CN106946367A - It is a kind of to be used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pretreating agent of crystallization - Google Patents

It is a kind of to be used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pretreating agent of crystallization Download PDF

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Publication number
CN106946367A
CN106946367A CN201710198212.9A CN201710198212A CN106946367A CN 106946367 A CN106946367 A CN 106946367A CN 201710198212 A CN201710198212 A CN 201710198212A CN 106946367 A CN106946367 A CN 106946367A
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CN
China
Prior art keywords
ethylene glycol
waste liquid
coal
pretreating agent
tower bottom
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710198212.9A
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Chinese (zh)
Inventor
成兰兴
霍二福
王伯楠
师传兴
郝凌云
李迎春
赵增兵
程伟琴
王毅楠
冯明
王延花
谷中鸣
李胜军
侯占峰
魏新军
王留栓
孟立山
宁红军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD
Original Assignee
HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD
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Publication date
Application filed by HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD filed Critical HENAN CHEMICAL INDUSTRY RESEARCH INSTITUTE CO LTD
Priority to CN201710198212.9A priority Critical patent/CN106946367A/en
Publication of CN106946367A publication Critical patent/CN106946367A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F5/00Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
    • C02F5/08Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
    • C02F5/14Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing phosphorus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • B01D3/4211Regulation; Control of columns
    • B01D3/4283Bottom stream
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00Specific treatment goals
    • C02F2303/22Eliminating or preventing deposits, scale removal, scale prevention

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Polyethers (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of pretreating agent for being used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, crystallization.The pretreating agent is prepared from by DBSA, dodecyl sodium sulfonate, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylene glycol, and its weight ratio is 02: 02: 02: 12.The pretreating agent of the present invention is added in waste liquid by weight the ratio for 0.1 1.8% is sufficiently mixed it, the coal-ethylene glycol waste liquid that can be stablized is used for the separation and recovery of next step, it is to avoid the polymerization of pipeline of the coal-ethylene glycol waste liquid during separation and recovery, pump and rectifying column is blocked.Enable recovery system continuous and steady operation.

