CN208933239U - A kind of formamide separation system - Google Patents

A kind of formamide separation system Download PDF

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Publication number
CN208933239U
CN208933239U CN201821647373.8U CN201821647373U CN208933239U CN 208933239 U CN208933239 U CN 208933239U CN 201821647373 U CN201821647373 U CN 201821647373U CN 208933239 U CN208933239 U CN 208933239U
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formamide
tower
heat exchanger
product
shell side
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李卓谦
李可根
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CHENGDU ZHUOLI RUIXING TECH Co
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CHENGDU ZHUOLI RUIXING TECH Co
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Abstract

The utility model discloses a kind of formamide separation systems.Separation system includes feeder and separation unit, wherein feeder is separated for being heated to the formamide head product comprising methanol and methyl formate and being transported to separation unit;Separation unit includes primary distillation tower and product rectifying column, and the methyl formate in head product can be fractionated by primary distillation tower, and product rectifying column can separate methanol and formamide.Using the separation system and separating technology in the utility model, energy consumption can be not only reduced, formamide of the purity 99.9% or more can also be obtained, and can be recycled to by-product carbinol, remarkable in economical benefits.

Description

A kind of formamide separation system
Technical field
The utility model belongs to formamide production technical field, and in particular to a kind of formamide separation system.
Background technique
The industrialized preparing process of formamide is methyl formate, ammonia is passed through in aminating reaction kettle, is being lower than 40 DEG C of item Aminating reaction is carried out under part, generates formamide.In the system due to ammonia be it is excessive, the conversion ratio of methyl formate is 95.0% ~98.0% and without side reaction occur, therefore in reaction solution be mainly methanol, formamide, methyl formate mixture.
Since the production of methyl formate is reacted dependent on methanol dehydrogenation, therefore it is necessary for refining the methanol in recycling reaction solution , therefore two tower processes are used in traditional handicraft, by the method for secondary rectifying, realize the separation of methyl formate, methanol, formamide Recycling.
Utility model content
In order to achieve the above object, the technical scheme adopted by the utility model is providing a kind of formamide separation system, Including feeder and separation unit, wherein
Feeder includes ageing tank, First Heat Exchanger, the second heat exchanger and the heating furnace that goes into operation, and the outlet of ageing tank is provided with The tube side of feed pump, First Heat Exchanger and the second heat exchanger is interconnected and is sequentially connected in series in the downstream of feed pump, and go into operation heating The inlet and outlet of furnace is connected to the primary distillation tower in the tube side and separation unit of the second heat exchanger respectively;
Separation unit includes primary distillation tower and product rectifying column, and the tower top of primary distillation tower is connected to fuel pipe network, and tower reactor is connected with The tube side of reboiler, reboiler is connected to product rectifying column, and the tower top airtight connection of product rectifying column has vacuum pump, and tower top is logical It crosses methanol loop pump to be connected to Methanol Recovery tank, tower reactor is connected to the shell side of reboiler, the shell side of reboiler and the second heat exchange The shell side of device is connected to, and the shell side of the second heat exchanger is connected to by product pump with formamide storage tank.
Separation system in the utility model includes feeder and separation unit, include in feeder two be sequentially connected in series change Hot device, head product are flowed through from the tube side of heat exchanger, are exchanged heat with the fluid flowed through in heat exchanger shell pass, more than product Heat can heat head product, realize the utilization to waste heat, not only can be energy saving, but also can shorten the heating furnace that goes into operation Heating time, promote separative efficiency, reduce the operating pressure of heating furnace of going into operation.
Separation unit in the utility model includes primary distillation tower and product rectifying column, and rectifying column is used for the formic acid in head product Methyl esters is separated, and product rectifying column is arranged two fractionating columns not only and can reduce point for separating to methanol and formamide The load of tower is evaporated, and may be implemented to separate step by step, separation is more thorough, and finally obtained product purity is higher, meets industry It needs, the substance isolated may be directly applied to industrialized production.
Based on the above technical solution, the utility model can also do following improvement.
Further, the heating furnace that goes into operation is the steam heater that goes into operation comprising shell side and the tube side coated by shell side, tube side In the shape of a spiral, steam inlet and steam (vapor) outlet are offered on shell side, are connected to respectively with steam generator and boiler room.
