CN112321397A - Novel method for increasing yield of triethylene glycol by EOEG device - Google Patents
Novel method for increasing yield of triethylene glycol by EOEG device Download PDFInfo
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- CN112321397A CN112321397A CN202011119862.8A CN202011119862A CN112321397A CN 112321397 A CN112321397 A CN 112321397A CN 202011119862 A CN202011119862 A CN 202011119862A CN 112321397 A CN112321397 A CN 112321397A
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- glycol
- diethylene glycol
- ethylene oxide
- triethylene glycol
- rectifying tower
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/02—Preparation of ethers from oxiranes
- C07C41/03—Preparation of ethers from oxiranes by reaction of oxirane rings with hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/02—Preparation of ethers from oxiranes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
Abstract
Compared with the prior art, the novel method only adds a diethylene glycol circulating loop pipeline or a crude diethylene glycol and triethylene glycol mixed liquid loop pipeline, so that the circulating diethylene glycol or the crude diethylene glycol and triethylene glycol mixed liquid enters a hydration reactor to be hydrated with ethylene oxide to generate triethylene glycol, the concentration of the diethylene glycol in the hydration reactor is improved, and the aim of increasing the yield of the triethylene glycol is fulfilled.
Description
Technical Field
The invention relates to the technical field of triethylene glycol production, in particular to a novel method for increasing the yield of triethylene glycol by an EOEG device.
Background
Triethylene glycol (also known as triethylene glycol, abbreviated as TEG) can be used as a solvent for extracting aromatic hydrocarbon, a solvent for rubber and nitrocellulose, a diesel additive and rocket fuel. In addition, the dye has wide application in the industries of medicine, coating, textile, printing and dyeing, food, paper making, cosmetics, leather making, photography, printing, metal processing and the like. Domestic TEG products are mainly derived from ethylene glycol plants, which are by-products of ethylene glycol plants.
The production technology of ethylene oxide glycol (EO/EG) device is mature, the Ethylene Oxide (EO) and water are mixed and then enter into an Ethylene Glycol (EG) reactor, and in the ethylene glycol reactor, the ethylene oxide containing acetaldehyde reacts with water and is completely converted into ethylene glycol (M EG). Since the moles of water in the reaction feed are much higher than ethylene oxide, very small amounts of diethylene glycol (DEG), triethylene glycol (TEG) and polyethylene glycol are produced. The reaction solution is subjected to multiple-effect evaporation, rectification, drying and dehydration to obtain the ethylene glycol product. And a small amount of diethylene glycol, triethylene glycol and polyethylene glycol are produced as byproducts. In the prior art, the triethylene glycol yield of an EOEG device is the minimum, and is about 0.4% of the monoethylene glycol yield and 5% of the diethylene glycol yield. The EOEG product has a diethylene glycol market price of 4600 yuan and an industrial grade triethylene glycol market price of 10300 yuan. The existing EOEG device products, namely monoethylene glycol and diethylene glycol, are at profit and loss edges, triethylene glycol has strong profit and profit capacity, and if diethylene glycol with low additional value can be converted into triethylene glycol, the economic benefit of the device can be obviously increased, and the competitiveness of the EOEG device is enhanced. The triethylene glycol mainly comes from byproducts produced in the process of preparing ethylene glycol by hydrating ethylene oxide, has low yield and can not meet the market demand.
Disclosure of Invention
The invention provides a novel method for increasing the yield of triethylene glycol by an EOEG device, aiming at the problems in the prior art, and the method can be used for continuously increasing the yield of TEG of the EOEG device.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a novel method for increasing the yield of triethylene glycol by an EOEG device, which comprises the following process flows:
reacting ethylene oxide with water in an ethylene oxide hydration reactor, and feeding the reacted components into a multi-effect evaporation unit, a monoethylene glycol rectifying tower and a diethylene glycol rectifying tower;
and (2) boosting the pressure of diethylene glycol extracted from the top of the diethylene glycol rectifying tower or crude diethylene glycol and triethylene glycol mixed liquor extracted from the bottom of the monoethylene glycol rectifying tower by a pump, then sending all or part of the mixture to the ethylene oxide hydration reactor for reaction, directly reacting diethylene glycol and ethylene oxide to generate triethylene glycol, allowing the reaction liquid to leave the ethylene oxide hydration reactor and enter the multi-effect evaporation unit, evaporating excessive water, removing monoethylene glycol by the monoethylene glycol rectifying tower, and removing diethylene glycol by the diethylene glycol rectifying tower, wherein all or part of tower bottom liquid obtained after removing monoethylene glycol by the monoethylene glycol rectifying tower or diethylene glycol removed by the diethylene glycol rectifying tower is recycled, and tower bottom components of the diethylene glycol rectifying tower enter the triethylene glycol rectifying tower to obtain a triethylene glycol product at the top of the tower.