Description

It is a kind of to be used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pre- place of crystallization Manage agent
Technical field
The present invention relates to a kind of pretreating agent for being used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, crystallization, category In chemical technology field.
Background technology
Coal-ethylene glycol is the device for producing ethylene glycol by processes such as gasification, coupling, hydrogenation, rectifying by raw material of coal, In the critical role of occupying of China's coal chemical industry, the built coal-ethylene glycol device of the cut-off end of the year 2015 China has 1,600,000 Just there are three sets of devices for producing 200000 tons per year the production scale of ton, only Henan area, and production capacity, 2016 will be newly-built up to 600,000 tons Into 1,660,000 tons of coal-ethylene glycol devices.41 covering devices will be built up to the year two thousand twenty is estimated, aggregated capacity reaches 10,260,000 tons.
In the distillation process of coal-ethylene glycol, complicated component in a certain amount of waste liquid, waste liquid can be produced, contains nearly 40 A variety of contents not wait synthesising by-product, but wherein content it is higher be still ethylene glycol and diethylene glycol, both, which add up to, accounts for waste liquid 80% or so of total amount, therefore with higher value.Current processing method is all to carry out conventional distillation by waste liquid Ethylene glycol and diethylene glycol are reclaimed, but have a problem to be difficult to solve, that is, coal-ethylene glycol waste liquid storage and it is defeated Easily it polymerize and crystallizes during sending, causes to begin to gather in course of conveying of the raw material from storage tank to rectifying column and in rectifying column Close and crystallize, Severe blockage delivery pump and conveyance conduit and rectifying device, it is impossible to normally produced.
The solution of existing apparatus is first to install filter additional before rectifying to filter the waste liquid for having produced polymerization, The course of conveying that filtrate is entered before distillation system rectifying, but filtering again is still blocked seriously, and high energy consumption is caused because of waste liquid simultaneously The substantial amounts of polymerization waste residue of huge waste and generation for polymerizeing and producing can not be handled.
The content of the invention
The purpose of the present invention exactly be directed to above-mentioned prior art in the presence of weak point and provide a kind of raw material be easy to get, The good pretreating agent for solving the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, crystallization of low cost, effect.
The purpose of the present invention can be realized by following technique measures:
The pretreating agent for being used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, crystallize of the present invention is by detergent alkylate Sulfonic acid, dodecyl sodium sulfonate, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylene glycol are prepared from, and its weight ratio is 0-2: 0-2: 0-2: 1-2.
The addition of the pretreating agent of the present invention is the 0.1-1.8% of coal-ethylene glycol rectifying tower bottom waste liquid quality.
More specifically, using coal-ethylene glycol rectifying tower bottom waste liquid as raw material, 0.1-1.8% pretreating agent is added, makes it It is sufficiently mixed, the stable coal-ethylene glycol waste liquid for being difficult polymerization is made, pipe of the waste liquid in conveying and process is solved The problem of blocking, the coking of road and equipment.
Beneficial effects of the present invention are as follows:
The pretreating agent of the present invention is sufficiently mixed after reaction with coal-ethylene glycol rectifying tower bottom waste liquid, can make pretreating agent and original The compound of easy polymeric component formation rock-steady structure in material.The coal-ethylene glycol waste liquid of not polymerizable crystallizable steady in a long-term is made, The polymerizable crystallizable of waste liquid is prevented from source, it is ensured that the stabilization of next step rectification working process is normally run, do not do it is any heating and Control measure are cooled down, without any three waste discharge, energy-conserving and environment-protective, operating cost are low.
Embodiment
The present invention is further described below with reference to embodiment:
Embodiment 1:
It is prepared by A pretreating agents:6g DBSAs and 6g 90% ethylene glycol solution is taken to be put into container, it is agitated abundant Pretreating agent is obtained after mixing.
B pretreating effects:1000 grams of undressed coal-ethylene glycol rectifying tower bottoms are added in 2000ml beakers to give up Liquid, the after measured total content 82.66% containing ethylene glycol and diethylene glycol, wherein ethylene glycol 40.23%, diethylene glycol in waste liquid 42.43%.12 grams of pretreating agent is slowly added dropwise into coal-ethylene glycol rectifying tower bottom waste liquid under agitation to be sufficiently stirred for very Clock.Obtained sample is placed and is not any change for 480 hours, starts to go out from surface after placing 10 minutes without treated sample Now it polymerize, all polymerization is integrated in 2 hours.Preprocessed dose of treated 1012 grams of addition rectifying columns of sample are depressurized Rectifying, rectifying column tower top steams 376.5 grams of ethylene glycol, content 99.05%, the ethylene glycol rate of recovery 92.22%.Diethylene glycol 381.9 Gram, content 99.33%, the diethylene glycol rate of recovery 90.01%.Waste liquid ethylene glycol and diethylene glycol overall recovery 91.08%.
Embodiment 2:
It is prepared by A pretreating agents:8.4g 1-hydroxy ethylidene-1,1-diphosphonic acids and 8.4g 90% ethylene glycol solution is taken to be put into container, it is agitated Pretreating agent is obtained after being sufficiently mixed.
B pretreating effects:600 grams of undressed coal-ethylene glycol rectifying tower bottom waste liquids are added in 1000ml beakers, Total content 75.17% containing ethylene glycol and diethylene glycol, wherein ethylene glycol 38.39%, diethylene glycol 36.78% in waste liquid after measured. 9 grams of pretreating agent is slowly added dropwise into coal-ethylene glycol rectifying tower bottom waste liquid under agitation to be sufficiently stirred for 30 minutes.It is obtained Sample is placed and is not any change for 1080 hours, starts to polymerize from surface after placing 10 minutes without treated sample, 2 All polymerization is integrated in hour.Preprocessed dose of treated 609 grams of addition rectifying columns of sample are subjected to rectification under vacuum, rectifying Column overhead steams 220.9 grams of ethylene glycol, content 99.13%, the ethylene glycol rate of recovery 92.53%.198.6 grams of diethylene glycol, content 99.02%, the diethylene glycol rate of recovery 89.99%.Waste liquid ethylene glycol and diethylene glycol overall recovery 91.29%.
Embodiment 3:
It is prepared by A pretreating agents:5.1g dodecyl sodium sulfonates and 5.1g 90% ethylene glycol solution is taken to be put into container, it is agitated to fill Divide after mixing and obtain pretreating agent.、
B pretreating effects:300 grams of undressed coal-ethylene glycol rectifying tower bottom waste liquids are added in 500ml beakers, through surveying Determine the total content 80.51% containing ethylene glycol and diethylene glycol, wherein ethylene glycol 39.85%, diethylene glycol 40.66% in waste liquid.Will be pre- 3.5 grams of inorganic agent is slowly added dropwise to coal-ethylene glycol rectifying tower bottom waste liquid and is sufficiently stirred for 45 minutes under agitation.Obtained sample Product are placed and are not any change for 1500 hours, start to polymerize from surface after placing 10 minutes without treated sample, 2 is small When it is interior all polymerization be integrated.Preprocessed dose of treated 303.5 grams of addition rectifying columns of sample are subjected to rectification under vacuum, rectifying Column overhead steams 110.9 grams of ethylene glycol, content 99.18%, the ethylene glycol rate of recovery 88.96%.109.8 grams of diethylene glycol, content 99.25%, the diethylene glycol rate of recovery 90.00%.Waste liquid ethylene glycol and diethylene glycol overall recovery 89.65%.

