CN104262177B - A kind of separation purification method of thick diglycolamine - Google Patents
A kind of separation purification method of thick diglycolamine Download PDFInfo
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- CN104262177B CN104262177B CN201410442723.7A CN201410442723A CN104262177B CN 104262177 B CN104262177 B CN 104262177B CN 201410442723 A CN201410442723 A CN 201410442723A CN 104262177 B CN104262177 B CN 104262177B
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Abstract
The invention discloses a kind of separation purification method of thick diglycolamine, thick diglycolamine that glycol ether catalytic ammoniation is obtained under the condition of pressurization or normal pressure successively by eight tower continuous still batterys, diglycolamine, morpholine, glycol ether are separated from unreacted raw material and impurity, obtain the diglycolamine product of purity more than 99%, by-product morpholine, reclaims unreacted glycol ether simultaneously; Described eight towers are followed successively by deammoniation tower, normal pressure azeotrope column, vacuum dehydration column, vacuum morpholine recovery tower, vacuum diglycolamine lightness-removing column, vacuum diglycolamine tower, vacuum glycol ether lightness-removing column and vacuum glycol ether recovery tower.Separation and purification process energy consumption of the present invention is low, and flow process is simple, easy to operate, obtain the diglycolamine product of purity more than 99% and the morpholine byproduct of purity more than 99.5%, and productive rate reaches 99.5%.
Description
One, technical field
The present invention relates to a kind of process for purification, specifically a kind of separation purification method of thick diglycolamine.
Two, background technology
Diglycolamine, also known as 2-(2-amino ethoxy) ethanol, molecular formula C
4h
11nO
2, being colorless syrup liquid, is a kind of important solvent and organic raw material, energy and water dissolution, can dissolve aromatic hydrocarbons and absorb sour gas (H
2s and CO
2).The main absorption agent as sour gas, tensio-active agent and wetting agent, sweetening agent, also can be used as the raw material of polymkeric substance, extensive at industrial applications such as metal, electronics, medicine.
Catalytic ammoniation can be there is under catalyzer existent condition and be obtained by reacting in diglycolamine by glycol ether and ammonia, in building-up process, side reaction is many, except diglycolamine, also 20 plurality of impurities such as morpholine, N-methylmorpholine, N-ethylmorpholine, ethylene glycol monomethyl ether, glycol ether, water are contained in thick diglycolamine, and not easily separated.Also there is no a kind of method of effective separation diglycolamine at home under prior art, be only separated the report of diglycolamine in laboratory, but its separating effect is poor, can not be used for suitability for industrialized production.
Three, summary of the invention
The present invention aims to provide a kind of separation purification method of thick diglycolamine, and technical problem to be solved is by diglycolamine separating-purifying from numerous by product, obtains diglycolamine sterling.The inventive method can make the purity of diglycolamine reach more than 99%.
The thick diglycolamine that the present invention uses is catalytic ammoniation method self-control synthesis, and in thick diglycolamine, diglycolamine content is 35%, and concrete preparation process is as follows:
1, before reaction feeds intake, first use the air in nitrogen replacement reactor, then the hydrogen of preheating is continued to pass in reactor, make that the catalyst temperature in reactor rises to 180-240 DEG C, pressure in reactor rises to 1.60-1.75MPa;
2, gas mixture is mixed to get after liquid ammonia vaporization with hydrogen, by described charge heating to 240-280 DEG C;
3, glycol ether and soft water are mixed to get mixed solution, described mixed solution is preheated to 230-280 DEG C;
4, the mixed solution after the gas mixture after step 2 preheating and step 3 preheating is sent in reactor, liquid phase catalytic ammoniation reaction (reaction is successive reaction) is carried out in the presence of a catalyst at 1.60-1.75MPa, 180-240 DEG C, obtain crude product, through gas-liquid separator separates gas and liquid after obtained crude product cooling, gas main component is hydrogen and ammonia, can recycle; Liquid is thick diglycolamine, the content of diglycolamine about 35% in thick diglycolamine.