Further, the proportion of the diethylene glycol in recycling is 1-95%.
Further preferably, the proportion of the diethylene glycol used in the recycling is 15-60%
Further, diethylene glycol is fed back to the ethylene oxide hydration reactor either upstream or downstream of the ethylene oxide hydration feed pump.
Further, the inlet temperature of the ethylene oxide hydration reactor is 120-200 ℃ and the operating pressure is 10-25 barg.
Further preferably, the inlet temperature of the ethylene oxide hydration reactor is 140-160 degrees and the operating pressure is 15-21 barg.
Further, the reaction residence time of the ethylene oxide hydration reactor is 5-10min
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
compared with the prior art, the novel method for increasing the yield of the triethylene glycol by the EOEG device only adds one diethylene glycol circulating loop pipeline or a crude diethylene glycol and triethylene glycol mixed liquid loop pipeline, so that the circulating loop diethylene glycol or the crude diethylene glycol and triethylene glycol mixed liquid enters a hydration reactor to be hydrated with ethylene oxide to generate the triethylene glycol, the concentration of the diethylene glycol in the hydration reactor is increased, and the purpose of increasing the yield of the triethylene glycol is achieved.
Drawings
FIG. 1 is a process flow diagram of examples 1-3 of the present invention;
FIG. 2 is a process flow diagram of example 4 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1
As shown in figure 1, in a 7 kiloton/year ethylene glycol device, a DEG rectifying tower produces 110kg/hr diethylene glycol, wherein 65kg/hr MEG is pumped up and then mixed with 7550g/h EO aqueous solution (EO concentration 10%) conveyed by a hydration feed pump, the mixture is pumped up and then sent into a preheater (not shown in the figure), the mixture is preheated to 160 ℃ and then enters an EO hydration reactor, the reactor stays for 9min, the reaction pressure is 21barg, the reacted components enter a multi-effect evaporation unit (heated by steam), water in the reaction liquid is removed, the mixture of MEG, DEG and TEG which are not water is discharged from a tower bottom, the mixture is pumped into the MEG rectifying tower through a pump, 875kg/hr MEG is obtained at the tower top, 130kg of the mixture of DEG and TEG enters the DEG rectifying tower, 110kg/hr DEG is obtained at the tower top, 65kg/hr DEG is pumped up and then returned to the EO hydration reactor for recycling, 45kg/hr DEG is taken as a product, tower bottom liquid is sent into a TEG rectifying tower, 19kg/hr TEG product is obtained at the tower top, and the tower bottom liquid is 1kg/hr heavy component.
Example 2
As shown in figure 1, in a certain 7 kiloton/year ethylene glycol device, a DEG rectifying tower produces 65kg/hr diethylene glycol, 13kg/hr DEG is taken as a product, the rest 52kg/hr DEG is recycled, the DEG is mixed with 7550g/h EO aqueous solution (EO concentration is 10%) conveyed by a hydration feeding pump after being pumped up by a pump, the mixture is conveyed into a preheater (not shown) after being pumped up by a pump, the mixture is preheated to 160 ℃ and then enters an EO hydration reactor, the reactor stays for 9min, the reaction pressure is 21barg, the components after reaction enter a multi-effect evaporation unit (heated by steam), water in the reaction liquid is removed, the mixture containing no MEG, DEG and TEG is discharged from a tower bottom, the mixture is conveyed into the MEG rectifying tower through the pump, 875kg/hr of MEG is obtained at the tower top, the mixture of the DEG and the TEG in 117kg enters the DEG tower bottom, 98kg/hr of DEG product is obtained at the tower top, wherein 52kg/hr is pumped to increase pressure and then returned to the EO hydration reactor for recycling, tower bottom liquid is sent to a TEG rectifying tower, 18.5kg/hr TEG product is obtained at the tower top, and the tower bottom liquid is 0.8kg/hr heavy component.
