CN107089901A - A kind of 1,4 butynediols purification systems - Google Patents
A kind of 1,4 butynediols purification systems Download PDFInfo
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- CN107089901A CN107089901A CN201710497516.5A CN201710497516A CN107089901A CN 107089901 A CN107089901 A CN 107089901A CN 201710497516 A CN201710497516 A CN 201710497516A CN 107089901 A CN107089901 A CN 107089901A
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- butynediols
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- formaldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The invention discloses one kind 1, 4 butynediols purification systems, including butynediols product tower, the butynediols product tower is connected with solution to be purified, butynediols product tower is also sequentially connected the system of steaming, butynediols product tower vapor condensation system, formaldehyde tower and formaldehyde tower vapor condensation system, wherein, butynediols product tower through waste heat boiler respectively with the system of steaming, butynediols product tower vapor condensation system is connected, the butynediols product tower vapor condensation system through butynediols product tower reflux pump respectively with butynediols product tower, formaldehyde tower is connected, the formaldehyde tower is connected through formaldehyde tower top cooler with formaldehyde tower vapor condensation system;Flow of the present invention is simple, manipulation strength big, the cycle of operation is long, while fully reclaiming butynediols product tower gas phase heat again is used to produce steam, consumes low with operating cost.
Description
Technical field
The invention belongs to Isosorbide-5-Nitrae-butynediols purification field, more particularly to a kind of Isosorbide-5-Nitrae-butynediols purification system.
Background technology
Isosorbide-5-Nitrae-butynediols (Isosorbide-5-Nitrae-butynediol), also known as Isosorbide-5-Nitrae-dihydroxy -2- butine or 2- butine-Isosorbide-5-Nitrae-glycol,
English abbreviation BYD, molecular formula:C4H602, molecular weight:86.09,1,4- butynediols is usually white rhomboidal crystal or 35%
The aqueous solution, fusing point under normal pressure:57-58 DEG C, boiling point:238 DEG C, water, ethanol and propyl alcohol are dissolved in, toxicity is high, to the upper respiratory tract, eye
Mucous membrane, skin have narcoticness stimulation.
Isosorbide-5-Nitrae-butynediols is basic chemical raw materials, soluble in water, ethanol, insoluble in ether, hydro carbons, with binary primary alconol
Chemical property, mainly for the production of butanediol and its downstream product, such as polybutylene terephthalate(PBT), polyurethane
Chain extender and adhesive, tetrahydrofuran, gamma-butyrolacton, 1-METHYLPYRROLIDONE, 2-Pyrrolidone and polyvinyladehydes pyrrolidones
Product etc., while still producing the primary raw material of vitamin B6, industrially can be used as the brightener, preservative, inhibitor of nickel plating
Deng.
When producing BDO by Isosorbide-5-Nitrae-butynediols for raw material, Isosorbide-5-Nitrae-butynediols, which need to be hydrogenated with, could generate Isosorbide-5-Nitrae-fourth
Glycol, needs when before hydrogenation by harmful constituent:The method that formaldehyde, methanol, propilolic alcohol etc. are reminded by rectifying divides it in advance
From falling, in current domestic industry process units, there is butynediols product column overhead gas phase heat not using or using not filling
Point, the problems such as hydroxyl numerical value is higher, butynediols product tower tray floor is easily blocked in butyne diol solutions.
The content of the invention
Present invention seek to address that drawbacks described above is there is provided a kind of Isosorbide-5-Nitrae-butynediols purification system, in butynediols product
Waste heat boiler, heat pump assembly etc. are provided with column overhead vapor delivery line, abundant recovery has been carried out to gas-phase potential heat and Lowlevel thermal energy,
Solve the problem of butynediols product column overhead gas phase heat does not utilize or utilizes insufficient;Simultaneously in butynediols product tower
Bottom is connected with middle pressure steam, by supplementing clean water vapour adjustment operation operating mode, solves butanol glycol product tower bottom fourth
The problems such as hydroxyl numerical value is higher in acetylenic glycols solution and butanol glycol product tower tray floor is easily blocked.
In order to overcome defect present in background technology, the technical solution adopted for the present invention to solve the technical problems is:
A kind of Isosorbide-5-Nitrae-butynediols purification system, including butynediols product tower, the butynediols product tower connect with solution to be purified
Connect, butynediols product tower is also sequentially connected the system of steaming, butynediols product tower vapor condensation system, formaldehyde tower, formaldehyde tower
Vapor condensation system, wherein, the butynediols product tower through waste heat boiler respectively with the system of steaming, butynediols product tower gas
Phase condenser system connect, the butynediols product tower vapor condensation system through butynediols product tower reflux pump respectively with butine
Glycol product tower, the connection of formaldehyde tower, the formaldehyde tower are connected through formaldehyde tower top cooler with formaldehyde tower vapor condensation system.
