CN108299204A - The separation method and device of dimethyl carbonate in coal-ethylene glycol raffinate - Google Patents
The separation method and device of dimethyl carbonate in coal-ethylene glycol raffinate Download PDFInfo
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- CN108299204A CN108299204A CN201810316849.8A CN201810316849A CN108299204A CN 108299204 A CN108299204 A CN 108299204A CN 201810316849 A CN201810316849 A CN 201810316849A CN 108299204 A CN108299204 A CN 108299204A
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- C07—ORGANIC CHEMISTRY
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- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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Abstract
The present invention relates to chemical fields, more particularly to coal-ethylene glycol field, more particularly in a kind of coal-ethylene glycol raffinate dimethyl carbonate method and device, the separator includes lightness-removing column, thick DMC rectifying columns and essence DMC rectifying columns, the first pipe for being sent into raw material is connected at the centre entrance of lightness-removing column, lightness-removing column is connected to side take-off tank inlet by second pipe, side take-off tank is connected to thick DMC rectifying columns by third pipeline, thick DMC rectifying columns are connected to by the 4th pipeline on smart DMC rectifying columns, smart DMC rectifying columns are connected to by the 5th pipeline in dimethyl oxalate storage tank, smart DMC rectifying columns are connected to side take-off tank tower top inlet by the 6th pipeline.The present invention is mainly that the recycling separation of dimethyl carbonate in ethylene glycol raffinate is completed by lightness-removing column, thick DMC rectifying columns and essence DMC rectifying columns, and the equipment used is simple, and low energy consumption, small investment, the dimethyl carbonate purity isolated is high, significantly reduces production cost, improves the performance of enterprises.
Description
Technical field
The present invention relates to chemical fields, more particularly to coal-ethylene glycol field more particularly to a kind of coal-ethylene glycol raffinate
The separation method and device of middle dimethyl carbonate.
Background technology
Dimethyl carbonate, also known as DMC, methyl carbonate, carbonic acid ethane dimethyl carbonate (DMC) are a kind of important organise
Work intermediate due to containing carbonyl, methyl, methoxyl group and carbomethoxy in its molecular structure, thus can be widely used for carbonyl
Change, methylate, the organic synthesis such as methoxylation and carbonvlmethyl, for producing makrolon, isocyanates, poly- amino
Formic acid esters, polycarbonate glycol, allyl diglycol carbonates, methylamino formic acid naphthalene ester (sevin), methyl phenyl ethers anisole, tetramethyl alcohol
Ammonium, long-chain alkyl carbonate, carbohydrazide, malonate, the third two urethane, diethyl carbonate, triphosgene, furazolidone, diazanyl first
A variety of chemical products such as sour methyl esters, anilino- methyl formate.Since DMC is nontoxic, the phosgene of alternative severe toxicity, methylchloroformate,
Dimethyl suflfate etc. is used as methylating agent or carbonyl agent, improves the safety of production operation, reduces environmental pollution.As
Solvent, the alternative freons of DMC, trichloroethanes, trichloro ethylene, benzene, dimethylbenzene etc. are for paint, cleaning solvent etc..Make
For gasoline additive, its octane number and oxygen content can be improved in DMC, and then improves its anti-knock properties [1].In addition, DMC can also be cleaned
Agent, surfactant and softening agent additive.Since purposes is very extensive, DMC is known as current organic synthesis " new base
Stone ".
In the production process of coal-ethylene glycol, the substances such as meeting by-product dimethyl carbonate, methyl formate, dimethoxym ethane influence
System stable operation, the fusel that the raffinate of coal-ethylene glycol coproduction at present regards cheap dimethyl carbonate are sold, formic acid
On the one hand methyl esters, dimethoxym ethane emptying, generate greatly pollution to environment in this way；On the other hand a large amount of methanol can also be lost and its spread out
Biology.Therefore rationally recycling dimethyl carbonate raffinate has great importance for the friendly process for developing clean environment firendly；Simultaneously
The methanol isolated, dimethyl carbonate mixture return system can create considerable economic benefit, improve the added value of raffinate.
