CN105906524A - Industrial device and process for continuously producing N,N-diethyl formamide - Google Patents

Industrial device and process for continuously producing N,N-diethyl formamide Download PDF

Info

Publication number
CN105906524A
CN105906524A CN201610391555.2A CN201610391555A CN105906524A CN 105906524 A CN105906524 A CN 105906524A CN 201610391555 A CN201610391555 A CN 201610391555A CN 105906524 A CN105906524 A CN 105906524A
Authority
CN
China
Prior art keywords
tower
storage tank
distillation column
reactor
catalyst
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610391555.2A
Other languages
Chinese (zh)
Inventor
王立静
辛志国
张斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dezhou Dehua Chemical Industry Co Ltd
Original Assignee
Dezhou Dehua Chemical Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dezhou Dehua Chemical Industry Co Ltd filed Critical Dezhou Dehua Chemical Industry Co Ltd
Priority to CN201610391555.2A priority Critical patent/CN105906524A/en
Publication of CN105906524A publication Critical patent/CN105906524A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/10Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

Abstract

The invention relates to an industrial device and method for continuously producing N,N-diethyl formamide. The device comprises a catalytic agent storage groove, a DEA storage groove, a DEA/ethyl alcohol storage groove and a product tank and further comprises a synthesis reactor, a first rectifying tower, a second rectifying tower and a gas stripping tower. According to the technical scheme, sodium ethoxide is adopted as a catalyst, ethyl alcohol is used as a solvent, no catalyst promoter is adopted, diethylamine and CO are used as raw materials, DEF is directly synthesized under the conditions that the temperature is 90-130 DEG C and pressure is 1.3-2.0 MPa, and the DEF production selectivity is 99%. By means of the technical scheme, the raw material cost is greatly reduced, unreacted raw materials are directly conveyed to an ethylamine device to be recycled without separation, the recycling cost is low, implementation is easy, the product purity is high, DEF content reaches 99.98%, and the requirements of users at home and abroad can be met.

