CN105348043B - 含易结垢杂质的溶剂-水混合物的分离回收方法及装置 - Google Patents
含易结垢杂质的溶剂-水混合物的分离回收方法及装置 Download PDFInfo
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- CN105348043B CN105348043B CN201510848319.4A CN201510848319A CN105348043B CN 105348043 B CN105348043 B CN 105348043B CN 201510848319 A CN201510848319 A CN 201510848319A CN 105348043 B CN105348043 B CN 105348043B
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- 239000012535 impurity Substances 0.000 title claims abstract description 57
- 239000000203 mixture Substances 0.000 title claims abstract description 47
- 238000000926 separation method Methods 0.000 title claims abstract description 10
- 238000011084 recovery Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims description 43
- 239000002351 wastewater Substances 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 238000004821 distillation Methods 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 239000011780 sodium chloride Substances 0.000 claims abstract description 7
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 4
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims description 42
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- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound 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CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound data:image/svg+xml;base64,PD94bWwgdmVyc2lvbj0nMS4wJyBlbmNvZGluZz0naXNvLTg4NTktMSc/Pgo8c3ZnIHZlcnNpb249JzEuMScgYmFzZVByb2ZpbGU9J2Z1bGwnCiAgICAgICAgICAgICAgeG1sbnM9J2h0dHA6Ly93d3cudzMub3JnLzIwMDAvc3ZnJwogICAgICAgICAgICAgICAgICAgICAgeG1sbnM6cmRraXQ9J2h0dHA6Ly93d3cucmRraXQub3JnL3htbCcKICAgICAgICAgICAgICAgICAgICAgIHhtbG5zOnhsaW5rPSdodHRwOi8vd3d3LnczLm9yZy8xOTk5L3hsaW5rJwogICAgICAgICAgICAgICAgICB4bWw6c3BhY2U9J3ByZXNlcnZlJwp3aWR0aD0nMzAwcHgnIGhlaWdodD0nMzAwcHgnIHZpZXdCb3g9JzAgMCAzMDAgMzAwJz4KPCEtLSBFTkQgT0YgSEVBREVSIC0tPgo8cmVjdCBzdHlsZT0nb3BhY2l0eToxLjA7ZmlsbDojRkZGRkZGO3N0cm9rZTpub25lJyB3aWR0aD0nMzAwLjAnIGhlaWdodD0nMzAwLjAnIHg9JzAuMCcgeT0nMC4wJz4gPC9yZWN0Pgo8cGF0aCBjbGFzcz0nYm9uZC0wIGF0b20tMCBhdG9tLTEnIGQ9J00gMTc3LjAsMTUwLjAgTCAxMDMuOCwxNTAuMCcgc3R5bGU9J2ZpbGw6bm9uZTtmaWxsLXJ1bGU6ZXZlbm9kZDtzdHJva2U6I0U4NDIzNTtzdHJva2Utd2lkdGg6Mi4wcHg7c3Ryb2tlLWxpbmVjYXA6YnV0dDtzdHJva2UtbGluZWpvaW46bWl0ZXI7c3Ryb2tlLW9wYWNpdHk6MScgLz4KPHBhdGggY2xhc3M9J2JvbmQtMCBhdG9tLTAgYXRvbS0xJyBkPSdNIDEwMy44LDE1MC4wIEwgMzAuNSwxNTAuMCcgc3R5bGU9J2ZpbGw6bm9uZTtmaWxsLXJ1bGU6ZXZlbm9kZDtzdHJva2U6IzNCNDE0MztzdHJva2Utd2lkdGg6Mi4wcHg7c3Ryb2tlLWxpbmVjYXA6YnV0dDtzdHJva2UtbGluZWpvaW46bWl0ZXI7c3Ryb2tlLW9wYWNpdHk6MScgLz4KPHRleHQgeD0nMjIzLjEnIHk9JzE3MC4wJyBjbGFzcz0nYXRvbS0wJyBzdHlsZT0nZm9udC1zaXplOjQwcHg7Zm9udC1zdHlsZTpub3JtYWw7Zm9udC13ZWlnaHQ6bm9ybWFsO2ZpbGwtb3BhY2l0eToxO3N0cm9rZTpub25lO2ZvbnQtZmFtaWx5OnNhbnMtc2VyaWY7dGV4dC1hbmNob3I6c3RhcnQ7ZmlsbDojRTg0MjM1JyA+TzwvdGV4dD4KPHRleHQgeD0nMjUwLjcnIHk9JzE3MC4wJyBjbGFzcz0nYXRvbS0wJyBzdHlsZT0nZm9udC1zaXplOjQwcHg7Zm9udC1zdHlsZTpub3JtYWw7Zm9udC13ZWlnaHQ6bm9ybWFsO2ZpbGwtb3BhY2l0eToxO3N0cm9rZTpub25lO2ZvbnQtZmFtaWx5OnNhbnMtc2VyaWY7dGV4dC1hbmNob3I6c3RhcnQ7ZmlsbDojRTg0MjM1JyA+SDwvdGV4dD4KPC9zdmc+Cg== data:image/svg+xml;base64,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 OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
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O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B63/00—Purification; Separation; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
