CN109678666A - A kind of recovery method of synthesis gas preparing ethylene glycol waste liquid - Google Patents
A kind of recovery method of synthesis gas preparing ethylene glycol waste liquid Download PDFInfo
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- CN109678666A CN109678666A CN201910133452.XA CN201910133452A CN109678666A CN 109678666 A CN109678666 A CN 109678666A CN 201910133452 A CN201910133452 A CN 201910133452A CN 109678666 A CN109678666 A CN 109678666A
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- ethylene glycol
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- rectifying column
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- 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
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of methods that effective polyalcohol is recycled from the waste liquid of synthesis gas preparing ethylene glycol, using the rectifying column of two different heights, carry out rectifying to waste liquid according to corresponding rectifying column is opened to the selection of product different demands.This process flow can produce two kinds of other ethylene glycol products of concentration level of polyester grade and technical grade, meet different use demands, create higher economic value.
Description
Technical field
The present invention relates to coal chemical technology, specially a kind of recovery method of synthesis gas preparing ethylene glycol waste liquid.
Background technique
Ethylene glycol also known as glycol, abbreviation EG are colourless, pleasantly sweet liquid under room temperature, wash mainly for the manufacture of polyester
Synthetic fibre, polyester resin, hygroscopic agent, plasticizer, can also synthetic resin PET etc., be a kind of important Organic Chemicals.Industry at present
Production method has petroleum path, coal route and biochemical routes；Wherein, coal route is at low cost, and low energy consumption, and is suitble to China's oil short
It lacks, the country of rich coal resources is widely applied.Coal-ethylene glycol technique is mostly indirect method, i.e. synthesis gas second two
Alcohol.In this technique, in the waste liquid that the purifying stage of rectification after synthesizing glycol generates, still contain 55% ethylene glycol, 12% fourth
Glycol, 15% diethylene glycol and 11% triethylene glycol etc..Because total amount is less, large industry equipment recovery efficiency is low, traditional mode of production
Direct burning disposal is taken in the process.Ethylene glycol, which burns, generates carbon monoxide and carbon dioxide, and carbon monoxide is toxic, and titanium dioxide
Carbon can aggravate nowadays more serious greenhouse effects.If direct burning disposal, not only results in the wasting of resources, environment but will be caused
Pollution.For economic benefit and environmental angle, the present invention provides a kind of recovery methods of synthesis gas preparing ethylene glycol waste liquid, use
The method of rectifying recycles the polyalcohol in this part waste liquid.By recovery processing, 90% or more polyalcohol can be recycled,
The pollution to environment is reduced, while increasing economic benefit, meets wastes reduction instantly, recycling, innoxious development reason
It reads.
And in general technology removal process, rectifying tower height degree is fixed, therefore whole flow process can only distill out a kind of concentration
The ethylene glycol product of rank is unable to satisfy different productions to the use demand of various concentration rank ethylene glycol.The present invention provides
A method of it recycling effective polyalcohol from the waste liquid of synthesis gas preparing ethylene glycol, uses the rectifying column of two different heights, root
Rectifying is carried out to waste liquid according to corresponding rectifying column is opened to the selection of product different demands.This process flow can produce polyester grade and work
Two kinds of other ethylene glycol products of concentration level of industry grade, meet different use demands, create higher economic value.
Summary of the invention
For existing issue, the present invention provides a kind of recovery methods of synthesis gas preparing ethylene glycol waste liquid, are steamed using negative pressure
Principle is evaporated, 4 vacuum distillation processing are carried out to ethylene glycol waste liquid, isolate butanediol, ethylene glycol and diethylene glycol, triethylene glycol
Equal products；Its process flow are as follows:
(1) ethylene glycol waste liquid enters tempering tower regime flow through infusion pump, and dehydrating tower is entered after preheating, 60 DEG C of tower top temperature, is pressed
Power 30kpa enters return tank after the condensation of top gaseous phase material, and material removes overhead reflux through infusion pump when lower than standard liquid level, high
Enter storage tank after material condensation when standard liquid level, exhaust gas enters exhaust gas processing device after vacuum pump produces in return tank；
(2) dehydrating tower materials at bottom of tower enters polyester grade ethylene glycol rectifying column or technical grade ethylene glycol rectifying column, tower by infusion pump
123 DEG C of temperature, pressure 10kpa of top, top gaseous phase material enter return tank after condensing, and material is through being infused when lower than standard liquid level
Pump removes overhead reflux, and material is that polyester grade ethylene glycol or technical grade ethylene glycol convey after condensation and decoloration when higher than standard liquid level
To storage tank；
(3) polyester grade ethylene glycol rectifying column or technical grade ethylene glycol rectifying column materials at bottom of tower enter butanediol rectifying by infusion pump
Tower, enters return tank after the condensation of top gaseous phase material, material passes through when being lower than standard liquid level by 142 DEG C of tower top temperature, pressure 10kpa
Infusion pump removes overhead reflux, and when being higher than standard liquid level, butanediol is transported to storage tank after condensing in return tank；
(4) butanediol rectifying column materials at bottom of tower enters diethylene glycol rectifying column by infusion pump, and 157 DEG C of tower top temperature, pressure
10kpa, top gaseous phase material enter return tank after condensing, and material removes overhead reflux through infusion pump when lower than standard liquid level, high
Material is transported to storage tank as diethylene glycol product when standard liquid level after condensation, and return tank vacuum gas-phase truncates through vacuum pump
Flash Gas Compression Skid System, materials at bottom of tower are transported to storage tank after condensation and decoloration as triethylene glycol product.