The heating furnace that goes into operation in the utility model is preferentially using the steam heater that goes into operation, the pipe inside the steam heater that goes into operation Journey in the shape of a spiral, increases the contact area of steam and tube side, heats more uniform and rapid.Into in the heating furnace shell side that goes into operation Steam pressure be within the scope of 0.8~1.0MPa, temperature be in 125~130 DEG C within the scope of, steam, which can be rapidly filled with, to go into operation The shell side of heating furnace can be evenly heated the tube side of shell side intra helical, and the head product in tube side is heated evenly, It can reach the temperature of technique requirement in short time, separative efficiency improves.
Further, ageing tank is connected to aminating reaction kettle.
The beneficial effects of the utility model are:
1. the utility model effectively reduces the dosage of hot and cold public work, energy conservation and consumption reduction effects compared to traditional handicraft Significantly
2. compared to traditional handicraft, due to increasing heat exchange equipment, within the scope of Rectification Tower Design, mass flow disturbance In the case of, this technique can response storm as early as possible, product is interfered small.Therefore, the operating flexibility of this technique is big, and safety coefficient is high.
Detailed description of the invention
Fig. 1 is the utility model separation system schematic diagram;
Fig. 2 is the heating furnace cross-sectional view that goes into operation;
Wherein, V0101, ageing tank;V0102, Methanol Recovery tank;E0101, First Heat Exchanger;E0102, the second heat exchanger; E0103, go into operation heating furnace;K1, shell side;K2, tube side;K3, steam inlet;K4, steam (vapor) outlet;E0104, reboiler;P0101, Feed pump;P0102, methanol loop pump;P0103, product pump;P0104, vacuum pump;T0101, primary distillation tower;T0102, product rectifying Tower.
Specific embodiment
Specific embodiment of the present utility model is described in detail with reference to the accompanying drawing.
In the embodiments of the present invention, as shown in Fig. 1~2, a kind of formamide separation system is provided, in the utility model Separation system include feeder and separation unit.Wherein, feeder includes ageing tank V0101, First Heat Exchanger E0101, second The heat exchanger E0102 and heating furnace E0103 that goes into operation;The entrance of ageing tank V0101 is directly connected to aminating reaction kettle, outlet connection There is feed pump P0101, feed pump P0101 to be connected to the tube side of First Heat Exchanger E0101, the tube side of First Heat Exchanger E0101 with The tube side of second heat exchanger E0102 is connected to, the closed company of import of the tube side of the second heat exchanger E0102 and the heating furnace E0103 that goes into operation It connects, the outlet for the heating furnace E0103 that goes into operation is connected to the primary distillation tower T0101 in separation unit;The heating furnace that goes into operation in the utility model E0103 can go into operation electric furnace, but in order to enable head product uniformly quickly to be heated in the heating furnace E0103 that goes into operation, this reality The steam heater that goes into operation preferentially is used with the heating furnace E0103 that goes into operation in novel, i.e., head product is heated with steam;It goes into operation Steam heater includes shell side K1 and the tube side K2 that is coated by shell side K1, for the contact area for increasing steam and tube side K2, It is preferentially that tube side K2 setting is spiral in utility model, steam inlet K3 and steam (vapor) outlet K4, steam are offered on shell side K2 Import K3 is connected to steam generator, and steam (vapor) outlet K4 is connected to boiler room;Steam generator provides for the steam heater that goes into operation The steam that pressure is 0.8~1.0MPa, temperature is 125~130 DEG C.
Separation unit includes primary distillation tower T0101 and product rectifying column T0102.Production is provided in the middle part of the tower body of primary distillation tower T0101 Product import, product import are connected with the outlet for the heating furnace E0103 that goes into operation, head product in the middle part of the tower body of primary distillation tower T0101 into Enter in tower;The tower top of primary distillation tower T0101 is provided with pressure reducing valve, and pressure reducing valve is connected to by pipeline with fuel pipe network;It is set to fore-running The outlet of tower T0101 tower bottom is connected to the tube side of reboiler E0104, and the tube side and product rectifying column T0102 of reboiler E0104 connects Logical, product rectifying column T0102 is equipped with vacuum pump P0104, and vacuum pump P0104 airtight connection is in the tower of product rectifying column T0102 Top, for being vacuumized to product rectifying column T0102;The tower top of rectifying column T0102 pumps P0102 and Methanol Recovery by methanol loop Tank V0102 connection, tower reactor are connected to the shell side of reboiler E0104, the shell side of reboiler E0104 and the second heat exchanger E0102 Shell side connection, the shell side of the second heat exchanger E0102 is connected to by product pump P0103 with formamide storage tank.
