CN218485985U - Preparation device of polymethoxy dimethyl ether DMMn system - Google Patents

Preparation device of polymethoxy dimethyl ether DMMn system Download PDF

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CN218485985U
CN218485985U CN202222515653.6U CN202222515653U CN218485985U CN 218485985 U CN218485985 U CN 218485985U CN 202222515653 U CN202222515653 U CN 202222515653U CN 218485985 U CN218485985 U CN 218485985U
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王义成
冷东斌
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Dandong Mingzhu Special Resin Co ltd
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Abstract

The application provides a DMMn system preparation device, which takes trioxymethylene and methylal as raw materials to synthesize DMM 3～8 The device comprises a pre-reaction part, a catalytic distillation part and an output flow separation part, wherein the catalytic distillation part is a catalytic distillation tower, a feed inlet is arranged on the upper part of a reaction section and is connected with an output intermediate stream of the pre-reaction part, a tower top stream and a tower bottom stream of the catalytic distillation part are downwards connected with the output flow separation part, and a supplement feed inlet of a high-position, a middle-position and a low-position three-way methylal supplement stream is arranged on the reaction section at equal intervals downwards from the feed inlet. The technical scheme has the technical advantages of simple process flow and low equipment investment cost, particularly has the technical advantages of high selectivity and conversion rate, greatly reduces the amount of recycled materials and has low energy consumption.