The present invention a preferred embodiment in, the butynediols product tower bottom respectively with middle pressure steam, butine
Glycol solution is connected.
In the preferred embodiment of the present invention, the system of steaming is followed including waste heat boiler, hot water heat exchanger, hot water
Ring pump, heat pump assembly, waste heat boiler are sequentially connected hot water heat exchanger, heat pump assembly and hot water circulating pump, the hot water circulating pump
Hot water heat exchanger is connected to, the waste heat boiler, the bottom of heat pump assembly and top respectively connect with boiler water and steam pipe system
Connect.
In the preferred embodiment of the present invention, butynediols product tower vapor condensation system includes the water being sequentially connected
Cooler, exhaust gas cooler, gas-liquid separator, butynediols product tower return tank, butynediols product tower reflux pump, the tail gas
Cooler is reclaimed with acetylene tail gas and is connected, and the waste heat boiler and hot water heat exchanger are connected to the backflow of butynediols product tower
Tank.
In the preferred embodiment of the present invention, the formaldehyde tower bottom is connected with alkynes aldehyde reaction.
In the preferred embodiment of the present invention, the formaldehyde tower top that formaldehyde tower vapor condensation system includes being sequentially connected is cold
But device, formaldehyde tower return tank and formaldehyde tower reflux pump, the formaldehyde tower top cooler, formaldehyde tower return tank are vented with normal pressure to be connected
Connect, formaldehyde tower reflux pump is connected with formaldehyde tower and Methanol Recovery respectively.
The beneficial effects of the invention are as follows:The invention provides Isosorbide-5-Nitrae-butynediols purification system,
The problem of butynediols product column overhead gas phase heat does not utilize or utilizes insufficient is which solved, consumption is reduced, it is real
The maximization for having showed energy is recycled, and has saved operating cost low;Solve butanol glycol product tower bottom butine again simultaneously
The problems such as hydroxyl numerical value is higher in glycol solution and butanol glycol product tower tray floor is easily blocked, improve the stability of device with
The cycle of operation;It is applied to the industrialized production that 1,4- butynediols is purified.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is the structural representation of the present invention.
Embodiment
Presently preferred embodiments of the present invention is described in detail below in conjunction with the accompanying drawings, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art, apparent is clearly defined so as to be made to protection scope of the present invention.
A kind of Isosorbide-5-Nitrae-butynediols purification system as shown in Figure 1, including butynediols product tower 1, butynediols product tower 1
It is connected with solution to be purified, butynediols product tower 1 is also sequentially connected the system of steaming, butynediols product tower vapor condensation system
System, formaldehyde tower 11, formaldehyde tower vapor condensation system, wherein, the butynediols product tower 1 is through waste heat boiler 2 respectively with steaming
System, the connection of butynediols product tower vapor condensation system, the butynediols product tower vapor condensation system is through butynediols
Product tower reflux pump 7 is connected with butynediols product tower 1, formaldehyde tower 11 respectively, and the formaldehyde tower 11 is through formaldehyde tower top cooler
12 are connected with formaldehyde tower vapor condensation system.
The bottom of butynediols product tower 1 is connected with middle pressure steam, butyne diol solutions respectively.
System of steaming includes waste heat boiler 2, hot water heat exchanger 3, hot water circulating pump 4, heat pump assembly 5, and waste heat boiler 2 is successively
Hot water heat exchanger 3, heat pump assembly 5 and hot water circulating pump 4 are connected, hot water circulating pump 4 is connected to hot water heat exchanger 3, the used heat
Boiler 2, the bottom of heat pump assembly 5 are respectively connected with top with boiler water with steam pipe system.
Butynediols product tower vapor condensation system includes the water cooler 8, exhaust gas cooler 9, gas-liquid separation being sequentially connected
Device 10, butynediols product tower return tank 6, butynediols product tower reflux pump 7, exhaust gas cooler 9 is reclaimed with acetylene tail gas to be connected
Connect, waste heat boiler 2 and hot water heat exchanger 3 are connected to butynediols product tower return tank 6.
The bottom of formaldehyde tower 11 is connected with alkynes aldehyde reaction.
