CN106518633A - Method for producing high-purity triethylene glycol - Google Patents
Method for producing high-purity triethylene glycol Download PDFInfo
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- CN106518633A CN106518633A CN201610901096.8A CN201610901096A CN106518633A CN 106518633 A CN106518633 A CN 106518633A CN 201610901096 A CN201610901096 A CN 201610901096A CN 106518633 A CN106518633 A CN 106518633A
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- triethylene glycol
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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
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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
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- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for producing high-purity triethylene glycol. The method is mainly used for solving the problem in the prior art that the product quality is relatively poor. According to the method for producing the high-purity triethylene glycol, through adopting the technical scheme that a crude triethylene glycol solution enters a molecular still I so as to separate out a heavy component, distilled triethylene glycol distillate I serves as feedstock of a molecular still II, the molecular still I and the molecular still II are connected with a vacuumizing device, the heavy component separated by the molecular still I and a light component separated by the molecular still II are mixed so as to form a polyethylene glycol mixed solution, and triethylene glycol distillate II of the molecular still II is cooled by a product condenser and then enters an aftertreatment unit, the problem is solved in a relatively good manner; and the method can be applied to the production of the high-purity triethylene glycol.
Description
Technical field
The present invention relates to a kind of production method of high-purity triethylene glycol.
Background technology
Triethylene glycol (also known as triethylene glycol, is abbreviated as TEG) can as the solvent of Aromatics Extractive Project, rubber, cellulose nitrate it is molten
Agent and diesel fuel additives, rocket fuel.In addition in medicine, coating, weaving, printing and dyeing, food, papermaking, cosmetics, process hides, photograph
Extensive purposes is suffered from the industries such as phase, printing, intermetallic composite coating.It is commonly used to do the increasing of textile auxiliary, solvent, rubber and resin
Modeling agent, the Aromatics Extractive Project agent of the modifier of lubricating oil viscosity and reformation liquid.
Oxirane ethylene glycol (EO/EG) device production technology is ripe, and prior art mainly has the skills such as DOW, SD, Shell
Art, at home and abroad has knowhow for many years.Oxirane enters ethylene glycol reactor after mixing with water, in ethylene glycol reactor
In, the oxirane containing acetaldehyde is fully converted to ethylene glycol with water reaction.As the molal quantity of water in reaction feed is far above ring
Oxidative ethane, has minimal amount of diethylene glycol, triethylene glycol and many ethylene glycol to generate.Reactant liquor Jing multiple-effect evaporations, rectifying and dry
Dry dehydration obtains ethylene glycol product.In distillation process, minimal amount of diethylene glycol, triethylene glycol and many ethylene glycol are from rectifying column
Tower reactor is discharged.In prior art, many ethylene glycol solutions for mixing are undersold by most counting apparatus as byproduct.
Existing triethylene glycol production method typically uses fractional distillation refining.Highly purified triethylene glycol is wished to get, need to be by commercially available product
With vacuum distillation after anhydrous sodium sulfate dehydration 3 times, collect midbarrel and recrystallize 2 times again.The relatively low triethylene glycol price of purity
It is general at 8000 yuan/ton or so, content be more than 99.8% technical grade triethylene glycol price up to 11000～13000 yuan/
Ton.The present invention not only can recycle triethylene glycol, can also obtain good economic benefit.Document " the purposes of triethylene glycol
And preparation method " existing triethylene glycol production is introduced in (Sichuan chemical industry, the 1990, the 4th phase) essentially from epoxyethane water and second processed two
The accessory substance of alcohol, has following several synthetic methods in addition：1) epoxyethane water is legal；2) ethylene glycol is legal with epoxyethane water；
3) diethylene glycol (DEG) and ethylene oxide synthesis；4) triethylene glycol is prepared by raw material of alkylene carbonates.
The content of the invention
The technical problem to be solved is the poor problem of product quality in prior art, there is provided a kind of new height
The production method of purity triethylene glycol.The method has the preferable advantage of product quality.