Description

Preparation device of polymethoxy dimethyl ether DMMn system
Technical Field
The present application relates to a fine chemical manufacturing system apparatus, and more particularly, to a manufacturing system apparatus for DX polymer.
Background
DX is a low molecular weight acetal polymer with methoxyl as a main chain, and the structural general formula of DX is as follows: CH (CH) 3 O(CH 2 O)nCH 3 The polymer is DMMn, wherein when n = 3-8, the polymer does not contain sulfur elements, has higher cetane number and oxygen content, is a diesel oil oxygenator with excellent performance, can greatly reduce the emission of carbon monoxide and oxynitride in the tail gas of a diesel vehicle, and does not generate sulfides. The addition of the polymer also has the advantage that the combustion performance of the diesel can be improved without modifying a vehicle engine, and the popularization value is very high.
From the reaction raw materials, the synthesis of DMMn mainly comprises a methanol/formaldehyde synthesis process, a methylal/formaldehyde process, a methanol/trioxymethylene synthesis process, a methylal/trioxymethylene process and the like. Among them, the methanol/formaldehyde process and the methylal/formaldehyde process have high difficulty in the concentration technique of the formaldehyde solution because formaldehyde directly participates in the synthesis of DMMn, wherein a large amount of H is inevitably introduced into the reaction system 2 O reaction system, the first is not favorable for the synthesis of the target product, and the second reaction product is H 2 O participates in various azeotropic systems, which is not beneficial to the separation and purification of target products.
Patent CN110078599A discloses a reactive distillation process method and a technical scheme of a device for synthesizing DMMn from methanol and high-concentration formaldehyde. The scheme takes the mixture of industrially provided product chain-terminated methanol and trioxymethylene, paraformaldehyde, gas-phase formaldehyde, formaldehyde aqueous solution or substances which provide product chain growth as raw materials, the raw materials react in a reactive distillation column, a reaction product with the polymerization degree of more than 2 is extracted from a column kettle, and then a high-purity target product DMM 3-5 is obtained through a product refining column; light components generated by the reaction, unreacted reactants and water are extracted from the top of the tower and also need to be dehydrated through vapor permeation, and the residual material flow returns to the reaction rectifying tower to participate in the reaction again.
The invention provides a production process method of polymethoxy dimethyl ether, which comprises the steps of trioxymethylene synthesis, separation, solvent recovery, methylal synthesis, separation, DMMn synthesis and separation.
We find that the prior process technical route generally has core technical problems of low selectivity and influence on yield, and in addition, the prior process technical route is accompanied with technical defects of long flow, difficult product separation, low product concentration, high production cost and the like, so that the technical progress steps of large-scale production industrialization and economy of DMMn are greatly limited.
Disclosure of Invention
The invention of the present patent application aims to simplify the process flow, and effectively improve the conversion rate and the polymerization for preparing DMM on the basis of the simplified process flow 3～8 The preparation device of the DMMn system has the technical advantages of easy operation and control, low energy consumption and low equipment investment.
The application provides a preparation facilities technical scheme of poly methoxy dimethyl ether DMMn system, its main technical content is:
a preparation device of a polyoxymethylene dimethyl ether DMMn system comprises a pre-reaction part, a catalytic distillation part and an output flow separation part, and is characterized in that,
the pre-reaction part is a pre-reactor for the polymerization reaction of raw materials and outputs an output intermediate stream;
the main body of the catalytic distillation part is a catalytic distillation tower, a rectification section, a reaction section and a stripping section are arranged in the tower from top to bottom, a high-temperature-resistant catalyst is filled in the reaction section in a modular mode, a feed inlet is formed in the upper portion of the reaction section and is connected with an output intermediate stream of the pre-reaction part, and an overhead stream and a tower kettle stream of the catalytic distillation part are connected with an output stream separation part downwards;
and a supplementary feeding hole for three methylal supplementary material flows, namely a high-level methylal supplementary material flow, a middle-level methylal supplementary material flow and a low-level methylal supplementary material flow, is arranged on the reaction section at equal intervals from the feeding hole downwards.
In the above-mentioned whole technical scheme, the described product flow separation portion includes light component separation portion, heavy component separation portion and mixing portion,
the main body of the light component separation part is a light component rectifying tower which is fed and connected with the tower top material flow of the catalytic distillation tower, the light component tower top material flow is merged into the raw material flow of the pre-reaction part, the light component tower kettle material flow and the output intermediate material flow are connected to the mixing part, and the obtained mixed material flow is connected to the feeding port of the catalytic distillation tower:
the heavy component separation part mainly comprises a heavy component rectifying tower which is fed and connected with the bottom material flow of the catalytic distillation tower, and DMM is obtained by separation at the top of the tower 3-8 The product overhead stream of (a).
In a preferred embodiment of the above integral aspect, the catalytic distillation column further comprises:
20-30 layers of trays are arranged in the rectifying section; 25-35 layers of trays are arranged in the stripping section;
the reaction section is internally provided with a modularized filling of 8-14 sections of high temperature resistant catalysts, and the 4 th, 6 th and 8 th high temperature resistant catalyst sections are respectively provided with a replenishing feed inlet of methylal replenishing material flow.
In a preferred embodiment of the above integral aspect, the catalytic distillation column further comprises:
the rectifying section is internally provided with 24 layers of tower trays; 30 layers of trays are arranged in the stripping section;
the reaction section is internally provided with a modularized filling 10 sections of high temperature resistant catalysts.
In a preferred embodiment of the above integral aspect, the catalytic distillation column further comprises:
in the reaction section, the height of each section of high-temperature resistant catalyst is 1.5-2m.
In a preferred embodiment of the above integral aspect, the catalytic distillation column further comprises:
and in the reaction section, the height of each section of the high-temperature resistant catalyst is 2m.
The application discloses a gather methoxy dimethyl ether DMMn system preparation facilities technical scheme to trioxymethylene and methylal of analytically pure are raw materials synthesis DMM 3～8 The reaction section of the catalytic distillation part adopts sectional addition of methylal as the raw material to improve the reaction concentration of the methylal raw material in each section of the reaction section, thereby greatly improving the conversion rate of trioxymethylene and polymerizing DMM 3～8 The selectivity of the DMM 3-8 is over 99.5%, the conversion rate of trioxymethylene is 100%, and the yield is over 99%, and the production and operation of the system device also have the technical advantages of greatly reducing the amount of circulating materials and being low in energy consumption, and can effectively control the reaction temperature, the reaction residence time and the reaction degree, and the operation is convenient.
Drawings
Fig. 1 is a block diagram of the system components of the present patent application.
Detailed Description
The technical content of the preparation device of the DMMn system of polymethoxy dimethyl ether in the patent application is explained in detail below.
The preparation device of the polymethoxy dimethyl ether DMMn system is shown in figure 1, and the system comprises a pre-reaction part, a catalytic distillation part and an output flow separation part.
The main body of the pre-reaction part is a pre-reactor 1, trioxymethylene and methylal are used as raw materials, the upper part of the pre-reaction part is fed by an upper pipeline 15 to carry out polymerization reaction, and the reaction conditions are as follows: the molar ratio of trioxymethylene to methylal is 1:1, the reaction temperature is 80-100 ℃, the pressure is 0.5-5Mpa, and the airspeed is 0.5-5h -1 And the bottom is connected with an output intermediate stream 7 produced by the reaction.
The main body of the catalytic distillation part is a catalytic distillation tower 2, a rectifying section, a reaction section and a stripping section are arranged in the tower from top to bottom, a feed inlet of the tower is arranged at the upper part of the reaction section, and an intermediate stream 7 produced by the pre-reactor 1 is communicated with the feed inlet of the catalytic distillation tower 2; on the reaction section, three replenishing material inlets of high-level, middle-level and low-level methylal replenishing material flows are arranged at equal intervals from the material inlet downwards in sequence; the top stream 11 and the bottom stream 14 of the column are connected downward to the separation section of the product stream.
Wherein, the rectification section is internally assembled with 20-30 layers of trays, and the optimal tray is 24 layers;
the stripping section is internally assembled with 25-35 layers of trays, and the optimal tray is 30 layers;
the reaction section is internally assembled with modularized high-temperature-resistant catalysts of 8-14 sections, the optimal modularized loading amount of the high-temperature-resistant catalysts is 10 sections, and the supplementary feed inlets 10, 9 and 8 of high-position, middle-position and low-position three methylal supplementary streams are respectively arranged at the 4 th, 6 th and 8 th modularized loading sections of the high-temperature-resistant catalysts between the feed inlets and the bottom of the reaction section.
The height of each section of the modularized high-temperature-resistant catalyst is 1.5-2m, and the optimal height is 2m.
The operation pressure of the catalytic distillation tower 2 is 0.1-0.5Mpa.
The product flow separation part comprises a light component separation part for feeding and connecting the top material flow 11 of the catalytic distillation tower 2 to perform material flow separation, a heavy component separation part for feeding and connecting the bottom material flow 14 of the catalytic distillation tower 2 to perform material flow separation, and a mixing part 6, wherein the top and bottom products of the catalytic distillation tower 2 are separated, and a part of the products are recycled until the products are separated to obtain the required products.
The light component separation part mainly comprises a light component rectifying tower 3, and is internally assembled with 50-70 trays, and the operation process conditions are as follows: the pressure is 0.1-0.5Mpa, and the reflux ratio is 1-3h -1 The separated light component overhead stream 12 mainly contains formaldehyde, low methylal and a small amount of methanol, and is merged into the raw material stream 5 of the pre-reactor 1; the light component column bottom stream 13 obtained by the separation mainly contains unreacted methylal, and is connected to the mixing section 6 through the light component column bottom stream 13 and the output intermediate stream 7, and is mixed to obtain a mixed stream 17, which is connected to the feed port of the catalytic distillation column 2 as the feed of the catalytic distillation column 2.
The heavy component separation part mainly comprises heavy component rectificationThe optimal number of trays assembled in the tower 4 is 40, and the operation process conditions are as follows: the pressure is 0.02-0.07Mpa, the reflux ratio is 0.05-0.2h -1 The column bottom material flow 14 of the catalytic distillation column 2 is taken as a feed for separation, and DMM is obtained by separation at the top of the column 3-8 To product overhead stream 15.
Through practice, the system device is operated in production and DMM 3～8 The selectivity of the catalyst is more than 99.5 percent, the conversion rate of trioxymethylene is 100 percent, and the yield is more than 99 percent.