Description

Produce industrialized unit and the technique thereof of N, N-diethylformamide continuously
Technical field
The present invention relates to the process units of a kind of N, N-diethylformamide, particularly relate to one and produce N, N-bis-continuously The industrialized unit of ethyl-formamide and technique thereof.
Background technology
Being a kind of colourless or light yellow transparent liquid at normal temperatures about N, N-diethylformamide (DEF), molecular formula is C5H11NO, DEF's is of many uses, is currently mainly used as solvent, preservative, anthelmintic etc., along with the development of electronic industrial technology, DEF starts to be largely used to the fluoroscopic abluent of LED, is used for removing the photoresist remained in process.
At present, the industrialized unit of domestic production DEF it is not yet reported that, only experimentation report, is to make with Feldalat NM For catalyst, promoter made by expoxy propane, and with methanol as solvent, the selectivity producing DEF is 96%, produces in this way DEF cost of material high, unreacted raw materials recovery cost is high, and the difficulty of recovery is big, and poor product quality does not reaches user quality Requirement, does not commercially have competitiveness.
Summary of the invention
In view of this, present invention is primarily targeted at the industrialization providing one to produce N, N-diethylformamide continuously Device and technique thereof, by the technical program, use Sodium ethylate to make catalyst, with ethanol as solvent, need not any promoter, It is raw material with diethylamine and CO, under conditions of temperature 90-130 DEG C, pressure 1.3-2.0MPa, is directly synthesized DEF, produce DEF's Selectivity is 99%, by the technical program, greatly reduces cost of material, and unreacted raw material directly returns instead without separating Answering system to recycle, cost recovery is low and easily realizes, and product purity is high, and DEF content reaches 99.98%, can meet both at home and abroad The requirement of user.
In order to achieve the above object, the technical scheme is that and be achieved in that:
One produces the industrialized unit of N, N-diethylformamide continuously, includes catalyst storage tank, DEA storage tank, recycle stock Storage tank and products pot, also include synthesis reactor, the first rectifying column, Second distillation column and stripping tower, in described synthesis reactor It is provided with reactor liquid phase entrance and reactor outlet, the catalyst storage that catalyst storage tank, DEA storage tank and recycle stock storage tank are arranged Groove outlet, DEA reservoir outlet and recycle stock reservoir outlet are entered with the reactor liquid phase in synthesis reactor by connecting pipe Mouth is connected, and described first rectifying column and Second distillation column are respectively arranged with the first rectifying column charging aperture, the first rectifying tower top Discharging opening and the first tower bottom of rectifying tower discharging opening and Second distillation column charging aperture, Second distillation column top discharging opening and Second distillation column Tower reactor discharging opening, the first rectifying tower top discharging opening is by connecting the recycle stock storage tank charging of pipeline and recycle stock storage tank upper end Mouth is connected, and the reactor outlet in synthesis reactor is connected by connecting pipe and the first rectifying column charging aperture, the first essence Evaporating tower tower reactor discharging opening to be connected with Second distillation column charging aperture through connecting pipe, Second distillation column discharging opening passes through connecting pipe It is connected with the stripping tower material inlet of stripping tower, is positioned at the air stripping tower reactor discharging opening bottom stripping tower by connecting pipe and position Products pot import in the middle part of products pot is connected.
As further technical scheme, also including vaporizer and filter, described vaporizer and filter are arranged on Synthesis is sent out and is answered between device and the first rectifying column, and the evaporator inlet of described vaporizer is by connecting the anti-of pipeline and synthesis reactor Answering device outlet to be connected, the vaporizer gaseous phase outlet of vaporizer feeds by connecting the first rectifying column of pipeline and the first rectifying column Mouth is connected, and the vaporizer liquid-phase outlet of vaporizer is connected with the filter import of filter by connecting pipeline, and filter goes out Mouth is connected with the vaporizer refluxing opening of vaporizer by connecting pipeline.