Invention content
It is an object of the invention to overcome above-mentioned raw coal preparing ethylene glycol coproduction raffinate existing in the prior art cannot be reasonable
Recycling and processing and caused by environmental pollution, the wasting of resources the shortcomings of and a kind of energy saving, efficient coal-ethylene glycol raffinate is provided
The separation method and device of middle dimethyl carbonate.
To achieve the goals above, the technical scheme is that it is such：
The separation method and device of dimethyl carbonate in a kind of coal-ethylene glycol raffinate, this method comprises the following steps：
Step 1：The mixed material of the methanol, dimethyl carbonate of coproduction is from lightness-removing column centre entrance in coal-ethylene glycol production technology
Into lightness-removing column, tower reactor is the mixture of methanol, water and dimethyl carbonate, returns to intermediate tank farm methanol tank following as synthesis
Ring methanol uses, remaining removes light, heavy constituent material and is discharged into side take-off tank from lightness-removing column side take-off mouth；
Step 2：The side run-off of lightness-removing column enters thick DMC rectifying columns, methanol, carbon after rectifying from thick DMC rectifying columns centre entrance
Dimethyl phthalate and low boiler cut are discharged return fractionation zone intermediate storage tank from tower top and are used as recycle methanol, and content is higher than 90%
Dimethyl carbonate and methanol mixture from tower reactor be discharged；
Step 3：Higher than the mixture of 90% dimethyl carbonate and methanol from thick DMC tower bottom of rectifying tower by essence DMC rectifying columns
Upper entrance enters smart DMC rectifying columns, and methanol, azeotropic mixture flow into lightness-removing column side take-off tank from tower top；
Step 4：After dimethyl carbonate removes light, heavy constituent, the DMC addition flowed out from smart DMC rectifying columns side line is higher than
When 99.8% or more, side run-off is discharged into dimethyl oxalate storage tank, side take-off temperature is at 114-120 DEG C.
The method realizes that the device includes lightness-removing column, thick DMC rectifying columns and essence DMC rectifying columns, is taken off based on following apparatus
The first pipe for being sent into raw material, lightness-removing column side line outlet connection second pipe, second pipe are connected at the centre entrance of light tower
The other end be connected to side take-off tank inlet, the exit of side take-off tank connects third pipeline, and third pipeline is connected to
At the centre entrance of thick DMC rectifying columns, the tower reactor exit of thick DMC rectifying columns connects the 4th pipeline, and the 4th pipeline is connected to essence
On DMC rectifying columns, the 5th pipeline is connected at the centre exit of smart DMC rectifying columns, the 5th pipeline is connected to dimethyl oxalate storage tank
On, the upper end outlet of smart DMC rectifying columns connects the 6th pipeline, and the 6th pipeline is connected to side take-off tank tower top inlet.
The operating pressure of lightness-removing column is 6-10Kpa in the step 1, and tower top temperature is 42-49 DEG C, bottom temperature 65-
69℃。
The operating pressure of thick DMC rectifying columns is 1.0-1.1MPa, reflux ratio 0.5: 1-3: 1, tower top temperature in the step 2
Degree is 139-143 DEG C, and bottom temperature is 167-180 DEG C；The operating pressure of essence DMC rectifying columns is 0.01- in the step 3
0.014MPa, reflux ratio 3: 1-6: 1, bottom temperature are 118-125 DEG C, and tower top temperature is at 95-100 DEG C.
Lightness-removing column overhead fraction is the mixing of methyl formate, dimethoxym ethane and Trace Methanol, dimethyl carbonate in the step 1
Object is discharged into fusel storage tank.
The recombination that essence DMC tower bottom of rectifying tower is discharged in the step 3 is distributed into fusel storage tank.
The tower top outlet of lightness-removing column connects the 7th pipeline, and the 7th pipeline is connected on fusel storage tank, and the tower reactor of lightness-removing column goes out
The 8th pipeline is connected at mouthful, the 8th pipeline is connected between on the methanol tank of tank field and is used as synthesis system recycle methanol.
