CN205662479U - Continuous production N, N industrialization device of diethyl carboxamide - Google Patents

Abstract

The utility model relates to a continuous production N, N industrialization device of diethyl carboxamide, including the catalyst storage tank, the DEA storage tank, DEA ethanol storage tank and product jar, still include synthesis reactor, first rectifying column, second rectifying column and stripping tower, by the present technical scheme, adopt the sodium ethoxide to make the catalyst, percolation is carried out after immersion, need not any cocatalyst, use diethylamine and CO as the raw materials, in temperature 90 130 DEG C, pressure 1.3 2.0MPa the condition under directly synthesize DEF, production DEF's selectivity is 99%, by the present technical scheme, the the raw materials cost is greatly reduced, unreacted raw materials need not the separation and directly returns reaction system recycle, low and easy realization of cost recovery, the product purity is high, DEF content reaches 99.98%, can satisfy domestic and international user's requirement.

Description

Produce the industrialized unit of N, N-diethylformamide continuously

Technical field

This utility model relates to the process units of a kind of N, N-diethylformamide, particularly relates to one and produces N continuously, The industrialized unit of N-diethylformamide.

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 continuous production DEF it is not yet reported that, only related experiment report, is to use methanol Sodium makees promoter as catalyst, expoxy propane, and with methanol as solvent, the selectivity producing DEF is 96%, in this way The DEF cost of material produced is high, and unreacted raw materials recovery cost is high, and the difficulty of recovery is big, and poor product quality does not reaches user Prescription, does not commercially have competitiveness.

Utility model content

In view of this, main purpose of the present utility model is the work providing one to produce N, N-diethylformamide continuously Industry gasifying device, by the technical program, uses Sodium ethylate to make catalyst, with ethanol as solvent, need not any promoter, with two Ethamine and CO are raw material, are directly synthesized DEF under conditions of temperature 90-130 DEG C, pressure 1.3-2.0MPa, produce the selection of DEF Property be 99%, by the technical program, greatly reduce cost of material, unreacted raw material without separate directly return reaction be System recycles, and cost recovery is low and easily realizes, and product purity is high, and DEF content reaches 99.98%, can meet users at home and abroad Requirement.

In order to achieve the above object, the technical solution of the utility model is achieved in that one produces N, N-bis-continuously The industrialized unit of ethyl-formamide, includes catalyst storage tank, DEA storage tank, recycle stock storage tank and products pot, also includes synthesis Reactor, the first rectifying column, Second distillation column and stripping tower, described synthesis reactor is provided with reactor liquid phase entrance with anti- Device is answered to export, catalyst reservoir outlet, DEA reservoir outlet and the circulation that catalyst storage tank, DEA storage tank and recycle stock storage tank are arranged Material reservoir outlet is connected with the reactor liquid phase entrance in synthesis reactor by connecting pipe, described first rectifying column and The first rectifying column charging aperture, the first rectifying column discharging opening and the first tower bottom of rectifying tower discharging opening it is respectively arranged with on Second distillation column With Second distillation column charging aperture, Second distillation column discharging opening and Second distillation column tower reactor discharging opening, the first rectifying column discharging opening leads to Crossing connection pipeline to be connected with the recycle stock storage tank charging aperture of recycle stock storage tank upper end, the reactor in synthesis reactor goes out Mouth is connected by connecting pipe and the first rectifying column charging aperture, and the first tower bottom of rectifying tower discharging opening is through connecting pipe and the second essence Evaporating tower charging aperture to be connected, Second distillation column discharging opening is connected with the stripping tower material inlet of stripping tower by connecting pipe, It is positioned at the air stripping tower reactor discharging opening bottom stripping tower to be connected with the products pot import being positioned in the middle part of products pot by connecting pipe.

As further technical scheme, also including vaporizer and filter, described vaporizer and filter are arranged on Between synthesis reactor and the first rectifying column, 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.

In the technical program, described Second distillation column is negative pressure tower.

Provide the benefit that after using technique scheme: one produces the industry makeup of N, N-diethylformamide continuously Put, by the technical program, use Sodium ethylate to make catalyst, with ethanol as solvent, need not any promoter, with diethylamine and CO is raw material, is directly synthesized DEF under conditions of temperature 90-130 DEG C, pressure 1.3-2.0MPa, and the selectivity producing DEF is 99%, by the technical program, greatly reduce cost of material, unreacted raw material is fed directly to ethamine device without separation and returns Receiving and utilize, cost recovery is low and easily realizes, and product purity is high, and DEF content reaches 99.98%, can meet wanting of users at home and abroad Ask.

Accompanying drawing explanation

Fig. 1 is overall structure schematic diagram of the present utility model.