For solving the above problems, the technical solution used in the present invention is as follows：A kind of production method of high-purity triethylene glycol,
Thick triethylene glycol solution enters molecular still I, isolates heavy constituent therein, the triethylene glycol distillate I for distillating as point
The charging of sub- distiller II, molecular still I, molecular still II are connected with vacuum extractor, and molecular still I is isolated
The light component that heavy constituent and molecular still II are isolated is mixed to form many ethylene glycol mixtures；Three second two of molecular still II
Alcohol distillate II enters post-processing unit Jing after the cooling of product condenser；The post-processing unit includes bleacher and full gear tank,
Triethylene glycol distillate when the aldehyde contenting amount in triethylene glycol distillate II is 50～99.99ppm, after the cooling of product condenser
II only by bleacher, obtains high-purity triethylene glycol product；When the aldehyde contenting amount in triethylene glycol distillate II be 100～
During 300ppm, the triethylene glycol distillate II after the cooling of product condenser passes sequentially through bleacher, full gear tank, obtains high-purity three
Ethylene glycol product.
In above-mentioned technical proposal, it is preferable that the decolorising agent in bleacher is selected from activated carbon, basic resin or molecular sieve；It is de-
The operating condition of color tank is：Temperature 25-40 DEG C, pressure 150-250KPa.
In above-mentioned technical proposal, it is preferable that the operating condition of molecular still I is：50～100 DEG C of operation temperature, operation
5～2000Pa of absolute pressure.
In above-mentioned technical proposal, it is preferable that the operating condition of molecular still II is：50～100 DEG C of operation temperature, operation
5～2000Pa of absolute pressure.
In above-mentioned technical proposal, it is preferable that in thick triethylene glycol solution, the mass content of triethylene glycol is 90～95%.
In above-mentioned technical proposal, it is preferable that the operating condition of full gear tank is：Temperature 25-40 DEG C, pressure 145-245KPa.
In above-mentioned technical proposal, it is preferable that the triethylene glycol distillate II Jing products condenser cooling of molecular still II
Post-processing unit is entered to after 25～40 DEG C.
In above-mentioned technical proposal, it is preferable that the purity of high-purity triethylene glycol product is more than 99.8wt% (mass fraction).
In above-mentioned technical proposal, it is preferable that the rate of recovery of high-purity triethylene glycol product is more than 75%.
Many ethylene glycol mixtures of by-product in glycol unit are carried out separating, are purified by the present invention, prepare economy more preferable
High-purity triethylene glycol product, it is by carrying out vacuum distillation to raw material triethylene glycol solution, especially with molecular clock, right
Heavy constituent carries out pre-separation.Obtain meeting high-purity three second two of commercially available prod requirement by rectification under vacuum and full gear desolventing technology
Alcohol product.It is an object of the invention to provide a kind of production method of high-purity triethylene glycol, high with raw material availability, bar is produced
Part is gentle, and device modulability is strong, the characteristics of stable, it is adaptable to existing EO/EG process units, can improve its economy effect
Benefit, achieves preferable technique effect.
Description of the drawings
Schematic flow sheets of the Fig. 1 for the method for the invention.
In Fig. 1,1 is molecular still I, and 2 is molecular still II, and 3 is bleacher, and 4 is full gear tank, and 5 is vacuum means
Put, 6 is thick triethylene glycol solution, and 7 is triethylene glycol distillate I, and 8 is triethylene glycol distillate II, and 9 is triethylene glycol product,
10 is many ethylene glycol mixtures.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Specific embodiment
【Embodiment 1】
A kind of production method of high-purity triethylene glycol, as shown in figure 1, the thick triethylene glycol solution (quality of triethylene glycol
92%) content is, into molecular still I, to isolate heavy constituent therein, and the triethylene glycol distillate I for distillating is steamed as molecule
The charging of device II is evaporated, molecular still I, molecular still II are connected with vacuum extractor, the restructuring that molecular still I is isolated
The light component isolated with molecular still II is divided to be mixed to form many ethylene glycol mixtures；The triethylene glycol of molecular still II evaporates
Go out liquid II and enter post-processing unit Jing after product condenser is cooled to 30 DEG C；The post-processing unit includes bleacher and full gear
Tank.
The operating condition of molecular still I is：80 DEG C of operation temperature, operates absolute pressure 50Pa；The operation of molecular still II
Condition is：Operation absolute pressure 80Pa, 83 DEG C of operation temperature；Decolorising agent in bleacher is activated carbon；The operating condition of bleacher is：
30 DEG C of temperature, pressure 150KPa.It is 78ppm that on-line analysis measures aldehyde contenting amount in triethylene glycol distillate II, and triethylene glycol evaporates
Go out liquid II only by bleacher, obtain high-purity triethylene glycol product, product purity (wt%) is：99.8%, colourity 23, cobalt molybdenum
Colourity, the rate of recovery 83% of high-purity triethylene glycol product.