本发明涉及一种含易结垢杂质的溶剂‑水混合物的分离回收方法及装置，所述方法包括如下步骤：(1)将含易结垢杂质的溶剂‑水混合物进行减压提馏操作；(2)将减压提馏操作得到的产品进行精馏操作，得到质量分数为80％以上的溶剂产品。所述含易结垢杂质的溶剂‑水混合物中的易结垢杂质为蛋白质、盐类。本发明提供的方法及装置成功解决了料液内杂质易结垢堵塞塔板或填料的问题，保证了精馏塔内的清洁；节约了蒸汽用量；同时降低了废水的排放量，实现了高效节能环保。
Description
含易结垢杂质的溶剂-水混合物的分离回收方法及装置
技术领域
[0001] 本发明属于溶剂-水混合物分离技术领域，涉及一种含易结垢杂质的溶剂-水混合 物的分离回收方法及装置。
背景技术
[0002] 工业生产中会产生大量的工业废水，这些工业废水如果直接排放，一方面会严重 污染环境;另一方面，会造成严重浪费。因此，排放前需要对工业废水中的有机溶剂进行资 源化回收处理。其中，溶剂涉及丙酮、乙醇、甲醇、异丙醇，特别是涉及异丙醇。
[0003] 异丙醇作为一种性能优良的有机溶剂和化工原料被广泛应用于制药、化妆品、塑 料、香料、涂料、电子工业等领域，因此产生了大量含异丙醇的工业废水需回收处理。异丙醇 与水形成共沸物系，对于共沸物的分离，常用的方法有变压精馏和萃取精馏。萃取精馏需要 引入第三组分，而变压精馏不需要另外加入第三组分，只要通过对输入热量进行调节，便能 获得更高纯度的产品，但变压精馏总的经济成本较萃取精馏要高。
[0004] 然而，对于含有易结垢类杂质(如蛋白类及盐类杂质）的异丙醇-水混合溶液，目前 的工艺是物料入精馏塔内蒸馏，塔顶蒸出浓异丙醇去循环回用，塔釜直接出废水去环保，工 艺为常压及减压下操作，精馏塔采用板式塔，由于结垢的产生，使塔板极易发生堵塞，塔底 的再沸器也容易堵塞，使生产不稳定且能耗大收率低，影响生产的稳定进行。
[0005] 因此，本发明需要在变压精馈的基础上进行节能设计，同时要保证精馏过程温度 不能过高，使蛋白类及盐类等杂质不易结垢，并且要降低废水的排放量，实现高效节能环保 的目的。
发明内容
[0006] 本发明的目的之一在于提供一种含易结垢杂质的溶剂-水混合物的分离回收方 法，其特征在于，所述方法包括如下步骤：
[0007] (1)将含易结垢杂质的溶剂-水混合物进行减压提馏操作；
[0008] (2)将减压提馈操作得到的产品进行精馏操作，得到质量分数为80%以上的溶剂 产品。
[0009] 所述含易结垢杂质的溶剂-水混合物中的易结垢杂质为蛋白质、盐类。
[0010] 本发明所述减压提馏操作的热源为所述精馏操作产生的冷凝潜热；
[0011] 优选地，采用多级换热分别对所述减压提馏操作的进料和所述精馏操作的进料进 行预热；
[0012] 优选地，所述多级换热的热源通过外界提供，或通过系统内部提供，优选通过系统 内部提供；
[0013] 优选地，所述多级换热为二级换热。
[0014] 本发明所述减压提馏的操作压力为1〇〜50kPa;
[0015] 优选地，所述减压提馏的气相出料温度为20〜60°C ;所述减压提馏的回流比优选 为1〜5;所述减压提馏的回流温度优选为20〜50°C ;
[0016]优选地，所述精镏的操作压力高于所述减压提馈的操作压力，优选所述精馏的操 作压力为100〜2〇〇kPa;
[0017]优选地，所述精馏的气相出料温度为50〜12(TC;所述精馏的回流比优选为1〜5; 所述精馏的回流温度优选为30〜100°C。
[0018]本发明所述含易结垢杂质的溶剂-水混合物中的易结垢杂质的质量含量为0.5% 〜10%;
[0019]优选地，所述减压提馈操作得到的废水中溶剂含量低于0.01% ;
[0020] 优选地，所述精馏操作得到的废水中溶剂含量低于0.0001 %。
[0021] 本发明所述含易结垢杂质的溶剂-水混合物中的溶剂选自异丙醇、丙酮、乙醇、甲 醇中的任意1种，优选异丙醇；
[0022] 优选地，当所述含易结垢杂质的溶剂-水混合物中的溶剂为异丙醇时，异丙醇质量 含量为5%〜70%。
[0023]本发明目的之二在于提供一种含易结垢杂质的溶剂-水混合物的分离回收装置， 其特征在于，所述装置包括:依次连接的减压提馏单元和精馏单元;所述精馏单元连接有为 装置提供热量的供热单元。