The mol ratio of glycol ether, liquefied ammonia and soft water is 1:5:5.
Described catalyzer is copper-nickel catalyst, and producing 1 ton of diglycolamine needs spent catalyst 0.003m
3.
The separation purification method of the thick diglycolamine of the present invention, thick diglycolamine that glycol ether catalytic ammoniation is obtained under the condition of pressurization or normal pressure successively by eight tower continuous still batterys, diglycolamine, morpholine, glycol ether are separated from unreacted raw material and impurity, obtain the diglycolamine product of purity more than 99%, by-product morpholine, reclaims unreacted glycol ether simultaneously.Described eight towers are followed successively by deammoniation tower, normal pressure azeotrope column, vacuum dehydration column, vacuum morpholine recovery tower, vacuum diglycolamine lightness-removing column, vacuum diglycolamine tower, vacuum glycol ether lightness-removing column and vacuum glycol ether recovery tower.Technological process is as follows:
Thick diglycolamine is removed ammonia through deammoniation tower successively, normal pressure azeotrope column removes water, N-methylmorpholine, the by products such as N-ethylmorpholine, vacuum dehydration column removes part water, the impurity such as ethylene glycol monomethyl ether, vacuum morpholine recovery tower reclaims morpholine, vacuum diglycolamine lightness-removing column removes light constituent impurity, vacuum diglycolamine tower extraction diglycolamine, vacuum glycol ether lightness-removing column removes light constituent impurity, vacuum glycol ether recovery tower reclaims glycol ether, high boiling material bottom vacuum glycol ether recovery tower pumps in high boiling material tank, high boiling material main component is glycol ether, monomethyl morpholine, two methylmorpholines etc., sell outward.
The by product that deammoniation tower, normal pressure azeotrope column, vacuum dehydration column, vacuum morpholine recovery tower, vacuum diglycolamine lightness-removing column and vacuum glycol ether lightness-removing column remove and impurity are all discharged from the top of tower and collect, and the material of each tower bottom is sent in next tower reactor and continued separation and purification.
The diglycolamine purity of vacuum diglycolamine column overhead portion's extraction can reach more than 99%, the morpholine purity more than 99.5% of by-product.
Deammoniation tower bottom temperature is 170-180 DEG C, and tower top temperature is 35-40 DEG C, and tower internal pressure controls in 1.1-1.3MPa (absolute pressure).
Normal pressure azeotrope column bottom temperature is 115-120 DEG C, and tower top temperature is 95-98 DEG C, and tower internal pressure is normal pressure.
Vacuum dehydration column bottom temperature is 115-125 DEG C, and tower top temperature is 45-50 DEG C, and tower internal pressure is 0.08-0.085MPa (absolute pressure).
Vacuum morpholine recovery tower bottom temperature is 200-210 DEG C, and tower top temperature is 82-86 DEG C, and tower internal pressure is 0.08-0.085MPa (absolute pressure).
Vacuum diglycolamine lightness-removing column bottom temperature is 195-205 DEG C, and tower top temperature is 135-145 DEG C, and tower internal pressure is 0.09-0.095MPa (absolute pressure).
Vacuum diglycolamine tower bottom temperature is 205-215 DEG C, and tower top temperature is 150-155 DEG C, and tower internal pressure is 0.09-0.095MPa (absolute pressure).
Vacuum glycol ether lightness-removing column bottom temperature is 210-220 DEG C, and tower top temperature is 165-175 DEG C, and tower internal pressure is 0.09-0.095MPa (absolute pressure).
Vacuum glycol ether recovery tower bottom temperature is 215-225 DEG C, and tower top temperature is 170-180 DEG C, and tower internal pressure is 0.09-0.095MPa (absolute pressure).
Compared with the prior art, beneficial effect of the present invention is embodied in:
Separation and purification process energy consumption of the present invention is low, and flow process is simple, easy to operate, obtain the diglycolamine product of purity more than 99% and the morpholine byproduct of purity more than 99.5%, and productive rate reaches 99.5%.