Using the production system in the utility model, a kind of completely new cyclohexyl benzene production technology can be developed, is now led to Embodiment is crossed production technology in the utility model is described in detail.
Embodiment 1
(1) it by feeder will in ageing tank include that methanol and methyl formate formamide head product is heated to 90 DEG C, and It is delivered in primary distillation tower and is fractionated with the feed pressure of 0.16MPa, control primary distillation tower bottom temperature is 100 DEG C, tower top temperature Be 70 DEG C, molar reflux ratio 2.2, full tower pressure drop be 0.02MPa, distillate methyl formate from tower top, from tower reactor distillate methanol and The mixture of formamide;
(2) methyl formate distillated in step (1) feeding fuel pipe network is subjected to burning processing, by methanol and formamide Mixture is delivered in product rectifying column and is fractionated, and control product tower bottom of rectifying tower temperature is 170 DEG C, tower top temperature 40 DEG C, molar reflux ratio 1.0, top vacuum degree is 0.04MPa, distillates methanol from tower top, distillates formamide from tower reactor;
(3) methanol distillated in step (2) be fed through Methanol Recovery tank preservation, the formamide distillated successively with reboiler and Enter formamide storage tank after the heat exchange of second heat exchanger to save.
Embodiment 2
(1) it by feeder will in ageing tank include that methanol and methyl formate formamide head product is heated to 90 DEG C, and It is delivered in primary distillation tower and is fractionated with the feed pressure of 0.16MPa, control primary distillation tower bottom temperature is 105 DEG C, tower top temperature For 75 DEG C, molar reflux ratio 2.5, full tower pressure drop is 0.02MPa, distillates methyl formate from tower top, from tower reactor distillate methanol and The mixture of formamide;
(2) methyl formate distillated in step (1) feeding fuel pipe network is subjected to burning processing, by methanol and formamide Mixture is delivered in product rectifying column and is fractionated, and control product tower bottom of rectifying tower temperature is 185 DEG C, tower top temperature 45 DEG C, molar reflux ratio 0.8, top vacuum degree is 0.035MPa, distillates methanol from tower top, distillates formamide from tower reactor;
(3) methanol distillated in step (2) be fed through Methanol Recovery tank preservation, the formamide distillated successively with reboiler and Enter formamide storage tank after the heat exchange of second heat exchanger to save.
Embodiment 3
(1) it by feeder will in ageing tank include that methanol and methyl formate formamide head product is heated to 80 DEG C, and It is delivered in primary distillation tower and is fractionated with the feed pressure of 0.16MPa, control primary distillation tower bottom temperature is 95 DEG C, and tower top temperature is 65 DEG C, molar reflux ratio 2.2, full tower pressure drop is 0.02MPa, distillates methyl formate from tower top, distillates methanol and first from tower reactor The mixture of amide;
(2) methyl formate distillated in step (1) feeding fuel pipe network is subjected to burning processing, by methanol and formamide Mixture is delivered in product rectifying column and is fractionated, and control product tower bottom of rectifying tower temperature is 160 DEG C, tower top temperature 35 DEG C, molar reflux ratio 1.0, top vacuum degree is 0.045MPa, distillates methanol from tower top, distillates formamide from tower reactor;
(3) methanol distillated in step (2) be fed through Methanol Recovery tank preservation, the formamide distillated successively with reboiler and Enter formamide storage tank after the heat exchange of second heat exchanger to save.
Embodiment 4
(1) it by feeder will in ageing tank include that methanol and methyl formate formamide head product is heated to 85 DEG C, and It is delivered in primary distillation tower and is fractionated with the feed pressure of 0.16MPa, control primary distillation tower bottom temperature is 105 DEG C, tower top temperature Be 65 DEG C, molar reflux ratio 2.5, full tower pressure drop be 0.02MPa, distillate methyl formate from tower top, from tower reactor distillate methanol and The mixture of formamide;
(2) methyl formate distillated in step (1) feeding fuel pipe network is subjected to burning processing, by methanol and formamide Mixture is delivered in product rectifying column and is fractionated, and control product tower bottom of rectifying tower temperature is 185 DEG C, tower top temperature 35 DEG C, molar reflux ratio 1.5, top vacuum degree is 0.045MPa, distillates methanol from tower top, distillates formamide from tower reactor;
(3) methanol distillated in step (2) be fed through Methanol Recovery tank preservation, the formamide distillated successively with reboiler and Enter formamide storage tank after the heat exchange of second heat exchanger to save.
Although being described in detail in conjunction with the accompanying drawings and embodiments to specific embodiment of the present utility model, do not answer It is interpreted as the restriction to the protection scope of this patent.In range described by claims, those skilled in the art without Various modifications and deformation that creative work can make still belong to the protection scope of this patent.