As further technical scheme, described Second distillation column is negative pressure tower.
One produces the industrialization process of N, N-diethylformamide continuously, and reaction equation is:
Catalyst
(CH3CH2)2NH+CO——————→(CH3CH2)2NCOH + Q
1.3-2.0MPaG, 90~130 DEG C.
The described industrialization process producing N, N-diethylformamide continuously, is carried out in following processing steps:
(1) preparation: by catalyst discharging pump, the ethanol solution of 20% Sodium ethylate is squeezed into catalyst storage tank, and liquid level reaches 50-80%, Catalyst storage tank is passed through N2 protection, and catalyst storage tank operating pressure is 0.07-0.2MpaG;Diethylamine is sent into EDA storage tank by irrigated area, Liquid level reaches 50-80%;
(2) inject synthesis reactor: in catalyst storage tank, ethanol solution passes through catalyst feed pump, through effusion meter with flow as 4-7L/ The speed of h enters in synthesis reactor;DEA pressurizes through DEA feed pump, is entered for 1000-1200Kg/h with flow by effusion meter Enter synthesis reactor;The CO come through membrance separation passes through the effusion meter speed entrance synthesis reactor with flow as 430-520Kg/h In;
(3) synthetic reaction: (2) entered into CO, DEA and the CAT in synthesis reactor by step, in 1.3-2.0Mpa pressure, temperature Circular response under the conditions of spending 90-130 DEG C, the material after synthetic reaction enters evaporative filtration operation through circulating pump extraction, the most anti- The condensed rear liquid-phase reflux of gas phase that should fall is in synthesis reactor, and gas phase goes boiler combustion;
Evaporative filtration separate: above-mentioned steps (3) in through circulating pump extraction enter evaporative filtration operation synthesis liquid by evaporation Device, the liquid material being positioned at base of evaporator removes sodium salt and catalyst through filter, and the clear liquid after filtration steams at 2.5MPa Vapour is as adding thermal medium, and steam flow is to enter rectification working process, the liquid in vaporizer in the case of 700-800Kg/h after gasification Material enters base of evaporator, repeats above-mentioned filtration, heating, separation process;
(5) rectification: above-mentioned steps (4) in isolated gas enter the first rectifying column, through the light component such as the DEA of rectification, ethanol Entering condensation from the first rectifying tower top, a condensed condensed fluid part flow back in the first rectifying column, at the bottom of the first rectifying tower Extraction be about 99% DEF enter the Second distillation column of rectification again, DEF from Second distillation column overhead extraction after pump boosts Send into air stripping operation;
(6) air stripping qualified products: above-mentioned steps (5) in, the DEF of Second distillation column overhead extraction enters the top of stripping tower, nitrogen Being entered stripping tower by bottom, two phase countercurrent flow contacts, and makes DEF reach product requirement after nitrogen air stripping, and qualified products are by air stripping Extraction at the bottom of tower tower, after pump boosts, is sent in products pot.
The step of above-mentioned power 5 (5) described in a condensed condensed fluid part flow back in the first rectifying column, another portion Point from first rectifying column top enter recycle stock storage tank, and with power 5 steps (2) in other CO, DEA and CAT together right of access 5 Step (3), carry out synthetic reaction again.
The step of above-mentioned power 5 (5) described in Second distillation column be negative pressure tower (≤180mmHg absolute pressure), Second distillation column is again Boiling uses 2.5MPa steam as adding thermal medium, and flow is 700-800Kg/h, and the mixture through rectification heavy constituent and DEF reaches During to 130 DEG C, by extraction at the bottom of Second distillation column tower to heavy component tank, after utilizing nitrogen pressurization, deliver to boiler combustion.
The step of above-mentioned power 5 (6) in, boiler combustion is delivered in the gas emptying not being condensed at stripping tower tower top.
