CN104876808A - Device and process for producing methylal by utilizing novel catalytic distilled and structured packing - Google Patents
Device and process for producing methylal by utilizing novel catalytic distilled and structured packing Download PDFInfo
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- CN104876808A CN104876808A CN201510306276.7A CN201510306276A CN104876808A CN 104876808 A CN104876808 A CN 104876808A CN 201510306276 A CN201510306276 A CN 201510306276A CN 104876808 A CN104876808 A CN 104876808A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention discloses a device and process for producing methylal by utilizing novel catalytic distilled and structured packing. The device comprises a prereactor, a catalytic reaction distillation tower and a decompression and distillation tower, wherein an in-tower distillation section and a etherification reaction section in the catalytic reaction distillation tower adopt a windowing flow-guiding type structured packing. Condensation reaction occurs on methanol and formaldehyde solution to generate methylal in the prereactor, reacted materials are conveyed to the catalytic reaction distillation tower by a pump, new methanol is supplied into the tower, condensation reaction is further carried out continuously, a main product (methylal) flows out of the top part of the catalytic reaction distillation tower by the distillation action, and the methylal with the purity being more than 99.7 percent can be produced by adopting a decompression and distillation technology. The device and the process disclosed by the invention have the advantages that the method is simple, the effect is good, the operability is strong, the formaldehyde conversion rate is high, the large-scale industrial production is easy, and the market prospect is wide.
Description
Technical field
The present invention relates to device and technique that a kind of catalytic reaction rectification produces methylal, belong to technical field of petrochemical industry.
Background technology
Methylal has another name called Methylal(dimethoxymethane), it is a kind of important industrial chemicals, owing to having good physicochemical property, be widely used in the industries such as daily use chemicals, industrial automotive articles for use, makeup, medicine, household, rubber, paint, simultaneously, methylal has good ability of cleaning greasy dirt and volatility, and alternative F11 and F113 and chlorinated solvents, as novel cleaning, are the environmentfriendly products of replacement fluorine Leon.
The traditional preparation methods of methylal is that methyl alcohol and formaldehyde condensation reaction preparation occur under sulphuric acid catalysis and obtains, but this catalytic erosion is strong, and facility investment is high, and environmental pollution is serious, with present Green Development grave fault.In recent years, by using solid acid catalyst to prepare methylal, but the method product purity was lower, only can reach 85% ~ 93%, and methyl alcohol and methylal can form azeotropic again simultaneously, are difficult to obtain high-purity methylal.
Chinese patent CN102417442A, disclose a kind of preparation method of high-purity methylal, the method has highlighted the technological process preparing methylal, and the relevant information of catalytic filler in not mentioned catalytic rectifying tower, the inner stuffing for catalytic rectifying tower is not yet clear and definite.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, provides a kind of device and the technique that utilize new catalytic rectifying structured packing production methylal, effectively reduces the discharge of formaldehyde.
Technical scheme: a kind of device utilizing new catalytic rectifying structured packing to produce methylal of the present invention, comprises pre-reactor, catalytic rectifying column and vacuum rectification tower;
Described pre-reactor is provided with pre-reactor opening for feed, pre-reactor discharge port;
Described catalytic rectifying column tower top is provided with catalytic rectifying column tower top discharge port, and middle part is provided with catalytic rectifying column methanol feeding mouth and catalytic rectifying column opening for feed, is provided with discharge port at the bottom of catalytic rectifying column tower at the bottom of tower;
Be provided with vacuum rectification tower opening for feed in the middle part of described vacuum rectification tower, tower top is provided with rectification under vacuum column overhead discharge port, is provided with discharge port at the bottom of vacuum rectification tower tower at the bottom of tower;
The pre-reactor discharge port of described pre-reactor connects the catalytic rectifying column opening for feed of catalytic rectifying column, the catalytic rectifying column tower top discharge port of described catalytic rectifying column connects the vacuum rectification tower opening for feed of vacuum rectification tower, and at the bottom of the vacuum rectification tower tower of described vacuum rectification tower, discharge port connects pre-reactor opening for feed;
The pre-reactor opening for feed of described pre-reactor is connected with pre-reactor methanol feed line, recycle methanol feeding line and formaldehyde solution feeding line.