Four, accompanying drawing explanation
The process flow diagram of the present invention that Fig. 1-1 to Fig. 1-4 shows for segmentation.
In figure, 1 thick diglycolamine storage tank, 2 deammoniation towers, 3 deamination overhead condensers, 4 deammoniation tower reboilers, 5 deammoniation tower pan feeding pumps, 6 normal pressure azeotrope column, 7 normal pressure azeotropic overhead condensers, 8 normal pressure azeotrope column return tanks, 9 normal pressure azeotrope column reflux pumps, 10 normal pressure azeotrope column reboilers, 11 normal pressure azeotropic tower reactor flow containers, 12 vacuum dehydration column pan feeding pumps, 13 vacuum dehydration column, 14 is vacuum hydro-extraction tower top condensers, 15 vacuum dehydration column return tanks, 16 vacuum dehydration column reflux pumps, 17 vacuum dehydration column reboilers, 18 vacuum hydro-extraction tower reactor flow containers, 19 vacuum morpholine recovery tower pan feeding pumps, 20 vacuum morpholine recovery towers, 21 vacuum morpholines reclaim overhead condenser, 22 vacuum morpholine recovery tower return tanks, 23 vacuum morpholine recovery tower reflux pumps, 24 vacuum morpholine recovery tower reboilers, 25 vacuum morpholines reclaim tower reactor flow container, 26 vacuum diglycolamine lightness-removing column pan feeding pumps, 27 vacuum diglycolamine lightness-removing columns, 28 vacuum diglycolamine lightness-removing column top condensers, 29 vacuum diglycolamine lightness-removing column return tanks, 30 vacuum diglycolamine lightness-removing column reflux pumps, 31 vacuum diglycolamine lightness-removing column reboilers, 32 vacuum diglycolamine lightness-removing column still flow containers, 33 vacuum diglycolamine tower pan feeding pumps, 34 vacuum diglycolamine towers, 35 vacuum diglycolamine overhead condensers, 36 vacuum diglycolamine tower return tanks, 37 vacuum diglycolamine tower reflux pumps, 38 vacuum diglycolamine tower reboilers, 39 vacuum diglycolamine tower reactor flow containers, 40 vacuum glycol ether lightness-removing column pan feeding pumps, 41 vacuum glycol ether lightness-removing columns, 42 vacuum glycol ether lightness-removing column top condensers, 43 vacuum glycol ether lightness-removing column return tanks, 44 vacuum glycol ether lightness-removing column reflux pumps, 45 vacuum glycol ether lightness-removing column reboilers, 46 is vacuum glycol ether lightness-removing column still flow containers, 47 vacuum glycol ether tower pan feeding pumps, 48 vacuum glycol ether towers, 49 vacuum glycol ether overhead condensers, 50 vacuum glycol ether tower return tanks, 51 vacuum glycol ether tower reflux pumps, 52 vacuum glycol ether tower reboilers, 53 vacuum glycol ether tower reactor flow containers, 54 high boiling material pumps, 55 temperature measurers, 56 tensimeters.