[0024]本发明所述装置在所述减压提馏单元和精馏单元之间设置换热单元；
[0025]优选地，所述换热单元包括热流股进料管与精馏单元出气口连接的第一换热器， 以及与所述第一换热器的热流股出料管连接的液相回流罐;所述第一换热器冷流股进料管 与所述减压提馏单元的出液口连接;所述第一换热器冷流股出料管与所述减压提馏单元的 进气口连接；
[0026] 本发明所述第一换热器可以是加热器、冷却器、蒸发器、冷凝器、冷凝/再沸器中的 任一种；
[0027] 优选地，所述换热单元的第一换热器为降膜蒸发器；
[0028] 降膜蒸发具有高传热效率，液体循环使加热面接触时间短且连续冲洗避免加热面 结垢堵塞。
[0029] 本发明所述减压提馏单元包括减压提馏塔，设置于所述减压提馏塔进料口之前的 第一预热单元，设置于所述减压提馏塔出气口的塔顶冷凝器；
[0030] 优选地，所述第一预热单元的热源由外界提供，或者由系统内部提供，优选由减压 提馈单元产物的显热和/或精馏单元产物的显热提供；
[0031] 优选地，所述第一换热器的冷流股进料管与所述减压提馏塔的出液口连接，所述 第一换热器冷流股出料管与所述减压提馏塔的进气口连接；
[0032] 优选地，所述第一预热单元包括至少一个换热器；
[0033] 优选地，所述第一预热单元包括:依次连接的两个换热器。
[0034] 本发明所述精馏单元包括精馏塔和设置于所述精馏塔进料口之前的第二预热单 元；
[0035] 优选地，所述第二预热单元的热源由外界提供，或者由系统内部提供，优选由减压 提馏单元产物的显热和/或精馏单元产物的显热提供；
[0036] 优选地，所述第一换热器的热流股进料管与所述精馏塔的出气口连接，所述液相 回流罐的出料管与所述精馈塔的进液口连接；
[0037]优选地，所述第二预热单元包括至少一个换热器；
[0038]优选地，所述第二预热单元包括:依次连接的两个换热器。
[0039]本发明涉及的减压提馏塔和精馏塔均为普通精馏塔，可以为板式塔或填料塔;本 发明涉及的换热器可以是加热器、冷却器、蒸发器、冷凝器、冷凝/再沸器中的任一种；
[0040]与现有技术相比，本发明具有如下有益效果：
[0041] (1)本发明利用低温蒸馏下蛋白类及盐类等杂质不易结垢的特点，使减压提馏塔 在低温下操作，大大减少了结垢的发生；同时，精馏塔内料液完全脱除了结垢等杂质，操作 为洁净条件下进行，成功解决了料液内杂质易结垢堵塞塔板或填料的问题，保证了精馏塔 内的清洁；
[0042] ⑵本发明将精馏塔产生的冷凝潜热回收，并将其作为减压提馏塔的热源；同时采 用多级换热实现热量的有效利用，节约了蒸汽用量；当所述含易结垢杂质的溶剂-水混合物 中的溶剂为质量含量为5 %〜70 %的异丙醇时，与原常压精馏工艺相比，蒸汽用量减少了 30% 〜70%;
[0043] (3)本发明同时降低了废水的排放量，实现了高效节能环保。
附图说明
[0044]图1为具体实施方式一提供的含易结垢杂质的溶剂-水混合物的分离回收装置的 结构示意图；
[0045] 其中，100减压提馏单元，200精馏单元，300换热单元，400供热单元；
[0046]图2为具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置的 结构不意图；
[0047]其中，101减压提馏塔，102进料栗，103冷凝预热器，104热水预热器，105塔顶冷凝 器，106废水泵;201精馏塔，202凝水预热器，203精馏釜液预热器;301降膜蒸发器，302循环 栗，303液相回流罐，304出料杲;401再沸器。
具体实施方式
[0048] 为便于理解本发明，本发明列举实施例如下。本领域技术人员应该明了，所述实施 例仅仅是帮助理解本发明，不应视为对本发明的具体限制。
[0049]含易结垢杂质的溶剂-水混合物的分离回收装置的具体实施方式一
