CN104926675A - 低浓度二甲基乙酰胺的回收工艺 - Google Patents
低浓度二甲基乙酰胺的回收工艺 Download PDFInfo
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- CN104926675A CN104926675A CN201510254388.2A CN201510254388A CN104926675A CN 104926675 A CN104926675 A CN 104926675A CN 201510254388 A CN201510254388 A CN 201510254388A CN 104926675 A CN104926675 A CN 104926675A
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N DMA Chemical compound 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CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 238000011084 recovery Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000011552 falling film Substances 0.000 claims abstract description 23
- 238000009834 vaporization Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 32
- 239000006200 vaporizer Substances 0.000 claims description 28
- 238000000605 extraction Methods 0.000 claims description 25
- 239000012530 fluid Substances 0.000 claims description 11
- 229910004007 HAc Inorganic materials 0.000 claims description 8
- 238000007906 compression Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound 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C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- -1 dimethylacetamide amine Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
本发明公开一种低浓度二甲基乙酰胺的回收工艺,包括预热、浓缩、汽化、精馏、脱酸以及回收六大工序。通过将浓缩塔中的蒸汽进行压缩机压缩升温,作为降膜蒸发器热源,从而减少了鲜蒸汽的消耗量,能够将质量分数为1%~5%的DMAc溶液进行提纯回收,且回收同浓度DMAc溶液的单耗只是原有技术的1/6~1/5,其热能利用率极高,很好地节约了能源。该工艺设备成本以及工艺条件容易实现,较易实现自动化控制,操作简单易控;DMAc回收率高,损失少,减少了环境污染,适于广泛应用于实际工业生产过程中。
Description
技术领域
[0001] 本发明涉及二甲基乙酰胺回收工艺技术领域,尤其涉及一种低浓度二甲基乙酰胺 的回收工艺。
背景技术
[0002] 二甲基乙酰胺是N,N-二甲基乙酰胺的简称,英文简称DMAc。作为一种重要的化 工原料和优良的有机溶剂,在石油化工、有机合成工业、塑料薄膜、丙烯腈纺丝、聚醚砜纺 丝、医药、农药和染颜料等领域中应用广泛。DMAc的需求量大,且在使用后多以稀水溶液的 形式存在,如何经济有效地对其进行回收并降低单位能耗,具有重要的经济效益、社会效益 和环境效益。