Further, the rectifying section of described catalytic rectifying column and conversion zone adopt window diversion type structured packing.
As preferably, assembly A and the assembly B of two kinds of different structures is comprised in every layer of packing layer, assembly A be window diversion packing sheet external parcel silk screen, in fill out ion-exchange resin catalyst, assembly B is structured packing sheet, assembly A and assembly B stacks and curling, then fix with banding sheet, form catalytic rectification packing.
As replacement, assembly A and assembly B also can be alternately arranged vertical placement in every layer of packing layer.
Adopt the above-mentioned device utilizing new catalytic rectifying structured packing to produce methylal to carry out the technique of methylal production, comprise the steps:
1.1, formaldehyde solution and methanol solution are entered pre-reactor by pre-reactor opening for feed, carry out preliminary condensation reaction, reacted mixture is by the extraction of pre-reactor discharge port;
1.2, the mixture of step 1.1 extraction and the new methyl alcohol supplemented are entered in catalytic rectifying column by catalytic rectifying column opening for feed, catalytic rectifying column methanol feeding mouth respectively, there is condensation reaction further in unreacted formaldehyde and methyl alcohol, through refinery distillation, heavy constituent mixture distillates from discharge port at the bottom of catalytic rectifying column tower, and light constituent mixture distillates from catalytic rectifying column tower top discharge port;
1.3, the light constituent mixture that step 1.2 distillates enters vacuum rectification tower, and after rectifying, containing methylal from the extraction of rectification under vacuum column overhead discharge port, remaining ingredient is by discharge port extraction at the bottom of vacuum rectification tower tower;
1.4, the remaining ingredient of extraction in step 1.3 enters pre-reactor by recycle feed pipeline, circulating reaction.
As preferably, the working temperature of described pre-reactor is 50-85 DEG C, and pre-reactor working pressure is 0.01-0.5MPa, preferred 0.1-0.2MPa.
As preferably, the theoretical plate number of described catalytic rectifying column is 20-50 block, and working pressure is 0.01-0.2MPa, preferred 0.05-0.1MPa.
As preferably, the theoretical plate number of described vacuum rectification tower is 30-80 block, and working pressure is 0.01-0.08MPa, preferred 0.01-0.04MPa.
Compared with prior art, its beneficial effect is in the present invention:
(1) structural shape of catalytic rectifying column adopts window diversion type structured packing catalyzer, effectively increases gas-liquid mass transfer area, improves gas-liquid mass transfer speed, improve mass-transfer efficiency further.
(2) whole technique and device, achieves being separated of methyl alcohol and methylal azeotropic system, by variable-pressure rectification technology, without the need to introduce the third material can extraction purity reach more than 99.7% methylal, and the rate of recovery of methylal reaches 99.0%.
(3) the inventive method is simple, effective, transformation efficiency is high, is conducive to alternative chlorinated solvents, freonll-11, reduces topsoil, is an energy-conserving and environment-protective technology, meets industry development relevant policies.
Accompanying drawing explanation
The structural representation of Fig. 1 for utilizing new catalytic rectifying structured packing to produce the device of methylal described in embodiment 1.
Fig. 2 is that catalytic rectifying column packing layer assembly A and assembly B stacks and the vertical view of curling placement.
Fig. 3 to be catalytic rectifying column packing layer assembly A with assembly B be alternately arranged vertical vertical view placed.
Fig. 4 is the center section schematic diagram of Fig. 3.
In figure: 1-pre-reactor, 2-catalytic rectifying column, 3-vacuum rectification tower, 6-assembly A, 7-assembly B, a-methanol feeding, the charging of b-formaldehyde solution, c-supplements methanol feeding, by-product discharging after d-condensation, product discharge after e-condensation, the charging of f-Cycle Component, g-methylal product discharge, the discharging of h-remaining ingredient.