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 this utility model is described in further detail.

As it is shown in figure 1, the industrialized unit producing N, N-diethylformamide continuously that this utility model 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 7, second Rectifying column 8 and stripping tower 9, described synthesis reactor 4 is provided with reactor liquid phase entrance 41 and reactor outlet 42, and catalyst stores up Catalyst reservoir outlet 11, DEA reservoir outlet 21 and the recycle stock storage tank arranged on groove 1, DEA storage tank 2 and recycle stock storage tank 3 Outlet 32 is connected with the reactor liquid phase entrance 41 in synthesis reactor 4 by connecting pipe 110, described first rectifying column 7 Be respectively arranged with the first rectifying column charging aperture the 73, first rectifying column discharging opening 72 and the first rectifying tower on Second distillation column 8 Still discharging opening 71 and Second distillation column charging aperture 83, Second distillation column discharging opening 81 and Second distillation column tower reactor discharging opening 82, the One rectifying column discharging opening 81 is connected with the recycle stock storage tank charging aperture 31 of recycle stock storage tank 3 upper end by connecting pipeline 110 Logical, the reactor outlet 42 in synthesis reactor 4 is connected with the first rectifying column charging aperture 73 by connecting pipe 110, and first Tower bottom of rectifying tower discharging opening 71 is connected with Second distillation column charging aperture 83 through connecting pipe 110, Second distillation column discharging opening 81 It is connected with the stripping tower material inlet 94 of stripping tower 9 by connecting pipe 110, is positioned at the air stripping tower reactor bottom stripping tower 9 and goes out Material mouth 91 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.

In specific embodiment of the utility model, the ethanol solution of A. Sodium ethylate squeezes into catalyst storage tank by catalyst discharging pump 1 temporarily stores, and catalyst storage tank 1 takes N₂Protection, make catalyst all the time with air exclusion；Ethanol solution catalyst warp containing Sodium ethylate Cross catalyst reservoir outlet 11 and connection pipeline 110 enters catalyst feed pump, through inflow-rate of water turbine meter meter after being pressurizeed by catalyst feed pump Enter in synthesis reactor 4 after amount；B. DEA is to be sent into DEA storage tank 2 by ethamine workshop section or irrigated area and temporarily stored, DEA storage tank 2 DEA reservoir outlet 21 by connecting pipe 110 enter into after DEA feed pump is pressurized to synthesis pressure by effusion meter measure into Enter in synthesis reactor 4；C. from the reactor gas phase entrance 43 of synthesis reactor 4 bottom after CO gas is measured by effusion meter Enter in synthesis reactor 4；D. enter in synthesis reactor 4 by three kinds of materials (CO, DEA, CAT) of metering, at 1.3- Circular response under the conditions of 2.0Mpa pressure, temperature 90-130 DEG C, enters into vaporized through synthesis cycle pump through synthesis reactor 4 In filter operation；D. the synthesis liquid come from synthesis reactor 4 initially enters vaporizer 5, is positioned at vaporizer 5 bottoms material through steaming Entering filter 6 after sending out circulating pump pressurization and remove sodium salt and catalyst, clear liquid enters vaporizer 5, uses steam to be situated between as heating Matter, gas phase after heating enters distillation system, and the liquid at separation enters bottom vaporizer 5, repeat above-mentioned filtration, heat, point From process；E. from vaporizer 4 top, gas out initially enters the first rectifying column 7, in the first rectifying column 7 isolated gently Component enters overhead condenser condensation from tower top, and a condensed fluid part flows back to first rectifying column 7 backflow as this tower, separately Being partly into recycle stock storage tank 3, then participate in reaction with pumped back response system, at the bottom of the first rectifying column 7 tower, extraction is The DEF of about 99% enters Second distillation column 8, and Second distillation column 8 is a negative pressure tower (≤180mmHg absolute pressure), through rectification weight The mixture of component and DEF is adopted into heavy constituent storage tank from interruption at the bottom of Second distillation column 8 tower, delivers to boiler after then pressurizeing with nitrogen Burning, product DEF sends into stripping tower 9 after pump boosts from Second distillation column 8 overhead extraction, and being positioned at stripping tower 9 tower top does not has The gas being condensed sends into boiler combustion, Second distillation column 8 material pushed up enters stripping tower 9, and nitrogen is by bottom stripping tower Gas phase import 92 enters stripping tower 9, and two phase countercurrent flow contacts, and reaches product requirement after nitrogen air stripping, and qualified products are by air stripping Air stripping tower reactor discharging opening 91 extraction bottom tower 9, after pump boosts, is sent in products pot 10.

The above, preferable possible embodiments the most of the present utility model, it is not limited to of the present utility model Scope.

Claims (3)

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.