[0003] 目前最主要的处理方法是采用传统的"蒸发+精馏",该法对较高浓度的DMAc回收 具有一定的价值和可行性,但对浓度低于5%的DMAc溶液,采用该法处理能耗巨大,即便是 采用多效精馏,其能耗还是偏高。而直接排放,则造成严重的环境污染、且资源浪费严重。
[0004] 在中国发明专利申请号为"CN102993039A",名称为" 一种回收聚醚砜纺丝废水中 二甲基乙酰胺的方法"的专利文件中公开了一种回收低浓度二甲基乙酰胺的方法,该方法 属于二甲基乙酰胺的分离纯化技术领域。该方法主要包括超滤,反渗透和常减压精馏三个 主要工序。具体工艺流程是:将聚醚砜纺丝生产过程中所产生的含DMAc废水投入到料液 罐中,废水经料液泵进入超滤复合膜组件中以除去聚醚砜和聚乙烯吡咯烷酮高分子聚合 物,滤液进入储罐中,截留液回流至料液罐中;储罐中滤液经料液泵进入反渗透复合膜组件 中进行初步脱水浓缩,待浓缩至DMAc质量分数为10-15.%后,进入精馏工序进行进一步 的分离,在精馏工序得到质量分数在99.0%以上的二甲基乙酰胺产品。本发明操作相对简 便,不引入其它溶剂,节能效果比较明显,而且可以节省资源,并为企业带来良好的经济效 益,具有良好的推广应用前景。
[0005] 然而,现如今这种回收方法依然不能大范围的应用于生产实际过程中,因为该方 法对于超滤与反渗透设备的要求极高,而这些设备的成本也相当高,所以很多时候回收成 本大于了回收价值,所以新型的节能效果好、成本低的二甲基乙酰胺回收工艺亟待开发。
发明内容
[0006] 针对上述技术中存在的不足之处,本发明提供一种成本低、能耗小的低浓度二甲 基乙酰胺的回收工艺。
[0007] 为了达到上述目的,本发明一种低浓度二甲基乙酰胺的回收工艺,包括以下工艺 步骤: 51、 预热:将DMAc溶液经原料泵送入原料预热器进行预热处理,所述原料预热器采用 后序工艺中的降膜蒸发器冷凝液作为热介质; 52、 浓缩:预热后溶液进入浓缩塔,所述浓缩塔采用降膜蒸发器作为再沸器,塔顶采出 蒸汽经压缩机压缩后作为再沸器热源; 53、 汽化:浓缩后的溶液经转料泵打入汽化器,在汽化器中进一步加热升温; 54、 精馏:溶液汽化后,进入精馏塔,控制精馏塔塔底与塔顶温度,使高沸点DMAc溶液 与低沸点杂质进一步分离; 55、 脱酸:所述精馏塔塔底采出混有少量HAc的DMc溶液,经脱酸进料泵进入脱酸塔去 除HAc; 56、 回收:脱酸后的DMAc溶液进行冷却,高纯度的DMAc溶液进入DMAc成品罐回收利 用。
[0008] 其中,Sl中的原料含有浓度为1%~5%的DMAc溶液经原料泵送入原料预热器,由降 膜蒸发器冷凝液作为热介质传热,原料温度提高到75°C。
[0009] 其中,S2中浓缩塔的塔底温度为80°C,塔顶温度为75°C,浓缩后DMAc浓度达到 40% 〇
[0010] 其中,在S2中,浓缩塔塔顶蒸汽采出后,进入压缩机压缩,温度升高为9rc,升温 后的蒸汽进入降膜蒸发器中作为再沸器热源提供热量。
[0011] 其中,所述浓缩塔塔顶蒸汽采出后,先进入第一压缩机压缩,该压缩机压强为 14. 8KPa,蒸汽温度升高为83°C,一次压缩后的蒸汽再进入第二压缩机进行进一步压缩升 温,第二压缩机压强为19. 4KPa,蒸汽温度升高为91°C。
[0012] 其中,在S3中汽化器的热源为鲜蒸汽,浓缩液由汽化器的下端打入,从汽化器的 上端输出,打入汽化器的浓缩液经加热后温度维持80°C。
[0013] 其中,在S4中使用的精馏塔为板式精馏塔,从汽化器输出的浓缩液从精馏塔中间 的进料口进入,经精馏提纯后由塔底输出进入下一工序,所述精馏塔塔顶温度为54°C,精馏 塔塔底温度为9rc。
[0014] 其中,在S5中混有少量HAc的DMAc溶液在脱酸塔塔顶由热风分配器均匀地送入 塔内,塔内中和HAc的溶液为碳酸钠溶液,脱酸后的高纯度DMc溶液由脱酸塔塔底进入下 一工序。
[0015] 其中,在步骤S5和步骤S6之间还包括步骤S7,即溶液的冷却,脱酸后的高纯度 DMAc溶液先进入产品冷凝器进行冷却处理,冷却后合格产品才进入DMAc成品罐进行回收。
[0016] 其中,所述高纯度DMAc溶液在产品冷凝器中走管程,冷凝液体走壳程,冷凝液体 将DMAc溶液中的热量吸走后进入其他工程作业的加热过程中。