Embodiment
Below in conjunction with accompanying drawing, technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
Utilize new catalytic rectifying structured packing to produce a device for methylal, comprise pre-reactor, catalytic rectifying column and vacuum rectification tower.
Described pre-reactor is provided with pre-reactor opening for feed, pre-reactor discharge port.
Described catalytic rectifying column tower top is provided with catalytic rectifying column tower top discharge port, and middle part is provided with catalytic rectifying column methanol feeding mouth and catalytic rectifying column opening for feed, is provided with discharge port at the bottom of catalytic rectifying column tower at the bottom of tower.
The rectifying section of described catalytic rectifying column and etherification reaction section adopt window diversion type structured packing, assembly A and the assembly B of two kinds of different structures is comprised in every layer of packing layer, assembly A be window diversion packing sheet external parcel silk screen, in fill out ion-exchange resin catalyst, assembly B is structured packing sheet, assembly A and assembly B stacks and curling, then fix with banding sheet, form catalytic rectification packing, as shown in Figure 2.
As replacement, assembly A and assembly B also can be alternately arranged vertical placement in every layer of packing layer, as shown in Figures 3 and 4.
Be provided with vacuum rectification tower opening for feed in the middle part of described vacuum rectification tower, tower top is provided with rectification under vacuum column overhead discharge port, is provided with discharge port at the bottom of vacuum rectification tower tower at the bottom of tower;
The pre-reactor discharge port of described pre-reactor connects the catalytic rectifying column opening for feed of catalytic rectifying column, the catalytic rectifying column tower top discharge port of described catalytic rectifying column connects vacuum rectification tower opening for feed, the circulation line opening for feed of the rectification under vacuum column overhead discharge port pre-reactor of described vacuum rectification tower;
The pre-reactor opening for feed of described pre-reactor is connected with pre-reactor methanol feed line, recycle methanol feeding line and formaldehyde solution feeding line.
In the present embodiment, the processing step adopting the above-mentioned device utilizing new catalytic rectifying structured packing to produce methylal to carry out methylal production is:
1.1, formaldehyde solution (massfraction is the formalin of 41.70%) and methyl alcohol are entered pre-reactor by pre-reactor opening for feed, carry out preliminary condensation reaction and generate methylal, wherein: methyl alcohol is 3.76 × 10 to the feed flow rates of pre-reactor
3kg/h, formaldehyde solution is 6.49 × 10 to the feed flow rates of pre-reactor
3kg/h, pre-reactor temperature is 55 DEG C, and pre-reactor working pressure is 0.10MPa, and reacted mixture is by the extraction of pre-reactor discharge port;
1.2, the mixture of step 1.1 extraction and the new methyl alcohol supplemented are entered in catalytic rectifying column by catalytic rectifying column opening for feed, catalytic rectifying column methanol feeding mouth respectively, there is condensation reaction further and produce methylal in unreacted formaldehyde and methyl alcohol, through refinery distillation, heavy constituent mixture distillates from discharge port at the bottom of catalytic rectifying column tower, and light constituent mixture distillates from catalytic rectifying column tower top discharge port; Heavy constituent mixture comprises a small amount of unreacted first alcohol and water, and light constituent mixture comprises methylal and a small amount of methyl alcohol and formaldehyde;
The stage number of catalytic rectifying column is 25 blocks of (rectifying section column plates 2nd ~ 5 pieces, catalyst reaction section column plate 6th ~ 19 pieces, stripping section column plate 20th ~ 24 pieces), the feed entrance point supplementing methyl alcohol is the 19th block of column plate, and the feed entrance point of the mixture of step 1.1 extraction is the 16th block of column plate.
Supplementary methyl alcohol is 2.03 × 10 to the feed flow rates of catalytic rectifying column
3kg/h, the working pressure of catalytic rectifying column is 0.10MPa.
1.3, the light constituent mixture that step 1.2 distillates enters vacuum rectification tower, and after rectifying, methylal product is from the extraction of rectification under vacuum column overhead discharge port, and remaining ingredient is by discharge port extraction at the bottom of vacuum rectification tower tower, and remaining ingredient is mainly methyl alcohol.
