CN111450553A - Dimethyl formamide evaporation system and production process - Google Patents
Dimethyl formamide evaporation system and production process Download PDFInfo
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- CN111450553A CN111450553A CN202010229455.6A CN202010229455A CN111450553A CN 111450553 A CN111450553 A CN 111450553A CN 202010229455 A CN202010229455 A CN 202010229455A CN 111450553 A CN111450553 A CN 111450553A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0011—Heating features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0064—Feeding of liquid into an evaporator
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
- B01D1/305—Demister (vapour-liquid separation)
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Abstract
The invention particularly relates to an evaporation system and a production process of dimethylformamide. The method for preparing the dimethylformamide by using the carbon monoxide and the dimethylamine as raw materials under the catalytic action of methanol/sodium methoxide has the advantages of good product quality and low cost, but the sodium methoxide is easy to generate crystals when dissolved in water, and can catalyze the DMF to generate reverse reaction in an evaporation process to generate the dimethylamine. The invention provides a DMF (dimethyl formamide) evaporation system suitable for the production mode and a production process, wherein the production process comprises the following steps: after crude DMF of a DMF synthesis tower enters a separator for preliminary concentration, the crude DMF is divided into two paths to be forcibly circulated with a filter, one path is added with water at an inlet of a second circulating pump, normal operation of an evaporation circulating pump is ensured by adding water, and the other path is carried out by inhibiting reverse reaction of the DMF. The first circulating pump of the other path plays a role in filtering and discharging the salt mud of the system. The production process can effectively improve the operation period of DMF and improve the yield.
Description
Technical Field
The invention belongs to the technical field of chemical production methods, particularly relates to an evaporation system of dimethylformamide, provides a production process applying the evaporation system, and has the technical effect of improving the production period of the dimethylformamide.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Dimethyl formamide (DMF) is a good solvent for many organic and inorganic substances, so that the dimethyl formamide is commonly used as a reaction catalyst or a cocatalyst in the reaction, so that the yield of a reaction product can be improved, and the generation rate of a byproduct can be reduced. The process for producing DMF is to use anhydrous dimethylamine and carbon monoxide (CO) as raw materials to carry out gas-liquid contact by using sodium methoxide and methanol as catalyst solvents at a certain temperature and under a certain pressure to complete acylation reaction.
The acylation reaction comprises the following two steps:
the first step is as follows: CH (CH)3OH+CO→HCOOCH3
The second step is that: HCOOCH3+(CH3)2NH→HCON(CH3)2+CH3OH
The general reaction formula is as follows: CO + (CH)3)2NH→HCON(CH3)2
The first step has a relatively slow reaction rate and the second step has a relatively fast reaction rate. The DMF product prepared by the process has good quality and low cost, but methanol and sodium methoxide are required to be catalyzed together, otherwise, the reaction cannot be carried out. Methanol is an intermediate raw material in the system and also plays a role of a solvent, and meanwhile, methanol and sodium methoxide are added, so that the defects exist, for example, in the reaction process, the catalyst sodium methoxide is easy to react with impurity water, oxygen and carbon dioxide brought by the raw material to generate sodium formate and sodium carbonate crystals, and the crystals are easy to attach to the wall and the pipe wall of a reaction tower in the system and further accumulate, so that the physical performance and the gas-liquid flowing performance of liquid are deteriorated, and the operation period of the system is influenced; meanwhile, the reaction of dimethylamine and CO to generate DMF is a reversible reaction, and DMF moves in the reverse reaction direction due to the existence of sodium methoxide serving as a catalyst in a DMF evaporation process, so that a part of DMF is decomposed to generate dimethylamine, the content of dimethylamine in DMF is increased, the yield of DMF is influenced, and the energy consumption for generating DMF is increased.