The formaldehyde tower vapor condensation system include be sequentially connected formaldehyde tower top cooler 12, formaldehyde tower return tank 13,
Formaldehyde tower reflux pump 14, the formaldehyde tower top cooler 12, formaldehyde tower return tank 13 are connected with normal pressure emptying, the backflow of formaldehyde tower
Pump 14 is connected with formaldehyde tower 11 and Methanol Recovery respectively.
Embodiment:
Solution to be purified(1,4- butynediols:43.5%, methanol:1.2%, formaldehyde:1.8%, propilolic alcohol:0.65%)Into butanol two
Alcohol product tower 1, the column bottom temperature of butanol glycol product tower 1 is controlled by the tower bottom reboiler of butanol glycol product tower 1 and middle pressure steam
At 138-142 DEG C, control butanol glycol product tower 1 bottom of towe hydroxyl numerical value < 2.5mg KOH/g, fourth into butyne diol solutions
The top gaseous phase of alcohol glycol product tower 1 enters to cool in waste heat boiler 2 through boiler water, recovery section gas-phase potential heat by-product
0.185MPa.g steam delivers to uncooled gas phase in steam pipe system, waste heat boiler 2 and carries out hot water heat exchanger 3, through hot water circulating pump 4
Reclaim remaining low grade residual heat and 90 DEG C of hot water are made into heat pump assembly 5, fill into boiler water and enter generation after heat pump assembly 5
0.185MPa.g steam delivers to steam pipe system, and waste heat boiler 2,3 times Partial Liquid Phases of hot water heat exchanger carry out producing into butynediols
In product tower return tank 6, uncooled gas phase carries out water cooler 8 in hot water heat exchanger 3, and gas phase temperature temperature is 70 after control cooling
DEG C, in water cooler 8 uncooled gas phase enter exhaust gas cooler 9, control cooling after 35 DEG C of gas phase temperature temperature <, water cooler 8 with
9 times Partial Liquid Phases of exhaust gas cooler are carried out into gas-liquid separator 10, liquid phase in gas-liquid separator 10 after separation gas phase, into fourth
It is most of to enter butynediols product tower through the pressurized delivered of butynediols product tower reflux pump 7 in acetylenic glycols product tower return tank 6
Backflow is participated in, small part enters formaldehyde tower 11 in addition, control the column bottom temperature of formaldehyde tower 11 to exist by the tower bottom reboiler of formaldehyde tower 11
102-105 DEG C, the bottom of towe solution of formaldehyde tower 11(Contain formaldehyde, propilolic alcohol, water)Alkynes aldehyde reaction is delivered to, formaldehyde and propilolic alcohol is realized
Recycling, the top gaseous phase of formaldehyde tower 11 enter formaldehyde tower top cooler 12 in, after cooling liquid phase enter formaldehyde tower backflow
In tank 13, through the pressurized delivered of formaldehyde tower reflux pump 14, most of formaldehyde tower 11 that enters participates in backflow, the tower overhead gas of control formaldehyde tower 11
Phase temperature is at 70-75 DEG C, and small part delivers to Methanol Recovery in addition(Methanol content≤95%), formaldehyde tower top cooler 12 and formaldehyde
The uncooled fixed gas in the top of tower return tank 13 delivers to normal pressure emptying.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related skills
Art field, is included within the scope of the present invention.
Claims (6)
1. a kind of Isosorbide-5-Nitrae-butynediols purification system, it is characterised in that including butynediols product tower, the butynediols product
Tower is connected with solution to be purified, and butynediols product tower is also sequentially connected the system of steaming, butynediols product tower vapor condensation system
System, formaldehyde tower and formaldehyde tower vapor condensation system, wherein, butynediols product tower through waste heat boiler respectively with the system of steaming, fourth
Acetylenic glycols product tower vapor condensation system is connected, and the butynediols product tower vapor condensation system is returned through butynediols product tower
Stream pump is connected with butynediols product tower, formaldehyde tower respectively, and the formaldehyde tower is cold through formaldehyde tower top cooler and formaldehyde tower gas phase
Solidifying system connection.
2. Isosorbide-5-Nitrae as claimed in claim 1-butynediols purification system, it is characterised in that part under the butynediols product tower
It is not connected with middle pressure steam, butyne diol solutions.
3. Isosorbide-5-Nitrae as claimed in claim 1-butynediols purification system, it is characterised in that the system of steaming includes waste heat boiler
Stove, hot water heat exchanger, hot water circulating pump and heat pump assembly, the waste heat boiler be sequentially connected hot water heat exchanger, heat pump assembly and
Hot water circulating pump, the hot water circulating pump is connected to hot water heat exchanger, and the waste heat boiler, the bottom of heat pump assembly and top are equal
It is connected respectively with boiler water with steam pipe system.