Provide the benefit that after using technique scheme: one produces the industry makeup of N, N-diethylformamide continuously Put and method, by the technical program, use Sodium ethylate to make catalyst, with ethanol as solvent, need not any promoter, use Diethylamine and CO are raw material, are directly synthesized DEF under conditions of temperature 90-130 DEG C, pressure 1.3-2.0MPa, produce the choosing of DEF Selecting property is 99%, by the technical program, greatly reduces cost of material, and unreacted raw material directly send recycle without separating Batch can dereaction system participates in reaction, and cost recovery is low and easily realizes, and product purity is high, and DEF content reaches 99.98%, can be full The requirement of foot users at home and abroad.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of the present invention.
In figure, 1 catalyst storage tank, 11 catalyst reservoir outlet, 2 DEA storage tanks, 21 DEA reservoir outlet, 3 recycle stock storages Groove, 31 recycle stock storage tank charging apertures, 32 recycle stock reservoir outlet, 4 synthesis reactor, 41 reactor liquid phase entrances, 42 Reactor outlet, 43 reactor gas phase entrances, 5 vaporizers, 51 vaporizer gaseous phase outlets, 52 vaporizer liquid-phase outlets, 53 evaporations Device refluxing opening, 54 evaporator inlets, 6 filters, 61 filter outlets, 62 filter imports, 7 first rectifying columns, 71 first essences Evaporate tower tower reactor discharging opening, 72 first rectifying column discharging openings, 73 first rectifying column charging apertures, 8 Second distillation columns, 81 Second distillation columns Discharging opening, 82 Second distillation column tower reactor discharging openings, 83 Second distillation column charging apertures, 9 stripping towers, 91 air stripping tower reactor discharging openings, 92 Stripping tower gas phase import, 94 stripping tower material inlets, 10 products pots, 101 products pot imports, 110 connecting pipes.
Detailed description of the invention
Below in conjunction with accompanying drawing, specific embodiment in the present invention is described in further detail.
As it is shown in figure 1, the industrialized unit producing N, N-diethylformamide continuously that the present invention relates to, include catalyst Storage tank 1, DEA storage tank 2, recycle stock storage tank 3 and products pot 10, also include synthesis reactor the 4, first rectifying column the 7, second rectification Tower 8 and stripping tower 9, described synthesis reactor 4 is provided with reactor liquid phase entrance 41 and reactor outlet 42, catalyst storage tank 1, Catalyst reservoir outlet 11, DEA reservoir outlet 21 and the recycle stock reservoir outlet arranged on DEA storage tank 2 and recycle stock storage tank 3 32 are connected with the reactor liquid phase entrance 41 in synthesis reactor 4 by connecting pipe 110, described first rectifying column 7 and the It is respectively arranged with first rectifying column charging aperture the 73, first rectifying column discharging opening 72 on two rectifying columns 8 and the first tower bottom of rectifying tower goes out Material mouth 71 and Second distillation column charging aperture 83, Second distillation column discharging opening 81 and Second distillation column tower reactor discharging opening 82, the first essence Evaporate tower discharging opening 81 and be connected with the recycle stock storage tank charging aperture 31 of recycle stock storage tank 3 upper end by connecting pipeline 110, close The reactor outlet 42 on reactor 4 is become to be connected with the first rectifying column charging aperture 73 by connecting pipe 110, the first rectifying column Tower reactor discharging opening 71 is connected with Second distillation column charging aperture 83 through connecting pipe 110, and Second distillation column discharging opening 81 is by even Thread a pipe and 110 be connected with the stripping tower material inlet 94 of stripping tower 9, be positioned at the air stripping tower reactor discharging opening 91 bottom stripping tower 9 It is connected with the products pot import 101 being positioned in the middle part of products pot 10 by connecting pipe 110.
As further technical scheme, also including vaporizer 5 and filter 6, described vaporizer 5 and filter 6 set Putting to send out in synthesis answers between device 4 and the first rectifying column 7, and the evaporator inlet 54 of described vaporizer 5 is by connecting pipeline 110 and closing The reactor outlet 42 becoming reactor 4 is connected, and the vaporizer gaseous phase outlet 51 of vaporizer 5 is by connecting pipeline 110 and first First rectifying column charging aperture 73 of rectifying column 7 is connected, the vaporizer liquid-phase outlet 52 of vaporizer 5 by connect pipeline 110 with The filter import 62 of filter 6 is connected, and filter outlet 61 is by connecting the vaporizer refluxing opening of pipeline 110 and vaporizer 5 53 are connected.