The existing dimethylformamide production device generally comprises a separator, an evaporation circulating pump, a filter and an evaporation heater, and impurities such as a catalyst in dimethylformamide are removed by the device. For example, patent CN207203493U provides an operation mode of a dimethylformamide evaporation system, in which a material is returned to an evaporator through a separator and a circulating pump via a heater, and a filter and the heater work in turn to realize cleaning without stopping. Patent CN2728587Y also provides a way of connecting a heater, a separator, a circulation pump loop in parallel with a separator, a filter, and a circulation pump loop, so that the liquid in the heater can always maintain a large flow rate, and deposition caused by slow flow rate is avoided. The inventor believes that the heater is arranged in parallel with the filter to ensure the normal operation of the production, since the salt slurry is easily deposited on the filter or the heater part during the evaporation of the dimethylformamide. When the production process is adopted for production, sodium methoxide is easily dissolved in water, so that a product is crystallized and decomposed in a system, and impurities are introduced again.
Disclosure of Invention
In view of the above background art, the present invention provides an evaporation system and a production process of Dimethylformamide (DMF) that is more suitable for using sodium methoxide as a catalyst, and provides the following technical solutions:
in a first aspect, an evaporation system of dimethylformamide is provided, which comprises a separator, a first circulating pump, a second circulating pump, a filter and a heater; the separator, the first circulating pump, the filter and the heater are connected in series to form a loop for circulating and evaporating DMF materials; and introducing steam into the second circulating pump for forcing the DMF material to circulate in the evaporation system.
Aiming at the synthesis scheme using sodium methoxide as a catalyst, the invention is provided with a first circulating pump and a second circulating pump which are arranged in parallel, the first circulating pump participates in the evaporation and circulation of the materials of the whole system, and because steam is not introduced into the first circulating pump, the water content in an evaporation circulation loop is obviously reduced, so that salty mud carried by DMF materials can be precipitated in a pipeline, and the purification effect of DMF is realized. The second evaporation pump is used for introducing steam, so that the normal work of the circulating pump is ensured, power is provided for the evaporation system, and the DMF material is forced to circulate in the evaporation system. In addition, because sodium methoxide is easily dissolved in water, steam in the second circulating pump can take away sodium methoxide in an evaporation loop, so that residual sodium methoxide in an evaporation system is hydrolyzed, and DMF is inhibited from going to a reverse reaction, thereby achieving the purposes of improving yield and reducing consumption.
As the evaporation proceeds, salt sludge deposition gradually occurs in the evaporation system pipeline and the device. Through the setting of first circulating pump, can realize under the condition of not stopping, pause first circulating pump gets rid of the partial salt mud in first circulating pump and the pipeline through the washing, extension system operation cycle. Preferably, the first circulating pumps arranged in parallel can be adopted to alternately operate, so that the complete non-stop work is realized.
In a second aspect, there is provided a production method of the evaporation system of dimethylformamide described in the first aspect, the production method comprising the steps of: introducing DMF materials into the separator to reach a certain liquid level, and sequentially opening a second circulating pump and a first circulating pump to construct circulation in an evaporation system; and (3) preheating a heater to ensure that the temperature of the separator reaches 155-165 ℃, then keeping the continuous addition of the DMF material, and when the temperature in the separator reaches 170-180 ℃, normally operating the system.
In a third aspect, a process for producing dimethylformamide is provided, the process comprising a production method using the evaporation system of dimethylformamide of the first aspect and/or the evaporation system of dimethylformamide of the second aspect.
The beneficial effects of one or more technical schemes are as follows:
1. the evaporation system ingeniously realizes the effects of ensuring the normal operation of the system and inhibiting the reverse reaction in the system by the parallel design of circulating pumps aiming at the synthesis process of adopting methanol/sodium methoxide as a catalyst, and well solves the problem of evaporation separation caused by the preparation process.
2. The production method realizes the improvement of the operation period of the DMF, can improve the operation period of the DMF by two months on average, can improve the yield by 4-7% under the condition of the same feeding, saves the production cost and has good market popularization significance.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of the structure of an evaporation system for dimethylformamide described in example 1;
wherein, 1 is a separator, 2 is a first circulating pump, 3a is a second circulating pump a, 3b is a second circulating pump b, 4a is a filter a, 4b is a filter b, 5a is a heater a, 5b is a heater b, 6 is a DMF synthesis tower, 7 is a first steam source, 8 is a second steam source, 9 is a pushing liquid storage tank, and 11 is a demister.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As the introduction of the background art, aiming at the defects in the prior art, the invention provides an evaporation system and a production process of dimethylformamide, aiming at solving the technical problems.
