CN101481190B - 氯醇化法皂化废水处理方法 - Google Patents
氯醇化法皂化废水处理方法 Download PDFInfo
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- CN101481190B CN101481190B CN200910096097XA CN200910096097A CN101481190B CN 101481190 B CN101481190 B CN 101481190B CN 200910096097X A CN200910096097X A CN 200910096097XA CN 200910096097 A CN200910096097 A CN 200910096097A CN 101481190 B CN101481190 B CN 101481190B
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- water
- treatment
- chlorohydrination
- pond
- electrodialysis
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- 239000002351 wastewater Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000007127 saponification reaction Methods 0.000 title claims description 23
- 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 claims abstract description 56
- 238000000909 electrodialysis Methods 0.000 claims abstract description 26
- GOOHAUXETOMSMM-UHFFFAOYSA-N propylene oxide Chemical compound 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CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 238000005188 flotation Methods 0.000 claims abstract description 4
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound 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- VZIQXGLTRZLBEX-UHFFFAOYSA-N 2-Chloro-1-propanol Chemical compound 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- KNKRKFALVUDBJE-UHFFFAOYSA-N 1,2-Dichloropropane Chemical compound 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CC(Cl)CCl KNKRKFALVUDBJE-UHFFFAOYSA-N 0.000 description 1
- WZKYSMVCTDJJAR-UHFFFAOYSA-N 1,2-dichloro-2-(1,2-dichloropropan-2-yloxy)propane Chemical compound 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ClCC(Cl)(C)OC(C)(Cl)CCl WZKYSMVCTDJJAR-UHFFFAOYSA-N 0.000 description 1
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound 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Abstract