The 9th pipeline of tower reactor outlet connection of smart DMC rectifying columns, the 9th pipeline are connected on fusel storage tank.
The lightness-removing column includes mainly lightness-removing column main body, reboiler, overhead condenser, tail condenser, return tank, kettle liquid
Pump, lateral line discharging pump and reflux pump, lightness-removing column include two reboilers, and the heat source of two reboilers is respectively by thick DMC rectifying columns
And essence DMC rectifying tower top gaseous phases provide.
The thick DMC rectifying columns include mainly thick DMC rectifying columns main body, reboiler, overhead condenser, return tank and reflux
Pump, wherein overhead condenser are lightness-removing column kettle reboiler；The essence DMC rectifying columns include reboiler, overhead condenser, return tank
And reflux pump, wherein overhead condenser is lightness-removing column kettle reboiler.
The good effect that technical scheme of the present invention generates is as follows：As a result of rationally efficient industrialization recycling separation
Method has the following advantages：
1, the heat source of lightness-removing column is provided by thick DMC rectifying columns, essence DMC rectifying tower top gaseous phases, and energy is utilized effectively；
2, light component methyl formate, the dimethoxym ethane in system are separated from lightness-removing column, keep synthesis system light component balance,
Synchronous fluorimetry synthesis system recycle methanol quality；
3, it by the side reaction product DMC separating-purifyings of synthesis, is sold as product, to maintain synthesis system dimethyl carbonate to contain
Amount is stablized；
4, the present invention has the characteristics that flow is simple, investment is small, the rate of recovery is high, and products obtained therefrom is the carbonic acid for meeting high-class product index
Dimethyl ester, dimethyl carbonate purity are higher than 99.9%.
Description of the drawings
Fig. 1 is the connection diagram of the separator of dimethyl carbonate in coal-ethylene glycol raffinate of the present invention.
Fig. 2 is the flow chart of the separation method of dimethyl carbonate in coal-ethylene glycol raffinate of the present invention.
It is labeled as in figure：1, lightness-removing column；2, thick DMC rectifying columns；3, essence DMC rectifying columns；4, side take-off tank；5, carbonic acid two
Methyl esters storage tank；6, fusel storage tank；101, first pipe；102, second pipe；103, third pipeline；104, the 4th pipeline；105、
5th pipeline；106, the 6th pipeline；107, the 7th pipeline；108, the 8th pipeline；109, the 9th pipeline.
Specific implementation mode
With reference to specific embodiments and the drawings to the separation side of dimethyl carbonate in the coal-ethylene glycol raffinate of the present invention
Method and device are further elaborated and illustrate.
The separator of dimethyl carbonate in a kind of coal-ethylene glycol raffinate, as shown in Figure 1, a kind of coal-ethylene glycol raffinate
The separator of middle dimethyl carbonate, the separator include lightness-removing column 1, thick DMC rectifying columns 2 and essence DMC rectifying columns 3, are taken off light
The first pipe 101 for being sent into raw material is connected at the centre entrance of tower, the tower top outlet of lightness-removing column connects the 7th pipeline 107, the
Seven pipelines are connected on fusel storage tank 6；The tower reactor exit of lightness-removing column connects the 8th pipeline 108, and the 8th pipeline is connected between
It is used as synthesis system recycle methanol on the methanol tank of tank field.The 9th pipeline of tower reactor outlet connection of smart DMC rectifying columns, the 9th
Pipeline is connected on fusel storage tank.Lightness-removing column side line outlet connection second pipe, the other end of second pipe are connected to side line and adopt
Go out tank inlet, the exit of side take-off tank connects third pipeline, and third pipeline is connected to the centre entrance of thick DMC rectifying columns
The tower reactor exit at place, thick DMC rectifying columns connects the 4th pipeline, and the 4th pipeline is connected on smart DMC rectifying columns, smart DMC rectifying
The 5th pipeline is connected at the centre exit of tower, the 5th pipeline is connected in dimethyl oxalate storage tank, is brought out on smart DMC rectifying columns
Mouthful the 6th pipeline of connection, the 6th pipeline are connected to side take-off tank tower top inlet, the tower reactor outlet connection of smart DMC rectifying columns the
Nine pipelines, the 9th pipeline are connected on the second fusel storage tank.