Five, embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As shown in Figure 1, to pump in deammoniation tower 2 through deammoniation tower pan feeding pump 5 from the thick diglycolamine of thick diglycolamine storage tank 1 and carry out deamination, with middle pressure steam (2.5MPa, 300 DEG C), the thick glycol ether material in deammoniation tower reboiler 4 is heated, to control tower top temperature for 35-40 DEG C, bottom temperature is 170-180 DEG C, and deammoniation tower internal pressure is 1.1-1.3MPa (absolute pressure).From deammoniation tower 2 top gas ammonia out after deamination overhead condenser 3 cooling becomes liquefied ammonia, get back in deammoniation tower 2, need to regulate according to technique, a part of liquefied ammonia backflow is as phegma, and a part of liquefied ammonia extraction is to liquid ammonia storage tank.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
Material bottom deammoniation tower 2 is delivered continuously in normal pressure azeotrope column 6 under the effect of pressure reduction, by low-pressure steam (1.2MPa, 190 DEG C), the material in normal pressure azeotrope column reboiler 10 is heated, to control tower top temperature for 95-98 DEG C, bottom temperature is 115-120 DEG C, and normal pressure azeotrope column internal pressure is normal pressure.From normal pressure azeotrope column top gaseous substance out after condenser 7 cooling in normal pressure azeotrope column top becomes liquid phase, enter normal pressure azeotrope column return tank 8, need to regulate according to technique, under the effect of normal pressure azeotrope column reflux pump 9, a part is back to as phegma in normal pressure azeotrope column 6, and a part of extraction is to sewage disposal.Thick diglycolamine removes the impurity such as most of water, N-methylmorpholine, N-ethylmorpholine contained in normal pressure azeotrope column 6.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
By the material continus convergence bottom normal pressure azeotrope column 6 to normal pressure azeotropic tower reactor liquid storage tank 11, be continuously pumped in vacuum dehydration column 13 through vacuum dehydration column pan feeding pump 12, by low-pressure steam (1.2MPa, 190 DEG C), the material in vacuum dehydration column reboiler 17 is heated, vacuumized from vacuum dehydration column return tank 15 and vacuum hydro-extraction tower reactor flow container 18 continuously by vacuum pump, control tower top temperature is 45-50 DEG C, bottom temperature is 115-125 DEG C, and vacuum dehydration column internal pressure is 0.08-0.085MPa (absolute pressure).From vacuum dehydration column 13 top gaseous substance out after the cooling of vacuum hydro-extraction tower top condenser 14 becomes liquid phase, enter vacuum dehydration column return tank 15, need to regulate according to technique, under the effect of vacuum dehydration column reflux pump 16, a part is back to as phegma in vacuum dehydration column 13, and a part of extraction is to sewage disposal.Thick diglycolamine removes the impurity such as a small amount of water, ethylene glycol monomethyl ether contained in vacuum dehydration column 13.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
By the material continus convergence bottom vacuum dehydration column 13 to vacuum hydro-extraction tower reactor liquid storage tank 18, be continuously pumped in vacuum morpholine recovery tower 20 through vacuum morpholine recovery tower pan feeding pump 19, with middle pressure steam (2.5MPa, 300 DEG C), the material in vacuum morpholine recovery tower reboiler 24 is heated, reclaim tower reactor flow container 25 from vacuum morpholine recovery tower return tank 22 and vacuum morpholine continuously by vacuum pump to vacuumize, control tower top temperature is 82-86 DEG C, bottom temperature is 200-210 DEG C, and vacuum morpholine recovery tower internal pressure is 0.08-0.085MPa (absolute pressure).Reclaim after overhead condenser 21 cooling becomes liquid phase from vacuum morpholine recovery tower 20 top gaseous substance out through vacuum morpholine, enter vacuum morpholine recovery tower return tank 22, need to regulate according to technique, under the effect of vacuum morpholine recovery tower reflux pump 23, a part is back to as phegma in vacuum morpholine recovery tower 20, and a part of extraction is to morpholine finished pot.Thick diglycolamine removes the morpholine contained in vacuum morpholine recovery tower 20, forms morpholine product, purity more than 99.5%.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
