CN104086386A - Method and device for extracting dimethyl dipentene aldehyde from propionaldehyde waste liquid - Google Patents

Method and device for extracting dimethyl dipentene aldehyde from propionaldehyde waste liquid Download PDF

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Publication number
CN104086386A
CN104086386A CN201410326905.8A CN201410326905A CN104086386A CN 104086386 A CN104086386 A CN 104086386A CN 201410326905 A CN201410326905 A CN 201410326905A CN 104086386 A CN104086386 A CN 104086386A
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China
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tower
dimethyl
rectifying tower
olefine aldehydr
liquid
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CN201410326905.8A
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CN104086386B (en
Inventor
王涛
贾露露
李刚
汤雯
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NANJING RONGXIN CHEMICAL INDUSTRIAL Co.,Ltd.
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NANJING RONGXIN CHEMICAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a method for extracting dimethyl dipentene aldehyde from propionaldehyde waste liquid. The method comprises the steps of (1) filtering waste liquid produced in the propionaldehyde preparation process through a membrane unit to remove matters of which molecules are greater than dimethyl dipentene aldehyde molecules; (2) delivering the filtered mixture to a rectifying tower, heating the tower kettle of the rectifying tower to ensure the mixture is azeotropic, separating a gaseous-phase matter from the tower top, and discharging residual liquid from the tower bottom; (3) condensing the gaseous-phase matter separated out from the tower top into a liquid phase and delivering the liquid phase to a storage tank; (4) detecting the dimethyl dipentene aldehyde content of the liquid in the storage tank, delivering the unqualified liquid back to the rectifying tower, and repeating steps (2)-(3); (5) delivering the liquid qualified in the content detection in the step (4) to a product tank, thus obtaining the dimethyl dipentene aldehyde. By adopting the method for extracting the dimethyl dipentene aldehyde from the waste liquid produced in propionaldehyde preparation, the production cost is greatly reduced and waste of resources is avoided.

