CN107141196A - A kind of 1,4 butynediols two-stage hydrogenation systems - Google Patents

A kind of 1,4 butynediols two-stage hydrogenation systems Download PDF

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Publication number
CN107141196A
CN107141196A CN201710497533.9A CN201710497533A CN107141196A CN 107141196 A CN107141196 A CN 107141196A CN 201710497533 A CN201710497533 A CN 201710497533A CN 107141196 A CN107141196 A CN 107141196A
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CN
China
Prior art keywords
hydrogenation
hydrogen
hydrogenation plant
flash tank
butynediols
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Application number
CN201710497533.9A
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Chinese (zh)
Inventor
杨延奇
王读彬
孙乃良
高向国
张可
张一可
张驰
毛富彬
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Inquiry (shanghai) Technology Co Ltd
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Inquiry (shanghai) Technology Co Ltd
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Priority to CN201710497533.9A priority Critical patent/CN107141196A/en
Publication of CN107141196A publication Critical patent/CN107141196A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/17Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds
    • C07C29/172Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds with the obtention of a fully saturated alcohol

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)

Abstract

The invention discloses one kind 1, 4 butynediols two-stage hydrogenation systems, including device for producing hydrogen, first hydrogenation plant, second hydrogenation plant and entrance separator, described device for producing hydrogen one end connects raw hydrogen, the other end is sequentially connected the first hydrogenation plant, catalyst recovery devices, second hydrogenation plant, first flash tank and the second flash tank, second flash tank connects low pressure hydrogen compressor by entrance separator, the low pressure hydrogen compressor is connected to device for producing hydrogen import, first flash tank connects the first hydrogenation plant, agitator is provided with first hydrogenation plant, and first hydrogenation plant top be provided with gas-liquid separator, the gas-liquid separator also connects entrance separator, the device for producing hydrogen also connects the second hydrogenation plant top by high pressure hydrogen compressor;Flow of the present invention is simple, manipulation strength big and emptying end gas is fully reclaimed, and consumes low with operating cost.

