CN1398843A - Acraldehyde recovering method - Google Patents
Acraldehyde recovering method Download PDFInfo
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- CN1398843A CN1398843A CN 02132797 CN02132797A CN1398843A CN 1398843 A CN1398843 A CN 1398843A CN 02132797 CN02132797 CN 02132797 CN 02132797 A CN02132797 A CN 02132797A CN 1398843 A CN1398843 A CN 1398843A
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- hydroxy propanal
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Abstract
The present invention is a method of separating and recovering unreacted acraldehyde from the reacted liquid of hydrolyzing acraldehyde to prepare 3-hydroxy propionic aldehyde. The recovering process includes preheating an aqueous solution of 3-hydroxy propionic aldehyde with 2-10 wt% of acraldehyde to 50-75 deg.C; and treating in the middle part of a refining tower under the solution speed of 0.1-2.0 m/hr and vacuum degree of 0.066-0.092 MPa while introducing inert gas of 5-25 times the volume of the aqueous solution and heated to 50-75 deg.C from the bottom of the tower; cooling the distrilled liquid from the top of the tower to obtain the aqueous, solution of rich acraldehyde content. The said method can reduce the consumption of acraldehyde and prolong the service life of the catalyst.
Description
Technical field: the present invention relates to a kind ofly prepare the reaction solution that 3-hydroxy propanal reaction process produces the method for Separation and Recovery unreacting propylene aldehyde from acrolein hydration.
Background technology: what the recovery of propenal was adopted substantially at present is traditional fractionation, rectificating method, because the chemical property of propenal and 3-hydroxy propanal is active, so the rate of recovery is very low.The acrolein hydration reaction is given birth under the catalyst action in acidity and is carried out generally speaking, this reaction is reversible reaction, the 3-hydroxy propanal aqueous solution that produces contains the unreacted propenal of 2～10% (weight) approximately, if this part propenal is not reclaimed, can in next step 3-hydroxypropyl aldehyde hydrogenation reaction, form multiple by product, the active of hydrogenation catalyst reduced rapidly, influence the life-span of hydrogenation catalyst, increased the norm quota of consumption.Along with steaming of propenal, the 3-hydroxy propanal can be decomposed into propenal and water, and 3-hydroxypropyl aldehyde is very unstable, under heating condition self or be easy to take place polymerization and condensation reaction with propenal etc., cause the content of propenal in the 3-hydroxy propanal aqua liquid to be difficult to be reduced to and meet the hydrogenation requirement, liquid after the separation should not be as hydrogenating materials because of containing superpolymer, and therefore existing method is unsuitable for separating the propenal in the 3-hydroxy propanal aqueous solution.And US3518310, US5015789, US5093537, US6140543 patent have all been mentioned and are adopted thin-film evaporator to separate propenal in the 3-hydroxy propanal aqua liquid, shorten the duration of contact of aqua liquid and thermal source as far as possible, to avoid the generation of side reaction, though the rate of recovery of propenal increases, but required thin-film evaporator facility investment is big, and operation is also relatively more difficult.