Claims (3)

1. a kind of formamide separation system, it is characterised in that: including feeder and separation unit, wherein
Feeder includes ageing tank (V0101), First Heat Exchanger (E0101), the second heat exchanger (E0102) and the heating furnace that goes into operation (E0103), the outlet of the ageing tank (V0101) is provided with feed pump (P0101), the First Heat Exchanger (E0101) and the The tube side of two heat exchangers (E0102) is interconnected and is sequentially connected in series in the downstream of the feed pump (P0101), the heating that goes into operation The inlet and outlet of furnace (E0103) connects with the primary distillation tower (T0101) in the tube side and separation unit of the second heat exchanger (E0102) respectively It is logical;
Separation unit includes primary distillation tower (T0101) and product rectifying column (T0102), the tower top and fuel of the primary distillation tower (T0101) Pipe network connection, tower reactor are connected with reboiler (E0104), the tube side and product rectifying column (T0102) of the reboiler (E0104) Connection, the tower top airtight connection of the product rectifying column (T0102) have vacuum pump (P0104), and tower top is pumped by methanol loop (P0102) it is connected to Methanol Recovery tank (V0102), tower reactor is connected to the shell side of the reboiler (E0104), the reboiler (E0104) shell side is connected to the shell side of second heat exchanger (E0102), and the shell side of second heat exchanger (E0102) is logical Product pump (P0103) is crossed to be connected to formamide storage tank.
2. formamide separation system according to claim 1, it is characterised in that: the heating furnace that goes into operation (E0103) is to open Work steam heater comprising shell side (K1) and by shell side (K1) coat tube side (K2), the tube side (K2) in the shape of a spiral, Steam inlet (K3) and steam (vapor) outlet (K4) are offered on the shell side (K2), is connected to respectively with steam generator and boiler room.
3. formamide separation system according to claim 1, it is characterised in that: the ageing tank (V0101) and amination are anti- Kettle is answered to be connected to.
CN201821647373.8U 2018-10-11 2018-10-11 A kind of formamide separation system Active CN208933239U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109020824A (en) * 2018-10-11 2018-12-18 成都科特瑞兴科技有限公司 A kind of formamide separation system and formamide separating technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109020824A (en) * 2018-10-11 2018-12-18 成都科特瑞兴科技有限公司 A kind of formamide separation system and formamide separating technology

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