Description

A kind of 1,4- butynediols two-stage hydrogenation system
Technical field
The invention belongs to Isosorbide-5-Nitrae-butynediols field of hydrogenation, more particularly to a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system System.
Background technology
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, industrial at present is two-stage hydrogenation on Isosorbide-5-Nitrae-butynediols hydrogenation, and two-stage hydrogenation is divided into again:Two sections are that high pressure adds Hydrogen and first paragraph are that low-voltage hydrogenation string second segment is two kinds of techniques of high-pressure hydrogenation.
In current domestic industry process units, during two-stage hydrogenation is the technique of high-pressure hydrogenation, exist because first paragraph adds Hydrogen intensity is excessive and causes the problem of catalyst inactivation is too fast;And first paragraph is the work that low-voltage hydrogenation string second segment is high-pressure hydrogenation Skill, though solving the problem of first paragraph hydrogenation catalyst inactivation is too fast in two-stage hydrogenation technique, it is present does not add to first paragraph The problem of emptying end gas in hydrogen technique is recycled with the final stage flash distillation emptying end gas in second segment hydrogenation technique.
The content of the invention
Present invention seek to address that drawbacks described above is there is provided Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system, which solves two sections and add The problem of first paragraph hydrogenation catalyst inactivation is too fast in hydrogen technique;It is that low-voltage hydrogenation string second segment is high pressure to solve first paragraph again In the technique of hydrogenation, the problem of emptying end gas is recycled;It is applied to the industrialized production that 1,4- butynediols is hydrogenated with.
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 two-stage hydrogenation system, including device for producing hydrogen, the first hydrogenation plant, the second hydrogenation plant and entrance separation Device, described device for producing hydrogen one end connects raw hydrogen, and the other end is sequentially connected the first hydrogenation plant, catalyst recovery devices, the Two hydrogenation plants, the first flash tank and the second flash tank, the second flash tank connect low pressure hydrogen compressor by entrance separator, Low pressure hydrogen compressor is connected to device for producing hydrogen import, and the first flash tank is connected to be set in the first hydrogenation plant, the first hydrogenation plant There is agitator, and the first hydrogenation plant top is provided with gas-liquid separator, the gas-liquid separator also connects entrance separator, described Device for producing hydrogen also connects the second hydrogenation plant top by high pressure hydrogen compressor.
In the preferred embodiment of the present invention, device for producing hydrogen is connected with resolution gas.
In the preferred embodiment of the present invention, the first hydrogenation plant is with treating that hydrogenating materials are connected.
In the preferred embodiment of the present invention, the second flash tank is connected with product after hydrogenation.
In the preferred embodiment of the present invention, the top end of the first hydrogenation plant is provided with deeply to its internal stirring Device, propeller-blade is 1-5 layers, preferably 3-4 layers.
The beneficial effects of the invention are as follows:The invention provides Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system, two sections are which solved The problem of first paragraph hydrogenation catalyst inactivation is too fast in hydrogenation technique, improves stability and the cycle of operation of device;Solve again First paragraph is that the problem of emptying end gas is recycled reduces and disappeared during low-voltage hydrogenation string second segment is the technique of high-pressure hydrogenation Consumption, has saved operating cost low;It is applied to the industrialized production that 1,4- butynediols is hydrogenated with.
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 two-stage hydrogenation system as shown in Figure 1, including device for producing hydrogen 1, the first hydrogenation plant 2, the Two hydrogenation plants 6 and entrance separator 10, the one end of device for producing hydrogen 1 connection raw hydrogen, the other end are sequentially connected the first hydrogenation dress 2, catalyst recovery devices 5, the second hydrogenation plant 6, the first flash tank 8 and the second flash tank 9 are put, the second flash tank 9 is by entering The mouth connection low pressure hydrogen of separator 10 compressor 11, low pressure hydrogen compressor 11 is connected to the import of device for producing hydrogen 1, the first flash tank Agitator 3 is provided with 8 the first hydrogenation plants 2 of connection, the first hydrogenation plant 2, and the top of the first hydrogenation plant 2 is provided with gas-liquid separation Device 4, gas-liquid separator 4 also connects entrance separator 10, and device for producing hydrogen 1 is also hydrogenated with by the connection of high pressure hydrogen compressor 7 second The top of device 6;Device for producing hydrogen 1 is connected with resolution gas.
First paragraph hydrogenation reactor 2 is with treating that hydrogenating materials are connected;Second flash tank 9 is connected with product after hydrogenation.
The top end of first paragraph hydrogenation reactor 2 is provided with deeply to its internal agitator 3, the blade of agitator 3 is 1-5 Layer, preferably 3-4 layers.
Embodiment:
Raw hydrogen obtains high-purity hydrogen through the purification of device for producing hydrogen 1(Hydrogen content:99.9%, CO+CO2 < 10ppm), High Purity Hydrogen Gas is with treating hydrogenating materials(Isosorbide-5-Nitrae-butynediols content 32-37%, PH:8.0-9.0, catalyst solid thing content:5-25g/ l00ml)Enter the first hydrogenation plant 2 together, in agitator 3(4 layers of blade)Participation reaction, control are thoroughly mixed under effect The temperature of first hydrogenation plant 2 at 55-65 DEG C, pressure after 2.2-2.5MPa.g, reaction solution through the first hydrogenation plant 2 inside Interpolation pipe with sleeve is drawn and delivers to catalyst recovery devices 5, and through multi-stage separation and filtering, the catalyst of recovery is back to first The suction line of hydrogenation plant 2 is to recycle, solution after the reaction without catalyst(Solids particle diameter < 0.5um)With through high pressure Hydrogen after the pressurization of hydrogen gas compressor 7(Pressure:25MPa.g), progress deep hydrogenation in the second hydrogenation plant 6 is entered together anti- Should, the control temperature of the second hydrogenation plant 6 at 55-65 DEG C, pressure 2.2-2.5MPa.g Isosorbide-5-Nitraes-butynediols conversion ratio >= 99.99%, the solution reacted through two-stage hydrogenation enters the first flash tank 8, the hydrogen after the flash distillation of the top of the first flash tank 8(Pressure: 2.5 MPa.g)Enter the first hydrogenation plant 2 together with the high-purity hydrogen that device for producing hydrogen 1 comes out, hydrogen is recycled, first dodges The material of the bottom of steaming pot 8 enters the second flash tank 9, the hydrogen after the flash distillation of the top of the second flash tank 9(Pressure:0.1-0.25 MPa.g)Enter entrance separator 10 together with through the top of gas-liquid separator 4 hydrogen out, the hydrogen after separating liquid from The top of entrance separator 10 enters low pressure air compressor 11, is pressurizeed through low pressure hydrogen compressor 11(Pressure:2.8-3.0 MPa.g) The hydrogen delivered to afterwards in the suction line of device for producing hydrogen 1, emptying end gas is reclaimed through device for producing hydrogen 1, realizes the circulation profit of hydrogen With.
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 (5)