In the technical program, described Second distillation column 8 is negative pressure tower.
The industrialization process producing N, N-diethylformamide continuously of the present invention, reaction equation is:
Catalyst
(CH3CH2)2NH+CO——————→(CH3CH2)2NCOH + Q
1.3-2.0MPaG, 90~130 DEG C.
The described industrialization process producing N, N-diethylformamide continuously, is carried out in following processing steps:
(1) preparation: by catalyst discharging pump, the ethanol solution of 20% Sodium ethylate is squeezed into catalyst storage tank 1, and liquid level reaches 50-80%, Catalyst storage tank 1 is passed through N2 protection, and catalyst storage tank 1 operating pressure is 0.07-0.2MpaG;Diethylamine is sent into EDA storage tank by irrigated area 2, liquid level reaches 50-80%;
(2) inject synthesis reactor: in catalyst storage tank 1, ethanol solution passes through catalyst feed pump, through effusion meter with flow as 4- The speed of 7L/h enters in synthesis reactor 4;DEA pressurizes through DEA feed pump, by effusion meter with flow as 1000-1200Kg/ H enters synthesis reactor 4;The CO come through membrance separation passes through the effusion meter speed entrance synthesis with flow as 430-520Kg/h instead Answer in device 4;
(3) synthetic reaction: (2) enter into CO, DEA and the CAT in synthesis reactor 4 by step, in 1.3-2.0Mpa pressure, temperature Circular response under the conditions of spending 90-130 DEG C, the material after synthetic reaction enters evaporative filtration operation through circulating pump extraction, the most anti- The condensed rear liquid-phase reflux of gas phase that should fall is in synthesis reactor 4, and gas phase goes boiler combustion;
Evaporative filtration separate: above-mentioned steps (3) in through circulating pump extraction enter evaporative filtration operation synthesis liquid pass through vaporizer 5, it is positioned at the liquid material bottom vaporizer 5 and removes sodium salt and catalyst through filter 6, the clear liquid after filtration steams at 2.5MPa Vapour is as adding thermal medium, and steam flow is to enter rectification working process, the liquid in vaporizer 5 in the case of 700-800Kg/h after gasification Body material enters bottom vaporizer 5, repeats above-mentioned filtration, heating, separation process;
(5) rectification: above-mentioned steps (4) in isolated gas enter the first rectifying column 7, through the light component such as the DEA of rectification, ethanol Entering condensation from the first rectifying column 7 jacking, a condensed condensed fluid part flow back in the first rectifying column 7, the first rectifying column 7 Extraction at the bottom of tower be about 99% DEF enter the Second distillation column 8 of rectification again, DEF from Second distillation column 8 overhead extraction through pump Air stripping operation is sent into after boosting;
(6) air stripping qualified products: above-mentioned steps (5) in, the DEF of Second distillation column 8 overhead extraction enters the top of stripping tower 9, nitrogen Gas is entered stripping tower 9 by bottom, and two phase countercurrent flow contacts, and makes DEF reach product requirement after nitrogen air stripping, and qualified products are by gas Extraction at the bottom of stripper 9 tower, after pump boosts, is sent in products pot 10.
The step of above-mentioned power 5 (5) described in a condensed condensed fluid part flow back in the first rectifying column 7, another portion Point from first rectifying column 7 top enter recycle stock storage tank 3, and with power 5 steps (2) in other CO, DEA and CAT together right of access (3) the step of 5, carries out synthetic reaction again.
The step of above-mentioned power 5 (5) described in Second distillation column 8 be negative pressure tower (≤180mmHg absolute pressure), Second distillation column 8 Boiling uses 2.5MPa steam as adding thermal medium again, and flow is 700-800Kg/h, through rectification heavy constituent and the mixture of DEF When reaching 130 DEG C, by extraction at the bottom of Second distillation column 8 tower to heavy component tank, after utilizing nitrogen pressurization, deliver to boiler combustion.
The step of above-mentioned power 5 (6) in, boiler combustion is delivered in the gas emptying not being condensed at stripping tower 9 tower top.
The above, only the preferable possible embodiments of the present invention, is not limited to the scope of the present invention.