The lightness-removing column includes mainly lightness-removing column main body, reboiler, overhead condenser, tail condenser, return tank, kettle liquid
Pump, lateral line discharging pump and reflux pump, lightness-removing column include two reboilers, and the heat source of two reboilers is respectively by thick DMC rectifying columns
And essence DMC rectifying tower top gaseous phases provide.
The thick DMC rectifying columns include mainly thick DMC rectifying columns main body, reboiler, overhead condenser, return tank and reflux
Pump, wherein overhead condenser are lightness-removing column kettle reboiler；The essence DMC rectifying columns include reboiler, overhead condenser, return tank
And reflux pump, wherein overhead condenser is lightness-removing column kettle reboiler.
A kind of separation method using the separator of dimethyl carbonate in above-mentioned coal-ethylene glycol raffinate, as shown in Fig. 2,
This method comprises the following steps：
Step 1：The mixed material of the methanol, dimethyl carbonate of coproduction enters from 1 middle part of lightness-removing column in coal-ethylene glycol production technology
Mouth enters lightness-removing column, and methanol accounts for 56% or so in mixed material, dimethyl carbonate 38% or so；Lightness-removing column overhead fraction is 60% left
Right methyl formate, more than 30% dimethoxym ethane and 5% or so methanol, 1% or so the mixture of dimethyl carbonate be discharged into fusel storage
Tank 6, tower reactor are that the mixture of 54% or so methanol, 45% or so dimethyl carbonate and 1% or so water returns to intermediate tank farm methanol
Storage tank is used as recycle methanol, remaining removing is light, 65% or so methanol of heavy constituent and 33% or so dimethyl carbonate from
Lightness-removing column side line is discharged into side take-off tank 4；The operating pressure of lightness-removing column is 6-10Kpa in the step 1, and tower top temperature is
42-49 DEG C, bottom temperature is 65-69 DEG C；
Step 2：The side run-off of lightness-removing column enters thick DMC rectifying columns 2,80% first after rectifying from thick DMC rectifying columns centre entrance
Alcohol, 20% dimethyl carbonate and micro low boiler cut from tower top discharge intermediate tank farm methanol storage tank as synthesis system cycle
Methanol uses, and the mixture of dimethyl carbonate of the content higher than 90% and methanol is discharged from tower reactor；Thick DMC rectifying in the step 2
The operating pressure of tower is 1.0-1.1MPa, and reflux ratio 0.5: 1-3: 1, tower top temperature is 139-143 DEG C, bottom temperature 167-
180℃；
Step 3：Higher than the mixture of 90% dimethyl carbonate and methanol smart DMC rectifying is passed into from thick DMC tower bottom of rectifying tower
3 middle and upper part entrance of tower enters smart DMC rectifying columns, and methanol content is less than the slave tower top stream that 20%, DMC addition is more than 80%
Enter lightness-removing column side take-off tank, 90% or more dimethyl carbonate of tower reactor discharge is sent into fusel storage tank；Essence DMC in the step 3
The operating pressure of rectifying column is 0.01-0.014MPa, and reflux ratio 3: 1-6: 1, bottom temperature is 118-125 DEG C, tower top temperature
At 95-100 DEG C；
Step 4：After dimethyl carbonate removes light, heavy constituent, the material flowed out from smart DMC rectifying columns side line meets following index：
Appearance is that water white transparency is more than 99.8%, methanol content and is less than less than 0.05%, water content without mechanical admixture, DMC addition
0.02%, acidity is less than 25mmol/100g, coloration is less than 5#, side run-off is discharged into dimethyl oxalate storage tank 5, side take-off
Temperature is at 114-120 DEG C.