Material continus convergence bottom vacuum morpholine recovery tower 20 is reclaimed tower reactor liquid storage tank 25 to vacuum morpholine, be continuously pumped in vacuum diglycolamine lightness-removing column 27 through vacuum diglycolamine lightness-removing column pan feeding pump 26, with middle pressure steam (2.5MPa, 300 DEG C) material in vacuum diglycolamine lightness-removing column reboiler 31 is heated, vacuumized from vacuum diglycolamine lightness-removing column return tank 29 and vacuum diglycolamine lightness-removing column still flow container 32 continuously by vacuum pump, control tower top temperature is 135-145 DEG C, bottom temperature is 195-205 DEG C, vacuum diglycolamine lightness-removing column internal pressure is 0.09-0.095MPa (absolute pressure).From vacuum diglycolamine lightness-removing column 27 top gaseous substance out after condenser 28 cooling in vacuum diglycolamine lightness-removing column top becomes liquid phase, enter vacuum diglycolamine lightness-removing column return tank 29, need to regulate according to technique, under the effect of vacuum diglycolamine lightness-removing column reflux pump 30, a part is back to as phegma in vacuum diglycolamine lightness-removing column 27, and a part of extraction is to high boiling material tank.Light constituent before thick diglycolamine removes diglycolamine in vacuum diglycolamine lightness-removing column 27.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
By the material continus convergence bottom vacuum diglycolamine lightness-removing column 27 to vacuum diglycolamine lightness-removing column still liquid storage tank 32, be continuously pumped in vacuum diglycolamine tower 34 through vacuum diglycolamine tower pan feeding pump 33, with middle pressure steam (2.5MPa, 300 DEG C) mixture in vacuum diglycolamine tower reboiler 38 is heated, vacuumized from vacuum diglycolamine tower return tank 36 and vacuum diglycolamine tower reactor flow container 39 continuously by vacuum pump, control tower top temperature is 150-155 DEG C, bottom temperature is 205-215 DEG C, vacuum diglycolamine tower internal pressure is 0.09-0.095MPa (absolute pressure).From vacuum diglycolamine tower 34 top gaseous substance out after the cooling of vacuum diglycolamine overhead condenser 35 becomes liquid phase, enter vacuum diglycolamine tower return tank 36, need to regulate according to technique, under the effect of vacuum diglycolamine tower reflux pump 37, a part is back in vacuum diglycolamine tower 34 as phegma, part extraction is to diglycolamine finished pot, and purity can reach more than 99%.Diglycolamine is separated in vacuum diglycolamine tower 34, forms diglycolamine product.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
By the material continus convergence bottom vacuum diglycolamine tower 34 to vacuum diglycolamine tower bottoms storage tank 39, be continuously pumped in vacuum glycol ether lightness-removing column 41 through vacuum glycol ether lightness-removing column pan feeding pump 40, with middle pressure steam (2.5MPa, 300 DEG C) material in glycol ether lightness-removing column reboiler 45 is heated, vacuumized from vacuum glycol ether lightness-removing column return tank 43 and vacuum glycol ether lightness-removing column still flow container 46 continuously by vacuum pump, control tower top temperature is 165-175 DEG C, bottom temperature is 210-220 DEG C, vacuum glycol ether lightness-removing column internal pressure is 0.09-0.095MPa (absolute pressure).From vacuum glycol ether lightness-removing column 41 top gaseous substance out after condenser 42 cooling in vacuum glycol ether lightness-removing column top becomes liquid phase, enter vacuum glycol ether lightness-removing column return tank 43, need to regulate according to technique, under the effect of vacuum glycol ether lightness-removing column reflux pump 44, a part is back to as phegma in vacuum glycol ether lightness-removing column 41, and a part of extraction is to high boiling material tank.The light constituent of mixture before vacuum glycol ether lightness-removing column 41 removes glycol ether.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
By the material continus convergence bottom vacuum glycol ether lightness-removing column 41 to vacuum glycol ether lightness-removing column still liquid storage tank 47, be continuously pumped in vacuum glycol ether tower 48 through vacuum glycol ether tower pan feeding pump 47, with middle pressure steam (2.5MPa, 300 DEG C), the material in vacuum glycol ether tower reboiler 52 is heated, vacuumized from vacuum glycol ether tower return tank 50 and vacuum diglycolamine tower reactor flow container 53 continuously by vacuum pump, control tower top temperature is 170-180 DEG C, bottom temperature is 215-225 DEG C, and vacuum glycol ether tower internal pressure is 0.09-0.095MPa (absolute pressure).From vacuum glycol ether tower 48 top gaseous substance out after the cooling of vacuum glycol ether overhead condenser 49 becomes liquid phase, enter vacuum glycol ether tower return tank 50, need to regulate according to technique, under the effect of vacuum glycol ether tower reflux pump 51, as phegma in part backflow vacuum glycol ether tower 48, a part of extraction is to glycol ether finished pot.Glycol ether is separated in vacuum glycol ether tower 48, recycle.Temperature is measured by temperature measurer 55, and pressure is measured by tensimeter 56, and needs to regulate according to technique.
