CN102503789A - Method for distilling, separating and purifying ketone alcohol mixture by utilizing separating plate - Google Patents

Method for distilling, separating and purifying ketone alcohol mixture by utilizing separating plate Download PDF

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Publication number
CN102503789A
CN102503789A CN2011103083163A CN201110308316A CN102503789A CN 102503789 A CN102503789 A CN 102503789A CN 2011103083163 A CN2011103083163 A CN 2011103083163A CN 201110308316 A CN201110308316 A CN 201110308316A CN 102503789 A CN102503789 A CN 102503789A
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China
Prior art keywords
tower
distilling
distillation
separating
alcohol mixture
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CN2011103083163A
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Chinese (zh)
Inventor
刘修华
杨辉
秦国栋
谭立文
张建梅
李义田
郑洪军
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WEIFANG CITY YUANLI CHEMICAL INDUSTRY Co Ltd
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WEIFANG CITY YUANLI CHEMICAL INDUSTRY Co Ltd
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Priority to CN2011103083163A priority Critical patent/CN102503789A/en
Publication of CN102503789A publication Critical patent/CN102503789A/en
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Abstract

The invention discloses a method for distilling, separating and purifying a ketone alcohol mixture by utilizing a separating plate. A distilling separating process is finished in first and second distilling towers which are serially connected with each other; the separating plate is vertically arranged at the top of the first distilling tower; an upper cavity of the first distilling tower is divided into a first tower chamber on one side of a material inlet and a second tower chamber on the other side of the material inlet; and material inlet of the first distilling tower is located above the bottom of the separating plate. The distilling separating process comprises the following steps: placing the raw material, namely, the ketone alcohol mixture, into the first and second distilling towers in serial connection; separating light components from the top of the first tower chamber of the first distilling tower and separating octanone from the top of the second tower chamber; placing the materials at the bottom of the first distilling tower into the second distilling tower; separating octanol from the top of the second distilling tower; and discharging weight components from the bottom of the second distilling tower, wherein the pressures of the first and second distilling towers are respectively 18-20kPa and 15-17kPa, and the temperatures of the gas phases at the tower top are respectively 110-120 DEG C and 120-130 DEG C.