Summary of the invention: the present invention is the recovery method of a kind of propenal of development, and the content that this recovery method can reduce propenal in the 3-hydroxy propanal aqua liquid makes the solution after the separation meet the hydrogenation requirement, and this method facility investment is few, is convenient to operation.The recovery method of propenal of the present invention is: earlier the 3-hydroxy propanal aqueous solution that contains 2～10% (weight) propenal in the acrolein hydration reaction is fed in the head tank 1, open vacuum pump 11, by vacuum in the tower with solution after under meter 2 metering, enter and be preheated to 50～75 ℃ in the preheater 3, preferably be preheated to 55～65 ℃, enter the middle part of rectifying tower 4 then, making 3-hydroxypropyl aldehyde aqueous solution void tower liquid speed is 0.1～2.0m/h, preferably selecting liquid speed is 0.2～0.8m/h, the stage number of rectifying tower 4 is 5～25, preferably stage number is 10～21, vacuum tightness is-0.066～-0.092Mpa, preferably vacuum tightness be-0.072～-0.086Mpa, bottom feeding from rectifying tower 4 simultaneously is heated to 50～75 ℃ through under meter 5 meterings and through preheater 6, preferably is preheated to 55～65 ℃, and volume is 5～25 times of the 3-hydroxy propanal aqueous solution, 10～20 times reactionlessness gas preferably, described rare gas element can be hydrogen, nitrogen, air, argon gas, helium, water vapour.The liquid that is steamed by rectifying tower 4 cats head is after water cooler 7 coolings, and what obtain is rich in aqueous acrolein solution, enters in the receiving tank 8 again, finishes the recovery operation of unreacting propylene aldehyde.By obtaining the aqueous acrolein solution that level of acrolein is lower than 0.9% (weight) at the bottom of rectifying tower 4 towers, this liquid is to meet hydrogenation preparing 1, the 3-hydroxypropyl aldehyde reaction liquid that the ammediol reaction requires, and this liquid is after water cooler 9 coolings, enter receiving tank 10, as the raw material of hydrogenation reaction.The recovery method of the propenal that the present invention relates to is easy to realize, and it is simple to operate, the required equipment less investment, at propenal, the chemical property of 3-hydroxy propanal is active, unsettled characteristics, add an amount of rare gas element, the content of propenal in the 3-hydroxy propanal is reduced, utilize this recovery method the content of propenal in the 3-hydroxy propanal aqueous solution can be reduced to below 0.9% (weight) by original 2～10% (weight), can reach the requirement of hydrogenation reaction fully, the present invention not only can reduce the norm quota of consumption of propenal, and has prolonged the work-ing life of 3-hydroxy propanal catalyst for hydrogenation.
Description of drawings: Fig. 1 is the synoptic diagram of recovery method equipment therefor of the present invention.
Embodiment one: present embodiment is earlier the 3 hydroxy propanal aqueous solution that contain 2.9% (weight) propenal in the acrolein hydration reaction to be fed in the head tank 1, open vacuum pump 11 by vacuum in the tower, solution is after under meter 2 meterings, enter in the preheater 3, feeding temperature is 55～58 ℃, enter the middle part of rectifying tower 4 then, make 3-hydroxy propanal aqueous solution void tower liquid speed be 0.5m/h, the stage number of rectifying tower 4 is 17～21, the vacuum tightness of rectifying tower 4 is-0.076～-0.080Mpa, feeding is preheated to 55～58 ℃ air, gas-liquid volume ratio is 10～12 times, separates the level of acrolein of the back 3-hydroxy propanal aqueous solution and reduces to 0.9% (weight) by 2.9% (content).
Embodiment two: what present embodiment and embodiment one were different is, the level of acrolein of the 3-hydroxy propanal aqueous solution is 3.5% (weight), feeding temperature is 58～62 ℃, the fast 0.6m/h of being of void tower liquid, the stage number of rectifying tower 4 is 12～16, the vacuum tightness of rectifying tower 4 is-0.084～-0.086Mpa, feeding is preheated to 58～62 ℃ air, gas-liquid volume ratio is 14～16 times, after the separation, the content of the propenal of the 3-hydroxyl hydroxy propanal aqueous solution is reduced to 0.8% (weight) by 3.5% (weight).Its removal process is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is, the level of acrolein of the 3-hydroxy propanal aqueous solution is 6.1% (weight), feeding temperature is 62～65 ℃, void tower liquid speed is 0.6m/h, and the stage number of rectifying tower 4 is 12～16, vacuum tightness is-0.082～-0.084Mpa, feeding is preheated to 62～65 ℃ air, gas-liquid volume ratio is 14～16 times, and after the separation, the level of acrolein of the 3-hydroxy propanal aqueous solution is reduced to 0.8% (weight) by 6.1% (content).Its removal process is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is, the level of acrolein of the 3-hydroxy propanal aqueous solution is 3.0% (weight), feeding temperature is 58～62 ℃, void tower liquid speed is 0.3m/h, and the stage number of rectifying tower 4 is 12～16, vacuum tightness is-0.080～-0.082Mpa, feeding is preheated to 58～62 ℃ nitrogen, gas-liquid volume ratio is 16～20 times, and after the separation, the level of acrolein of the 3-hydroxy propanal aqueous solution is reduced to 0.6% (weight) by 3.0% (weight).Its removal process is identical with embodiment one.