Description

In a kind of propionic aldehyde waste liquid, extract method and the device of dimethyl diamyl olefine aldehydr
Technical field
The present invention relates to a kind of method and device that extracts dimethyl diamyl olefine aldehydr, in especially a kind of propionic aldehyde waste liquid, extract method and the device of dimethyl diamyl olefine aldehydr.
Background technology
In the preparation method of propionic aldehyde, low pressure oxo synthesis is current main method and developing direction, and in the preparation system of low pressure oxo synthesis, thereby propionic aldehyde can condensation produce dimethyl diamyl olefine aldehydr.
Dimethyl diamyl olefine aldehydr is important organic synthesis intermediate, and for example strawberriff is synthetic.Simultaneously dimethyl diamyl olefine aldehydr has stronger toxicity, easy firing and have pungency.
In existing propionic aldehyde preparation technology, the dimethyl diamyl olefine aldehydr being condensed into by propionic aldehyde is blended in waste liquid, with waste liquid, processes together discharge, not only enterprise is caused the waste of resource, and the waste liquid of discharge also can pollute bad border simultaneously.
Summary of the invention
Goal of the invention: the object of the invention is for the deficiencies in the prior art, and the method and the device that extract dimethyl diamyl olefine aldehydr in a kind of waste liquid preparing propionic aldehyde generation are provided.
Technical scheme: extract the method for dimethyl diamyl olefine aldehydr in propionic aldehyde waste liquid of the present invention, comprise the following steps:
(1) by preparing the waste liquid producing in propionic aldehyde process, by film unit, filter, the material that molecule is wherein greater than to dimethyl diamyl olefine aldehydr molecule filters out;
(2) mixture after filtering is transported in rectifying tower, heating tower bottom of rectifying tower, makes mixture form azeotropic, by tower top, isolates gaseous substance, discharges raffinate at the bottom of tower;
(3) the isolated gaseous substance of tower top being condensed into liquid phase is transported in hold-up vessel;
(4) detect and store dimethyl limonene aldehyde in pot liquid, underproof conveying is got back in rectifying tower, repeats (2) ~ (3) step;
(5) transport of liquid that in step (4), content detection is qualified, to products pot, obtains described dimethyl diamyl olefine aldehydr.
Preferably, raffinate described in step (2) is transmitted back to rectifying again in rectifying tower.In described raffinate, have and fail to form in time the dimethyl diamyl olefine aldehydr of gas phase, can again return to rectifying in rectifying tower.
Preferably, in step (2), the temperature of tower bottom of rectifying tower is 110 ~ 130 ℃, and the temperature of tower top is 90 ~ 100 ℃.
The device that extracts dimethyl diamyl olefine aldehydr in propionic aldehyde waste liquid of the present invention, comprises filtration unit, rectifying tower and condenser, and the entrance of described filtration unit is connected with waste liquid outlet, and the outlet of described filtration unit is connected with described rectifying tower import by delivery tube; Described rectifying tower tower top is provided with vapour outlet, is provided with raffinate outlet at the bottom of tower, and described vapour outlet is connected with described condenser inlet by delivery tube, and described condensator outlet is connected with products pot by delivery tube;
Described filtration unit is the strainer that is provided with two-layer above film unit, and described film unit is provided with the hole consistent with dimethyl diamyl olefine aldehydr molecular size.
Further, between described rectifying tower and described products pot, be also provided with reflux, described reflux import is connected by delivery tube with condensator outlet, and described reflux outlet is connected by delivery tube with products pot, rectifying tower respectively.
Further, in the delivery tube between described reflux and described products pot, described rectifying tower, be respectively arranged with valve.Can select to open or close valve according to the detected result of dimethyl limonene aldehyde, liquid in hold-up vessel is conveyed into products pot or is back in rectifying tower.
Preferably, described rectifying tower raffinate outlet is provided with valve.The valve of rectifier bottoms can conveniently be controlled the reaction times of mixture in rectifying tower, effluent discharge in time after fully reacting.
Preferably, described film unit is molecular sieve.
Preferably, described rectifying tower is atmospheric distillation tower.
Beneficial effect: (1) the present invention extracts dimethyl diamyl olefine aldehydr in the waste liquid of preparing propionic aldehyde generation, greatly reduces production cost, can not cause the wasting of resources; (2) the present invention can effectively reduce discharging of waste liquid amount, reduces environmental pollution; (3) technique of the present invention is simple, is conducive to large-scale industrialization and produces.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation.
Embodiment
Below by accompanying drawing, technical solution of the present invention is elaborated, but protection scope of the present invention is not limited to described embodiment.
embodiment 1:in propionic aldehyde waste liquid, extract a device for dimethyl diamyl olefine aldehydr, comprise filtration unit 1, atmospheric distillation tower 3 and condenser 5;
The entrance of described filtration unit 1 is connected with waste liquid outlet, and the outlet of described filtration unit 1 is connected with described atmospheric distillation tower 3 imports by delivery tube; Described atmospheric distillation tower 3 tower tops are provided with vapour outlet 4, are provided with raffinate outlet at the bottom of tower, and described vapour outlet 4 is connected with described condenser 5 imports by delivery tube; Described condenser 5 outlets are connected with the import of reflux 6 by delivery tube; The outlet of described reflux 6 is connected by delivery tube with products pot 7, atmospheric distillation tower 3 respectively, is respectively arranged with valve 8 in described delivery tube;
Described filtration unit is the strainer that is provided with two-layer above molecular sieve 2, and described molecular sieve 2 is provided with the hole consistent with dimethyl diamyl olefine aldehydr molecular size.
Step during specific works:
(1) by preparing the waste liquid producing in propionic aldehyde process, by molecular sieve 2, filter, the material that molecule is wherein greater than to dimethyl diamyl olefine aldehydr molecule filters out;
(2) mixture after filtering is transported in atmospheric distillation tower 3, heating rectifying tower 3, makes the temperature of tower bottom of rectifying tower reach 110 ~ 130 ℃, and tower top reaches 90 ~ 100 ℃, thereby makes mixture form azeotropic, by tower top 4, isolates gaseous substance, discharges raffinate at the bottom of tower;
(3) the isolated gaseous substance of tower top 4 being condensed into liquid phase by condenser 5 is transported in hold-up vessel 6;
(4) detect dimethyl limonene aldehyde in the interior liquid of hold-up vessel 6, underproof conveying is got back in rectifying tower 3, repeats (2) ~ (3) step;
(5) transport of liquid that in step (4), content detection is qualified, to products pot 7, obtains described dimethyl diamyl olefine aldehydr.
As mentioned above, although represented and explained the present invention with reference to specific preferred embodiment, it shall not be construed as the restriction to the present invention self.Not departing under the spirit and scope of the present invention prerequisite of claims definition, can make in the form and details various variations to it.

Claims (9)