本发明公开了一种化学处理方法,具体是指一种对氯醇化法产生的皂化废水进行回收利用的处理方法。本发明是通过把氯醇化法产生的皂化废水经新型膜法处理、盐与水回用的方法,在该方法中将运用气浮、防结晶、陶瓷膜过滤、热交换、电渗析浓缩、蒸发回收等工艺设计实现的。本发明的优点是基本达到废水零排放、盐与水可以回收、占地面积小、运行费用低、经济及社会效益好的目的。本发明可在氯醇法生产环氧丙烷的工厂广泛使用。
Description
氯醇化法皂化废水处理方法
技术领域
[0001] 本发明涉及一种化学处理方法,具体是指一种对氯醇化法产生的皂化废水进行回 收利用的处理方法。
背景技术
[0002] 通过技术查新,目前国内对该类废水处理的方法主要有直接排到城市污水处理厂 统一处理、生物法与物理、物化组合工艺等。
[0003] 环氧丙烷生产主要分二步,第一步为氯醇化,此步需要大量的新鲜水;第二步为皂 化反应,氯醇化法皂化废水主要来自于皂化反应过程。在氯醇法生产环氧化物的过程中从 皂化工序排出的大量污水,由于含盐浓度较高(CaCl2质量分数为3. 5% ),给处理带来一定 的困难。国外环氧化物污水一般进城市污水处理厂统一处理,在混流时被其他污水将盐稀 释,减轻了污水生化处理的难度。
[0004] 由于在环氧化物生产时,需要周期性清理皂化塔,造成排放的污水有较大的波动。 盐浓度的变化,可导致污泥流失,生化处理失败。一般用清水稀释,稀释水量约为污水量的 30-50%,控制生化处理进水的盐浓度在2%左右,以减轻盐浓度的波动对生化处理造成的 冲击。
[0005] 中石化集团公司北京化工研究院从1972年开始,对氯醇法生产环氧化合物的污 水(环氧乙烷、环氧丙烷和环氧氯丙烷)进行专项研究,根据污水的特点研究出氯醇法生 产环氧化合物污水的处理方法,目前该项研究成果在国内得到了普遍的应用。但到目前为 止,国内环氧化物生产厂污水能稳定处理的不多,并且处理效果也不理想,一是盐含量没有 减少,从而增加市政污水处理厂的负担;二是COD去除率低,处理后出水的COD还在400mg/ L左右;三是处理费用高,由于要按1 : 0.6-0. 8的淡水进行稀释,浪费大量的淡水资源。
[0006] 氯醇法生产环氧丙烷工艺中产生的废水主要是从氯丙醇皂化和粗环氧丙烷精制 两个工序中排出的。氯丙醇皂化通常用石灰为原料,废水特点是:
[0007] 1)高pH,pH值高达11以上;
[0008] 2)高盐,废水中含有大量氯化钙等无机盐类,仅氯化钙含量就高达4% ;
[0009] 3)高C0D,通常COD浓度在1000_2000mg/L左右,废水中所含的氯丙烷,二氯异丙 醚,二氯丙烷等有机氯化物,属于难生化降解的物质;
[0010] 4)高温,废水温度高达60_80°C ;
[0011] 5)高 SS,悬浮物高达 1000 〜5000mg/L ;
[0012] 6)易结晶结垢,虽然盐的浓度远未达到结晶结垢的浓度,但在废水流经的水渠与 管道都容易出现结晶结垢现象,使管道堵塞。
[0013] 据了解一套2万吨/年的PO生产装置,每年排出的废水约120-190万吨。以2008 年全国10家企业PO产量约100万吨计,年排废水量约7000-9000万吨。
[0014] 如果采用电渗析法除盐,将会取得较好的效果,但要对废水进行预处理,至少要解 决高SS与易结晶的问题。另的高PH、高温、高COD也应进行适当的预处理才能进行电渗析浓缩处理。
[0015] 环氧丙烷工业废水的成分复杂,排放量也大,给环境带来了极大的污染,由于其有 高温、高盐、高COD、易局部结晶等问题,给废水的处理造成了极大的困难。本发明首先进行 解决去除SS、防止结晶的问题,接下去进行电渗析浓缩氯化钙回收以及淡水回用处理,实现 资源回收利用以及零排放的目标。
[0016] 随着国内水资源短缺日益严重以及环保意识的增强,国家对节能减排也越来越重 视。我国所用的氯醇法生产环氧丙烷的生产工艺属于高耗水行业。如果不在生产工艺或废 水回收利用上进行突破性改造,将使环氧丙烷的生产提出严峻考验,而环氧丙烷又是新型 工业材料聚胺聚的必需原材料,故对氯醇法生产环氧丙烷(PO)系产生的废水进行处理并 回用有其重要的意义与必要性。
[0017] 发明内容
[0018] 本发明针对现有技术中的不足,提出了一种高效处理方法,实现循环使用的效果, 本发明专利的目的是针对氯醇化法皂化废水的高PH、高温、高盐度、高COD、易结垢等特点 以及现有技术的不足,设计开发了一种氯醇化法皂化废水新型膜法处理、盐与水回用的方 法。在该方法中将运用气浮、防结晶、陶瓷膜过滤、热交换、电渗析浓缩、蒸发回收等工艺设 计,基本达到废水零排放、盐与水可以回收、占地面积小、运行费用低、经济及社会效益好的 目的。