In a first aspect of the present invention, an evaporation system for dimethylformamide is provided, which includes a separator, a first circulation pump, a second circulation pump, a filter and a heater. The separator, the first circulating pump, the filter and the heater are connected in series to form a loop for circulating and evaporating DMF materials; and introducing steam into the second circulating pump for forcing the DMF material to circulate in the evaporation system.
Preferably, the separator is communicated with a DMF synthesis tower and is used for receiving crude DMF materials synthesized by the DMF synthesis tower and carrying out evaporation separation; the top part is provided with a filter screen and a demister and is used for purifying gas-phase DMF; the bottom of the separator is communicated with a first circulating pump.
Preferably, the first circulation pump and/or the second circulation pump is an evaporation circulation pump.
Preferably, the first circulation pump does not introduce steam.
Preferably, the number of the first circulating pumps is 1-4, and when the number is not 1, the first circulating pumps are arranged in parallel.
Preferably, the second circulation pump is arranged in parallel with the first circulation pump.
Preferably, the number of the second circulating pumps is two or more, and the second circulating pumps are arranged in parallel; more preferably, the number of the cells is 2 to 4.
Preferably, the number of the filter is two or more, and the filter is arranged in parallel; more preferably, the number of the cells is 2 to 4.
Preferably, the number of the heaters is two or more, and the heaters are arranged in parallel; more preferably, the number of the cells is 2 to 4.
Preferably, the heater is an evaporation heater, and the temperature is regulated by introducing steam.
In a second aspect, there is provided a production method of the evaporation system of dimethylformamide described in the first aspect, the production method comprising the steps of: introducing DMF materials into the separator to reach a certain liquid level, and sequentially opening a second circulating pump and a first circulating pump to construct circulation in an evaporation system; and (3) preheating a heater to ensure that the temperature of the separator reaches 155-165 ℃, then keeping the continuous addition of the DMF material, and when the temperature in the separator reaches 170-180 ℃, normally operating the system.
Preferably, the production method comprises the following specific steps:
(1) confirming that the evaporation system has good air tightness;
(2) enabling the DMF material to flow into the separator to reach a liquid level of 2-2.5m, stopping adding the DMF material, opening a second circulating pump, a filter and a first circulating pump, and establishing a circulating path in the evaporation system;
(3) preheating a heater, and recovering DMF material to be continuously added after the temperature in the heater reaches 155-165 ℃;
(4) and raising the temperature of the separator until the temperature in the separator reaches 170-180 ℃, and normally operating the system.
Further preferably, the preheating heater process is controlled to be 30-40 ℃/hour.
Further preferably, the heater is a steam heater, and the temperature is adjusted by controlling the steam introduction amount.
In a third aspect, a process for producing dimethylformamide is provided, the process comprising a production method using the evaporation system of dimethylformamide of the first aspect and/or the evaporation system of dimethylformamide of the second aspect.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
In the embodiment, an evaporation system of dimethylformamide is provided, and the structure of the evaporation system is shown in fig. 1, and the evaporation system comprises a separator 1, a first circulating pump 2, a second circulating pump 3, a filter 4 and a heater 6. The DMF material flows back to the separator 1 after passing through the separator 1, the first circulating pump 2, the filter 4 and the heater 6.
The separator 1 is provided with a liquid level high-low limit alarm, the liquid level is controlled to be 1.2-2.5m, the internal temperature is about 173 ℃, and the pressure is controlled to be about 0.08 MPa. The separator 1 receives DMF crude material from a DMF synthesis tower 6, the DMF crude material is subjected to primary evaporation separation under the action of temperature and pressure, and the DMF in a gas phase enters a primary distillation tower through a filter screen at the top of the separator 1 and a demister 11 and enters the next working procedure for purification of the DMF.
The liquid phase DMF flows out from the lower opening of the separator, enters a first circulating pump 2, sequentially flows through a filter 4 and a heater 5 through the first circulating pump 2, returns to the separator 1, and is evaporated and separated again. The liquid phase DMF is purified by the forced circulation of the first circulating pump 2 and the filter 4, and the flow rate of the forced circulation is about 80 square/h. First circulating pump 2 is open impeller, can eliminate the influence of salt mud to the pipeline, the exit linkage of first circulating pump 2 is 4 imports of filter, the filter is the leaf filter, thick DMF after the concentration can form one deck filter cake on the filter element surface, filter out the system with salt mud in the thick DMF, thick DMF filters the back through the filter, with the export of second circulating pump and be in the same place, in getting into 5 tube passes of heater, the shell pass of heater 5 is medium pressure steam, can evaporate the thick DMF in 5 tube passes of heater to evaporating in the vapour and liquid separator, accomplish the evaporation filtration flow of DMF.
