CN208471945U - Dimethylformamide preparation facilities - Google Patents

Dimethylformamide preparation facilities Download PDF

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CN208471945U
CN208471945U CN201821157878.6U CN201821157878U CN208471945U CN 208471945 U CN208471945 U CN 208471945U CN 201821157878 U CN201821157878 U CN 201821157878U CN 208471945 U CN208471945 U CN 208471945U
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tower
dmf
rectifying
outlet
column
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刘海艳
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Abstract

Dimethylformamide preparation facilities, it is connected in the middle part of the outlet of methylamine reaction tower tower bottom and first rectifying column, the outlet of first rectifying column top gaseous phase is connected with methylamine reaction tower top material inlet pipeline, first rectifying column tower bottom liquid-phase outlet is connected with Second distillation column centre inlet, the outlet of Second distillation column top gaseous phase is connected with DMF synthetic tower bottom inlet, the outlet of DMF synthetic tower top gaseous phase is connected with cooler, it is connected in the middle part of DMF synthetic tower lower part reacting product outlet and DMF rectifying knockout tower, the outlet of DMF rectifying knockout tower top gaseous phase and cooler liquid-phase outlet are connected with methylamine reaction tower top material inlet pipeline respectively.Utility model device realizes being carried out continuously for synthetic methylamine and DMF purifying products, it is only necessary to which two rectifying columns can realize the dimethylamine purification process of current four tower rectifying, simplify technique, reduce plant construction cost.