[0019] 本发明是通过下述技术方案得以实现的:
[0020] 氯醇化法皂化废水处理方法,其特征在于包括下述步骤:
[0021] (1)把环氧丙烷生产中的皂化废水作为处理料液:pH为11〜12、盐含量为2. 0% wt 〜4. 0% wt、温度为 75 〜85°C、CODcr 为 1000mg/L 〜3000mg/L、SS 含量为 2000mg/L 〜 5000mg/L,进入增稠池初步沉降;
[0022] (2)经初步沉降后,上清液用离心泵送至气浮沉降联合池,气浮池所用的压缩空气 的压力为1. 5-3. 5kir,气泡直径20-200微米,沉降时间为1-5小时;
[0023] (3)经气浮沉降联合池后,底部污泥用压滤机压滤后成滤饼外运;上清液经中和 处理,其中中和处理后pH达到9. 5-10. 5,再把上清液输入陶瓷超滤膜装置过滤,其中陶瓷 膜的孔径为0. 2-1. 0微米,处理压力为Hbar,浓产比为0. 1-0. 6,经陶瓷超滤膜过滤的浓 液回到气浮沉降联合池循环;
[0024] (4)陶瓷超滤膜的产水经热交换器热交换后,水温降至40〜45°C,再经pH调节到 7. 5-8. 5 ;
[0025] (5)再进入电渗析装置浓缩处理,电渗析电压为15〜50V ;
[0026] (6)经循环浓缩,电渗析装置出口的电渗析浓液中,氯化钙的浓度提升到9. 0% wt〜18. 0% wt,而淡水出口的浓度为0. wt〜0. 5% wt ;
[0027] (7)电渗析装置的氯化钙浓液在热交换器中预热至60°C以上,后送至蒸发塔蒸发 回收氯化钙;电渗析产水和蒸发塔出来的蒸馏水一起作为生产用水回用。
[0028] 作为优选,上述处理方法中的步骤O)中,经气浮沉降联合池处理后的清液的SS 为800mg/L以下。
[0029] 作为优选,上述处理方法中的步骤(3)中,进入陶瓷超滤膜过滤前,对清液经过, 进行防结晶处理,这样可以为下面步骤的设备减轻处理污染物的负担,更利于保持设备的长期运行。
[0030] 作为更优选择,上述处理方法中的步骤(3)中的防结晶结垢装置为磁化装置。
[0031] 作为优选,上述处理方法中的步骤(4)进行PH调节后,再用纳滤膜预处理装置进 行预浓缩,达到盐含量为3. 0% wt以上。
[0032] 作为优选,上述处理方法中的步骤(6)中电渗析装置采用的膜为聚乙烯异相离子 交换膜。对于电渗析装置所采用的膜很多,在本发明中,采用聚乙烯异相离子交换膜在实际 使用过程中有更好的脱盐等效果。
[0033] 有益效果:
[0034] 1.利用气浮技术使废水的pH、COD、SS都大幅下降;
[0035] 2.运用磁化防结晶技术,使废水在管道中的结晶结垢大为降低,为后面的各种处 理能顺利进行;
[0036] 3.采用陶瓷超滤膜过滤,可以在80度以上的水温中能长期稳定的运行,而其他超 滤膜基本不能在50度以上的水温中运行;
[0037] 4.采用电渗析技术,使氯化钙浓度得以极大的提高,使最后用蒸发法回收成为经 济可行的方案;
[0038] 由于本处理工艺是针对氯醇法皂化废水的各种特点而开发,最后可以回收氯化钙 晶体,而水能循环使用,基本达到零排放的效果,最终达到较好的社会与经济效益。
[0039] 说明书附图
[0040] 图1氯醇化法生产环氧丙烷皂化废水回收利用的工艺流程图
[0041] 1、皂化废水 2、增稠池 3、气浮沉降联合池 4、压滤后滤饼外运 5、中和池 6、防结晶结垢装置 7、陶瓷膜超滤装置8、浓液9、热交换器10、热交换后余热11、纳 滤预浓缩装置12、电渗析装置13、电渗析浓液14、电渗析淡水15、蒸发塔16、氯化 钙晶体17、环氧丙烷生产用水
具体实施方式
[0042] 下面结合附图,对本发明的具体实施作进一步的说明:
[0043] 如图1所示,从氯醇法环氧丙烷生产车间出来的皂化废水1进入增稠池2,进行部 分石灰乳与部分废水回用,其余大部分废水进入气浮沉降联合池3。经过气浮去除部分小颗 粒悬浮物,大颗粒悬浮物经沉降后压滤后滤饼外运4。上清液经中和池5进行酸中和及防结 晶结垢装置6处理后,进入陶瓷膜超滤装置7过滤,浓液8回到气浮沉降联合池3,产水为较 干净的氯化钙溶液,经热交换器9进行热交换后,使水温降低后再进行纳滤预浓缩装置11 处理。预处理后进行电渗析装置12浓缩处理,氯化钙的电渗析浓液13利用热交换器9产 生的热交换后余热10进行预加热后进入蒸发塔15,蒸发后回收氯化钙晶体16,纳滤淡水以 及电渗析淡水14与蒸发后产生的蒸馏水一起作为环氧丙烷生产用水17,从而实现资源回 收与水循环利用的目的。
