CN109020824A - A kind of formamide separation system and formamide separating technology - Google Patents

A kind of formamide separation system and formamide separating technology Download PDF

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Publication number
CN109020824A
CN109020824A CN201811181086.7A CN201811181086A CN109020824A CN 109020824 A CN109020824 A CN 109020824A CN 201811181086 A CN201811181086 A CN 201811181086A CN 109020824 A CN109020824 A CN 109020824A
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China
Prior art keywords
formamide
tower
product
methanol
primary distillation
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CN201811181086.7A
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李卓谦
李忠俐
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CHENGDU ZHUOLI RUIXING TECH Co
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CHENGDU ZHUOLI RUIXING TECH Co
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Priority to CN201811181086.7A priority Critical patent/CN109020824A/en
Publication of CN109020824A publication Critical patent/CN109020824A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/22Separation; Purification; Stabilisation; Use of additives
    • C07C231/24Separation; Purification
    • 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
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of formamide separation system and formamide separating technologies.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.When being separated to head product, first head product is heated, then is sequentially sent in primary distillation tower and product rectifying column, the conditions such as the bottom temperature of primary distillation tower and product rectifying column, tower top temperature, full tower pressure drop are controlled, it is separated from each other each component in mixture, realizes the purpose of formamide separation.Using the separation system and separating technology in the present invention, 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 and formamide separating technology
Technical field
The invention belongs to formamide production technical fields, and in particular to a kind of formamide separation system and formamide separate work Skill.
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.
Summary of the invention
In order to achieve the above object, the technical scheme adopted by the invention is that: a kind of formamide separation system is provided, 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 present invention includes feeder and separation unit, includes two heat exchange being sequentially connected in series in feeder 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, are utilized the waste heat of product Head product can be heated, realize the utilization to waste heat, not only can be energy saving, but also the heater that goes into operation can be shortened Heating time promotes separative efficiency, reduces the operating pressure for the heater that goes into operation.
Separation unit in the present invention includes primary distillation tower and product rectifying column, and rectifying column is used for the methyl formate in head product It is separated, for product rectifying column for separating to methanol and formamide, two fractionating columns, which are arranged, can not only reduce fractionating column Load, and may be implemented to separate step by step, separate more thorough, finally obtained product purity is higher, meet industrial needs, The substance isolated may be directly applied to industrialized production.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the heater 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.
Preferentially using the steam heater that goes into operation, the tube side inside the steam heater that goes into operation is in the heater that goes into operation in the present invention Helical form increases the contact area of steam and tube side, heats more uniform and rapid.Steaming into the heater shell side that goes into operation Steam pressure is within the scope of 0.8~1.0MPa, and temperature is within the scope of 125~130 DEG C, and steam can be rapidly filled with the heating that goes into operation The shell side of device can be evenly heated the tube side of shell side intra helical, and the head product in tube side is heated evenly, in short-term The interior temperature that can reach technique requirement, separative efficiency improve.
Further, ageing tank is connected to aminating reaction kettle.
The ageing tank that head product is contained in the present invention is directly connected to aminating reaction kettle, and it is straight that product is gone out after the completion of aminating reaction It taps into ageing tank, product is avoided to consume in transport process.
In the present invention using formamide separation system separation formamide technique the following steps are included:
(1) the formamide head product comprising methanol and methyl formate in ageing tank is heated to 80~90 by feeder DEG C, and be delivered in primary distillation tower and be fractionated with the feed pressure of 0.16MPa, control primary distillation tower bottom temperature is 95~105 DEG C, Tower top temperature is 65~75 DEG C, and molar reflux ratio is greater than 2.0, and full tower pressure drop is 0.02MPa, distillates methyl formate from tower top, from Tower reactor distillates the mixture of methanol and 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 160~185 DEG C, tower top temperature It is 35~45 DEG C, molar reflux ratio is greater than 0.5, and top vacuum degree is 0.035~0.045MPa, methanol is distillated from tower top, from tower Stilling goes out formamide;
(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.It is heated to 80~90 DEG C, then
In the present invention when carrying out formamide separation, head product is sent into primary distillation tower with the feed pressure of 0.16MPa, can be made Head product to be separated is full of primary distillation tower in a short time, and primary distillation tower is avoided the case where dry plate occur;And the temperature of head product The molar reflux ratio for cooperating primary distillation tower between primary distillation tower bottom temperature and tower top temperature and full tower pressure drop are, it can be achieved that formic acid The quick separating of methyl esters, and the thermic load of reboiler can be reduced, and quantity of steam used in reboiler greatly reduces, and reduces energy The consumption in source.
The pressure of product the top of the distillation column is controlled in 0.035~0.045MPa, and within this range, the temperature of tower top material exists It 40 DEG C or so, is able to use this cheap cooling medium of recirculated cooling water and is cooled down, cooling cost is greatly lowered.
The beneficial effects of the present invention are:
1. the invention patent 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.
3., reasonably using the material heat of transformation and included heat, being rationally designed, reduction is produced into compared to traditional handicraft This.
Detailed description of the invention
Fig. 1 is separation system schematic diagram of the present invention;
Fig. 2 is the heater 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 embodiments of the present invention will be described in detail with reference to the accompanying drawing.
In the embodiment of the present invention, as shown in Fig. 1~2, a kind of formamide separation system, the segregative line in the present invention are provided System includes feeder and separation unit.Wherein, feeder includes ageing tank V0101, First Heat Exchanger E0101, the second heat exchanger The E0102 and heating furnace E0103 that goes into operation;The entrance of ageing tank V0101 is directly connected to aminating reaction kettle, and outlet is connected with charging P0101 is pumped, feed pump P0101 is connected to the tube side of First Heat Exchanger E0101, and the tube side of First Heat Exchanger E0101 is changed with second The tube side of hot device E0102 is connected to, and the import airtight connection of the tube side of the second heat exchanger E0102 and the heating furnace E0103 that goes into operation goes into operation The outlet of heating furnace E0103 is connected to the primary distillation tower T0101 in separation unit;The heating furnace E0103 that goes into operation in the present invention can be opened Work electric furnace, but in order to enable head product uniformly quickly to be heated in the heating furnace E0103 that goes into operation, going into operation in the present invention adds Hot stove E0103 preferentially using the steam heater that goes into operation, i.e., heats head product with steam;The steam heater that goes into operation includes shell The journey K1 and tube side K2 coated by shell side K1, for the contact area for increasing steam and tube side K2, it is of the invention in preferentially by tube side K2 setting is spiral, and steam inlet K3 and steam (vapor) outlet K4 are offered on shell side K2, and steam inlet K3 and steam generator connect Logical, steam (vapor) outlet K4 is connected to boiler room;Steam generator for the steam heater that goes into operation provide pressure be 0.8~1.0MPa, temperature The steam that degree 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 present invention, a kind of completely new cyclohexyl benzene production technology can be developed, reality is now passed through Example is applied production technology in the present invention 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 Be 75 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 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 a specific embodiment of the invention, should not be understood For the restriction of the protection scope to this patent.In range described by claims, those skilled in the art are without creation Property the various modifications that can make of labour and deformation still belong to the protection scope of this patent.