1. a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system, it is characterised in that including device for producing hydrogen, the first hydrogenation plant, second Hydrogenation plant and entrance separator, described device for producing hydrogen one end connect raw hydrogen, the other end be sequentially connected the first hydrogenation plant, Catalyst recovery devices, the second hydrogenation plant, the first flash tank and the second flash tank, second flash tank are separated by entrance Device connects low pressure hydrogen compressor, and the low pressure hydrogen compressor is connected to device for producing hydrogen import, the first flash tank connection Agitator is provided with first hydrogenation plant, first hydrogenation plant, and the first hydrogenation plant top is provided with gas-liquid separator, institute State gas-liquid separator and also connect entrance separator, the device for producing hydrogen also connects the second hydrogenation plant by high pressure hydrogen compressor Top.
2. a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system as claimed in claim 1, it is characterised in that the device for producing hydrogen with Resolution gas is connected.
3. a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system as claimed in claim 1, it is characterised in that the first hydrogenation dress Put and treat that hydrogenating materials are connected.
4. a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system as claimed in claim 1, it is characterised in that second flash tank It is connected with product after hydrogenation.
5. a kind of Isosorbide-5-Nitrae-butynediols two-stage hydrogenation system as claimed in claim 1, it is characterised in that the first hydrogenation dress The top end put is provided with deeply to its internal agitator, propeller-blade is 1-5 layers.
CN201710497533.9A 2017-06-27 2017-06-27 A kind of 1,4 butynediols two-stage hydrogenation systems Withdrawn CN107141196A (en)

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CN201710497533.9A CN107141196A (en) 2017-06-27 2017-06-27 A kind of 1,4 butynediols two-stage hydrogenation systems

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112457160A (en) * 2019-09-06 2021-03-09 南京延长反应技术研究院有限公司 Preparation system and process of 1, 4-butanediol
CN114409504A (en) * 2022-01-15 2022-04-29 山西大学 Method for preparing 1, 4-butanediol by hydrogenation of 1, 4-butynediol
CN114874071A (en) * 2022-05-06 2022-08-09 河南能源化工集团鹤壁煤化工有限公司 BDO (boron-containing organic compound) circulating hydrogenation process

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3449445A (en) * 1967-03-17 1969-06-10 Gaf Corp Process of preparing 1,4-butanediol
CN1081174A (en) * 1992-07-08 1994-01-26 化学工业部北京化工研究院 Butynediol medium-pressure hydrocracking system butyleneglycol Process
CN101348235A (en) * 2007-07-19 2009-01-21 中国石油化工集团公司 Hydrogen recovery method for hydrogenation plant
CN103113190A (en) * 2013-02-05 2013-05-22 中国五环工程有限公司 Butynediol low-pressure hydrogenation catalyst recycling process and system
CN106232561A (en) * 2014-04-24 2016-12-14 因温斯特技术公司 The butanediol manufacture method improved

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3449445A (en) * 1967-03-17 1969-06-10 Gaf Corp Process of preparing 1,4-butanediol
CN1081174A (en) * 1992-07-08 1994-01-26 化学工业部北京化工研究院 Butynediol medium-pressure hydrocracking system butyleneglycol Process
CN101348235A (en) * 2007-07-19 2009-01-21 中国石油化工集团公司 Hydrogen recovery method for hydrogenation plant
CN103113190A (en) * 2013-02-05 2013-05-22 中国五环工程有限公司 Butynediol low-pressure hydrogenation catalyst recycling process and system
CN106232561A (en) * 2014-04-24 2016-12-14 因温斯特技术公司 The butanediol manufacture method improved

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112457160A (en) * 2019-09-06 2021-03-09 南京延长反应技术研究院有限公司 Preparation system and process of 1, 4-butanediol
CN114409504A (en) * 2022-01-15 2022-04-29 山西大学 Method for preparing 1, 4-butanediol by hydrogenation of 1, 4-butynediol
CN114409504B (en) * 2022-01-15 2023-12-26 山西大学 Method for preparing 1, 4-butanediol by hydrogenating 1, 4-butynediol
CN114874071A (en) * 2022-05-06 2022-08-09 河南能源化工集团鹤壁煤化工有限公司 BDO (boron-containing organic compound) circulating hydrogenation process

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