Description

Dimethylformamide preparation facilities
Technical field
The utility model belongs to chemical device technical field, and in particular to a kind of dimethylformamide preparation facilities.
Background technique
Dimethylformamide, abbreviation DMF, be both a kind of industrial chemicals that purposes is extremely wide and it is a kind of have many uses it is excellent Good solvent.Dimethylformamide is good to a variety of high polymers such as polyethylene, polyvinyl chloride, polyacrylonitrile, polyamide etc. Solvent, can be used for the synthesis of the wet spinning silk, polyurethane of the synthetic fibers such as polyacrylonitrile fibre;It is film-made for plastics;It can also make Remove the paint stripper of paint-removing;It can also dissolve the pigment of certain low solubilities, make the characteristics of pigment is with dyestuff.Dimethyl formyl Amine is for Aromatics Extractive Project and for separating and recovering isoamyl two from separation and recovery butadiene in C-4-fraction and from C5 fraction Alkene also acts as the potent agent that non-dydrocarbon constituents is separated from paraffin.
Dimethylformamide is to carry out being catalyzed to react being prepared with carbon monoxide by dimethylamine at present, and catalyst is general For the methanol solution of sodium methoxide, raw material dimethylamine must have very high purity, because if containing water in dimethylamine, methanol Sodium is reacted with water can generate methanol and sodium hydroxide, lead to the loss of catalyst, influence react yield, furthermore in dimethylamine if Containing ammonia or other amine substances, various amides byproducts can be also generated in DMF synthesis process, these amides by-products Product thermostabilization is weaker than DMF, these byproducts can thermally decompose in DMF purification process, make in DMF product containing ammonia or other Amine impurities, therefore DMF production is very high to dimethylamine purity requirement, dimethylamine is that preparation is reacted with liquefied ammonia by methanol at present Mixed methylamine is obtained, mixes and contains monomethyl amine and trimethylamine byproduct in methylamine, because of monomethyl amine, dimethylamine, trimethylamine and not anti- The ammonia answered will form azeotropic mixture, and the separation of dimethylamine must be separated using multistage rectification, and dimethylamine purifying plant is by first at present Pure and mild ammonia catalytic reaction products are sent to first rectifying column, and tower top obtains unreacted ammonia and is recycled in reaction system, materials at bottom of tower It send into Second distillation column, is wherein separated trimethylamine by water extracting rectifying, and by tower bottom by monomethyl amine, dimethylamine Go out with hydromining, materials at bottom of tower send to third distillation column be carried out dehydrating again, and monomethyl amine and diformazan amine blends are by overhead extraction It is sent again to the 4th rectifying column and carries out conventional rectification, monomethyl amine overhead extraction, the extraction of dimethylamine tower bottom, such high-purity dimethylamine is It can send into DMF synthetic tower, such separator equipment investment is big, complex process, and operation regulation is difficult, large steam consumption.
Utility model content
The utility model aims at the problems existing in the prior art, and provides a kind of dimethylformamide preparation facilities.
The technical scheme adopted by the utility model to solve the technical problem is as follows:
A kind of dimethylformamide preparation facilities, is synthesized by methylamine reaction tower, first rectifying column, Second distillation column, DMF Tower, cooler and DMF rectifying knockout tower composition, the outlet of methylamine reaction tower tower bottom and first rectifying column middle part are connected, the first rectifying Column overhead gaseous phase outlet is connected with methylamine reaction tower top material inlet pipeline, first rectifying column tower bottom liquid-phase outlet and the second essence It evaporates tower centre inlet to be connected, the outlet of Second distillation column top gaseous phase is connected with DMF synthetic tower bottom inlet, and DMF synthesizes column overhead Gaseous phase outlet is connected with cooler, is connected in the middle part of DMF synthetic tower lower part reacting product outlet and DMF rectifying knockout tower, DMF rectifying The outlet of knockout tower top gaseous phase and cooler liquid-phase outlet are connected with methylamine reaction tower top material inlet pipeline respectively.
Above-mentioned first rectifying column uses packed tower or plate column, and board-like tower tray floor number is 40 ~ 120.
Above-mentioned Second distillation column uses packed tower or plate column, and board-like tower tray floor number is 30 ~ 80.
The working principle of utility model device is: material benzenemethanol and liquefied ammonia are sent into synthetic methylamine tower in dehydration catalyst In the presence of monomethyl amine, dimethylamine and trimethylamine is prepared, these mixed methylamines, which are sent into first rectifying column, carries out rectifying separation, First rectifying column top, ammonia, monomethyl amine and trimethylamine form azeotropic mixture and are distilled by tower top, and azeotropic mixture is it is ensured that contain There is the dimethylamine of synthetic methylamine reaction product quality 1%, can guarantee that the monomethyl amine in reaction product is kept completely separate out in this way, the One rectifying tower top gaseous phase is back in methylamine reaction tower, such first rectifying column materials at bottom of tower contain dimethylamine, trimethylamine and Water, first rectifying column bottoms, which is sent into Second distillation column, carries out dehydration distillation, and water and other high boiling components are in the second rectifying Tower tower bottom is isolated, and dimethylamine and trimethylamine are sent again by overhead extraction, dimethylamine and front three amine blends into DMF synthetic tower, Wherein using gas-liquid contact technique under sodium methoxide catalyst effect with reaction of carbon monoxide, DMF synthetic tower top gaseous phase contains There is most of gasification trimethylamine to send to be fully cooled into cooler, unreacting gas and inert gas be separated, cooler Liquid phase is returned to be recycled in methylamine reaction tower for trimethylamine is converted into dimethylamine, and DMF synthetic tower lower part obtains thick DMF product, thick DMF Product is sent into DMF rectifying knockout tower, and DMF rectifying separation column overhead obtains low boiling mixture and is back in synthetic methylamine tower, DMF rectifying knockout tower tower bottom sub-argument goes out high boiling mixture, can obtain high-purity DMF product in this way.
Utility model device realizes being carried out continuously for synthetic methylamine and DMF purifying products, it is only necessary to two rectifying columns The dimethylamine purification process that can realize current four tower rectifying, simplifies technique, reduces plant construction cost.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the structural schematic diagram of utility model device.
1 methylamine reaction tower, 2 first rectifying columns, 3 Second distillation columns, 4DMF synthetic tower, 5 coolers, 6DMF rectifying point in figure From tower.
Specific embodiment
As shown, a kind of dimethylformamide preparation facilities, by methylamine reaction tower 1, first rectifying column 2, the second rectifying Tower 3, DMF synthetic tower 4, cooler 5 and DMF rectifying knockout tower 6 form, in the outlet of 1 tower bottom of methylamine reaction tower and first rectifying column 2 Portion is connected, and the outlet of 2 top gaseous phase of first rectifying column is connected with 1 top material inlet pipeline of methylamine reaction tower, 2 tower of first rectifying column Bottom liquid-phase outlet is connected with 3 centre inlet of Second distillation column, 3 top gaseous phase of Second distillation column outlet with 4 bottom of DMF synthetic tower into Mouth is connected, and the outlet of 4 top gaseous phase of DMF synthetic tower is connected with cooler 5,4 lower part reacting product outlet of DMF synthetic tower and DMF essence Evaporate in the middle part of knockout tower 6 be connected, 6 top gaseous phase of DMF rectifying knockout tower outlet and 5 liquid-phase outlet of cooler respectively with methylamine reaction tower 1 top material inlet pipeline is connected, and first rectifying column uses packed tower or plate column, and board-like tower tray floor number is 40 ~ 120, the Two rectifying columns use packed tower or plate column, and board-like tower tray floor number is 30 ~ 80
The working principle of utility model device is: material benzenemethanol and liquefied ammonia are sent into synthetic methylamine tower in dehydration catalyst In the presence of monomethyl amine, dimethylamine and trimethylamine is prepared, these mixed methylamines, which are sent into first rectifying column, carries out rectifying separation, First rectifying column top, ammonia, monomethyl amine and trimethylamine form azeotropic mixture and are distilled by tower top, and azeotropic mixture is it is ensured that contain There is the dimethylamine of synthetic methylamine reaction product quality 1%, can guarantee that the monomethyl amine in reaction product is kept completely separate out in this way, the One rectifying tower top gaseous phase is back in methylamine reaction tower, such first rectifying column materials at bottom of tower contain dimethylamine, trimethylamine and Water, first rectifying column bottoms, which is sent into Second distillation column, carries out dehydration distillation, and water and other high boiling components are in the second rectifying Tower tower bottom is isolated, and dimethylamine and trimethylamine are sent again by overhead extraction, dimethylamine and front three amine blends into DMF synthetic tower, Wherein using gas-liquid contact technique under sodium methoxide catalyst effect with reaction of carbon monoxide, DMF synthetic tower top gaseous phase contains There is most of gasification trimethylamine to send to be fully cooled into cooler, unreacting gas and inert gas be separated, cooler Liquid phase is returned to be recycled in methylamine reaction tower for trimethylamine is converted into dimethylamine, and DMF synthetic tower lower part obtains thick DMF product, thick DMF Product is sent into DMF rectifying knockout tower, and DMF rectifying separation column overhead obtains low boiling mixture and is back in synthetic methylamine tower, DMF rectifying knockout tower tower bottom sub-argument goes out high boiling mixture, can obtain high-purity DMF product in this way.