[0050] 图1提供了含易结垢杂质的溶剂-水混合物的分离回收装置的具体实施方式一的 结构示意图，所述装置包括依次连接的减压提镏单元100和精馏单元200,精馏单元200连接 有为装置提供热量的供热单元400,在减压提馏单元100和精馏单元2〇〇之间设置换热单元 300,换热单元3〇〇用于收集精馏单元200的产物的冷凝潜热作为减压提馏单元100的热源。 从减压提馏单元1〇〇和精馏单元200可以回收废水，从换热单元300可以得到所需要的溶剂 产物。
[0051] 含易结垢杂质的溶剂-水混合物的分离回收装置的具体实施方式二
[0052] 图2提供了含易结垢杂质的溶剂-水混合物的分离回收装置的具体实施方式二的 结构示意图，如具体实施方式一所述，其中，所述减压提馏单元包括:减压提馏塔101，进料 泵102，冷凝预热器103，热水预热器104，塔顶冷凝器105，废水栗106;所述精馏单元包括:精 馏塔201，凝水预热器2〇2，精馏釜液预热器203;所述换热单元包括:降膜蒸发器301，循环泵 302，液相回流罐303，出料栗304;所述供热单元为再沸器401。
[0053]料液由进料泵102送入冷凝预热器103和热水预热器104,经过二级预热后送入减 压提馏塔101的进料口；减压提馏塔101塔顶采出进入塔顶冷凝器105，冷凝后液相在经过凝 水预热器2〇2和精馏釜液预热器2〇3的二级预热后送去精镏塔201的进料口，气相送去真空 系统。精馏塔201内料液完全脱除了结垢等杂质，操作为洁净条件下进行。降膜蒸发器301的 热流股进料管与精馏塔2〇1的出气口连接，热流股出料管与液相回流罐303的进料口连接， 液相回流罐3〇3的出料口与出料栗3〇4连接，通过出料泵304部分液相回流至精馏塔201，部 分液相采出作为产品回收。精馏塔201塔底采用再沸器401加热，精馏塔201塔顶采出作为降 膜蒸发器3〇1的热源，减压提馏塔101塔底采用降膜蒸发器301加热；降膜蒸发器301的底部 分别连接有循环泵3〇2和废水泵106,减压提馏塔101塔底废水经降膜蒸发器301处理后通过 废水栗1〇6送入冷凝预热器1〇3冷凝，然后送去环保处理。精馏塔201塔釜液经过精馏釜液预 热器203冷却换热后可去回用。热水预热器104和凝水预热器202顺次连接于再沸器401，利 用再沸器的热量进行换热。
[OOM]以具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置为例简 述含易结垢杂质的溶剂-水混合物的分离回收方法：
[0055]将易结垢杂质(蛋白质、盐类)的质量含量为0.5%〜10%的溶剂-水混合物经过二 级预热后送入减压提馏塔101，塔底废水送去环保处理，塔顶采出冷凝后的液相一部分回流 至减压提馏塔101，一部分经过二级预热后进入精馏塔201，精馏塔201内为不含易结垢杂质 的溶剂-水混合物。
[0056]本发明减压提馈塔101的操作压力为10〜5〇kPa;塔顶物料温度为20〜6(TC;所述 减压提馏塔101的回流比为1〜5、回流温度为2〇〜5(TC;所述精馏塔201的操作压力为1〇〇〜 200kPa;精馏塔2〇 1的塔顶物料温度为5〇〜12(TC、回流比为1〜5、回流温度为3〇〜1〇〇 X：。精 馏塔201塔顶得到质量分数为80%以上的溶剂，减压提馏塔1〇1的塔底废水中溶剂含量低于 〇 • 01 %，精馏塔201的塔底废水中溶剂含量低于0.0001 %。
[0057]本发明所述含易结垢杂质的溶剂-水混合物中的溶剂选自异丙醇、丙酮、乙醇、甲 醇中的任意1种，优选异丙醇；当所述含易结垢杂质的溶剂-水混合物中的溶剂为异丙醇时， 异丙醇质量含量为5%〜70%。
[0058] 实施例1
[0059]利用具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的异丙醇-水混合物，包括如下步骤：
[0060] 丨、将异丙醇质量含量为5%的料液送入减压提馏塔，经过二级预热后温度为55。(：； 减压提馏塔的操作压力为15kPa、塔顶物料温度为50-C、回流比为2、回流温度为40 °C;
[0061] 2、将减压提馏塔塔顶采出送入精馏塔，经过二级预热后温度为9〇。(：；精馏塔的操 作压力为120kPa、塔顶物料温度为85。(：、回流比为2、回流温度为60。(：；