1. in propionic aldehyde waste liquid, extract a method for dimethyl diamyl olefine aldehydr, it is characterized in that comprising the following steps:
(1) by preparing the waste liquid producing in propionic aldehyde process, by film unit, filter, the material that molecule is wherein greater than to dimethyl diamyl olefine aldehydr molecule filters out;
(2) mixture after filtering is transported in rectifying tower, heating tower bottom of rectifying tower, makes mixture form azeotropic, by tower top, isolates gaseous substance, discharges raffinate at the bottom of tower;
(3) the isolated gaseous substance of tower top being condensed into liquid phase is transported in hold-up vessel;
(4) detect and store dimethyl limonene aldehyde in pot liquid, underproof conveying is got back in rectifying tower, repeats (2) ~ (3) step;
(5) transport of liquid that in step (4), content detection is qualified, to products pot, obtains described dimethyl diamyl olefine aldehydr.
2. the method for extraction dimethyl diamyl olefine aldehydr according to claim 1, is characterized in that: raffinate described in step (2) is transmitted back to rectifying again in rectifying tower.
3. the method for extraction dimethyl diamyl olefine aldehydr according to claim 1, is characterized in that: in step (2), the temperature of tower bottom of rectifying tower is 110 ~ 130 ℃, and the temperature of tower top is 90 ~ 100 ℃.
4. in a propionic aldehyde waste liquid, extract the device of dimethyl diamyl olefine aldehydr, it is characterized in that: comprise filtration unit, rectifying tower and condenser, the entrance of described filtration unit is connected with waste liquid outlet, and the outlet of described filtration unit is connected with described rectifying tower import by delivery tube; Described rectifying tower tower top is provided with vapour outlet, is provided with raffinate outlet at the bottom of tower, and described vapour outlet is connected with described condenser inlet by delivery tube, and described condensator outlet is connected with products pot by delivery tube;
Described filtration unit is the strainer that is provided with two-layer above film unit, and described film unit is provided with the hole consistent with dimethyl diamyl olefine aldehydr molecular size.
5. the device of extraction dimethyl diamyl olefine aldehydr according to claim 4, it is characterized in that: between described rectifying tower and described products pot, be also provided with reflux, described reflux import is connected by delivery tube with condensator outlet, and described reflux outlet is connected by delivery tube with products pot, rectifying tower respectively.
6. the device of extraction dimethyl diamyl olefine aldehydr according to claim 5, is characterized in that: in the delivery tube between described reflux and described products pot, described rectifying tower, be respectively arranged with valve.
7. the device of extraction dimethyl diamyl olefine aldehydr according to claim 4, is characterized in that: described rectifying tower raffinate outlet is provided with valve.
8. the device of extraction dimethyl diamyl olefine aldehydr according to claim 4, is characterized in that: described film unit is molecular sieve.
9. the device of extraction dimethyl diamyl olefine aldehydr according to claim 4, is characterized in that: described rectifying tower is atmospheric distillation tower.
CN201410326905.8A 2014-07-09 2014-07-09 Method and the device of 2-methyl-2-pentenal serving is extracted in a kind of propionic aldehyde waste liquid Active CN104086386B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970530A (en) * 2019-05-07 2019-07-05 四川大学 A method of strawberriff is prepared using propionic aldehyde industrial wastes

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336638A (en) * 2011-07-20 2012-02-01 南京荣欣化工有限公司 Technical method for producing propyl aldehyde through hydroformylation of ethylene
CN102344349A (en) * 2011-08-22 2012-02-08 无锡百川化工股份有限公司 Method for preparing 2-methyl-2-pentena

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336638A (en) * 2011-07-20 2012-02-01 南京荣欣化工有限公司 Technical method for producing propyl aldehyde through hydroformylation of ethylene
CN102344349A (en) * 2011-08-22 2012-02-08 无锡百川化工股份有限公司 Method for preparing 2-methyl-2-pentena

Non-Patent Citations (1)

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Title
赵兴武: "南京宣判一起企业污染环境邢事案", 《人民法院报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970530A (en) * 2019-05-07 2019-07-05 四川大学 A method of strawberriff is prepared using propionic aldehyde industrial wastes

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Effective date of registration: 20181211

Address after: Room 1129, 11th floor, Traffic Bureau Building, 95 Yingbin Avenue, Xinhua Street, Huadu District, Guangzhou City, Guangdong 510800

Patentee after: Guangzhou New Century New Energy Development Co., Ltd.

Address before: 210047 No. 99 Munifeng Road, Nanjing Chemical Park, Nanjing, Jiangsu Province

Patentee before: Nanjing Rongxin Chemical Co., Ltd.

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Address after: Room 1129, 11th floor, Traffic Bureau Building, 95 Yingbin Avenue, Xinhua Street, Huadu District, Guangzhou City, Guangdong 510800

Patentee after: Guangzhou New Century New Energy Development Co., Ltd.

Address before: 210047 No. 99 Munifeng Road, Nanjing Chemical Park, Nanjing, Jiangsu Province

Patentee before: Nanjing Rongxin Chemical Co., Ltd.

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Patentee after: NANJING RONGXIN CHEMICAL INDUSTRIAL Co.,Ltd.

Address before: Room 1129, 11th floor, Traffic Bureau Building, 95 Yingbin Avenue, Xinhua Street, Huadu District, Guangzhou City, Guangdong 510800

Patentee before: GUANGZHOU XINSHIJI NEW ENERGY DEVELOPMENT Co.,Ltd.

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