Claims (9)
1. the separation method and device of dimethyl carbonate in a kind of coal-ethylene glycol raffinate, it is characterised in that：This method includes such as
Lower step：
Step 1：The mixed material of the methanol, dimethyl carbonate of coproduction is from lightness-removing column centre entrance in coal-ethylene glycol production technology
Into lightness-removing column, tower reactor is the mixture of methanol, water and dimethyl carbonate, returns to intermediate tank farm methanol tank following as synthesis
Ring methanol uses, remaining removes light, heavy constituent material and is discharged into side take-off tank from lightness-removing column side take-off mouth；
Step 2：The side run-off of lightness-removing column enters thick DMC rectifying columns, methanol, carbon after rectifying from thick DMC rectifying columns centre entrance
Dimethyl phthalate and low boiler cut are discharged return fractionation zone intermediate storage tank from tower top and are used as recycle methanol, and content is higher than 90%
Dimethyl carbonate and methanol mixture from tower reactor be discharged；
Step 3：Higher than the mixture of 90% dimethyl carbonate and methanol from thick DMC tower bottom of rectifying tower by essence DMC rectifying columns
Upper entrance enters smart DMC rectifying columns, and methanol, azeotropic mixture flow into lightness-removing column side take-off tank from tower top；
Step 4：After dimethyl carbonate removes light, heavy constituent, the DMC addition flowed out from smart DMC rectifying columns side line is higher than
When 99.8% or more, side run-off is discharged into dimethyl oxalate storage tank, side take-off temperature is at 114-120 DEG C；
The method realizes that the device includes lightness-removing column, thick DMC rectifying columns and essence DMC rectifying columns, lightness-removing column based on following apparatus
Centre entrance at be connected be sent into raw material first pipe, lightness-removing column side line outlet connection second pipe, second pipe it is another
One end is connected to side take-off tank inlet, and the exit of side take-off tank connects third pipeline, and third pipeline is connected to thick DMC
At the centre entrance of rectifying column, the tower reactor exit of thick DMC rectifying columns connects the 4th pipeline, and the 4th pipeline is connected to smart DMC essences
It evaporates on tower, the 5th pipeline is connected at the centre exit of smart DMC rectifying columns, the 5th pipeline is connected in dimethyl oxalate storage tank, essence
The upper end outlet of DMC rectifying columns connects the 6th pipeline, and the 6th pipeline is connected to side take-off tank tower top inlet.
2. the separation method and device of dimethyl carbonate, feature exist in coal-ethylene glycol raffinate according to claim 1
In：The operating pressure of lightness-removing column is 6-10Kpa in the step 1, and tower top temperature is 42-49 DEG C, and bottom temperature is 65-69 DEG C.
3. the separation method and device of dimethyl carbonate, feature exist in coal-ethylene glycol raffinate according to claim 1
In：The operating pressure of thick DMC rectifying columns is 1.0-1.1MPa in the step 2, and reflux ratio 0.5: 1-3: 1, tower top temperature is
139-143 DEG C, bottom temperature is 167-180 DEG C；The operating pressure of essence DMC rectifying columns is 0.01- in the step 3
0.014MPa, reflux ratio 3: 1-6: 1, bottom temperature are 118-125 DEG C, and tower top temperature is at 95-100 DEG C.
4. the separation method and device of dimethyl carbonate, feature exist in coal-ethylene glycol raffinate according to claim 1
In：Lightness-removing column overhead fraction is methyl formate, dimethoxym ethane and Trace Methanol in the step 1, the mixture of dimethyl carbonate is arranged
Enter fusel storage tank.
5. the separation method and device of dimethyl carbonate, feature exist in coal-ethylene glycol raffinate according to claim 1
In：The recombination that essence DMC tower bottom of rectifying tower is discharged in the step 3 is distributed into fusel storage tank.
6. according to the separation method and device of dimethyl carbonate in the coal-ethylene glycol raffinate described in claim 1, feature
It is：The tower top outlet of lightness-removing column connects the 7th pipeline, and the 7th pipeline is connected on fusel storage tank, the tower reactor exit of lightness-removing column
The 8th pipeline is connected, the 8th pipeline is connected between on the methanol tank of tank field and is used as synthesis system recycle methanol.