The stage number of vacuum rectification tower is 48 pieces, and feed entrance point is the 46th block of column plate, and working pressure is 0.015MPa.
1.4, the remaining ingredient of extraction in step 1.3 enters pre-reactor by recycle feed pipeline, circulating reaction.
The material of pre-reactor, catalytic rectifying column, vacuum rectification tower passes through pump delivery.
In pre-reactor, the transformation efficiency of formaldehyde is 46.04%, and after catalytic distillation reaction, the transformation efficiency of formaldehyde is 99.61%; After condensation reaction, the massfraction of the methylal of extraction is 97.21%.
Table 1: the flow rate of extraction at the bottom of pre-reactor discharge port, catalytic rectifying column tower top and tower in embodiment 1, the extraction of vacuum rectification tower product and cycling stream stock and composition
Embodiment 2:
What adopt in the present embodiment a kind ofly utilizes new catalytic rectifying structured packing to produce the device of methylal, identical with embodiment 1.
In the present embodiment, the processing step adopting the above-mentioned device utilizing new catalytic rectifying structured packing to produce methylal to carry out methylal production is:
1.1, formaldehyde solution (massfraction is the formalin of 36.70%) and methyl alcohol are entered pre-reactor by pre-reactor opening for feed, carry out preliminary condensation reaction and generate methylal, wherein: methyl alcohol is 1.28 × 10 to the feed flow rates of pre-reactor
3kg/h, formaldehyde solution is 2.18 × 10 to the feed flow rates of pre-reactor
3kg/h, pre-reactor temperature is 60 DEG C, and pre-reactor working pressure is 0.10MPa, and reacted mixture is by the extraction of pre-reactor discharge port;
1.2, the mixture of step 1.1 extraction and the new methyl alcohol supplemented are entered in catalytic rectifying column by catalytic rectifying column opening for feed, catalytic rectifying column methanol feeding mouth respectively, there is condensation reaction further and produce methylal in unreacted formaldehyde and methyl alcohol, through refinery distillation, heavy constituent mixture distillates from discharge port at the bottom of catalytic rectifying column tower, and light constituent mixture distillates from catalytic rectifying column tower top discharge port; Heavy constituent mixture comprises a small amount of unreacted first alcohol and water, and light constituent mixture comprises methylal and a small amount of methyl alcohol and formaldehyde;
The stage number of catalytic rectifying column is 30 blocks of (rectifying section column plates 2nd ~ 7 pieces, catalyst reaction section column plate 8th ~ 28 pieces, stripping section column plate 28th ~ 29 pieces), the feed entrance point supplementing methyl alcohol is the 28th block of column plate, and the feed entrance point of the mixture of step 1.1 extraction is the 7th block of column plate.
Supplementary methyl alcohol is 314kg/h to the feed flow rates of catalytic rectifying column, and the working pressure of catalytic rectifying column is 0.1MPa.
1.3, the light constituent that step 1.2 distillates enters vacuum rectification tower, and after rectifying, methylal product is from the extraction of rectification under vacuum column overhead discharge port, and remaining ingredient is by discharge port extraction at the bottom of vacuum rectification tower tower, and remaining ingredient is mainly methyl alcohol.
The stage number of vacuum rectification tower is 70 pieces, and feed entrance point is the 70th block of column plate, and working pressure is 0.02MPa.
1.4, the remaining ingredient of extraction in step 1.3 enters pre-reactor by recycle feed pipeline, circulating reaction.
The material of pre-reactor, catalytic rectifying column, vacuum rectification tower passes through pump delivery.
In pre-reactor, the transformation efficiency of formaldehyde is 56.14%, and after catalytic distillation reaction, the transformation efficiency of formaldehyde is 99.74%; After condensation reaction, the massfraction of the methylal of extraction is 96.91%.
Table 2: the flow rate of extraction at the bottom of pre-reactor discharge port, catalytic rectifying column tower top and tower in embodiment 2, the extraction of vacuum rectification tower product and cycling stream stock and composition
Embodiment 3:
What adopt in the present embodiment a kind ofly utilizes new catalytic rectifying structured packing to produce the device of methylal, identical with embodiment 1.