Claims (8)

1. the industrialized unit of a continuous production N, N-diethylformamide, includes catalyst storage tank, DEA storage tank, recycle Material storage tank and products pot, it is characterised in that also include synthesis reactor, the first rectifying column, Second distillation column and stripping tower, described Reactor liquid phase entrance and reactor outlet it is provided with, on catalyst storage tank, DEA storage tank and recycle stock storage tank in synthesis reactor Catalyst reservoir outlet, DEA reservoir outlet and the recycle stock reservoir outlet arranged is by connecting pipe and synthesis reactor Reactor liquid phase entrance is connected, described first rectifying column and Second distillation column are respectively arranged with the first rectifying column charging aperture, First rectifying tower top discharging opening and the first tower bottom of rectifying tower discharging opening and Second distillation column charging aperture, Second distillation column top discharging opening With Second distillation column tower reactor discharging opening, the first rectifying tower top discharging opening is by connecting the circulation of pipeline and recycle stock storage tank upper end Material storage tank charging aperture is connected, and the reactor outlet in synthesis reactor passes through connecting pipe and the first rectifying column charging aperture phase Connection, the first tower bottom of rectifying tower discharging opening is connected with Second distillation column charging aperture through connecting pipe, Second distillation column discharging opening It is connected with the stripping tower material inlet of stripping tower by connecting pipe, is positioned at the air stripping tower reactor discharging opening bottom stripping tower and passes through Connecting pipe is connected with the products pot import being positioned in the middle part of products pot.
The industrialized unit of continuous production N, N-diethylformamide the most according to claim 1, it is characterised in that also wrap Having included vaporizer and filter, described vaporizer and filter are arranged on synthesis and answer between device and the first rectifying column, described steaming The evaporator inlet sending out device is connected with the reactor outlet of synthesis reactor by connecting pipeline, the vaporizer gas phase of vaporizer Exporting and be connected by the first rectifying column charging aperture of connection pipeline and the first rectifying column, the vaporizer liquid-phase outlet of vaporizer leads to Crossing connection pipeline to be connected with the filter import of filter, filter outlet is by connecting the vaporizer backflow of pipeline and vaporizer Mouth is connected.
The industrialized unit of continuous production N, N-diethylformamide the most according to claim 1, it is characterised in that described Second distillation column is negative pressure tower.
4. the industrialization process of a continuous production N, N-diethylformamide, it is characterised in that reaction equation is:
Catalyst
(CH3CH2)2NH+CO——————→(CH3CH2)2NCOH + Q
1.3-2.0MPaG, 90~130 DEG C.
The industrialization process of continuous production N, N-diethylformamide the most according to claim 4, it is characterised in that by with Lower processing step is carried out:
(1) preparation.: by catalyst discharging pump, the ethanol solution of 20% Sodium ethylate is squeezed into catalyst storage tank, and liquid level reaches 50-80%, Catalyst storage tank is passed through N2 protection, and catalyst storage tank operating pressure is 0.07-0.2MpaG;Diethylamine is sent into EDA storage tank by irrigated area, Liquid level reaches 50-80%;
(2) inject synthesis reactor: in catalyst storage tank, ethanol solution passes through catalyst feed pump, through effusion meter with flow as 4-7L/ The speed of h enters in synthesis reactor;DEA pressurizes through DEA feed pump, is entered for 1000-1200Kg/h with flow by effusion meter Enter synthesis reactor;The CO come through membrance separation passes through the effusion meter speed entrance synthesis reactor with flow as 430-520Kg/h In;