Claims (3)

1. a kind of dimethylformamide preparation facilities, it is characterized in that by methylamine reaction tower, first rectifying column, Second distillation column, DMF Synthetic tower, cooler and DMF rectifying knockout tower composition, the outlet of methylamine reaction tower tower bottom and first rectifying column middle part are connected, and first Rectifying tower top gaseous phase outlet is connected with methylamine reaction tower top material inlet pipeline, first rectifying column tower bottom liquid-phase outlet and the Two rectifying column centre inlets are connected, and the outlet of Second distillation column top gaseous phase is connected with DMF synthetic tower bottom inlet, DMF synthetic tower Top gaseous phase outlet is connected with cooler, is connected in the middle part of DMF synthetic tower lower part reacting product outlet and DMF rectifying knockout tower, DMF The outlet of rectifying knockout tower top gaseous phase and cooler liquid-phase outlet are connected with methylamine reaction tower top material inlet pipeline respectively.
2. dimethylformamide preparation facilities according to claim 1, it is characterized in that first rectifying column using packed tower or Plate column, board-like tower tray floor number are 40 ~ 120.
3. dimethylformamide preparation facilities according to claim 1, it is characterized in that Second distillation column using packed tower or Plate column, board-like tower tray floor number are 30 ~ 80.
CN201821157878.6U 2018-07-18 2018-07-18 Dimethylformamide preparation facilities Active CN208471945U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201821157878.6U CN208471945U (en) 2018-07-18 2018-07-18 Dimethylformamide preparation facilities

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Application Number Priority Date Filing Date Title
CN201821157878.6U CN208471945U (en) 2018-07-18 2018-07-18 Dimethylformamide preparation facilities

Publications (1)

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CN208471945U true CN208471945U (en) 2019-02-05

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