Description

The method of dividing plate fractionation by distillation purification keto-alcohol mixture
Technical field
The present invention relates to organic mixture purification technique field, relate in particular to a kind of the purification and prepare the method for secondary octanone and secondary octanol by the keto-alcohol mixture separation.
Background technology
Secondary octanol is a kind of important straight chain C 8Alcohol, the secondary octanol that purity is high are oily liquids colourless, that aromatising flavour is arranged, inflammable, low toxicity, are slightly soluble in water, and is miscible with ethanol, ether.Secondary octanol, also is mainly used in and produces plastic plasticizer, synthetic perfume etc. not only as mineral flotation agent, skimmer, solvent as important straight chain alcohol.
Secondary octanone is a kind of important chemical material equally, is mainly used in fields such as fiber, medicine, agricultural chemicals, spices, chemical industry, and as synthetic fiber oiling agent, foam killer and produce tensio-active agent, the colliery is with flotation agent etc.
The keto-alcohol mixture that contains secondary octanol and secondary octanone is to produce the by product in the sebacic acid process with Viscotrol C, contains the light constituent and the heavy constituent of some amount simultaneously, from the keto-alcohol mixture, secondary octanone is separated with secondary octanol, makes higher secondary octanol of purity and secondary octanone; And separate and remove light constituent and heavy constituent, traditional tripping device and separation method obtain two kinds of purity high product; At least need accomplish in placed in-line three distillation towers each other, light constituent is removed in tower separation, gets into two towers after the condensation of bottoms material; Two column overhead separate purify secondary octanone, get into three towers after the two Tata substrate material condensations, three column overhead separate purify secondary octanol; At the bottom of three Tatas heavy constituent, because the boiling-point difference of secondary octanol and secondary octanone is less, therefore; If will obtain the purity high product, just require the theoretical plate number of distillation tower higher relatively, adopt traditional water distilling apparatus and method; Not only Production Flow Chart is complicated, and higher relatively to the investment of devices such as tower, cost of investment is bigger; And each tower restriction is stronger in the still-process, and energy consumption is high, unstable product quality.
Summary of the invention
Technical problem to be solved by this invention is: to the deficiency that prior art exists, the method for the dividing plate fractionation by distillation purification keto-alcohol mixture that a kind of production technique is simple, facility investment is little, energy consumption is low is provided.
For solving the problems of the technologies described above, technical scheme of the present invention is:
The method of dividing plate fractionation by distillation purification keto-alcohol mixture; Said fractionation by distillation is accomplished in placed in-line first and second distillation towers each other; The top of said first distillation tower vertically is provided with dividing plate; The upper cavity of first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side, and the material inlet of said first distillation tower is positioned at the top of said dividing plate bottom, and said fractionation by distillation may further comprise the steps:
The raw ketone alcohol mixture is got into placed in-line first distillation tower each other; Light constituent is separated from the first tower chamber cat head of first distillation tower; Secondary octanone is separated from the second tower chamber cat head; The bottoms material gets into second column, and secondary octanol is separated from the after-fractionating column overhead, and heavy constituent are discharged at the bottom of the after-fractionating Tata;
The pressure of said first distillation tower and second column is respectively 18~20kPa and 15~17kPa, and the cat head gas phase temperature is respectively 110~120 ℃ and 120~130 ℃.
Said first distillation tower and second column column bottom temperature are respectively 140~150 ℃ and 145~160 ℃.
The purity of said secondary octanone of separating and secondary octanol is respectively 99.1wt% and more than the 99.6wt%.
The first tower chamber of said second column is consistent with the pressure of the second tower chamber.
Owing to adopted technique scheme, the invention has the beneficial effects as follows:
The present invention separates the keto-alcohol mixture and each other accomplishes in placed in-line two distillation towers, and wherein the top of first distillation tower vertically is provided with dividing plate, and the upper cavity of said first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side; Light constituent is separated from the first tower chamber cat head gaseous phase outlet; Secondary octanone and secondary octanol are separated from the cat head gaseous phase outlet of the second tower chamber and second column respectively, and heavy constituent liquid phase outlet at the bottom of the tower of the second tower chamber is separated, and has realized with three kinds of components of tower separation; Thereby can realize isolating four kinds of components with two distillation towers; Compare prior art, shortened Production Flow Chart, omitted in traditional separating technology and need from first distillation tower, get into second column distillatory operation after the condensation again; Practiced thrift the energy of reheat; Reduce energy consumption, reduced production cost, and reduced facility investment.
The present invention adopts continuous still battery separate to purify secondary octanol and secondary octanone, and owing to technology is moved continuously, each material equiblibrium mass distribution in tower has guaranteed the stability of product.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention;
Among the figure: 1. first distillation tower; 11. first material inlet; 12. first liquid phase outlet; 13. the first tower chamber gaseous phase outlet; 14. the second tower chamber gaseous phase outlet; 15. dividing plate; 16. the first tower chamber; 17. the second tower chamber; 2. second column; 21. second material inlet; 22. second liquid phase outlet; 23. second gaseous phase outlet.
Embodiment
Below in conjunction with accompanying drawing and embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Shown in accompanying drawing; The raw ketone alcohol mixture is got into first distillation tower from first material inlet 11; Light constituent is separated from the first tower chamber gaseous phase outlet 13 at 16 tops, the first tower chamber; Secondary octanone is separated from the second tower chamber gaseous phase outlet 14 at 17 tops, the second tower chamber, and the bottoms material is discharged from first liquid phase outlet 12, gets into second column 2 through second material inlet 21; Secondary octanol is discharged from second gaseous phase outlet 23 at second column 2 tops, and heavy constituent are discharged from second liquid phase outlet 22 of second column 2 bottoms.
Embodiment 1
The raw ketone alcohol mixture is at first got into placed in-line first distillation tower each other; The top of first distillation tower vertically is provided with dividing plate; The upper cavity of first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side; And the material inlet of first distillation tower is positioned at the top of dividing plate bottom, and the tower internal pressure of first distillation tower is that 18kPa, cat head gas phase temperature are that liquidus temperature is 140 ℃ at the bottom of 110 ℃, tower, and the light constituent first tower chamber cat head is separated; Secondary octanone is separated from the second tower chamber cat head; The bottoms material gets into second column, and the tower internal pressure of second column is that 15kPa, cat head gas phase temperature are that liquidus temperature is 150 ℃ at the bottom of 120 ℃, tower, and secondary octanol is separated from the after-fractionating column overhead; Heavy constituent are discharged at the bottom of the after-fractionating Tata, and the secondary octanone of separating and the purity of secondary octanol are seen table 1.
Embodiment 2
The raw ketone alcohol mixture is at first got into placed in-line first distillation tower each other; The top of first distillation tower vertically is provided with dividing plate; The upper cavity of first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side; And the material inlet of first distillation tower is positioned at the top of dividing plate bottom, and the tower internal pressure of first distillation tower is that 19kPa, cat head gas phase temperature are that liquidus temperature is 145 ℃ at the bottom of 115 ℃, tower, and the light constituent first tower chamber cat head is separated; Secondary octanone is separated from the second tower chamber cat head; The bottoms material gets into second column, and the tower internal pressure of second column is that 16kPa, cat head gas phase temperature are that liquidus temperature is 155 ℃ at the bottom of 125 ℃, tower, and secondary octanol is separated from the after-fractionating column overhead; Heavy constituent are discharged at the bottom of the after-fractionating Tata, and the secondary octanone of separating and the purity of secondary octanol are seen table 1.
Embodiment 3
The raw ketone alcohol mixture is at first got into placed in-line first distillation tower each other; The top of first distillation tower vertically is provided with dividing plate; The upper cavity of first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side; And the material inlet of first distillation tower is positioned at the top of dividing plate bottom, and the tower internal pressure of first distillation tower is that 20kPa, cat head gas phase temperature are that liquidus temperature is 150 ℃ at the bottom of 120 ℃, tower, and the light constituent first tower chamber cat head is separated; Secondary octanone is separated from the second tower chamber cat head; The bottoms material gets into second column, and the tower internal pressure of second column is that 17kPa, cat head gas phase temperature are that liquidus temperature is 160 ℃ at the bottom of 130 ℃, tower, and secondary octanol is separated from the after-fractionating column overhead; Heavy constituent are discharged at the bottom of the after-fractionating Tata, and the secondary octanone of separating and the purity of secondary octanol are seen table 1.
Table 1
Product Embodiment 1 Embodiment 2 Embodiment 3
Secondary octanone purity (wt%) 99.13 99.16 99.25
Secondary octanol purity (wt%) 99.61 99.75 99.67