Claims (10)
1, the recovery method of propenal, it is characterized in that earlier the 3-hydroxy propanal aqueous solution that contains 2～10% (weight) propenal in the acrolein hydration reaction being fed in the head tank (1), open vacuum pump (11) by vacuum in the tower, solution is after under meter (2) metering, enter in the preheater (3) and be preheated to 50～75 ℃, enter the middle part of rectifying tower (4) then, making 3-hydroxy propanal aqueous solution void tower liquid speed is 0.1～2.0m/h, the stage number of rectifying tower (4) is 5～25, vacuum tightness is-0.066～-0.092Mpa, bottom feeding from rectifying tower (4) simultaneously is heated to 50～75 ℃ through under meter (5) metering and through preheater (6), volume is the reactionlessness gas of 5～25 times of the 3-hydroxy propanal aqueous solution, the liquid that is steamed by rectifying tower (4) cat head is after water cooler (7) cooling, what obtain is rich in aqueous acrolein solution, enters in the receiving tank (8) again.
2, the recovery method of propenal according to claim 1 is characterized in that behind preheater (3), the preheating temperature of the 3-hydroxy propanal aqueous solution is preferably 55～65 ℃, and 3-hydroxy propanal aqueous solution void tower liquid speed is preferably 0.2～0.8m/h.
3, the recovery method of propenal according to claim 1 is characterized in that the stage number of rectifying tower (4) is preferably 10～21, vacuum tightness is preferably-0.072～-0.086Mpa.
4, the recovery method of propenal according to claim 1 is characterized in that behind preheater (6), the preheating temperature of gas is preferably 55～65 ℃, and the volume of gas is preferably 10～20 times of the 3-hydroxy propanal aqueous solution.
5, the recovery method of propenal according to claim 1, it is characterized in that by obtaining the aqueous acrolein solution that level of acrolein is lower than 0.9% (weight) at the bottom of rectifying tower (4) tower, this liquid is to meet hydrogenation preparing 1, the 3-hydroxy propanal reaction solution that the ammediol reaction requires, this liquid is after water cooler (9) cooling, enter receiving tank (10), as the raw material of hydrogenation reaction.
6, the recovery method of propenal according to claim 1, it is characterized in that earlier (3) the hydroxy propanal aqueous solution that contains 2.9% (weight) propenal in the acrolein hydration reaction being fed in the head tank (1), pass through the interior vacuum of tower again after under meter (2) metering, enter in the preheater (3), feeding temperature is 55～58 ℃, enter the middle part of rectifying tower (4) then, make 3-hydroxy propanal aqueous solution void tower liquid speed be 0.5m/h, the stage number of rectifying tower (4) is 17～21, the vacuum tightness of rectifying tower (4) is-0.076～-0.080Mpa, feeding is preheated to 55～58 ℃ air, and gas-liquid volume ratio is 10～12 times.
7, the recovery method of propenal according to claim 1, the level of acrolein that it is characterized in that the 3-hydroxy propanal aqueous solution is 3.5% (weight), feeding temperature is 58～62 ℃, the fast 0.6m/h of being of void tower liquid, the stage number of rectifying tower (4) is 12～16, the vacuum tightness of rectifying tower (4) is-0.084～-0.086Mpa, feeding is preheated to 58～62 ℃ air, and gas-liquid volume ratio is 14～16 times.
8, the recovery method of propenal according to claim 1, the level of acrolein that it is characterized in that the 3-hydroxy propanal aqueous solution is 6.1% (weight), feeding temperature is 62～65 ℃, void tower liquid speed is 0.6m/h, the stage number of rectifying tower (4) is 12～16, vacuum tightness is-0.082～-0.084Mpa, feed and be preheated to 62～65 ℃ air, gas-liquid volume ratio is 14～16 times.
