CN115991634A - Production method of triethylene glycol - Google Patents
Production method of triethylene glycol Download PDFInfo
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- CN115991634A CN115991634A CN202111215045.7A CN202111215045A CN115991634A CN 115991634 A CN115991634 A CN 115991634A CN 202111215045 A CN202111215045 A CN 202111215045A CN 115991634 A CN115991634 A CN 115991634A
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Abstract
The invention provides a production method of triethylene glycol, which belongs to the technical field of chemical industry and comprises the steps of boosting Ethylene Oxide (EO) through an EO feed pump, boosting diethylene glycol (DEG) through the DEG feed pump, mixing with the diethylene glycol (DEG) in a static mixer, heating to a reaction temperature in a preheater, and directly reacting diethylene glycol with ethylene oxide in a triethylene glycol (TEG) reactor to generate triethylene glycol. The invention can be used for the transformation of the existing EO/EG device, has small modification and strong adaptability, can obviously increase the quantity of the byproduct TEG, has simple preparation process and high yield, can be flexibly produced according to market change, and has larger market application and popularization value.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a production method of triethylene glycol.
Background
Triethylene glycol (also known as triethylene glycol, abbreviated as TEG) can be used as a solvent for aromatic hydrocarbon extraction, a solvent for rubber and nitrocellulose, a diesel additive and rocket fuel. In addition, the coating 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. The aromatic hydrocarbon extractant is commonly used as textile auxiliary, solvent, plasticizer of rubber and resin, modifier of lubricating oil viscosity and aromatic hydrocarbon extractant of reformate.
With the development of natural gas chemical industry, triethylene glycol is mainly used for natural gas dehydration, and compared with other solvents, the triethylene glycol solvent has a series of advantages of good thermal stability and the like, and the market is in short supply.
Domestic TEG products are mainly byproducts in the production of ethylene glycol. The production technology of ethylene oxide/ethylene glycol (EO/EG) is mature, the prior art mainly comprises the production technology of large chemical companies such as DOW, SD, shell, and has production experience for many years at home and abroad. The production technology mainly comprises the following steps: ethylene Oxide (EO) is mixed with water and fed to an Ethylene Glycol (EG) reactor where the acetaldehyde-containing ethylene oxide is fully converted to ethylene glycol by reaction with water. Since the molar number of water in the reaction feed is much higher than that of ethylene oxide, very small amounts of diethylene glycol, triethylene glycol and polyethylene glycol are formed. The reaction liquid is subjected to multi-effect evaporation, rectification, drying and dehydration to obtain an ethylene glycol product. By-products of little diethylene glycol, triethylene glycol and polyethylene glycol. In the prior art, the production of triethylene glycol in EO/EG production technology is minimum, about 0.4% of the ethylene glycol production and 5% of the diethylene glycol production. Diethylene glycol market price 4600 yuan, technical grade triethylene glycol market price 10300 yuan. At present, ethylene glycol, diethylene glycol is at the edges of profit and deficiency, triethylene glycol has strong profit capability, but the yield is small, and the market demand can not be met far, and if diethylene glycol with low added value can be converted into triethylene glycol, the economic benefit can be obviously increased.
Patent CN201610903407.4 discloses a method for continuously producing high-purity triethylene glycol, which adopts a high-vacuum wiped film evaporator, and can obtain triethylene glycol with the purity (wt%) of 99.8%; patent CN201610901096.8 only solves the problem of poor product quality in the prior art, but does not fundamentally solve the problems of low triethylene glycol yield and inability to meet the market dosage. Patent CN201610901096.8 provides a method for continuously producing high-purity triethylene glycol, which is complicated in production apparatus and does not solve the problem of low triethylene glycol yield.
Disclosure of Invention
The invention aims to provide a production method of triethylene glycol, which has good anti-aging effect.
The technical scheme of the invention is realized as follows:
the invention provides a production method of triethylene glycol, ethylene oxide is boosted by an EO feed pump and then is mixed with diethylene glycol by a DEG feed pump, the mixture is fed into a static mixer, then is fed into a preheater, is heated to the reaction temperature, and is fed into a TEG reactor, and diethylene glycol and ethylene oxide are directly reacted in the reactor to generate triethylene glycol.
As a further improvement of the present invention, the diethylene glycol is pure diethylene glycol or an aqueous diethylene glycol solution.
As a further improvement of the invention, the mass ratio of the diethylene glycol to the ethylene oxide is 2-15:1.