Claims (3)

1. the method for dividing plate fractionation by distillation purification keto-alcohol mixture; It is characterized in that: said fractionation by distillation is accomplished in placed in-line first and second distillation towers each other; The top of said first distillation tower vertically is provided with dividing plate; The upper cavity of first distillation tower is divided into the first tower chamber that is positioned at material inlet one side and the second tower chamber of opposite side, and the material inlet of said first distillation tower is positioned at the top of said dividing plate bottom, and said fractionation by distillation may further comprise the steps:
The raw ketone alcohol mixture is got into placed in-line first distillation tower each other; Light constituent is separated from the first tower chamber cat head of first distillation tower; Secondary octanone is separated from the second tower chamber cat head; The bottoms material gets into second column, and secondary octanol is separated from the after-fractionating column overhead, and heavy constituent are discharged at the bottom of the after-fractionating Tata;
The pressure of said first distillation tower and second column is respectively 18~20kPa and 15~17kPa, and the cat head gas phase temperature is respectively 110~120 ℃ and 120~130 ℃.
2. the method for dividing plate fractionation by distillation purification keto-alcohol mixture as claimed in claim 1 is characterized in that: said first distillation tower and second column column bottom temperature are respectively 140~150 ℃ and 145~160 ℃.
3. the method for dividing plate fractionation by distillation purification keto-alcohol mixture as claimed in claim 1 is characterized in that: the purity of said secondary octanone of separating and secondary octanol is respectively 99.1wt% and more than the 99.6wt%.
CN2011103083163A 2011-10-12 2011-10-12 Method for distilling, separating and purifying ketone alcohol mixture by utilizing separating plate Pending CN102503789A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108774106A (en) * 2018-06-13 2018-11-09 山东元利科技股份有限公司 A kind of method and its catalyst for producing sec-octyl alcohol by extracting secondary octanone hydrogenating in thick sec-octyl alcohol
CN111473916A (en) * 2020-04-10 2020-07-31 中国石油化工股份有限公司 Monitoring method for crystallizer corrosion leakage condition

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108774106A (en) * 2018-06-13 2018-11-09 山东元利科技股份有限公司 A kind of method and its catalyst for producing sec-octyl alcohol by extracting secondary octanone hydrogenating in thick sec-octyl alcohol
CN108774106B (en) * 2018-06-13 2021-06-18 山东元利科技股份有限公司 Method for extracting sec-octanone from crude sec-octanol and hydrogenating to prepare sec-octanol and catalyst thereof
CN111473916A (en) * 2020-04-10 2020-07-31 中国石油化工股份有限公司 Monitoring method for crystallizer corrosion leakage condition
CN111473916B (en) * 2020-04-10 2022-05-31 中国石油化工股份有限公司 Monitoring method for crystallizer corrosion leakage condition

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Address after: 262404, Shandong province Weifang County Changle Zhu Liu Street Industrial Park (309 State Road 355 kilometers)

Applicant after: Shandong Yuanli Technology Co., Ltd.

Address before: 262404 No. 37 Industrial Zone, Zhu Liu street, Changle County, Shandong, Weifang

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Free format text: CORRECT: APPLICANT; FROM: WEIFANG YUANLI CHEMICAL CO., LTD. TO: SHANDONG YUANLI SCIENCE AND TECHNOLOGY CO., LTD.

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Application publication date: 20120620