【Embodiment 2】
A kind of production method of high-purity triethylene glycol, as shown in figure 1, the thick triethylene glycol solution (quality of triethylene glycol
85%) content is, into molecular still I, to isolate heavy constituent therein, and the triethylene glycol distillate I for distillating is steamed as molecule
The charging of device II is evaporated, molecular still I, molecular still II are connected with vacuum extractor, the restructuring that molecular still I is isolated
The light component isolated with molecular still II is divided to be mixed to form many ethylene glycol mixtures；The triethylene glycol of molecular still II evaporates
Go out liquid II and enter post-processing unit Jing after product condenser is cooled to 25 DEG C；The post-processing unit includes bleacher and full gear
Tank.
The operating condition of molecular still I is：60 DEG C of operation temperature, operates absolute pressure 50Pa；The operation of molecular still II
Condition is：Operation absolute pressure 50Pa, 10 DEG C of operation temperature；Decolorising agent in bleacher is activated carbon；The operating condition of bleacher is：
25 DEG C of temperature, pressure 150KPa.The operating condition of full gear tank is：30 DEG C of temperature, pressure 145KPa.
It is 145ppm that on-line analysis measures aldehyde contenting amount in triethylene glycol distillate II, and triethylene glycol distillate II leads to successively
Bleacher, full gear tank is crossed, high-purity triethylene glycol product is obtained, product purity (wt%) is：99.5%, colourity 25, cobalt molybdenum color
Degree, the rate of recovery 69% of high-purity triethylene glycol product.
【Embodiment 3】
A kind of production method of high-purity triethylene glycol, as shown in figure 1, the thick triethylene glycol solution (quality of triethylene glycol
95%) content is, into molecular still I, to isolate heavy constituent therein, and the triethylene glycol distillate I for distillating is steamed as molecule
The charging of device II is evaporated, molecular still I, molecular still II are connected with vacuum extractor, the restructuring that molecular still I is isolated
The light component isolated with molecular still II is divided to be mixed to form many ethylene glycol mixtures；The triethylene glycol of molecular still II evaporates
Go out liquid II and enter post-processing unit Jing after product condenser is cooled to 35 DEG C；The post-processing unit includes bleacher and full gear
Tank.
The operating condition of molecular still I is：80 DEG C of operation temperature, operates absolute pressure 100Pa；The operation of molecular still II
Condition is：Operation absolute pressure 90Pa, 78 DEG C of operation temperature；Decolorising agent in bleacher is activated carbon；The operating condition of bleacher is：
35 DEG C of temperature, pressure 250KPa.
It is 56ppm that on-line analysis measures aldehyde contenting amount in triethylene glycol distillate II, and triethylene glycol distillate II only passes through
Bleacher, obtains high-purity triethylene glycol product, and product purity (wt%) is：99.8%, colourity 22, cobalt molybdenum colourity, high-purity
The rate of recovery 78% of triethylene glycol product.
【Embodiment 4】
A kind of production method of high-purity triethylene glycol, as shown in figure 1, the thick triethylene glycol solution (quality of triethylene glycol
89%) content is, into molecular still I, to isolate heavy constituent therein, and the triethylene glycol distillate I for distillating is steamed as molecule
The charging of device II is evaporated, molecular still I, molecular still II are connected with vacuum extractor, the restructuring that molecular still I is isolated
The light component isolated with molecular still II is divided to be mixed to form many ethylene glycol mixtures；The triethylene glycol of molecular still II evaporates
Go out liquid II and enter post-processing unit Jing after product condenser is cooled to 33 DEG C；The post-processing unit includes bleacher and full gear
Tank.
The operating condition of molecular still I is：65 DEG C of operation temperature, operates absolute pressure 200Pa；The operation of molecular still II
Condition is：Operation absolute pressure 180Pa, 63 DEG C of operation temperature；Decolorising agent in bleacher is resin；The operating condition of bleacher is：
33 DEG C of temperature, pressure 160KPa.The operating condition of full gear tank is：33 DEG C of temperature, pressure 155KPa.