Comparison Chinese invention patent (publication number CN201310167743) discloses a kind of coal-ethylene glycol production technology pair
The recovery method of raffinate, Chinese invention patent (publication number CN201510656923) disclose a kind of pair of synthesis gas preparing ethylene glycol
Product recycling technique, Chinese invention patent (publication number CN201710198209) disclose a kind of suitable for coal-ethylene glycol production
The rectifier unit of waste liquid commercial recovery system, technique use three-tower rectification, and benefit can not be divided to go out triethylene glycol contained in waste liquid,
And a kind of ethylene glycol product of rank can only be produced；Four tower rectifying technique used in the present invention, can isolate ethylene glycol,
Diethylene glycol, butanediol and triethylene glycol；In second of distillation process, Φ 1000cm*20500cm or Φ can be manually selected
Two kinds of specification rectifying columns of 1200cm*34487cm, to produce the ethylene glycol product of two kinds of ranks of technical grade or polyester grade.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the recovery method of synthesis gas preparing ethylene glycol waste liquid.
1 it is ethylene glycol waste liquid raw material storage tank in figure, 2 be feedstock pump, 3 be raw material tempering tower, 4 be preheater, 5 is de-
Water tower, 6 be rectifying column, 7 be reboiler, 8 be condenser, 9 be return tank, 10 be reflux/extraction pump, 11 be vacuum pump, 12 be
Exhaust gas processing device, 13 be water storage tank, 14 be technical grade ethylene glycol storage tank, 15 be polyester grade ethylene glycol storage tank, 16 be butanediol
Storage tank, 17 be diethylene glycol storage tank, 18 be triethylene glycol storage tank, 19 be bleaching tower, 20 be column bottoms pump.
Specific embodiment
The present invention is further described below with reference to embodiment and its attached drawing.
Ethylene glycol waste liquid is added with the flow of 3t/h, continuous production 10h in embodiment 1:
A. ethylene glycol waste liquid enters tempering tower, regime flow through infusion pump with 3t/h flow, preheater pre-heating temperature elevation heats de-
Water tower and reboiler, 60 DEG C of tower top temperature, pressure 30kpa；Top gaseous phase material enters condenser, enters reflux after material condensation
Tank, if liquid level is lower than 30% in return tank, material removes overhead reflux through infusion pump, if liquid level is higher than 30% in return tank, material
It is delivered to storage tank through reflux/extraction pump, exhaust gas enters exhaust gas processing device after vacuum pump produces in return tank；
B. dehydrating tower materials at bottom of tower enters polyester grade ethylene glycol rectifying column (Φ according to the selection of required product by infusion pump
1000*20500) or technical grade ethylene glycol rectifying column (Φ 1200*34487) is opened if required product is technical grade ethylene glycol
Technical grade ethylene glycol rectifying column closes polyester grade ethylene glycol rectifying column,；If required product is polyester grade ethylene glycol, open poly-
Ester grade ethylene glycol rectifying column closes technical grade ethylene glycol rectifying column；Rectifying column and reboiler are heated, at this time 123 DEG C of tower top temperature,
Pressure 10kpa, gas phase, through extraction pump extraction, are condensed, 25-45 DEG C of condenser uneven shell-side temperature, pipe by tower top into overhead condenser
Cheng Wendu 70-85 DEG C enters return tank after material condensation, if liquid level is lower than 30% in return tank, material is gone through reflux/extraction pump
Overhead reflux is higher by the material of liquid level as grade technical grade ethylene glycol or polyester grade second two if liquid level is higher than 30% in return pipe
Alcohol enters condenser through reflux/extraction pump, enters bleaching tower decolorization through infusion pump after condensation, material is delivered to after decoloration
Technical grade ethylene glycol storage tank or polyester grade ethylene glycol storage tank；Exhaust gas enters vent gas treatment after vacuum pump produces and fills in return tank
It sets；
C. polyester grade ethylene glycol rectifying column or technical grade ethylene glycol rectifying column materials at bottom of tower enter butanediol rectifying by column bottoms pump