In the present embodiment, the processing step adopting the above-mentioned device utilizing new catalytic rectifying structured packing to produce methylal to carry out methylal production is:
1.1, formaldehyde solution (massfraction is the formalin of 39.10%) and methyl alcohol are entered pre-reactor by pre-reactor opening for feed, carry out preliminary condensation reaction and generate methylal, wherein: methyl alcohol is 6.78 × 10 to the feed flow rates of pre-reactor
3kg/h, formaldehyde solution is 1.02 × 10 to the feed flow rates of pre-reactor
4kg/h, pre-reactor temperature is 55 DEG C, and pre-reactor working pressure is 0.10MPa, and reacted mixture is by the extraction of pre-reactor discharge port;
1.2, the mixture of step 1.1 extraction and the new methyl alcohol supplemented are entered in catalytic rectifying column by catalytic rectifying column opening for feed, catalytic rectifying column methanol feeding mouth respectively, there is condensation reaction further and produce methylal in unreacted formaldehyde and methyl alcohol, through refinery distillation, heavy constituent mixture distillates from discharge port at the bottom of catalytic rectifying column tower, and light constituent mixture distillates from catalytic rectifying column tower top discharge port; Heavy constituent mixture comprises a small amount of unreacted first alcohol and water, and light constituent mixture comprises methylal and a small amount of methyl alcohol and formaldehyde;
The stage number of catalytic rectifying column is 21 blocks of (rectifying section column plates 2nd ~ 5 pieces, catalyst reaction section column plate 6th ~ 18 pieces, stripping section column plate 19th ~ 20 pieces), the feed entrance point supplementing methyl alcohol is the 14th block of column plate, and the feed entrance point of the mixture of step 1.1 extraction is the 12nd block of column plate.
Supplementary methyl alcohol is 2.02 × 10 to the feed flow rates of catalytic rectifying column
3kg/h, the working pressure of catalytic rectifying column is 0.08MPa.
1.3, the light constituent that step 1.2 distillates enters vacuum rectification tower, and after rectifying, methylal product is from the extraction of rectification under vacuum column overhead discharge port, and remaining ingredient is by discharge port extraction at the bottom of vacuum rectification tower tower, and remaining ingredient is mainly methyl alcohol.
The stage number of vacuum rectification tower is 44 pieces, and feed entrance point is the 44th block of column plate, and working pressure is 0.015MPa.
1.4, the remaining ingredient of extraction in step 1.3 enters pre-reactor by recycle feed pipeline, circulating reaction.
Pre-reactor, material between catalytic rectifying column and vacuum rectification tower pass through pump delivery.
In pre-reactor, the transformation efficiency of formaldehyde is 54.51%, and after catalytic distillation reaction, the transformation efficiency of formaldehyde is 99.82%; After condensation reaction, the massfraction of the methylal of extraction is 96.70%.
Table 3: the flow rate of extraction at the bottom of pre-reactor discharge port, catalytic rectifying column tower top and tower in embodiment 3, the extraction of vacuum rectification tower product and cycling stream stock and composition
As mentioned above, although represented with reference to specific preferred embodiment and described the present invention, it shall not be construed as the restriction to the present invention self.Under the spirit and scope of the present invention prerequisite not departing from claims definition, various change can be made in the form and details to it.
Claims (8)
1. utilize new catalytic rectifying structured packing to produce a device for methylal, it is characterized in that: comprise pre-reactor, catalytic rectifying column and vacuum rectification tower;
Described pre-reactor is provided with pre-reactor opening for feed, pre-reactor discharge port;
Described catalytic rectifying column tower top is provided with catalytic rectifying column tower top discharge port, and middle part is provided with catalytic rectifying column methanol feeding mouth and catalytic rectifying column opening for feed, is provided with discharge port at the bottom of catalytic rectifying column tower at the bottom of tower;
Be provided with vacuum rectification tower opening for feed in the middle part of described vacuum rectification tower, tower top is provided with rectification under vacuum column overhead discharge port, is provided with discharge port at the bottom of vacuum rectification tower tower at the bottom of tower;
The pre-reactor discharge port of described pre-reactor connects the catalytic rectifying column opening for feed of catalytic rectifying column, the catalytic rectifying column tower top discharge port of described catalytic rectifying column connects vacuum rectification tower opening for feed, and discharge port at the bottom of the vacuum rectification tower tower of described vacuum rectification tower connects pre-reactor opening for feed;
The pre-reactor opening for feed of described pre-reactor is connected with pre-reactor fresh methanol feeding line, recycle methanol feeding line and formaldehyde solution feeding line.