Example 3
As shown in figure 1, in a certain 7 kiloton/year ethylene glycol device, 65kg/hr diethylene glycol is produced by a DEG rectifying tower, the diethylene glycol directly enters an EO hydration upstream buffer tank, is mixed with 7550g/h EO aqueous solution (EO concentration is 10%) in the tank, is sent into a preheater (not shown in the figure) after being pumped and boosted, is sent into an EO hydration reactor after being preheated to 160 ℃, is kept for 9min at the reactor with the reaction pressure of 21barg, is sent into a multi-effect evaporation unit (heated by steam) after reaction, removes water in reaction liquid, discharges a mixture of MEG, DEG and TEG without water from a tower bottom, is sent into an MEG rectifying tower by a pump, obtains 875kg/hr of MEG at the tower top, and 130kg of DEG mixed liquid of the DEG and the TEG enters a DEG tower, obtains 110kg/hr of DEG product at the tower top, wherein 65kg/hr is returned to the EO hydration reactor for circulation after being boosted by the pump, the bottom of the column is fed into a TEG rectifying column, 19kg/hr of TEG product is obtained at the top of the column, and 1kg/hr of heavy component is obtained at the bottom of the column.
Example 4
As shown in figure 2, in a 7 kiloton/year ethylene glycol device, 68kg/hr of diethylene glycol and triethylene glycol mixed alcohol is produced at the tower bottom of an MEG rectifying tower, the mixed alcohol is mixed with 7550g/h of EO aqueous solution (EO concentration is 10%) conveyed by a hydration feeding pump after being pumped up, the mixed alcohol is conveyed into a preheater (not shown in the figure) after being pumped up, the mixture is preheated to 160 ℃ and then enters an EO hydration reactor, the residence time of the reactor is 9min, the reaction pressure is 21barg, the components after the reaction enter a multi-effect evaporation unit (adopting steam heating), water in the reaction liquid is removed, the mixture of MEG, DEG and TEG which are not contained in water is discharged from the tower bottom, the mixture is conveyed into the MEG rectifying tower through a pump, 873kg/hr of MEG is obtained at the tower top, 133kg of the mixture of DEG and TEG in the tower bottom enters a DEG tower for circulation, 112kg/hr of DEG product is obtained at the tower top of the DEG, the tower liquid is conveyed into a TEG rectifying tower, 19kg/hr of TEG product was obtained at the top of the column and 1kg/hr of heavy components at the bottom of the column.
Comparative example
In a certain 7 kiloton/year ethylene glycol device, 7550g/h EO aqueous solution (EO concentration is 10%) is pumped and then sent into a preheater, preheated to 160 ℃ and then sent into an EO hydration reactor, the reactor stays for 9min, the reaction pressure is 21barg, the reaction liquid is sent into a dehydration tower after reaction, the dehydration tower is heated by steam, water in the reaction liquid is removed, a mixture of MEG, DEG and TEG which are not water is discharged from a tower bottom, the mixture is sent into an MEG rectifying tower through a pump, 875kg/hr of MEG is obtained at the tower top, 140kg of mixture of DEG and TEG enters a DEG tower, 65kg/hr of DEG product is obtained at the tower top, the tower bottom is sent into a TEG rectifying tower, 0.56kg/hr of TEG product is obtained at the tower top, and 1kg/hr of heavy component is obtained at the tower bottom.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (7)
1. A novel method for increasing the yield of triethylene glycol by an EOEG device is characterized by comprising the following process flows:
reacting ethylene oxide with water in an ethylene oxide hydration reactor, and feeding the reacted components into a multi-effect evaporation unit, a monoethylene glycol rectifying tower and a diethylene glycol rectifying tower;
and (2) boosting the pressure of diethylene glycol extracted from the top of the diethylene glycol rectifying tower or crude diethylene glycol and triethylene glycol mixed liquor extracted from the bottom of the monoethylene glycol rectifying tower by a pump, then sending all or part of the mixture to the ethylene oxide hydration reactor for reaction, directly reacting diethylene glycol and ethylene oxide to generate triethylene glycol, allowing the reaction liquid to leave the ethylene oxide hydration reactor and enter the multi-effect evaporation unit, evaporating excessive water, removing monoethylene glycol by the monoethylene glycol rectifying tower, and removing diethylene glycol by the diethylene glycol rectifying tower, wherein all or part of tower bottom liquid obtained after removing monoethylene glycol by the monoethylene glycol rectifying tower or diethylene glycol removed by the diethylene glycol rectifying tower is recycled, and tower bottom components of the diethylene glycol rectifying tower enter the triethylene glycol rectifying tower to obtain a triethylene glycol product at the top of the tower.