[0062] 3、精馏后得到质量分数为8〇%的异丙醇，减压提馏塔的塔底废水中异丙醇含量为 0-0〇9%，精馏塔的塔底废水中异丙醇含量为0.00005%。
[0063] 4、与原工艺相比，蒸汽用量减少30 %。 LU〇4」仕处獅目问的物料，达到相同的分离效果的情况下，每生产1吨质量分数为80%的 异丙醇，变压双效精馏工艺的蒸汽消耗量为14吨，而原常压精馏工艺的蒸汽消耗量为2吨， 与原工艺相比，蒸汽用量减少3〇%。
[0065] 实施例2
[0066]利用具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的异丙醇-水混合物，包括如下步骤： t0067] U将^丙醇质量含量为10%的料液送入减压提馏塔，经过二级预热后温度为55 °c;减压提馈塔的操作压力为15kPa、塔顶物料温度为5(rc、回流比为2、回流温度为4(rc; [0068] 2、将减压提馏塔塔顶采出送入精馏塔，经过二级预热后温度为9(TC;精馈塔的操 作压力为12〇kPa、塔顶物料温度为85〇c、回流比为2、回流温度为6〇；
[0069] 3、精馏后得到质量分数为85%的异丙醇，减压提馏塔的塔底废水中异丙醇含量为 0 _ 009 %，精馏塔的塔底废水中异丙醇含量为〇. 〇〇〇〇5%。
[0070] 4、与原工艺相比，蒸汽用量减少40%。
[0071]在处理相同的物料，达到相同的分离效果的情况下，每生产1吨质量分数为85%的 异丙醇，变压双效精馏工艺的蒸汽消耗量为丨.2吨，而原常压精馏工艺的蒸汽消耗量为2吨， 与原工艺相比，蒸汽用量减少40%。
[0072] 实施例3
[0073]利用具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的异丙醇-水混合物，包括如下步骤：
[0074] 1、将异丙醇质量含量为70 %的料液送入减压提馏塔，经过二级预热后温度为55 °C ;减压提馏塔的操作压力为丨5kPa、塔顶物料温度为5〇〇c、回流比为2、回流温度为4(rc ; [OO75] 2、将减压提馏塔塔顶采出送入精馏塔，经过二级预热后温度为9(rc;精馏塔的操 作压力为120kPa、塔顶物料温度为85 〇C、回流比为2、回流温度为6(rc ;
[0076] 3、精馏后得到质量分数为85%的异丙醇，减压提馏塔的塔底废水中异丙醇含量为 0 • 0001 %，精馏塔的塔底废水中异丙醇含量为〇. 〇〇〇〇5%。
[0077] 4、与原工艺相比，蒸汽用量减少7〇 %。
[0078]在处理相同的物料，达到相同的分离效果的情况下，每生产丨吨质量分数为85%的 异丙醇，变压双效精馏工艺的蒸汽消耗量为0.6吨，而原常压精馏工艺的蒸汽消耗量为2吨， 与原工艺相比，蒸汽用量减少70%。
[0079] 实施例4
[00S0]利用具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的甲醇-水混合物，包括如下步骤：
[0081] I将甲醇质量含量为的料液送入减压提馏塔，经过二级预热后温度为4〇r;减 压提馏塔的操作压力为UkPa、塔顶物料温度为4(TC、回流比为1、回流温度为3(TC;
[0082] 2、将减压提馏塔塔顶采出送入精馈塔，经过二级预热后温度为6(rc;精馏塔的操 作压力为110kPa、塔顶物料温度为7(TC、回流比为1、回流温度为4(TC;
[0083] 3、精馏后得到质量分数为99%的甲醇，减压提馏塔的塔底废水中甲醇含量为 0 • 00〇5%，精馏塔的塔底废水中甲醇含量为〇. 0001 %。
[0084] 实施例5 L J利用具体买施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的乙醇-水混合物，包括如下步骤：
[0086] 1、将乙醇质量含量为15%的料液送入减压提馏塔，经过二级预热后温度为4(rc; 减压提馏塔的操作压力为l5kPa、塔顶物料温度为35»C、回流比为丨、回流温度为3(rc ;