Tower (Φ 1000*29637), 142 DEG C of tower top temperature, pressure 10kpa, top gaseous phase material enters condensation after tower top pump extraction
Device, 25-45 DEG C of condenser uneven shell-side temperature, 70-85 DEG C of tube side temperature, material enters return tank after condensation, and liquid level is low in return tank
Material removes overhead reflux through infusion pump when 30%, and when being higher than 30%, material enters condenser in return tank, through conveying after condensation
Pump is transported to butanediol storage tank, and exhaust gas enters exhaust gas processing device after vacuum pump produces in return tank；
D. butanediol rectifying column materials at bottom of tower enters diethylene glycol rectifying column (Φ 1000*29637), tower top temperature by infusion pump
157 DEG C, pressure 10kpa of degree, top gaseous phase material enter condenser by tower top pump, and condensed material is pumped by tower top to be entered
Return tank, material reflux/extraction pump removes overhead reflux when liquid level is lower than 30% in return tank, and material is flowed back/adopted when higher than 30%
Pump enters condenser out, and it is diethylene glycol product that condensed material, which is transported to diethylene glycol storage tank through reflux/extraction pump,；It returns
It flows tank gas phase and enters exhaust gas processing device through vacuum pump extraction；Materials at bottom of tower enters condenser, condenser shell side by column bottoms pump
35-55 DEG C of temperature, 85-95 DEG C of tube side temperature, material enters bleaching tower by column bottoms pump after condensation, and material enters three after decoloration
Ethylene glycol storage tank is triethylene glycol product.
Products obtained therefrom yield is as follows:
| Product | Ethylene glycol | Diethylene glycol | Triethylene glycol | Butanediol | Water |
| Yield (t) | 16.0 | 4.2 | 3.9 | 3.5 | 2.1 |
Claims (4)
1. the technique that a kind of ethylene glycol devil liquor recovery recycles, specifically includes that ethylene glycol waste liquid raw material storage tank, tempering tower, preheating
Device, reboiler, dehydrating tower, rectifying column, return tank, condenser, feedstock pump, vacuum pump, reflux/extraction pump, vent gas treatment
Device, bleaching tower, storage tank；Four distillation processes, exhaust gas are separated including dehydration, ethylene glycol separation, butanediol separation, diethylene glycol
Treatment process；Wherein distillation process mainly includes the pre-heating temperature elevation of raw material, boiling, condensation, decoloration；It is characterized in that technical process
It is as follows:
A. ethylene glycol waste liquid enters tempering tower regime flow through infusion pump, after preheating enter dehydrating tower, 60 DEG C of tower top temperature, pressure
30kpa,
B. enter return tank after the condensation of top gaseous phase material, material removes overhead reflux, c. high through infusion pump when lower than standard liquid level
Enter storage tank after material condensation when standard liquid level,
D. exhaust gas enters exhaust gas processing device after vacuum pump produces in return tank.
2. the technique that a kind of ethylene glycol devil liquor recovery recycles according to claim 1, it is characterised in that: dehydrating tower bottoms
Material enters polyester grade grade diethylene glycol rectifying column or technical grade diethylene glycol rectifying column by infusion pump, 123 DEG C of tower top temperature, presses
Power 10kpa, top gaseous phase material enter return tank after condensing, and material removes overhead reflux through infusion pump when lower than standard liquid level,
Material is that polyester grade ethylene glycol or technical grade ethylene glycol are delivered to storage tank after condensation and decoloration when higher than standard liquid level.
3. the technique that a kind of ethylene glycol devil liquor recovery recycles according to claim 1, it is characterised in that: polyester grade grade diethyl
Glycol rectifying column or technical grade diethylene glycol rectifying column materials at bottom of tower enter butanediol rectifying column, tower top temperature by infusion pump
142 DEG C, pressure 10kpa, enter return tank after the condensation of top gaseous phase material, material removes tower top through infusion pump when lower than standard liquid level
Reflux, when being higher than standard liquid level, butanediol is transported to storage tank after condensing in return tank.