Claims (6)

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 heater 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.
4. utilizing the technique of the described in any item formamide separation systems of claims 1 to 33 separation formamide, which is characterized in that The following steps are included:
(1) it by feeder will in ageing tank include that methanol and methyl formate formamide head product is heated to 80~90 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 95~105 DEG C, tower top Temperature is 65~75 DEG C, and molar reflux ratio is greater than 2.0, and full tower pressure drop is 0.02MPa, methyl formate is distillated from tower top, from tower reactor Distillate the mixture of methanol and formamide;
(2) methyl formate distillated in step (1) feeding fuel pipe network is subjected to burning processing, by the mixing of methanol and formamide Object is delivered in product rectifying column and is fractionated, and control product tower bottom of rectifying tower temperature is 160~185 DEG C, tower top temperature 35 ~45 DEG C, molar reflux ratio is greater than 0.5, and top vacuum degree is 0.035~0.045MPa, distillates methanol from tower top, evaporates from tower reactor Formamide out;
(3) methanol distillated in step (2) be fed through Methanol Recovery tank preservation, the formamide distillated successively with reboiler and second Enter formamide storage tank after heat exchanger heat exchange to save.
5. the technique of separation formamide according to claim 4, it is characterised in that: primary distillation tower bottom temperature in step (1) It is 100 DEG C, tower top temperature is 70 DEG C, molar reflux ratio 2.2.
6. the technique of separation formamide according to claim 4, it is characterised in that: product tower bottom of rectifying tower in step (2) Temperature is 170 DEG C, and tower top temperature is 40 DEG C, molar reflux ratio 1.0, and top vacuum degree is 0.04MPa.
CN201811181086.7A 2018-10-11 2018-10-11 A kind of formamide separation system and formamide separating technology Pending CN109020824A (en)

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CN109438167A (en) * 2018-12-27 2019-03-08 成都科特瑞兴科技有限公司 A kind of cyclohexene production energy-saving system and production method
CN109761841A (en) * 2019-01-30 2019-05-17 上海阿拉丁生化科技股份有限公司 A kind of preparation process of order of spectrum formamide
CN111848351A (en) * 2020-08-20 2020-10-30 山东阿斯德科技有限公司 Methanol recovery treatment process for formamide production

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CN109761841A (en) * 2019-01-30 2019-05-17 上海阿拉丁生化科技股份有限公司 A kind of preparation process of order of spectrum formamide
CN111848351A (en) * 2020-08-20 2020-10-30 山东阿斯德科技有限公司 Methanol recovery treatment process for formamide production

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