The first circulating pump 2 and the second circulating pump 3 are arranged in parallel, the second circulating pump 3 is used for introducing steam, the addition amount of the steam is based on the emptying amount of the primary distillation tower, the emptying amount of the primary distillation tower is controlled to be about 30-50 square/h, when the emptying amount is reduced, the fact that more water is added in the system is proved, the product quality of DMF (dimethyl formamide) can be influenced, and when the emptying amount is increased, the reverse reaction of the DMF is increased, and the addition amount of the steam needs to be increased. When the pressure of first circulating pump 2 risees, the inside salt mud siltation that appears, through closing the valve, make the liquid phase of outflow directly flow into the filter in the separator and circulate, wash first circulating pump simultaneously, need not the parking operation.
As shown in fig. 1, the second circulation pump 3 is two parallel circulation pumps 3a and 3b, and steam is introduced into the second circulation pump through a first steam source 7. The filter 4 is two filters 4a and 4b connected in parallel, and when the pressure of one filter reaches or exceeds 0.4MPa, the filter is suspended to clean the salt mud in the filter. In other embodiments, three or four filters can be arranged in parallel, the filter with salt mud deposition stops to clean, and the whole system does not need to stop to operate.
The heater 5 is a heater 5a and a heater 5b which are connected in parallel, and are respectively connected with a second steam source 8a and a second steam source 8b, and are used for heating DMF liquid flowing out of the filter 4 and maintaining the temperature in the separator 1.
The shell side steam of the heater 5 is provided with the adjusting valve, the steam adjusting valve and the liquid level of the evaporation gas-liquid separator, and the automatic interlocking function is realized, so that the accurate operation of the whole system can be effectively controlled, the automatic control can be realized, a large amount of manpower can be saved, and the operation is convenient
Furthermore, the separator 1 is provided with a remote transmission liquid level, when the liquid level of the separator 1 is higher than 2.1m, the steam regulating valve of the heater 5 is automatically opened in an interlocking manner, the stability of the liquid level is ensured, and when the liquid level is lower than 1.9m, the steam regulating valve of the evaporation heater is automatically closed in an interlocking manner, so that the stability of the liquid level is ensured.
Furthermore, the valve and the equipment are made of stainless steel; the first circulating pump 2 is an open impeller high-temperature end face seal shield pump; the second circulating pump 3 is a closed impeller high-temperature end face seal shield pump, and is also provided with a thrust liquid storage tank which is respectively communicated with the first circulating pump 2 and the second circulating pump 3.
The heater 5 is a shell-and-tube heat exchanger, and the filter 4 is a leaf filter. The device in the evaporation system is made of stainless steel, so that on one hand, the service cycle of the device in normal operation is prolonged, and meanwhile, the device can be prevented from being corroded to cause leakage and cause production safety.
Example 2
In this example, there is provided a process for the production of the evaporation system of dimethylformamide as described in example 1, said process comprising the steps of:
(1) the opening condition of the valve and the sealing condition of the filter 4 are checked to ensure the sealing property of the evaporation system;
(2) opening valves of a DMF synthesis tower 6 and a heater 5, temporarily closing a discharge valve of the DMF synthesis tower 6 after the material in the separator 1 rises to 2.3m, opening an inlet valve of a second circulating pump 3, opening a valve of a circulating pump outlet which enters a filter a and a valve of the filter a to an evaporation heater, then opening a gas phase valve of the evaporation heater to ensure that a circulating passage valve of evaporation filtration is unblocked, and then opening an evaporation circulating pump a or b according to the operation rule of a shielding pump to establish system circulation;
(3) and similarly, the evaporation circulating pump c is started to ensure the circulation passage to be smooth.