2. A novel method for increasing triethylene glycol production by an EOEG plant as claimed in claim 1, wherein the proportion of the diethylene glycol used in the partial recycling is 1-95%.
3. A novel method for increasing triethylene glycol production by an EOEG plant as claimed in claim 2, wherein the proportion of the diethylene glycol used in the partial recycling is 15-60%.
4. A novel method for triethylene glycol stimulation by an EOEG plant of claim 1 wherein diethylene glycol is fed back to the ethylene oxide hydration reactor either upstream or downstream of an ethylene oxide hydration feed pump.
5. A novel method for triethylene glycol stimulation by an EOEG plant as claimed in claim 1 wherein the inlet temperature of the ethylene oxide hydration reactor is 120-200 ℃ and the operating pressure is 10-25 barg.
6. A novel method for triethylene glycol stimulation by an EOEG plant as claimed in claim 5 wherein the inlet temperature of the ethylene oxide hydration reactor is 140-160 ℃ and the operating pressure is 15-21 barg.
7. A novel method for triethylene glycol stimulation by an EOEG plant of claim 1 wherein the reaction residence time of the ethylene oxide hydration reactor is 5-10 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115155091A (en) * | 2022-07-08 | 2022-10-11 | 三江乐天化工有限公司 | Polyethylene glycol separation system and separation method |
Citations (6)
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|---|---|---|---|---|
| JPS60126241A (en) * | 1983-12-13 | 1985-07-05 | Mitsui Toatsu Chem Inc | Production of triethylene glycol |
| US20050119510A1 (en) * | 2003-09-26 | 2005-06-02 | Boons Petrus J.G. | Process of preparing an alkylene glycol |
| KR20120091594A (en) * | 2011-02-09 | 2012-08-20 | 삼성토탈 주식회사 | A method for producing diethylene glycol from ethylene oxide with high yield |
| JP2013129613A (en) * | 2011-12-20 | 2013-07-04 | Mitsubishi Chemicals Corp | Method of producing trialkylene glycol |
| CN106518633A (en) * | 2016-10-17 | 2017-03-22 | 中石化上海工程有限公司 | Method for producing high-purity triethylene glycol |
| CN106542975A (en) * | 2016-10-17 | 2017-03-29 | 中石化上海工程有限公司 | The method of continuous production high-purity triethylene glycol |
-
2020
- 2020-10-19 CN CN202011119862.8A patent/CN112321397A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| JPS60126241A (en) * | 1983-12-13 | 1985-07-05 | Mitsui Toatsu Chem Inc | Production of triethylene glycol |
| US20050119510A1 (en) * | 2003-09-26 | 2005-06-02 | Boons Petrus J.G. | Process of preparing an alkylene glycol |
| KR20120091594A (en) * | 2011-02-09 | 2012-08-20 | 삼성토탈 주식회사 | A method for producing diethylene glycol from ethylene oxide with high yield |
| JP2013129613A (en) * | 2011-12-20 | 2013-07-04 | Mitsubishi Chemicals Corp | Method of producing trialkylene glycol |
| CN106518633A (en) * | 2016-10-17 | 2017-03-22 | 中石化上海工程有限公司 | Method for producing high-purity triethylene glycol |
| CN106542975A (en) * | 2016-10-17 | 2017-03-29 | 中石化上海工程有限公司 | The method of continuous production high-purity triethylene glycol |
Non-Patent Citations (2)
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| 吕百龄: "《实用工业助剂全书》", 31 August 2001 * |
| 编辑部: "《化工百科全书 第18卷 锌和锌合金-硬质合金》", 30 September 1998 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115155091A (en) * | 2022-07-08 | 2022-10-11 | 三江乐天化工有限公司 | Polyethylene glycol separation system and separation method |
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