7. according to the separation method and device of dimethyl carbonate in the coal-ethylene glycol raffinate described in claim 1, feature
It is：The 9th pipeline of tower reactor outlet connection of smart DMC rectifying columns, the 9th pipeline are connected on fusel storage tank.
8. according to the separation method and device of dimethyl carbonate in the coal-ethylene glycol raffinate described in claim 1, feature
It is：The lightness-removing column includes mainly lightness-removing column main body, reboiler, overhead condenser, tail condenser, return tank, kettle liquid pump, side
Line discharging pump and reflux pump, lightness-removing column include two reboilers, and the heat source of two reboilers is respectively by thick DMC rectifying columns and essence
DMC rectifying tower top gaseous phases provide.
9. according to the separation method and device of dimethyl carbonate in the coal-ethylene glycol raffinate described in claim 1, feature
It is：The thick DMC rectifying columns mainly include thick DMC rectifying columns main body, reboiler, overhead condenser, return tank and reflux pump,
Wherein overhead condenser is lightness-removing column kettle reboiler；The essence DMC rectifying columns include reboiler, overhead condenser, return tank and
Reflux pump, wherein overhead condenser are lightness-removing column kettle reboiler.
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Cited By (7)
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| CN109970565A (en) * | 2019-03-05 | 2019-07-05 | 天津中昊天久工程技术有限公司 | The technique of pressurization coupling fusion-crystallization final cell liquid grade dimethyl carbonate |
| CN110124345A (en) * | 2019-05-16 | 2019-08-16 | 江苏凯美普瑞工程技术有限公司 | A kind of methyl formate separation system and methyl formate separation and purification technique |
| CN111170863A (en) * | 2020-03-16 | 2020-05-19 | 天津市新天进科技开发有限公司 | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration |
| CN112679352A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Refining method and system for mixed material flow containing dimethyl carbonate |
| CN113372222A (en) * | 2021-05-20 | 2021-09-10 | 山东华鲁恒升化工股份有限公司 | Method for separating coal-to-ethylene glycol coupling esterification process by-product |
| CN113636936A (en) * | 2021-08-16 | 2021-11-12 | 山西沃能化工科技有限公司 | Device and method for improving recovery rate of byproduct DMC in process of preparing ethylene glycol from synthesis gas |
| CN114957008A (en) * | 2021-02-18 | 2022-08-30 | 上海浦景化工技术股份有限公司 | Separation and purification method of byproducts in coal-to-ethylene glycol process |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970565A (en) * | 2019-03-05 | 2019-07-05 | 天津中昊天久工程技术有限公司 | The technique of pressurization coupling fusion-crystallization final cell liquid grade dimethyl carbonate |
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| CN110124345A (en) * | 2019-05-16 | 2019-08-16 | 江苏凯美普瑞工程技术有限公司 | A kind of methyl formate separation system and methyl formate separation and purification technique |
| CN112679352A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Refining method and system for mixed material flow containing dimethyl carbonate |
| CN112679352B (en) * | 2019-10-18 | 2023-04-07 | 中国石油化工股份有限公司 | Refining method and system for mixed material flow containing dimethyl carbonate |
| CN111170863A (en) * | 2020-03-16 | 2020-05-19 | 天津市新天进科技开发有限公司 | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration |
| CN114957008A (en) * | 2021-02-18 | 2022-08-30 | 上海浦景化工技术股份有限公司 | Separation and purification method of byproducts in coal-to-ethylene glycol process |
| CN114957008B (en) * | 2021-02-18 | 2024-03-19 | 上海浦景化工技术股份有限公司 | Separation and purification method of byproducts in coal-to-ethylene glycol process |
| CN113372222A (en) * | 2021-05-20 | 2021-09-10 | 山东华鲁恒升化工股份有限公司 | Method for separating coal-to-ethylene glycol coupling esterification process by-product |
| CN113636936A (en) * | 2021-08-16 | 2021-11-12 | 山西沃能化工科技有限公司 | Device and method for improving recovery rate of byproduct DMC in process of preparing ethylene glycol from synthesis gas |
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