As a further improvement of the invention, the purity of the ethylene oxide is not lower than 99.5 percent, and the temperature is between minus 5 ℃ and 60 ℃.
As a further improvement of the present invention, the purity of the pure diethylene glycol is not less than 99%.
As a further improvement of the present invention, the static mixer is selected from one of SK type static mixer, jet mixer, SMV static mixer.
As a further improvement of the present invention, the TEG reactor is a tubular reactor or a loop reactor.
As a further development of the invention, the residence time in the tube reactor is from 0.1 to 10 hours.
As a further improvement of the invention, the reaction temperature of the TEG reactor is 60-250 ℃ and the reaction pressure is 5-25 barg.
The invention further protects a device applied to the production method of triethylene glycol, the device comprises an EO feed pump and a DEG feed pump, the outlet ports of the EO feed pump and the DEG feed pump are respectively and simultaneously connected to a static mixer, and then a preheater and a TEG reactor are sequentially arranged.
The invention has the following beneficial effects: aiming at the low triethylene glycol yield in the existing market, the invention designs a new production flow, ethylene oxide is boosted by an EO feed pump and then is boosted by a DEG feed pump with diethylene glycol, the mixture is fed into a static mixer for mixing, then is fed into a preheater, is heated to the reaction temperature, and is fed into a TEG reactor, and diethylene glycol and ethylene oxide are directly reacted in the reactor to generate triethylene glycol. The invention can be used for the transformation of the existing EO/EG device, has small modification and strong adaptability, can obviously increase the quantity of the byproduct TEG, has simple preparation process and high yield, can be flexibly produced according to market change, and has larger market application and popularization value.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic view of a triethylene glycol production apparatus;
wherein, EO feed pump; DEG feed pump; 3. a static mixer; 4. a preheater; teg reactor.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, an apparatus for use in a process for producing triethylene glycol comprises an EO feed pump 1 and a DEG feed pump 2, the outlets of the EO feed pump 1 and the DEG feed pump 2 being simultaneously connected to a static mixer 3, respectively, followed by a preheater 4 and a TEG reactor 5 in this order.
Example 1
10kg/hr EO (purity 99.6%) at-5 deg.C is boosted to 16barg by EO feed pump 1, 50kg/hr DEG (purity 99.1%) is boosted to 16barg by DEG feed pump 2, mixed in static mixer 3, static mixer 3 adopts SK type static mixer, preheated by preheater 4 after uniform mixing, preheated by 10barg steam, the reaction liquid is heated to 140 deg.C and then enters TEG reactor 5, the reaction pressure of TEG reactor 5 is 15barg, residence time is 10min, the temperature after reaction is raised to 175 deg.C, the TEG content of reaction liquid at the outlet of the reactor is 44%, and the TEG yield is 26.4kg/hr.
Example 2
10kg/hr, EO (purity 99.6%) at-5 ℃ is boosted to 25barg by an EO feed pump, DEG (purity 99.1%) at 50kg/hr is boosted to 25barg by the DEG feed pump, and mixed in a static mixer, the static mixer adopts an SK type static mixer, the mixture is preheated by a preheater after uniform mixing, the preheater is heated by steam of 40barg, the reaction liquid is heated to 250 ℃ and then enters a TEG reactor, the reaction pressure of the TEG reactor is 25barg, the residence time is 6min, the temperature rise value after the reaction is 285 ℃, the TEG content at the outlet of the reactor is 45%, and the TEG yield is 27.0kg/hr.
Example 3
10kg/hr, EO (purity 99.6%) at-5 ℃ is boosted to 16barg by an EO feed pump, DEG (purity 99.1%) at-5 ℃ is boosted to 16barg by the DEG feed pump, and mixed in a static mixer, the static mixer adopts an SK type static mixer, the mixture is preheated by a preheater after uniform mixing, the preheater is heated by steam of 10barg, the reaction liquid is heated to 150 ℃ and then enters a TEG reactor, the reaction pressure of the TEG reactor is 15barg, the residence time is 18min, the temperature rise value after the reaction is 155 ℃, the TEG content of the reaction liquid at the outlet of the reactor is 8.5%, and the TEG yield is 26.35kg/hr.
