WO2022155781A1 - 环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法 - Google Patents

环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法 Download PDF

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WO2022155781A1
WO2022155781A1 PCT/CN2021/072663 CN2021072663W WO2022155781A1 WO 2022155781 A1 WO2022155781 A1 WO 2022155781A1 CN 2021072663 W CN2021072663 W CN 2021072663W WO 2022155781 A1 WO2022155781 A1 WO 2022155781A1
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dichloropropanol
epichlorohydrin
neutralization
dechlorination
production
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PCT/CN2021/072663
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English (en)
French (fr)
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夏燕
周焕恩
于振光
邱进瑞
李明福
相子喜
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汇智工程科技股份有限公司
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Priority to PCT/CN2021/072663 priority Critical patent/WO2022155781A1/zh
Publication of WO2022155781A1 publication Critical patent/WO2022155781A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/02—Synthesis of the oxirane ring
    • C07D301/24—Synthesis of the oxirane ring by splitting off HAL—Y from compounds containing the radical HAL—C—C—OY
    • C07D301/26—Y being hydrogen
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/32—Separation; Purification

Definitions

  • the invention relates to the technical field of epichlorohydrin production, in particular to a method for dechlorination of dichlorohydrin refining tank residue in epichlorohydrin production.
  • Epichlorohydrin is an important organic chemical raw material and fine chemical chlorine-consuming product. It is mainly used in the production of fine chemical products such as epoxy resin, synthetic glycerin, and chlorohydrin rubber. These products are widely used in chemical industry, light industry, Transportation, medicine, electronic appliances and other fields.
  • the dichloropropanol refining kettle residue liquid generated in the chlorination section of the conventional glycerol method to synthesize epichlorohydrin is directly discharged into the incinerator for incineration. Due to the relatively high chlorine content in the residual liquid of the dichloropropanol refining reactor, it is directly discharged into the incineration system, which not only pollutes the environment, but also seriously reduces the service life of the incinerator.
  • the technical problem to be solved by the present invention is: to overcome the deficiencies of the prior art, to provide a method for dechlorination of dichloropropanol refining tank residue in the production of epichlorohydrin, which greatly reduces the damage of organic chlorine to the incinerator, and prolongs the The service life of the incinerator is shortened, the equipment replacement cycle of the incinerator is reduced, and the economic benefit is improved; at the same time, the harmful substances during incineration are reduced, and the operation and maintenance are convenient.
  • the method for dechlorination of dichloropropanol refining still residue liquid in the production of epichlorohydrin comprises the following steps:
  • the chemical reaction equation of the present invention is:
  • the mass concentration of the liquid caustic soda is 30-32%.
  • step S1 after the dropwise addition of the residues of the dichloropropanol refining kettle is completed, the temperature of the system is maintained at 95-105° C., pH>12, and the temperature is kept for 2-3 hours.
  • the mass concentration of the hydrochloric acid is 31%.
  • step S2 after adjusting the pH to 5-8, the temperature is maintained for 2-3 hours.
  • step S3 before pumping the neutralization solution in the neutralization reactor into a filter press for filtration, the temperature is first lowered to 25-35°C.
  • the present invention Compared with the prior art, the present invention has the following beneficial effects: the present invention removes the organochlorine component therein before the residue of the dichloropropanol refining kettle enters the incinerator for incineration, greatly reduces the damage to the incinerator, prolongs the The service life of the incinerator is shortened, the equipment replacement cycle of the incinerator is reduced, and the economic benefit is improved; at the same time, the harmful substances during incineration are reduced, and the operation and maintenance are convenient.
  • Fig. 1 is a process flow diagram of the present invention.
  • 01-neutralization reactor 02-neutralization liquid delivery pump
  • 03-filter press 04-filtrate buffer tank
  • the present embodiment provides a kind of method for the dechlorination of dichloropropanol refining tank residue liquid in the production of epichlorohydrin, comprising the following steps:
  • the present embodiment provides a method for dechlorination of dichloropropanol refining tank residue in the production of epichlorohydrin, comprising the following steps:

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Epoxy Compounds (AREA)

Abstract

一种环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，属于环氧氯丙烷生产技术领域。其技术方案为：采用过量的氢氧化钠来处理二氯丙醇精制釜残液，使残液中的氯反应；而后用盐酸中和过量的氢氧化钠，反应生成的滤渣和污水均可采用简单常规的处理方法。大大降低了有机氯对焚烧炉的损害，延长了焚烧炉的使用寿命，减少了焚烧炉的设备更换周期，提高了经济效益；同时也减少了焚烧时的有害物质，操作维修方便。

Description

环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法 技术领域
本发明涉及环氧氯丙烷生产技术领域，具体涉及一种环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法。
背景技术
环氧氯丙烷是一种重要的有机化工原料和精细化工耗氯产品，主要用于生产环氧树脂、合成甘油、氯醇橡胶等精细化工产品，而这些产品又广泛应用于化工、轻工、交通运输、医药、电子电器等领域。常规的甘油法合成环氧氯丙烷的氯化工段中生成的二氯丙醇精制釜残液直接排入焚烧炉中进行焚烧。由于二氯丙醇精制釜残液含氯的成分比较高直接排入焚烧系统，不仅污染环境，同时严重降低焚烧炉的使用寿命。
发明内容
本发明要解决的技术问题是：克服现有技术的不足，提供一种环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，大大降低了有机氯对焚烧炉的损害，延长了焚烧炉的使用寿命，减少了焚烧炉的设备更换周期，提高了经济效益；同时也减少了焚烧时的有害物质，操作维修方便。
本发明的技术方案为：
环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，包括以下步骤：
S1：在中和反应釜中加入液碱，将二氯丙醇精制釜残液滴加到中和反应釜中进行中和反应；
S2：待反应结束后，向中和反应釜中滴加盐酸，调节pH至5-8；
S3：将中和反应釜中的中和液泵入压滤机进行过滤，过滤得到的滤液进入滤液缓冲罐并泵入污水处理站进行处理，过滤得到的滤渣装袋后送至焚烧车间焚烧处理。
本发明的化学反应方程式为：
Figure PCTCN2021072663-appb-000001
HCl+NaOH＝NaCl+H 2O
优选地，步骤S1中，所述液碱的质量浓度为30-32％。
优选地，步骤S1中，当二氯丙醇精制釜残液滴加完毕后，维持体系温度在95-105℃，pH>12，保温2-3h。
优选地，步骤S2中，所述盐酸的质量浓度为31％。
优选地，步骤S2中，调节pH至5-8至后，保温2-3h。
优选地，步骤S3中，将中和反应釜中的中和液泵入压滤机进行过滤之前，先降温至25-35℃。
本发明与现有技术相比，具有以下有益效果：本发明在二氯丙醇精制釜残液进入焚烧炉焚烧之前，先去除了其中的有机氯成分，大大降低了对焚烧炉的损害，延长了焚烧炉的使用寿命，减少了焚烧炉的设备更换周期，提高了经济效益；同时也减少了焚烧时的有害物质，操作维修方便。
附图说明
图1是本发明的工艺流程图。
图中，01-中和反应釜、02-中和液输送泵、03-压滤机、04-滤液缓冲罐、05-污水泵
具体实施方式
实施例1
如图1所示，本实施例提供了一种环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，包括以下步骤：
S1：将30％的液碱通过流量计控制进入中和反应釜01，并开启搅拌，将二氯丙醇精制釜 残液缓慢输送至中和反应釜01内，打开夹套循环水降温，维持体系温度在95℃，常压反应。当二氯丙醇精制釜残液滴加完毕后，取样监测体系pH值，通过向体系补加液碱，使pH>12，继续保温。保温2h后，打开釜底阀门，取样监测pH值，若pH>12则停止，若pH<12，则向体系补加液碱并继续保温2h。
S2：保温结束后，滴加31％盐酸到中和反应釜01，将体系pH降至5-8，保温2h。
S3：保温结束后，打开夹套循环水降温至25℃时，利用中和液输送泵02将中和液泵入板框压滤机03进行过滤，过滤得到的滤液进入滤液缓冲罐04并通过污水泵05输送到污水处理站处理，过滤得到的滤渣进行装袋送到焚烧车间。
实施例2
本实施例提供了一种环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，包括以下步骤：
S1：将32％的液碱通过流量计控制进入中和反应釜01，并开启搅拌，将二氯丙醇精制釜残液缓慢输送至中和反应釜01内，打开夹套循环水降温，维持体系温度在105℃，常压反应。当二氯丙醇精制釜残液滴加完毕后，取样监测体系pH值，通过向体系补加液碱，使pH>12，继续保温。保温3h后，打开釜底阀门，取样监测pH值，若pH>12则停止，若pH<12，则向体系补加液碱并继续保温3h。
S2：保温结束后，滴加31％盐酸到中和反应釜01，将体系pH降至5-8，保温3h。
S3：保温结束后，打开夹套循环水降温至35℃时，利用中和液输送泵02将中和液泵入板框压滤机03进行过滤，过滤得到的滤液进入滤液缓冲罐04并通过污水泵05输送到污水处理站处理，过滤得到的滤渣进行装袋送到焚烧车间。