Claims (6)

1. A preparation device of polymethoxy dimethyl ether DMMn system comprises a pre-reaction part, a catalytic distillation part and an output flow separation part, and is characterized in that,
the pre-reaction part is a pre-reactor (1) for the polymerization reaction of raw materials, and an output intermediate stream (7) is output;
the main body of the catalytic distillation part is a catalytic distillation tower (2), a rectification section, a reaction section and a stripping section are arranged in the tower from top to bottom, a high-temperature-resistant catalyst is filled in the reaction section in a modular mode, a feed inlet is formed in the upper portion of the reaction section and is connected with an output intermediate stream (7) of the pre-reaction part, and an overhead stream (11) and a tower kettle stream (14) of the catalytic distillation part are connected with an output stream separation part downwards;
and a supplementary feeding hole for three methylal supplementary material flows, namely a high-level methylal supplementary material flow, a middle-level methylal supplementary material flow and a low-level methylal supplementary material flow, is arranged on the reaction section at equal intervals from the feeding hole downwards.
2. The DMMn system preparation apparatus according to claim 1, wherein the effluent separation section comprises a light component separation section, a heavy component separation section and a mixing section (6),
the light component separation part is mainly a light component rectifying tower (3) which is fed and connected with an overhead material flow (11) of the catalytic distillation tower (2), a light component overhead material flow (12) of the light component rectifying tower is merged into a raw material flow (5) of the pre-reaction part, a light component tower kettle material flow (13) and an output intermediate material flow (7) are connected to the mixing part (6), and an obtained mixed material flow (17) is connected to a feeding hole of the catalytic distillation tower (2):
the heavy component separation part mainly comprises a heavy component rectifying tower (4) which is fed and connected with a tower kettle material flow (14) of the catalytic distillation tower (2), and DMM is obtained by separation at the top of the tower 3-8 The product overhead stream (15).
3. The DMMn system production plant according to claim 1, wherein the catalytic distillation column (2) comprises:
20-30 layers of trays are arranged in the rectifying section; 25-35 layers of trays are arranged in the stripping section;
the reaction section is internally provided with a modularized filling of 8-14 sections of high temperature resistant catalysts, and the 4 th, 6 th and 8 th high temperature resistant catalyst sections are respectively provided with a replenishing feed inlet of methylal replenishing material flow.
4. A dmem system production apparatus as claimed in claim 3, wherein said catalytic distillation column (2) comprises:
24 layers of tower trays are arranged in the rectifying section; 30 layers of trays are arranged in the stripping section;
the reaction section is internally provided with a modularized filling 10 sections of high temperature resistant catalysts.
5. The DMMn system preparation apparatus according to claim 1, 3 or 4, wherein the catalytic distillation column (2) has:
in the reaction section, the height of each section of high-temperature resistant catalyst is 1.5-2m.
6. The DMMn system preparation apparatus of claim 5, wherein the catalytic distillation column (2) comprises:
the height of each section of the high-temperature resistant catalyst in the reaction section is 2m.
CN202222515653.6U 2022-09-22 2022-09-22 Preparation device of polymethoxy dimethyl ether DMMn system Active CN218485985U (en)

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Application Number Priority Date Filing Date Title
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