回流至精馏塔(3)的塔顶;
蒸汽渗透透水膜设备(7),连接于塔顶冷凝器(5)的蒸汽出料口,用于对蒸汽物料进行脱水;
蒸汽渗透透水膜设备(7)和塔顶冷凝器(5)之间通过过热器(6)和/或热泵(8)连接;
蒸汽渗透透水膜设备(7)的物料侧的出口与精馏塔(3)的物料进口之间通过第一换热器(1)进行换热连接;
精馏塔(3)的塔底物料出口与精馏塔(3)的物料进口之间通过第二换热器(2)进行换热连接;
精馏塔(3)的塔底还设置再沸器(4);
所述的蒸汽渗透透水膜设备(7)中的蒸汽渗透膜的选自NaA分子筛膜;
还包括加盐萃取精馏塔(9),加盐萃取精馏塔(9)的塔顶出口连接至精馏塔(3)的原料进口,用于去除原料中的乙酸甲酯;
所述的乙醇生产方法包括如下步骤:
第1步,以合成气反应生成二甲醚,二甲醚羰基化生成乙酸甲酯,乙酸甲酯在催化剂的作用下加氢制得甲醇和乙醇;采用加盐萃取精馏方法分离乙酸甲酯,将加氢制得甲醇和乙醇反应产物送入加盐萃取精馏塔(9)中,加盐萃取精馏塔(9)塔顶设有回流口,回流的萃取剂为含有0.1g/ml的醋酸钾的水,反应产物与萃取剂的进料质量比为1:1,加盐萃取精馏塔内为常压,塔底温度87℃,塔顶温度73℃;塔顶蒸汽采出口经过冷凝器后与精馏塔(3)的进口连接,从加盐萃取精馏塔(9)塔顶蒸汽中获得除乙酸甲酯后的醇类产物;
第2步,将第1步中得到的醇类产物进行精馏分离,在精馏塔的塔顶或侧线采出含有乙醇的蒸汽;
第3步,将第2步得到的含有乙醇的蒸汽送入蒸汽渗透膜中进行脱水,得到乙醇产品;
合成气中含有65wt%H2和30wt%CO。
2.根据权利要求1所述的乙醇生产方法,其特征在于,所述的第2步中,含有乙醇的蒸汽中含水0.1~30wt%。
3.根据权利要求1所述的乙醇生产方法,其特征在于,所述的第3步中,乙醇产品中含水0.01~1wt%。
4.根据权利要求1所述的乙醇生产方法,其特征在于,所述的第3步中,蒸汽渗透膜的料液侧的操作压力为100~600 kPa,操作温度为进料的饱和蒸汽压对应的温度过热10~20℃。
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