[0017] 本发明的有益效果是: 与现有技术相比,本发明的低浓度二甲基乙酰胺的回收工艺,通过将浓缩塔中的蒸汽 进行压缩机压缩升温,作为再沸器热源,从而减少了鲜蒸汽的消耗量,能够将浓度为1°/p5% 的DMAc溶液进行提纯回收,且回收同浓度DMAc溶液的单耗只是原有技术的1/6~1/5,其热 能利用率极高,很好地节约了能源。该工艺设备成本以及工艺条件容易实现,较易实现自动 化控制,操作简单易控;DMc回收率高,损失少,减少了环境污染,适于广泛应用于实际工 业生产过程中。
附图说明
[0018] 图1为本发明低浓度二甲基乙酰胺的回收工艺的物料流程图; 图2为本发明低浓度二甲基乙酰胺的回收工艺的工艺流程图。
[0019] 主要元件符号说明如下: I、 原液罐 2、进料泵 3、原料预热器 4、降膜蒸发器 5、第一压缩机 6、第二压缩机 7、浓缩塔 8、转料泵 9、汽化器 10、精馏塔 II、 脱酸进料泵 12、脱酸塔 13、产品冷凝器 14、成品罐。
具体实施方式
[0020] 为了更清楚地表述本发明,下面结合附图对本发明作进一步地描述。
[0021] 第一实施例 参阅图1-2,本发明一种低浓度二甲基乙酰胺的回收工艺具体实施过程中的工艺步骤 为: 51、 将原液罐1中含DMAc质量分数为1. 8%的原液通过进料泵2以6t/h送入原料预热 器3,将原料温度预热到80°C,稳定运行时,原料预热器3使用降膜蒸发器4的冷凝水; 52、 经原料预热器3预热的物料进入浓缩塔7,同时通过控制降膜蒸发器4蒸汽的流 量,使浓缩塔7釜温度为80°C,并控制塔底物料采出为0. 29m3/h,此时可保证原物料浓缩到 40% 〇
[0022] S3、浓缩塔7顶采出的蒸汽,通过第一压缩机5和第二压缩机6的两次压缩,将其 温度提高到91°C,作为稳定运行时降膜蒸发器4的热源; S4、通过转料泵8将浓缩塔7底采出物泵入汽化器9,通过控制汽化器9鲜蒸汽的流量, 保持汽化器9的温度为80°C,压力为17kpa,在精馏段,控制回流量为220kg/h,其余进入下 一工序。
[0023] S5、通过控制精馏塔10再沸器蒸汽流量,保持塔釜温度为91°C。
[0024] S6、由于DMAc会分解,故需将精馏得到的DMAc进行脱酸处理,需要脱酸处理的物 料通过脱酸进料泵11泵入脱酸塔12,并控制脱酸塔12冷疑器回流量为45kg/h,其余进入 下一工序处理; S7、通过脱酸处理的物料,从脱酸塔12中部采出,由于采出的是DMAc的蒸汽,固使用产 品冷凝器13将其冷凝,送入DMAc成品罐14,得到的成品流量约为100kg/h。
[0025] 表IMVR技术在低浓度DMAc回收工艺中的应用与传统三效工艺比较:
备注:蒸汽按220元/吨,电按0.7元/度,水按3元/吨,DMc按11000元/吨,人工 费用未计算。
[0026] 第二实施例 本发明一种低浓度二甲基乙酰胺的回收工艺具体实施过程中的工艺步骤为: 51、 将原液罐1中含DMAc质量分数为1%的原液通过进料泵2以8t/h送入原料预热器 3,将原料温度预热到80°C,稳定运行时,原料预热器3使用降膜蒸发器4的冷凝水; 52、 经原料预热器3预热的物料进入浓缩塔7,同时通过控制降膜蒸发器4蒸汽的流 量,使浓缩塔7釜温度为80°C,并控制塔底物料采出为0. 22m3 /h,此时可保证原物料浓缩到 40% 〇
[0027] S3、浓缩塔7顶采出的蒸汽,通过第一压缩机5和第二压缩机6的压缩,将其温度 提高到91°C,作为稳定运行时降膜蒸发器4的热源; S4、通过转料泵8将浓缩塔7底采出物泵入汽化器9,通过控制汽化器9鲜蒸汽的流量, 保持汽化器9的温度为80°C,压力为17kpa,在精馏段,控制回流量为165kg/h,其余进入下 一工序。
[0028] S5、通过控制精馏塔10再沸器蒸汽流量,保持塔釜温度为91°C。
[0029]S6、由于DMAc会分解,故需将精馏得到的DMAc进行脱酸处理,需要脱酸处理的物 料通过脱酸进料泵11泵入脱酸塔12,并控制脱酸塔12冷疑器回流量为35kg/h,其余进入 下一工序处理; S7、通过脱酸处理的物料,从脱酸塔12中部采出,由于采出的是DMAc的蒸汽,固使用产 品冷凝器13将其冷凝,送入DMAc成品罐14,得到的成品流量约为80kg/h。