[0087] 2、将减压提馏塔塔顶采出送入精馏塔，经过二级预热后温度为6(TC;精馏塔的操 作压力为lOOkPa、塔顶物料温度为78»(：、回流比为2、回流温度为5〇〇c;
[0088] 3、精馏后得到质量分数为95 %的乙醇，减压提馏塔的塔底废水中乙醇含量为 0.0008%，精馏塔的塔底废水中乙醇含量为〇. 0001 %。
[0089] 实施例6
[0090]利用具体实施方式二提供的含易结垢杂质的溶剂-水混合物的分离回收装置分离 含易结垢杂质的丙酮-水混合物，包括如下步骤：
[0091] 1、将丙酮质量含量为10%的料液送入减压提馈塔，经过二级预热后温度为35。(：； 减压提馏塔的操作压力为3〇kPa、塔顶物料温度为3〇。(：、回流比为2、回流温度为25°C ;
[0092] 2、将减压提馏塔塔顶采出送入精馈塔，经过二级预热后温度为45t:;精馏塔的操 作压力为120kPa、塔顶物料温度为56°C、回流比为3、回流温度为35°C;
[0093] 3、精馏后得到质量分数为99%的丙酮，减压提馏塔的塔底废水中丙酮含量为 0 • 0005%，精馏塔的塔底废水中丙酮含量为〇. 〇〇〇1 %。
[0094]申请人声明，本发明通过上述实施例来说明本发明的详细工艺设备和工艺流程， 但本发明并不局限于上述详细工艺设备和工艺流程，即不意味着本发明必须依赖上述详细 工艺设备和工艺流程才能实施。所属技术领域的技术人员应该明了，对本发明的任何改进， 对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的 保护范围和公开范围之内。
Claims (15)
1. 一种含易结垢杂质的溶剂-水混合物的分离回收方法，其特征在于，所述方法包括如 下步骤： (1) 将含易结垢杂质的溶剂—水混合物进行减压提溜操作;所述减压提馈的操作压力为 10〜50kPa;所述减压提馏的气相出料温度为20〜6〇°C;所述减压提馏操作得到的废水中溶 剂含量低于〇.〇1 %; (2) 将减压提馏操作得到的产品进行精馏操作，得到质量分数为80%以上的溶剂产品； 所述精馏操作得到的废水中溶剂含量低于0 •0001 % ; 所述含易结垢杂质的溶剂-水混合物中的易结垢杂质的质量含量为0•5%〜10% ; 所述减压提馏操作的热源为所述精馏操作产生的冷凝潜热； 所述含易结垢杂质的溶剂-水混合物中的易结垢杂质为蛋白质、盐类。
2. 如权利要求1所述的方法，其特征在于，采用多级换热分别对所述减压提馈操作的进 料和所述精馏操作的进料进行预热。
3. 如权利要求2所述的方法，其特征在于，所述多级换热的热源由外界提供，或者由系 统内部提供。
4. 如权利要求3所述的方法，其特征在于，所述多级换热的热源由减压提馏操作产物的 显热和/或精馏操作的产物显热提供。
5. 如权利要求2所述的方法，其特征在于，所述多级换热为二级换热。
6. 如权利要求1或2所述的方法，其特征在于，所述减压提馈的回流比为1〜5。
7. 如权利要求1或2所述的方法，其特征在于，所述减压提馏的回流温度为20〜50°C。
8. 如权利要求1所述的方法，其特征在于，所述精馏的操作压力高于所述减压提馏的操 作压力。
9. 如权利要求8所述的方法，其特征在于，所述精馏的操作压力为100〜200kPa。
10. 如权利要求1所述的方法，其特征在于，所述精馏的气相出料温度为50〜120°C。
11. 如权利要求1所述的方法，其特征在于，所述精馏的回流比为1〜5。
12. 如权利要求1所述的方法，其特征在于，所述精馏的回流温度为3〇〜100°C。
13. 如权利要求1所述的方法，其特征在于，所述含易结垢杂质的溶剂-水混合物中的溶 剂选自异丙醇、丙酮、乙醇、甲醇中的任意1种。
14. 如权利要求13所述的方法，其特征在于，所述含易结垢杂质的溶剂-水混合物中的 溶剂为异丙醇。
15. 如权利要求14所述的方法，其特征在于，当所述含易结垢杂质的溶剂-水混合物中 的溶剂为异丙醇时，异丙醇质量含量为5%〜70%。
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