2. the device utilizing new catalytic rectifying structured packing to produce methylal according to claim 1, is characterized in that, the rectifying section of described catalytic rectifying column and conversion zone adopt window diversion type structured packing.
3. the device utilizing new catalytic rectifying structured packing to produce methylal according to claim 2, it is characterized in that, assembly A and the assembly B of two kinds of different structures is comprised in every layer of packing layer, assembly A be window diversion packing sheet external parcel silk screen, in fill out ion-exchange resin catalyst, assembly B is structured packing sheet, assembly A and assembly B stacks and curling, then fixes with banding sheet, forms catalytic rectification packing.
4. according to claim 3ly utilize new catalytic rectifying structured packing to produce the device of methylal, it is characterized in that, assembly A and assembly B also can be alternately arranged vertical placement in every layer of packing layer.
5. adopt the device utilizing new catalytic rectifying structured packing to produce methylal described in claim 1 or 2 to carry out the technique of methylal production, it is characterized in that, comprise the steps:
1.1, formaldehyde solution and methanol solution are entered pre-reactor by pre-reactor opening for feed, carry out preliminary condensation reaction, reacted mixture is by the extraction of pre-reactor discharge port;
1.2, the mixture of step 1.1 extraction and the new methyl alcohol supplemented are entered in catalytic rectifying column by catalytic rectifying column opening for feed, catalytic rectifying column methanol feeding mouth respectively, there is condensation reaction further in unreacted formaldehyde and methyl alcohol, through refinery distillation, heavy constituent mixture distillates from discharge port at the bottom of catalytic rectifying column tower, and light constituent mixture distillates from catalytic rectifying column tower top discharge port;
1.3, the light constituent mixture that step 1.2 distillates enters vacuum rectification tower, and after rectifying, product methylal is from the extraction of rectification under vacuum column overhead discharge port, and remaining ingredient is by discharge port extraction at the bottom of vacuum rectification tower tower;
1.4, the remaining ingredient of extraction in step 1.3 enters pre-reactor by recycle feed pipeline, circulating reaction.
6. technique of carrying out methylal production according to claim 5, is characterized in that, the working temperature of described pre-reactor is 50-85 DEG C, and pre-reactor working pressure is 0.01-0.5MPa.
7. technique of carrying out methylal production according to claim 5, is characterized in that, the theoretical plate number of described catalytic rectifying column is 20-50 block, and working pressure is 0.01-0.2MPa.
8. technique of carrying out methylal production according to claim 5, is characterized in that, the theoretical plate number of described vacuum rectification tower is 30-80 block, and working pressure is 0.01-0.08MPa.
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| CN201510306276.7A CN104876808B (en) | 2015-06-04 | 2015-06-04 | The device and technique of a kind of utilization new catalytic rectifying structured packing production dimethoxym ethane |
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| CN201510306276.7A CN104876808B (en) | 2015-06-04 | 2015-06-04 | The device and technique of a kind of utilization new catalytic rectifying structured packing production dimethoxym ethane |
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| CN116510332A (en) * | 2023-06-20 | 2023-08-01 | 江苏金茂源生物化工有限责任公司 | Solid acid catalytic reaction and rectification integrated device and method |
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| CN116510332A (en) * | 2023-06-20 | 2023-08-01 | 江苏金茂源生物化工有限责任公司 | Solid acid catalytic reaction and rectification integrated device and method |
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| CN104876808B (en) | 2017-10-20 |
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