(3) synthetic reaction: (2) entered into CO, DEA and the CAT in synthesis reactor by step, in 1.3-2.0Mpa pressure, temperature Circular response under the conditions of spending 90-130 DEG C, the material after synthetic reaction enters evaporative filtration operation through circulating pump extraction, the most anti- The condensed rear liquid-phase reflux of gas phase that should fall is in synthesis reactor, and gas phase goes boiler combustion;
Evaporative filtration separate: above-mentioned steps (3) in through circulating pump extraction enter evaporative filtration operation synthesis liquid by evaporation Device, the liquid material being positioned at base of evaporator removes sodium salt and catalyst through filter, and the clear liquid after filtration steams at 2.5MPa Vapour is as adding thermal medium, and steam flow is to enter rectification working process, the liquid in vaporizer in the case of 700-800Kg/h after gasification Material enters base of evaporator, repeats above-mentioned filtration, heating, separation process;
(5) rectification: above-mentioned steps (4) in isolated gas enter the first rectifying column, through the light component such as the DEA of rectification, ethanol Entering condenser from the first rectifying tower top, a condensed condensed fluid part flow back in the first rectifying column, the first rectifying tower End extraction be about 99% DEF enter the Second distillation column of rectification again, DEF boosts through pump from Second distillation column overhead extraction Rear feeding air stripping operation;
(6) air stripping qualified products: above-mentioned steps (5) in, the DEF of Second distillation column overhead extraction enters the top of stripping tower, nitrogen Being entered stripping tower by bottom, two phase countercurrent flow contacts, and makes DEF reach product requirement after nitrogen air stripping, and qualified products are by air stripping Extraction at the bottom of tower tower, after pump boosts, is sent in products pot.
The industrialization process of continuous production N, N-diethylformamide the most according to claim 5, it is characterised in that above-mentioned Power 5 step (5) described in a condensed condensed fluid part flow back in the first rectifying column, another part is from the first rectification Top of tower enter recycle stock storage tank, and with power 5 steps (2) in other CO, DEA and CAT together right of access 5 step (3), carry out Synthetic reaction again.
The industrialization process of continuous production N, N-diethylformamide the most according to claim 5, it is characterised in that above-mentioned Power 5 step (5) described in Second distillation column be negative pressure tower (≤180mmHg absolute pressure), Second distillation column again boil employing 2.5MPa Steam is as adding thermal medium, and flow is 700-800Kg/h, when the mixture through rectification heavy constituent and DEF reaches 130 DEG C, by At the bottom of Second distillation column tower, extraction is to heavy component tank, delivers to boiler combustion after utilizing nitrogen pressurization.
The industrialization process of continuous production N, N-diethylformamide the most according to claim 5, it is characterised in that above-mentioned The step of power 5 (6) in, boiler combustion is delivered in the gas emptying not being condensed at stripping tower tower top.
CN201610391555.2A 2016-06-06 2016-06-06 Industrial device and process for continuously producing N,N-diethyl formamide Pending CN105906524A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610391555.2A CN105906524A (en) 2016-06-06 2016-06-06 Industrial device and process for continuously producing N,N-diethyl formamide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610391555.2A CN105906524A (en) 2016-06-06 2016-06-06 Industrial device and process for continuously producing N,N-diethyl formamide