9, the recovery method of propenal according to claim 1, the level of acrolein that it is characterized in that the 3-hydroxy propanal aqueous solution is 3.0% (weight), feeding temperature is 58～62 ℃, void tower liquid speed is 0.3m/h, the stage number of rectifying tower (4) is 12～16, vacuum tightness is-0.080～-0.082Mpa, feed and be preheated to 58～62 ℃ nitrogen, gas-liquid volume ratio is 16～20 times.
10, the recovery method of propenal according to claim 1 is characterized in that described rare gas element can be hydrogen, nitrogen, air, argon gas, helium, water vapour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021327971A CN1176057C (en) | 2002-08-20 | 2002-08-20 | Acraldehyde recovering method |
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|---|---|---|---|
| CNB021327971A CN1176057C (en) | 2002-08-20 | 2002-08-20 | Acraldehyde recovering method |
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| CN1398843A true CN1398843A (en) | 2003-02-26 |
| CN1176057C CN1176057C (en) | 2004-11-17 |
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| CNB021327971A Expired - Fee Related CN1176057C (en) | 2002-08-20 | 2002-08-20 | Acraldehyde recovering method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376531C (en) * | 2006-01-23 | 2008-03-26 | 上海华谊丙烯酸有限公司 | Method for separating and reclaiming acrolein |
| CN110551013A (en) * | 2018-05-30 | 2019-12-10 | 中国石油集团东北炼化工程有限公司吉林设计院 | energy recovery method of acrolein refining process |
| CN112920031A (en) * | 2021-01-27 | 2021-06-08 | 浙江恒澜科技有限公司 | Method for separating and recycling acrolein in process of preparing 1, 3-propylene glycol |
| CN113277933A (en) * | 2021-06-04 | 2021-08-20 | 江苏扬农化工集团有限公司 | Method and device for preparing 3-hydroxypropionaldehyde by continuous catalytic distillation |
| CN116041162A (en) * | 2022-10-28 | 2023-05-02 | 江苏扬农化工集团有限公司 | Method for separating and recovering acrolein from product system for preparing 3-hydroxy propanal by hydration of acrolein |
-
2002
- 2002-08-20 CN CNB021327971A patent/CN1176057C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376531C (en) * | 2006-01-23 | 2008-03-26 | 上海华谊丙烯酸有限公司 | Method for separating and reclaiming acrolein |
| CN110551013A (en) * | 2018-05-30 | 2019-12-10 | 中国石油集团东北炼化工程有限公司吉林设计院 | energy recovery method of acrolein refining process |
| CN112920031A (en) * | 2021-01-27 | 2021-06-08 | 浙江恒澜科技有限公司 | Method for separating and recycling acrolein in process of preparing 1, 3-propylene glycol |
| CN112920031B (en) * | 2021-01-27 | 2022-07-08 | 浙江恒逸石化研究院有限公司 | Method for separating and recycling acrolein in process of preparing 1, 3-propylene glycol |
| CN113277933A (en) * | 2021-06-04 | 2021-08-20 | 江苏扬农化工集团有限公司 | Method and device for preparing 3-hydroxypropionaldehyde by continuous catalytic distillation |
| CN113277933B (en) * | 2021-06-04 | 2022-12-02 | 江苏扬农化工集团有限公司 | Method and device for preparing 3-hydroxypropionaldehyde by continuous catalytic distillation |
| CN116041162A (en) * | 2022-10-28 | 2023-05-02 | 江苏扬农化工集团有限公司 | Method for separating and recovering acrolein from product system for preparing 3-hydroxy propanal by hydration of acrolein |
| CN116041162B (en) * | 2022-10-28 | 2024-04-12 | 江苏扬农化工集团有限公司 | Method for separating and recovering acrolein from product system for preparing 3-hydroxy propanal by hydration of acrolein |
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| CN1176057C (en) | 2004-11-17 |
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