Material bottom vacuum glycol ether tower 48 drains into vacuum glycol ether tower reactor flow container 53, is delivered to high boiling material tank through high boiling material pump 54.
Claims (1)
1. a separation purification method for thick diglycolamine, is characterized in that:
Thick diglycolamine that glycol ether catalytic ammoniation is obtained under the condition of pressurization or normal pressure successively by eight tower continuous still batterys, diglycolamine, morpholine, glycol ether are separated from unreacted raw material and impurity, obtain the diglycolamine product of purity more than 99%, by-product morpholine, reclaims unreacted glycol ether simultaneously; Described eight towers are followed successively by deammoniation tower, normal pressure azeotrope column, vacuum dehydration column, vacuum morpholine recovery tower, vacuum diglycolamine lightness-removing column, vacuum diglycolamine tower, vacuum glycol ether lightness-removing column and vacuum glycol ether recovery tower;
Thick diglycolamine is removed ammonia through deammoniation tower successively, normal pressure azeotrope column removes water, N-methylmorpholine, N-ethylmorpholine by product, vacuum dehydration column removes part water, ethylene glycol monomethyl ether impurity, vacuum morpholine recovery tower reclaims morpholine, vacuum diglycolamine lightness-removing column removes light constituent impurity, vacuum diglycolamine tower extraction diglycolamine, vacuum glycol ether lightness-removing column removes light constituent impurity, vacuum glycol ether recovery tower reclaims glycol ether, and the high boiling material bottom vacuum glycol ether recovery tower pumps in high boiling material tank;
Deammoniation tower bottom temperature is 170-180 DEG C, and tower top temperature is 35-40 DEG C, and tower internal pressure controls at 1.1-1.3MPa;
Normal pressure azeotrope column bottom temperature is 115-120 DEG C, and tower top temperature is 95-98 DEG C, and tower internal pressure is normal pressure;
Vacuum dehydration column bottom temperature is 115-125 DEG C, and tower top temperature is 45-50 DEG C, and tower internal pressure is 0.08-0.085MPa;
Vacuum morpholine recovery tower bottom temperature is 200-210 DEG C, and tower top temperature is 82-86 DEG C, and tower internal pressure is 0.08-0.085MPa;
Vacuum diglycolamine lightness-removing column bottom temperature is 195-205 DEG C, and tower top temperature is 135-145 DEG C, and tower internal pressure is 0.09-0.095MPa;
Vacuum diglycolamine tower bottom temperature is 205-215 DEG C, and tower top temperature is 150-155 DEG C, and tower internal pressure is 0.09-0.095MPa;
Vacuum glycol ether lightness-removing column bottom temperature is 210-220 DEG C, and tower top temperature is 165-175 DEG C, and tower internal pressure is 0.09-0.095MPa;
Vacuum glycol ether recovery tower bottom temperature is 215-225 DEG C, and tower top temperature is 170-180 DEG C, and tower internal pressure is 0.09-0.095MPa.
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| EP3755692B1 (en) | 2018-02-22 | 2022-04-06 | Basf Se | Method for the depletion of 2-methoxyethanol (moe) |
| HUE058943T2 (en) | 2018-02-22 | 2022-09-28 | Basf Se | Method for the continuous destillative separation of mixtures comprising morpholine (mo), monoaminodiglycol (adg), ammonia, water and methoxyethanol (moe) |
| CN111801319A (en) | 2018-03-15 | 2020-10-20 | 巴斯夫欧洲公司 | Process for removing methoxyethanol from a mixture comprising methoxyethanol and morpholine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332142A (en) * | 2001-02-13 | 2002-01-23 | 安徽阜阳化工总厂 | Diglycol material for preparing morpholine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332142A (en) * | 2001-02-13 | 2002-01-23 | 安徽阜阳化工总厂 | Diglycol material for preparing morpholine |
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