[0030] 表2MVR技术在低浓度DMAc回收工艺中的应用与传统三效工艺比较:
备注:蒸汽按220元/吨,电按0.7元/度,水按3元/吨,DMc按11000元/吨,人工 费用未计算。
[0031] 第三实施例 本发明一种低浓度二甲基乙酰胺的回收工艺具体实施过程中的工艺步骤为: 51、 将原液罐1中含DMAc质量分数为5%的原液通过进料泵2以5t/h送入原料预热器 3,将原料温度预热到80°C,稳定运行时,原料预热器3使用降膜蒸发器4的冷凝水; 52、 经原料预热器3预热的物料进入浓缩塔7,同时通过控制降膜蒸发器4蒸汽的流 量,使浓缩塔7釜温度为80°C,并控制塔底物料采出为0. 67m3/h,此时可保证原物料浓缩到 40%〇
[0032]S3、浓缩塔7顶采出的蒸汽,通过第一压缩机5和第二压缩机6的压缩,将其温度 提高到91°C,作为稳定运行时降膜蒸发器4的热源; S4、通过转料泵8将浓缩塔7底采出物泵入汽化器9,通过控制汽化器9鲜蒸汽的流量, 保持汽化器9的温度为80°C,压力为17kpa,在精馏段,控制回流量为510kg/h,其余进入下 一工序。
[0033] S5、通过控制精馏塔10再沸器蒸汽流量,保持塔釜温度为91°C。
[0034] S6、由于DMAc会分解,故需将精馏得到的DMAc进行脱酸处理,需要脱酸处理的物 料通过脱酸进料泵11泵入脱酸塔12,并控制脱酸塔12冷疑器回流量为105kg/h,其余进入 下一工序处理; S7、通过脱酸处理的物料,从脱酸塔12中部采出,由于采出的是DMAc的蒸汽,固使用产 品冷凝器13将其冷凝,送入DMAc成品罐14,得到的成品流量约为250kg/h。
[0035] 表3MVR技术在低浓度DMAc回收工艺中的应用与传统三效工艺比较:
备注:蒸汽按220元/吨,电按0.7元/度,水按3元/吨,DMc按11000元/吨,人工 费用未计算。
[0036] 第四实施例 本发明一种低浓度二甲基乙酰胺的回收工艺具体实施过程中的工艺步骤为: 51、 将原液罐1中含DMAc质量分数为3%的原液通过进料泵2以6. 5t/h送入原料预热 器3,将原料温度预热到80°C,稳定运行时,原料预热器3使用降膜蒸发器4的冷凝水; 52、 经原料预热器3预热的物料进入浓缩塔7,同时通过控制降膜蒸发器4蒸汽的流 量,使浓缩塔7釜温度为80°C,并控制塔底物料采出为0. 52m3 /h,此时可保证原物料浓缩到 40% 〇
[0037]S3、浓缩塔7顶采出的蒸汽,通过第一压缩机5和第二压缩机6的压缩,将其温度 提高到91°C,作为稳定运行时降膜蒸发器4的热源; S4、通过转料泵8将浓缩塔7底采出物泵入汽化器9,通过控制汽化器9鲜蒸汽的流量, 保持汽化器9的温度为80°C,压力为17kpa,在精馏段,控制回流量为395kg/h,其余进入下 一工序。
[0038] S5、通过控制精馏塔10再沸器蒸汽流量,保持塔釜温度为91°C。
[0039] S6、由于DMAc会分解,故需将精馏得到的DMAc进行脱酸处理,需要脱酸处理的物 料通过脱酸进料泵11泵入脱酸塔12,并控制脱酸塔12冷疑器回流量为80kg/h,其余进入 下一工序处理; S7、通过脱酸处理的物料,从脱酸塔12中部采出,由于采出的是DMAc的蒸汽,固使用产 品冷凝器13将其冷凝,送入DMAc成品罐14,得到的成品流量约为195kg/h。
[0040] 表4MVR技术在低浓度DMAc回收工艺中的应用与传统三效工艺比较:
备注:蒸汽按220元/吨,电按0.7元/度,水按3元/吨,DMc按11000元/吨,人工 费用未计算。
[0041] 本发明各工序的温度控制要求高,在原料预热器3,降膜蒸发器4、压缩机、浓缩塔 7、汽化器9、精馏塔10、脱酸塔12、产品冷疑器等设备的外层均设置有一保温外罩,在蒸汽、 冷却液等溶液运输管道外层均套设有保温套以节能。
[0042] 以上公开的仅为本发明的几个具体实施例,但是本发明并非局限于此,任何本领 域的技术人员能思之的变化都应落入本发明的保护范围。
Claims (10)