4. Isosorbide-5-Nitrae as claimed in claim 3-butynediols purification system, it is characterised in that the butynediols product tower gas phase is cold
Solidifying system includes water cooler, exhaust gas cooler, gas-liquid separator, butynediols product tower return tank, the butine two being sequentially connected
Alcohol product tower reflux pump, the exhaust gas cooler is reclaimed with acetylene tail gas and is connected, and the waste heat boiler and hot water heat exchanger connect
It is connected to butynediols product tower return tank.
5. Isosorbide-5-Nitrae-butynediols purification system as described in right wants 1, it is characterised in that the formaldehyde tower bottom and alkynes aldehyde reaction
Connection.
6. Isosorbide-5-Nitrae as claimed in claim 1-butynediols purification system, it is characterised in that the formaldehyde tower vapor condensation system bag
Include the formaldehyde tower top cooler being sequentially connected, formaldehyde tower return tank and formaldehyde tower reflux pump, the formaldehyde tower top cooler, formaldehyde
Tower return tank is connected with normal pressure emptying, and formaldehyde tower reflux pump is connected with formaldehyde tower and Methanol Recovery respectively.
Priority Applications (1)
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CN201710497516.5A CN107089901A (en) | 2017-06-27 | 2017-06-27 | A kind of 1,4 butynediols purification systems |
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CN201710497516.5A CN107089901A (en) | 2017-06-27 | 2017-06-27 | A kind of 1,4 butynediols purification systems |
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ID=59640943
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112521252A (en) * | 2020-12-13 | 2021-03-19 | 天津大学 | Concentrated heat pump rectification process and equipment for propargyl alcohol and butynediol aqueous solution system |
CN112811984A (en) * | 2020-12-13 | 2021-05-18 | 天津大学 | Baffle plate rectification process and equipment for propynol and butynediol aqueous solution system |
CN115819187A (en) * | 2022-11-10 | 2023-03-21 | 中国石化长城能源化工(宁夏)有限公司 | Novel 1,4-butynediol purification treatment method |
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US3130236A (en) * | 1960-06-20 | 1964-04-21 | Gen Aniline & Film Corp | Process of removing formaldehyde from 1, 4-butynediol |
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US3130236A (en) * | 1960-06-20 | 1964-04-21 | Gen Aniline & Film Corp | Process of removing formaldehyde from 1, 4-butynediol |
US4180687A (en) * | 1978-04-24 | 1979-12-25 | E. I. Du Pont De Nemours And Company | Reaction of formaldehyde in butynediol |
EP0309915A1 (en) * | 1987-09-30 | 1989-04-05 | BASF Aktiengesellschaft | Process for removing formaldehyde from aqueous solutions of but-2-yn-1,4-diols |
CN103974924A (en) * | 2011-11-28 | 2014-08-06 | 因温斯特技术公司 | Caustic treatment of formaldehyde recycle column feed |
CN202754919U (en) * | 2012-06-27 | 2013-02-27 | 高猛 | 1, 4-butynediol stripping tower top steam latent heat recycle device |
WO2016036655A1 (en) * | 2014-09-04 | 2016-03-10 | Invista North America S.A.R.L. | Improved formaldehyde recovery method |
CN206843352U (en) * | 2017-06-27 | 2018-01-05 | 查都(上海)科技有限公司 | A kind of 1,4 butynediols purification systems |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112521252A (en) * | 2020-12-13 | 2021-03-19 | 天津大学 | Concentrated heat pump rectification process and equipment for propargyl alcohol and butynediol aqueous solution system |
CN112811984A (en) * | 2020-12-13 | 2021-05-18 | 天津大学 | Baffle plate rectification process and equipment for propynol and butynediol aqueous solution system |
CN112811984B (en) * | 2020-12-13 | 2023-09-26 | 天津大学 | Baffle rectification process and equipment for propynylol and butynyldiol aqueous solution system |
CN115819187A (en) * | 2022-11-10 | 2023-03-21 | 中国石化长城能源化工(宁夏)有限公司 | Novel 1,4-butynediol purification treatment method |
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Address after: 570000 No. a5002-323, A1 area, Fuxing City, 32 Binhai Avenue, Longhua District, Haikou City, Hainan Province Applicant after: Chadu (Hainan) Technology Co.,Ltd. Address before: Part 541, 5A / F, building B, 155 Fute West 1st Road, Shanghai pilot Free Trade Zone, Pudong New Area, Shanghai, 200120 Applicant before: CHADU (SHANGHAI) TECHNOLOGY Co.,Ltd. |
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