Claims (6)

  1. 环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，包括以下步骤：
    S1：在中和反应釜中加入液碱，将二氯丙醇精制釜残液滴加到中和反应釜中进行中和反应；
    S2：待反应结束后，向中和反应釜中滴加盐酸，调节pH至5-8；
    S3：将中和反应釜中的中和液泵入压滤机进行过滤，过滤得到的滤液进入滤液缓冲罐并泵入污水处理站进行处理，过滤得到的滤渣装袋后送至焚烧车间焚烧处理。
  2. 如权利要求1所述的环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，步骤S1中，所述液碱的质量浓度为30-32％。
  3. 如权利要求1所述的环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，步骤S1中，当二氯丙醇精制釜残液滴加完毕后，维持体系温度在95-105℃，pH>12，保温2-3h。
  4. 如权利要求1所述的环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，步骤S2中，所述盐酸的质量浓度为31％。
  5. 如权利要求1所述的环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，步骤S2中，调节pH至5-8至后，保温2-3h。
  6. 如权利要求1所述的环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法，其特征在于，步骤S3中，将中和反应釜中的中和液泵入压滤机进行过滤之前，先降温至25-35℃。
PCT/CN2021/072663 2021-01-19 2021-01-19 环氧氯丙烷生产中二氯丙醇精制釜残液脱氯的方法 WO2022155781A1 (zh)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101712661A (zh) * 2009-12-01 2010-05-26 宁波东港电化有限责任公司 一种环氧氯丙烷的生产方法
CN102399031A (zh) * 2010-09-07 2012-04-04 中国石油化工股份有限公司 一种有机氯化物的处理方法
US20150246895A1 (en) * 2012-09-28 2015-09-03 Conser Spa Continuous process for producing epichlorohydrin from glycerol
CN109851121A (zh) * 2017-11-30 2019-06-07 南通星辰合成材料有限公司 一种高盐含甘油有机废水的处理回收系统及方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101712661A (zh) * 2009-12-01 2010-05-26 宁波东港电化有限责任公司 一种环氧氯丙烷的生产方法
CN102399031A (zh) * 2010-09-07 2012-04-04 中国石油化工股份有限公司 一种有机氯化物的处理方法
US20150246895A1 (en) * 2012-09-28 2015-09-03 Conser Spa Continuous process for producing epichlorohydrin from glycerol
CN109851121A (zh) * 2017-11-30 2019-06-07 南通星辰合成材料有限公司 一种高盐含甘油有机废水的处理回收系统及方法

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