(4) Slightly opening a steam inlet valve of an evaporation heater, stopping when the air noise is heard, carrying out preheating equipment, controlling the preheating process at 30-40 ℃/and starting an inlet steam valve 1/3-1/2 when the preheating process is finished when the steam drained by the steam trap is finished, and heating the crude DMF by using the steam;
(5) and when the temperature in the evaporator heater reaches 160 ℃, opening the synthesis discharge valve to realize continuous feeding of DMF evaporation, gradually increasing the steam consumption of the evaporator according to the liquid level condition of the evaporation gas-liquid separator until the temperature of the evaporation gas-liquid separator reaches 175 ℃, and normally and continuously operating the evaporation system.
By adopting the device in the embodiment 1 and the production process in the embodiment 2, the operation period of DMF is improved from 3 months to 5 months, and meanwhile, under the condition of the same feeding, the yield is improved by about 5.5%, the unit product cost is reduced, and the market competitiveness is improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides an evaporation system of dimethyl formamide, its characterized in that, evaporation system includes separator, first circulating pump, second circulating pump, filter and heater. The separator, the first circulating pump, the filter and the heater are connected in series to form a loop for circulating and evaporating DMF materials; and introducing steam into the second circulating pump for forcing the DMF material to circulate in the evaporation system.
2. The dimethylformamide evaporation system of claim 1, wherein the separator is in communication with the DMF synthesis column for receiving the crude DMF stream from the DMF synthesis column and performing evaporative separation; the top part is provided with a filter screen and a demister and is used for purifying gas-phase DMF; the bottom of the separator is communicated with a first circulating pump.
3. The dimethylformamide evaporation system of claim 1, wherein the first circulation pump and/or the second circulation pump is an evaporation circulation pump;
or the first circulating pump does not feed steam;
or the number of the first circulating pumps is 1-4, and when the number is not 1, the first circulating pumps are arranged in parallel;
or the second circulating pump and the first circulating pump are arranged in parallel.
Or the number of the second circulating pumps is two or more, and the second circulating pumps are arranged in parallel; more preferably, the number of the cells is 2 to 4.
4. The dimethylformamide evaporation system according to claim 1, wherein the number of said filters is two or more, and said filters are arranged in parallel; more preferably, the number of the cells is 2 to 4.
5. The evaporation system of dimethylformamide as claimed in claim 1, wherein said heaters are two or more in number and arranged in parallel; more preferably, the number of the cells is 2 to 4.
6. The dimethylformamide evaporation system of claim 1, wherein the heater is an evaporation heater, and the temperature control is performed by introducing steam.
7. The process for the production of an evaporation system of dimethylformamide as claimed in any of claims 1 to 6, characterized in that it comprises the following steps: introducing DMF materials into the separator to reach a certain liquid level, and sequentially opening a second circulating pump and a first circulating pump to construct circulation in an evaporation system; and (3) preheating a heater to ensure that the temperature of the separator reaches 155-165 ℃, then keeping the continuous addition of the DMF material, and when the temperature in the separator reaches 170-180 ℃, normally operating the system.
8. The method for producing the evaporation system of dimethylformamide as claimed in claim 7, characterized in that the specific steps of said production method are as follows:
(1) confirming that the evaporation system has good air tightness;
(2) enabling the DMF material to flow into the separator to reach a liquid level of 2-2.5m, stopping adding the DMF material, opening a second circulating pump, a filter and a first circulating pump, and establishing a circulating path in the evaporation system;
(3) preheating a heater, and recovering DMF material to be continuously added after the temperature in the heater reaches 155-165 ℃;
(4) and raising the temperature of the separator until the temperature in the separator reaches 170-180 ℃, and normally operating the system.
9. The method for producing an evaporation system of dimethylformamide as claimed in claim 8, characterized in that said preheating heater process is controlled to 30-40 ℃/hr;
or the heater is a steam heater, and the temperature is adjusted by controlling the steam introduction amount.
10. A process for producing dimethylformamide, characterized in that the process comprises a production method using the evaporation system of dimethylformamide as described in any of claims 1 to 6 and/or the evaporation system of dimethylformamide as described in any of claims 7 to 9.
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Cited By (1)
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| CN113797716A (en) * | 2021-10-27 | 2021-12-17 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system of DMF (dimethyl formamide) production device, process and application |
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