4. the technique that a kind of ethylene glycol devil liquor recovery recycles according to claim 1, it is characterised in that: rectifying tower substrate
Material enters diethylene glycol rectifying column by infusion pump, and 157 DEG C of tower top temperature, pressure 10kpa, top gaseous phase material is laggard through condensing
Enter return tank, material removes overhead reflux through infusion pump when lower than standard liquid level, and material is as diethylene glycol when being higher than standard liquid level
Product is transported to storage tank after condensation, return tank vacuum gas-phase removes exhaust gas processing device through vacuum pump, and materials at bottom of tower is as three second two
Storage tank is transported to after alcohol product, condensation and decoloration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910133452.XA CN109678666A (en) | 2019-02-22 | 2019-02-22 | A kind of recovery method of synthesis gas preparing ethylene glycol waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910133452.XA CN109678666A (en) | 2019-02-22 | 2019-02-22 | A kind of recovery method of synthesis gas preparing ethylene glycol waste liquid |
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| Publication Number | Publication Date |
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| CN109678666A true CN109678666A (en) | 2019-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910133452.XA Withdrawn CN109678666A (en) | 2019-02-22 | 2019-02-22 | A kind of recovery method of synthesis gas preparing ethylene glycol waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804254A (en) * | 2022-04-08 | 2022-07-29 | 中自环保科技股份有限公司 | Method for recovering ethylene glycol from waste liquid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010294A (en) * | 2010-11-02 | 2011-04-13 | 宁波职业技术学院 | Method and device for recovering polyethylene glycol raffinate byproduct from ethylene glycol process |
| CN103254030A (en) * | 2013-05-17 | 2013-08-21 | 天津天中福大科技发展有限公司 | Device and method for recycling byproduct residual liquid in coal-to-ethylene-glycol production process |
| CN103265401A (en) * | 2013-04-24 | 2013-08-28 | 河南朝歌日光新能源股份有限公司 | Method for recovering coal-to-glycol technology byproduct raffinate |
| CN103553877A (en) * | 2013-10-22 | 2014-02-05 | 新疆天业（集团）有限公司 | Method for rectifying ethylene glycol during production of ethylene glycol from calcium carbide furnace gas |
| CN105330514A (en) * | 2015-10-12 | 2016-02-17 | 天津衡创工大现代塔器技术有限公司 | Purification process for preparation of ethylene glycol from synthesis gas |
| CN108329193A (en) * | 2018-04-03 | 2018-07-27 | 烟台国邦化工机械科技有限公司 | One kind being used for coal-ethylene glycol industry ethylene glycol recovery process method and system |
| CN109179542A (en) * | 2018-11-13 | 2019-01-11 | 重庆华峰化工有限公司 | Ethylene glycol, the Distallation systm of diethylene glycol and distillation technique in polyalcohol waste liquid |
-
2019
- 2019-02-22 CN CN201910133452.XA patent/CN109678666A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010294A (en) * | 2010-11-02 | 2011-04-13 | 宁波职业技术学院 | Method and device for recovering polyethylene glycol raffinate byproduct from ethylene glycol process |
| CN103265401A (en) * | 2013-04-24 | 2013-08-28 | 河南朝歌日光新能源股份有限公司 | Method for recovering coal-to-glycol technology byproduct raffinate |
| CN103254030A (en) * | 2013-05-17 | 2013-08-21 | 天津天中福大科技发展有限公司 | Device and method for recycling byproduct residual liquid in coal-to-ethylene-glycol production process |
| CN103553877A (en) * | 2013-10-22 | 2014-02-05 | 新疆天业（集团）有限公司 | Method for rectifying ethylene glycol during production of ethylene glycol from calcium carbide furnace gas |
| CN105330514A (en) * | 2015-10-12 | 2016-02-17 | 天津衡创工大现代塔器技术有限公司 | Purification process for preparation of ethylene glycol from synthesis gas |
| CN108329193A (en) * | 2018-04-03 | 2018-07-27 | 烟台国邦化工机械科技有限公司 | One kind being used for coal-ethylene glycol industry ethylene glycol recovery process method and system |
| CN109179542A (en) * | 2018-11-13 | 2019-01-11 | 重庆华峰化工有限公司 | Ethylene glycol, the Distallation systm of diethylene glycol and distillation technique in polyalcohol waste liquid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114804254A (en) * | 2022-04-08 | 2022-07-29 | 中自环保科技股份有限公司 | Method for recovering ethylene glycol from waste liquid |
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| PB01 | Publication | ||
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| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20200507 Address after: 253611 Recycling Economy Demonstration Park of Tieying Town, Leling City, Dezhou City, Shandong Province Applicant after: LELING LIWEI CHEMICALS Co.,Ltd. Address before: 253611 circular economy demonstration park, Tieying Town, Leling City, Dezhou City, Shandong Province Applicant before: LAOLING JUJIU ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. |
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| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190426 |