Claims (2)

1. a kind of be used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pretreating agent of crystallization, it is characterised in that:It is described Pretreating agent is prepared from by DBSA, dodecyl sodium sulfonate, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylene glycol, its weight Than for 0-2: 0-2: 0-2: 1-2.
2. it is used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pretreating agent of crystallization according to claim 1, its It is characterised by:The addition of the pretreating agent is the 0.1-1.8% of coal-ethylene glycol rectifying tower bottom waste liquid quality.
CN201710198212.9A 2017-03-29 2017-03-29 It is a kind of to be used to solve the waste liquid polymerization of coal-ethylene glycol rectifying tower bottom, the pretreating agent of crystallization Pending CN106946367A (en)

Priority Applications (1)

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Citations (7)

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CN1505599A (en) * 2001-04-25 2004-06-16 ������������ʽ���� Method of inhibiting polymerization of aromatic vinyl
FR2859988A1 (en) * 2003-09-18 2005-03-25 Nanoledge Dispersions of carbon nanotubes in organic solvents, useful in production of composites with e.g. electroconductive properties, prepared using stabilizing combination of surfactant and polymer
CN1761638A (en) * 2003-03-17 2006-04-19 伯东株式会社 Polymerization inhibitor for aromatic vinyl compounds and method for inhibiting the polymerization of the compounds
CN101056832A (en) * 2004-11-15 2007-10-17 伯东株式会社 Method of inhibiting polymerization for copolymer containing divinylbenzene and aromatic vinyl compound
CN101838058A (en) * 2009-12-31 2010-09-22 上海良田化工有限公司 Scale inhibitor of ethylene device process water system and using method thereof
CN102604762A (en) * 2012-02-15 2012-07-25 河南省化工研究所有限责任公司 Scavenger for clearing away PVC (polyvinyl chloride) polymer in top condenser of polymerization kettle
CN105483709A (en) * 2015-12-11 2016-04-13 青岛唐鹏钢结构工程有限公司 Steel product corrosion inhibitor

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1505599A (en) * 2001-04-25 2004-06-16 ������������ʽ���� Method of inhibiting polymerization of aromatic vinyl
CN1761638A (en) * 2003-03-17 2006-04-19 伯东株式会社 Polymerization inhibitor for aromatic vinyl compounds and method for inhibiting the polymerization of the compounds
FR2859988A1 (en) * 2003-09-18 2005-03-25 Nanoledge Dispersions of carbon nanotubes in organic solvents, useful in production of composites with e.g. electroconductive properties, prepared using stabilizing combination of surfactant and polymer
CN101056832A (en) * 2004-11-15 2007-10-17 伯东株式会社 Method of inhibiting polymerization for copolymer containing divinylbenzene and aromatic vinyl compound
CN101838058A (en) * 2009-12-31 2010-09-22 上海良田化工有限公司 Scale inhibitor of ethylene device process water system and using method thereof
CN102604762A (en) * 2012-02-15 2012-07-25 河南省化工研究所有限责任公司 Scavenger for clearing away PVC (polyvinyl chloride) polymer in top condenser of polymerization kettle
CN105483709A (en) * 2015-12-11 2016-04-13 青岛唐鹏钢结构工程有限公司 Steel product corrosion inhibitor

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Title
叶青萱等: "《胶粘剂》", 31 October 1999, 中国物资出版社 *

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