Example 4
10kg/hr, EO at-5 deg.C (purity 99.6%) is boosted to 16barg by EO feed pump, 100kg/hr DEG water solution (purity 50%) is boosted to 16barg by DEG feed pump, mixed with EO in static mixer, SMV type static mixer is adopted in static mixer, preheated by preheater after uniform mixing, heated by steam of 10barg, the reaction liquid is heated to 150 deg.C, then fed into TEG reactor, reaction pressure of TEG reactor is 15barg, residence time is 5h, temperature rise after reaction is 171 deg.C, TEG purity of reaction liquid at outlet of reactor is 8%, TEG yield is 8.8kg/hr.
Comparative example 1
A certain 7 kiloton/year glycol device is provided, 7550kg/h EO water solution (EO concentration is 10%) is pumped and sent to a preheater to be preheated to 160 ℃ and then enters an EO hydration reactor, the residence time of the reactor is 9min, the reaction pressure is 21barg, the reaction product enters a dehydration tower, the dehydration tower is heated by steam to remove water in the reaction liquid, the mixture of non-aqueous MEG, DEG and TEG is discharged from the tower bottom, the mixture is pumped to a MEG rectifying tower, 875kg/hr MEG is obtained at the tower top, the mixture of 140kg DEG and TEG at the tower bottom enters the DEG tower, 65kg/hr DEG product is obtained at the tower top, the tower bottom is sent to the TEG rectifying tower, and 0.56kg/hr TEG product is obtained at the tower top, so that the commercial requirement can be met, the operation of the process is complex, the equipment cost of the device is high, and the process energy consumption is high.
As is evident from the comparison of example 1 and comparative example 1, the method of the present invention can significantly increase TEG.
Compared with the prior art, the invention designs a new production flow aiming at low triethylene glycol yield in the existing market, ethylene oxide is boosted by an EO feed pump and then mixed with diethylene glycol by a DEG feed pump, and then enters a static mixer, and the mixture is heated to the reaction temperature and enters a TEG reactor, wherein diethylene glycol and ethylene oxide directly react in the reactor to generate triethylene glycol. The invention can be used for the transformation of the existing EO/EG device, has small modification and strong adaptability, can obviously increase the quantity of the byproduct TEG, has simple preparation process and high yield, can be flexibly produced according to market change, and has larger market application and popularization value.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A production method of triethylene glycol (TEG) is characterized in that Ethylene Oxide (EO) is boosted by an EO feed pump and then mixed with diethylene glycol (DEG) by a DEG feed pump, the mixture is fed into a static mixer, then fed into a preheater, heated to a reaction temperature, fed into a TEG reactor, and diethylene glycol and ethylene oxide directly react in the reactor to generate triethylene glycol.
2. The process for producing triethylene glycol according to claim 1, wherein the diethylene glycol is pure ethylene glycol or an aqueous diethylene glycol solution.
3. The process for producing triethylene glycol according to claim 1, wherein the mass ratio of diethylene glycol to ethylene oxide is 2 to 15:1.
4. The method for producing triethylene glycol according to claim 1, wherein the purity of ethylene oxide is not lower than 99.5% and the temperature is-5 to 60 ℃.
5. The method for producing triethylene glycol according to claim 2, wherein the purity of the pure diethylene glycol is not less than 99%.
6. The method for producing triethylene glycol according to claim 1, wherein the static mixer is one selected from the group consisting of SK type static mixer, jet mixer, SMV static mixer.
7. The process for producing triethylene glycol according to claim 1, wherein the TEG reactor is a tubular reactor or a loop reactor.
8. The process for producing triethylene glycol according to claim 7, wherein the residence time in the tubular reactor is 0.1 to 10 hours.
9. The process for producing triethylene glycol according to claim 1, wherein the reaction temperature of the TEG reactor is 60 to 250 ℃ and the reaction pressure is 5 to 25barg.
10. An apparatus for use in a process for producing triethylene glycol as claimed in claim 1, wherein the apparatus comprises an EO feed pump (1) and a DEG feed pump (2), and the outlets of the EO feed pump (1) and the DEG feed pump (2) are simultaneously connected to a static mixer (3) respectively, followed by a preheater (4) and a TEG reactor (5) in this order.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111215045.7A CN115991634A (en) | 2021-10-19 | 2021-10-19 | Production method of triethylene glycol |
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| CN202111215045.7A CN115991634A (en) | 2021-10-19 | 2021-10-19 | Production method of triethylene glycol |
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| CN115991634A true CN115991634A (en) | 2023-04-21 |
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