[0044] 实施例一
[0045] 以每小时2吨的处理量对整个工艺的各个处理装置设计与安装调试,最后进行实 地试验,对某环氧丙烷厂的皂化废水进行试验:
[0046] 经测定:其皂化废水排放量约1万吨/天,皂化废水的pH为11. 8、盐含量为2. 9%wt、C0D&为1800mg/L、悬浮物SS为2800mg/L,水温为81°C ;按下述步骤操作:
[0047] 1.皂化废水通过污泥泵送入增稠池2,进行灰乳回收,经测定,上清液的SS值为 850mg/L,上清液进入涡轮式气浮沉降联合池3去除部分小颗粒悬浮物与大颗粒悬浮物,沉 降时间为1. 5小时,沉淀物用压滤机压成滤饼外运,经气浮与沉降后,其pH降为9. 5,COD去 降率为80%,悬浮物去除率为92% ;
[0048] 2.气浮沉降联合池的上清液进入中和池5,再进入防结晶结垢装置6进行防结晶 处理,再进入陶瓷超滤膜装置7过滤,浓液回到气浮沉降联合池3,此时陶瓷超滤膜装置的 产水的SS总去除率在98%以上;
[0049] 3.陶瓷超滤膜装置的产水经热交换器9交换后,水温降到45°C左右,而后再进行 调节PH至7左右、纳滤预浓缩装置11等电渗析预处理;
[0050] 4.预处理后进行电渗析装置12处理,电渗膜采用聚乙烯异相离子交换膜,100对 阴阳模块,处理量每小时2吨,电压为15-50V,浓水水质:盐含量为10. 6% wt、CODcr为 500mg/L、悬浮物为50mg/L ;淡水水质:盐含量为0. 2% wt,C0DCr为50mg/L、悬浮物为IOmg/ L,浓淡比为0. 2-0.6 ;
[0051] 浓液进入蒸发塔15蒸发回收,浓液用热交换器9的余热预热至60度左右后再进 入蒸发塔15。蒸发塔15为20-50效多效蒸发塔,最后得到二水氯化钙晶体与蒸馏水,电渗 析装置12的淡水与蒸发塔15的蒸馏水共同回到环氧丙烷生产车间作为环氧丙烷生产用水 17进行回用。
[0052] 在整个处理过程中,对不同时间段的料液进行处理,得到如下数据:
[0053] 实施实例处理数据
[0054]
Claims (6)
1.氯醇化法皂化废水处理方法,其特征在于包括下述步骤:(1)把环氧丙烷生产中的皂化废水作为处理料液:pH为11〜12、盐含量为2. 0% wt〜 4. 0% wt、温度为 75 〜85°C、CODtt 为 1000mg/L 〜3000mg/L、SS 含量为 2000mg/L 〜5000mg/ L,进入增稠池初步沉降;(2)经初步沉降后,上清液用离心泵送至气浮沉降联合池,气浮池所用的压缩空气的压 力为1. 5-3. 5kir,气泡直径20-200微米,沉降时间为1-5小时;(3)经气浮沉降联合池后,底部污泥用压滤机压滤后成滤饼外运;上清液经中和处理, 其中中和处理后pH达到9. 5-10. 5,再把上清液输入陶瓷超滤膜装置过滤,其中陶瓷膜的孔 径为0. 2-1. 0微米,处理压力为Hbar,浓产比为0. 1-0. 6,经陶瓷超滤膜过滤的浓液回到 气浮沉降联合池循环;(4)陶瓷超滤膜的产水经热交换器热交换后,水温降至40〜45°C,再经pH调节到 7. 5-8. 5 ;(5)再进入电渗析装置浓缩处理,电渗析电压为15〜50V ;(6)经循环浓缩,电渗析装置出口的电渗析浓液中,氯化钙的浓度提升到9. 0% wt〜 18. 0% wt,而淡水出口的浓度为0. wt〜0.5% wt ;(7)电渗析装置的氯化钙浓液在热交换器中预热至60°C以上,后送至蒸发塔蒸发回收 氯化钙;电渗析产水和蒸发塔出来的蒸馏水一起作为生产用水回用。
2.根据权利要求1所述的处理方法,其特征在于所述的步骤O)中经气浮沉降联合池 处理后的清液的SS为800mg/L以下。
3.根据权利要求1所述的处理方法,其特征在于所述的步骤C3)中,进入陶瓷超滤膜过 滤前,对上清液经过防结晶结垢装置,进行防结晶处理。
4.根据权利要求3所述的处理方法,其特征在于所述的步骤(3)中的防结晶结垢装置 为磁化装置。
5.根据权利要求1所述的处理方法,其特征在于所述的步骤(4)进行pH调节后,再用 纳滤膜预处理装置进行预浓缩,达到盐含量为3. 0% wt以上。
6.根据权利要求1所述的处理方法,其特征在于所述的步骤(6)中电渗析装置采用的 膜为聚乙烯异相离子交换膜。
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