Publications (1)

Publication Number Publication Date
CN105906524A true CN105906524A (en) 2016-08-31

Family

ID=56742111

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610391555.2A Pending CN105906524A (en) 2016-06-06 2016-06-06 Industrial device and process for continuously producing N,N-diethyl formamide

Country Status (1)

Country Link
CN (1) CN105906524A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108997156A (en) * 2018-08-06 2018-12-14 浙江新化化工股份有限公司 A kind of method of one-step method continuous production N, N- diethylformamide
CN110256273A (en) * 2019-07-08 2019-09-20 德州市德化化工有限公司 A kind of industrialized unit and technique of coproduction DEF, NEF, NMF
CN111961205A (en) * 2020-08-13 2020-11-20 江西蓝星星火有机硅有限公司 Process for continuously producing various low-viscosity methyl silicone oils by comprehensively utilizing methyl silicone oil polymerization material
CN115043750A (en) * 2022-06-27 2022-09-13 中国科学院山西煤炭化学研究所 Method for preparing formamide under low pressure

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003277338A (en) * 2002-01-18 2003-10-02 Mitsubishi Rayon Co Ltd Method for producing dialkylformamide
CN2704410Y (en) * 2004-06-16 2005-06-15 山东华鲁恒升化工股份有限公司 Dimethylformamide reactors
CN101050188A (en) * 2006-04-07 2007-10-10 山东华鲁恒升化工股份有限公司 New installation for producing dimethyl formamide, and new technique of using the installation
CN103214387A (en) * 2013-05-03 2013-07-24 山东华鲁恒升化工股份有限公司 Method for preparing N,N-diethylformamide
CN103435508A (en) * 2013-08-16 2013-12-11 山东华鲁恒升化工股份有限公司 Preparation process and device for N,N-diethylformamide
CN205662479U (en) * 2016-06-06 2016-10-26 德州市德化化工有限公司 Continuous production N, N industrialization device of diethyl carboxamide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003277338A (en) * 2002-01-18 2003-10-02 Mitsubishi Rayon Co Ltd Method for producing dialkylformamide
CN2704410Y (en) * 2004-06-16 2005-06-15 山东华鲁恒升化工股份有限公司 Dimethylformamide reactors
CN101050188A (en) * 2006-04-07 2007-10-10 山东华鲁恒升化工股份有限公司 New installation for producing dimethyl formamide, and new technique of using the installation
CN103214387A (en) * 2013-05-03 2013-07-24 山东华鲁恒升化工股份有限公司 Method for preparing N,N-diethylformamide
CN103435508A (en) * 2013-08-16 2013-12-11 山东华鲁恒升化工股份有限公司 Preparation process and device for N,N-diethylformamide
CN205662479U (en) * 2016-06-06 2016-10-26 德州市德化化工有限公司 Continuous production N, N industrialization device of diethyl carboxamide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘兴泉,吴玉塘,贾朝霞,于作龙: "二乙胺液相催化羰化制备二乙基甲酰胺", 《应用化学》 *
沈炎芳: "二甲基甲酰胺的生产", 《湖北化工》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108997156A (en) * 2018-08-06 2018-12-14 浙江新化化工股份有限公司 A kind of method of one-step method continuous production N, N- diethylformamide
CN108997156B (en) * 2018-08-06 2021-01-05 浙江新化化工股份有限公司 Method for continuously producing N, N-diethylformamide by one-step method
CN110256273A (en) * 2019-07-08 2019-09-20 德州市德化化工有限公司 A kind of industrialized unit and technique of coproduction DEF, NEF, NMF
CN111961205A (en) * 2020-08-13 2020-11-20 江西蓝星星火有机硅有限公司 Process for continuously producing various low-viscosity methyl silicone oils by comprehensively utilizing methyl silicone oil polymerization material
CN111961205B (en) * 2020-08-13 2021-12-14 江西蓝星星火有机硅有限公司 Process for continuously producing various low-viscosity methyl silicone oils by comprehensively utilizing methyl silicone oil polymerization material
CN115043750A (en) * 2022-06-27 2022-09-13 中国科学院山西煤炭化学研究所 Method for preparing formamide under low pressure
CN115043750B (en) * 2022-06-27 2023-12-26 中国科学院山西煤炭化学研究所 Method for preparing formamide by low pressure

Similar Documents

Publication Publication Date Title
CN105906524A (en) Industrial device and process for continuously producing N,N-diethyl formamide
CN102030622B (en) Method for synthesizing propyl aldehyde by ethylene hydroformylation
CN204932911U (en) A kind of continuous rectification apparatus for maleic anhydride production
CN109053355B (en) Method for purifying biphenyl by continuous rectification
CN105037094A (en) Energy coupling distillation method for preparing ethyl alcohol by means of acetic acid ester hydrogenation
CN105669379B (en) A kind of technique of ethyl acetate preparation of ethanol through hydrogenation
CN107793293B (en) Method for separating methanol-isopropanol-water by intermittent extraction and rectification and control structure
CN205662479U (en) Continuous production N, N industrialization device of diethyl carboxamide
JP3748668B2 (en) Distillation method and distillation apparatus
CN219579904U (en) Recovery device for ethanol as byproduct of coal glycol synthesis
CN101391153A (en) Double-kettle batch extraction rectification device and method for separating ethanol-water azeotropic system
CN104262177B (en) A kind of separation purification method of thick diglycolamine
CN110078582A (en) Cyclohexane separation device and method for cyclohexanone and cyclohexanol production
CN208166883U (en) A kind of system of separating alcohol, ethyl acetate and aqueous mixtures
CN102502697B (en) Method for recovering ammonia in morpholine solution
CN113233982B (en) Device and method for obtaining high-purity methyl salicylate through continuous rectification purification
CN104844420A (en) Continuous treatment process and device of neopentyl glycol condensed washing mother liquor
CN210331712U (en) Steam condensate waste heat recovery device in alcohol ether production
CN207294646U (en) A kind of process units of methyl tertiary butyl ether(MTBE)
CN106316793A (en) Alcohol preparing device and method based on the double rectification column and six-column and four-effect distillation
CN101342426A (en) Mounting connection structure for rectification column and condenser of novel distillation equipment
CN207429733U (en) A kind of rectifying device for being used to prepare watermelon ketone
CN111921219A (en) Gas phase separation device and separation method for low-boiling-point impurities in titanium tetrachloride
CN205635427U (en) Continuous negative pressure of acetonitrile distillation extraction device
CN110590506A (en) Crude butanol recovery system and process

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160831