It is 138ppm that on-line analysis measures aldehyde contenting amount in triethylene glycol distillate II, and triethylene glycol distillate II leads to successively
Bleacher, full gear tank is crossed, high-purity triethylene glycol product is obtained, product purity (wt%) is：99.6%, colourity 25, cobalt molybdenum color
Degree, the rate of recovery 81% of high-purity triethylene glycol product.
【Embodiment 5】
A kind of production method of high-purity triethylene glycol, as shown in figure 1, the thick triethylene glycol solution (quality of triethylene glycol
93%) content is, into molecular still I, to isolate heavy constituent therein, and the triethylene glycol distillate I for distillating is steamed as molecule
The charging of device II is evaporated, molecular still I, molecular still II are connected with vacuum extractor, the restructuring that molecular still I is isolated
The light component isolated with molecular still II is divided to be mixed to form many ethylene glycol mixtures；The triethylene glycol of molecular still II evaporates
Go out liquid II and enter post-processing unit Jing after product condenser is cooled to 25 DEG C；The post-processing unit includes bleacher and full gear
Tank.
The operating condition of molecular still I is：95 DEG C of operation temperature, operates absolute pressure 280Pa；The operation of molecular still II
Condition is：Operation absolute pressure 125Pa, 85 DEG C of operation temperature；Decolorising agent in bleacher is resin；The operating condition of bleacher is：
25 DEG C of temperature, pressure 220KPa.
It is 88ppm that on-line analysis measures aldehyde contenting amount in triethylene glycol distillate II, and triethylene glycol distillate II only passes through
Bleacher, obtains high-purity triethylene glycol product, and product purity (wt%) is：99.6%, colourity 23, cobalt molybdenum colourity, high-purity
The rate of recovery 76% of triethylene glycol product.
【Comparative example】
According to art methods：Mass content be 93% thick triethylene glycol solution into after with anhydrous sodium sulfate dehydration
Carry out vacuum distillation, after vacuum distillation 3 times, midbarrel is carried out into recrystallization 2 times again.Obtain triethylene glycol product, product purity
(wt%) it is：99.5%, colourity 25, the triethylene glycol rate of recovery are 65%, can reach commercially available requirement, and process operation is complicated, device
Cost of equipment is high, and process energy consumption is higher.
Claims (9)
1. a kind of production method of high-purity triethylene glycol, thick triethylene glycol solution enter molecular still I, isolate therein
Heavy constituent, chargings of the triethylene glycol distillate I for distillating as molecular still II, molecular still I, molecular still II with
Vacuum extractor connects, and the light component that the heavy constituent and molecular still II that molecular still I is isolated is isolated is mixed to form
Many ethylene glycol mixtures；It is single that the triethylene glycol distillate II of molecular still II enters post processing Jing after the cooling of product condenser
Unit；The post-processing unit includes bleacher and full gear tank, when the aldehyde contenting amount in triethylene glycol distillate II be 50～
During 99.99ppm, the triethylene glycol distillate II after the cooling of product condenser obtains high-purity triethylene glycol only by bleacher
Product；When the aldehyde contenting amount in triethylene glycol distillate II is 100～300ppm, the triethylene glycol after the cooling of product condenser evaporates
Go out liquid II and pass sequentially through bleacher, full gear tank, obtain high-purity triethylene glycol product.
2. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that the decolorising agent choosing in bleacher
From activated carbon, basic resin or molecular sieve；The operating condition of bleacher is：Temperature 20-55 DEG C, pressure 100-500KPa.
3. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that the operation bar of molecular still I
Part is：50～100 DEG C of operation temperature, operates 5～2000Pa of absolute pressure.
4. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that the operation of molecular still II
Condition is：50～100 DEG C of operation temperature, operates 5～2000Pa of absolute pressure.
5. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that three in thick triethylene glycol solution
The mass content of ethylene glycol is 80-95%.
6. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that the operating condition of full gear tank is：
Temperature 20-55 DEG C, pressure 100-500KPa.
7. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that three second of molecular still II
Glycol distillate II enters post-processing unit Jing after product condenser is cooled to 20-55 DEG C.
8. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that high-purity triethylene glycol product
Purity be more than 99.5wt%.
9. the production method of high-purity triethylene glycol according to claim 1, it is characterised in that high-purity triethylene glycol product
The rate of recovery be more than 50%.
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Cited By (1)
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| CN112321397A (en) * | 2020-10-19 | 2021-02-05 | 中国石油化工股份有限公司 | Novel method for increasing yield of triethylene glycol by EOEG device |
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