1. 一种低浓度二甲基乙酰胺的回收工艺,其特征在于,包括以下工艺步骤: 51、 预热:将DMAc溶液经原料泵送入原料预热器进行预热处理,所述原料预热器采用 后序工艺中的降膜蒸发器冷凝液作为热介质; 52、 浓缩:预热后溶液进入浓缩塔,所述浓缩塔采用降膜蒸发器作为再沸器,塔顶采出 蒸汽经压缩机压缩后作为再沸器热源; 53、 汽化:浓缩后的溶液经转料泵打入汽化器,在汽化器中进一步加热升温; 54、 精馏:溶液汽化后,进入精馏塔,控制精馏塔塔底与塔顶温度,使高沸点DMAc溶液 与低沸点杂质进一步分离; 55、 脱酸:所述精馏塔塔底采出混有少量HAc的DMc溶液,经脱酸进料泵进入脱酸塔去 除HAc; 56、 回收:脱酸后的DMAc溶液进行冷却,纯度大于98%的DMAc溶液进入DMAc成品罐回 收利用。
2. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,Sl中的原料 含有浓度为1°/p5%的DMAc溶液经原料泵送入原料预热器,由降膜蒸发器冷凝液作为热介质 传热,原料温度提高到75 °C。
3. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,S2中浓缩塔 的塔底温度为80°C,塔顶温度为75°C,浓缩后DMAc浓度达到40%。
4. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,在S2中,浓缩 塔塔顶蒸汽采出后,进入压缩机压缩,温度升高为91°C,升温后的蒸汽进入降膜蒸发器中作 为再沸器热源提供热量。
5. 根据权利要求4所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,所述浓缩塔 塔顶蒸汽采出后,先进入第一压缩机压缩,该压缩机提供压差为14. 8KPa,蒸汽温度升高为 83°C,一次压缩后的蒸汽再进入第二压缩机进行进一步压缩升温,第二压缩机提供压差为 19. 4KPa,蒸汽温度升高为91 °C。
6. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,在S3中汽化 器的热源为鲜蒸汽,浓缩液由汽化器的下端打入,从汽化器的上端输出,打入汽化器的浓缩 液经加热后温度维持在80°C。
7. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,在S4中使用 的精馏塔为板式精馏塔,从汽化器输出的浓缩液从精馏塔中间的进料口进入,经精馏提纯 后由塔底输出进入下一工序,所述精馏塔塔顶温度为54°C,精馏塔塔底温度为91°C。
8. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,在S5中混有 少量HAc的DMAc溶液在脱酸塔塔顶由热风分配器均匀地送入塔内,塔内中和HAc的溶液为 碳酸钠溶液,脱酸后的高纯度DMAc溶液由脱酸塔塔底进入下一工序。
9. 根据权利要求1所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,在步骤S5和 步骤S6之间还包括步骤S7,即溶液的冷却,脱酸后的高纯度DMAc溶液先进入产品冷凝器进 行冷却处理,冷却后合格产品才进入DMAc成品罐进行回收。
10. 根据权利要求9所述的低浓度二甲基乙酰胺的回收工艺,其特征在于,所述高纯度 DMAc溶液在产品冷凝器中走管程,冷凝液体走壳程,冷凝液体将DMAc溶液中的热量吸走后 进入其他工程作业的加热过程中。
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CN109096140A (zh) * | 2018-09-21 | 2018-12-28 | 深圳市瑞升华科技股份有限公司 | 节能型二甲基乙酰胺精馏提纯工艺及设备 |
CN110452125A (zh) * | 2019-09-03 | 2019-11-15 | 天津科技大学 | 一种基于机械式蒸汽再压缩mvr的甲苯二胺脱水方法及装置 |
CN110862330A (zh) * | 2019-11-20 | 2020-03-06 | 浙江省天正设计工程有限公司 | 一种用于dmac废液回收的高效节能精馏工艺 |
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