CN209669096U

CN209669096U - A kind of one-step synthesis method DMM3-8Device

Info

Publication number: CN209669096U
Application number: CN201821832941.1U
Authority: CN
Inventors: 毛进池; 刘文飞; 张勇; 高永林
Original assignee: Kai Rui Environmental Protection Science And Technology Co Ltd
Current assignee: Kai Rui Environmental Protection Science And Technology Co Ltd
Priority date: 2018-11-08
Filing date: 2018-11-08
Publication date: 2019-11-22
Anticipated expiration: 2028-11-08

Abstract

The utility model discloses a kind of one-step synthesis method DMM_3‑8Device, evaporator, extraction catalytic tower, fractionating column including sequentially connected formalin, the formalin that concentration is 5-99% is after evaporator evaporation gasification, with gas phase state enter extraction catalytic tower in be dehydrated, formaldehyde trimerization, synthesize DMMn physical-chemical reaction, DMMn monomer product is obtained, then obtains target product DMM after being fractionated_3‑8.In the utility model, formalin is after gasifying, under the synergistic effect of functional membrane catalytic dehydration, using dehydration, catalyzing cooperation coupling technique, high-purity DMMn product is produced, is overcome existing: concentration technique, sulfuric acid catalysis technology, extraction, defect and drawback existing for drying technology, it is mild a process conditions have been started, process flow is short, and investment is small, quick；Efficient low-consume, novel technique route both with clean and environmental protection many advantages.

Description

A kind of one-step synthesis method DMM3-8Device

Technical field

The utility model relates to the devices of one-step synthesis method DMMn a kind of, belong to technical field of fine.

Background technique

DMMn product is universally acknowledged environment-friendly type oil dope, but its production method is considerably complicated, needs to give birth to first Metaformaldehyde, dimethoxym ethane, dimethyl ether etc. are produced, also to obtain purer raw material using technologies such as concentration, extraction, rectifying, drying Or semi-finished product, qualified DMMn finished product can be finally obtained, and this technology is: through formalin after gasifying, into one In a multifunctional membrane component tubulation bed catalytic tower for filling resin catalyst, integrates dehydration, polymerize, catalyze and synthesize, a step Synthesize a kind of new technology of DMMn.

Summary of the invention

Technical problem to be solved in the utility model be in the prior art synthesize DMMn existing for inadequate natural endowment, and The device and method of one-step synthesis method DMMn a kind of are provided, existing water absorption techniques, concentration technique, sulfuric acid catalysis skill are overcome Defect and drawback existing for art, extraction drying technology etc., having started one, process conditions are mild, process flow is short, investment is small, see Imitate fast, efficient low-consume, clean and environmental protection method and device.

To achieve the goals above, the utility model adopts the following technical solution:

A kind of one-step synthesis method DMM_3-8Device, evaporator including sequentially connected formalin, extraction catalysis are anti- Tower, fractionating column are answered, the formalin that concentration is 5-99% enters extraction with gas phase state and urge after evaporator evaporation gasification It is dehydrated in change reaction tower, formaldehyde trimerization, the physical-chemical reaction for synthesizing DMMn, obtains DMMn series monomers product, then pass through Target product DMM is obtained after fractionation_3-8；It is characterized by:

The evaporator of the formalin, top is equipped with discharge port 1A, bottom is equipped with feed inlet 1B, in side wall on Portion is equipped with outlet 1C, the middle and lower part of another side wall is equipped with import 1D, in which: feed inlet 1B and the dress for being capable of providing formalin It sets and is connected；Outlet 1C is connected with the system for being capable of providing condensed water, and is connected with the import for the system for being capable of providing condensed water It connects；Import 1D is connected with the device for being capable of providing steam, and is connected with the outlet for the device for being capable of providing steam；

The extraction catalytic tower, top is equipped with gaseous phase outlet 2B, bottom is equipped with discharge port 2D, and side wall upper part is equipped with First refluxing opening 2C, middle part are equipped with the second refluxing opening 2E, middle and lower part is equipped with discharge outlet 2F, bottom sidewall is equipped with feed inlet 2A；Its In: feed inlet 2A is connected with the discharge port 1A of evaporator；Gaseous phase outlet 2B is connected with condenser I, return tank I, reflux in turn I is pumped, the pump discharge of reflux pump I is connected with the second refluxing opening 2E；Discharge outlet 2F is connected with sewage disposal system, the water body of removing It is drained into sewage disposal system and is handled through discharge outlet 2F；The second refluxing opening 2E also be capable of providing fresh first The device of acetal (M1) is connected；

The fractionating column, top is equipped with gaseous phase outlet 3B, bottom is equipped with discharge port 3D, is equipped with feed inlet in the middle part of side wall 3A, side wall middle and upper part are equipped with third refluxing opening 3C, in which: feed inlet 3A is connected with the discharge port 2D of extraction catalytic tower； Gaseous phase outlet 3B is connected with condenser II, return tank II, reflux pump II in turn；The pump discharge of reflux pump II is divided into two-way, all the way It is connected with third refluxing opening 3C, another way is connected with the first refluxing opening 2C of extraction catalytic tower；Bottom discharge port 3D It is connected with the device for acquiring or receiving finished product DMMn.

In above-mentioned technical proposal, the extraction catalytic tower, side wall lower section is equipped with reboiler I.

In above-mentioned technical proposal, the extraction catalytic tower, internals include: demister, distributor, filler assembly； The top in the reaction tower be equipped with demister, its have distributor；Multistage filler assembly is loaded under the distributor, and Redistributor is designed between each section of filler assembly；The filler assembly and the adjacent distributor, the redistribution Device connection；

The filler assembly is multifunction module component: in column including multiple vertically arranged tubulation arrangements up and down Pipe bed is fixed by tube sheet, and the tubulation whole body is provided with multiple apertures, the function up and down that insertion is fired into the tubulation Pipe, functional membrane made of the compound firing of function pipe internal surface, the function pipe is interior to fill filler；

The upper and lower side setting sealing material in the gap between the tubulation and function pipe, which seals, to be fixed；The filler assembly with The adjacent distributor, the redistributor pass through function pipe connection and constitute reaction channel；It is the filler assembly, described Redistributor constitutes dehydration runner with described react between tower side wall；

The reaction tower, top is equipped with the gaseous phase outlet 2B, bottom is equipped with the discharge port 2D, the reaction The tower bottom side wall setting feed inlet 2A, the filler assembly position of the bottom row described in reaction tower side wall setting Mouth of a river 2F, the reaction tower topmost distributor are connected to the first refluxing opening 2C being arranged on the reaction tower side wall；Position Redistributor in the middle part of the reaction tower is connected to the second refluxing opening 2E being arranged on the reaction tower side wall；

Tube sheet described in the bottom is closed water-accepting board, and each tube sheet more than bottom is connected to by downspout, most Be provided with vacuum orifice on the high-rise tube sheet, and connect external pumped vacuum systems, it is outside each section of tubulation, connected by downspout It is pumped into negative pressure in logical all spaces.

The diameter of the apertureFor 1-50mm.

The function pipe Ceramics material sintering is made；The functional membrane Ceramics class material, diatom earthen materia, In ZSM-5, SAPO-34 or zeolite molecular sieve any one with the function pipe internal surface is compound is made.

The filler is catalyst module, produces poly- methoxy with full chamber bed technology in patent CN201620189748.5 The module catalyst of base dimethyl ether: the module catalyst includes catalyst, wire mesh, wire mesh corrugated plating, the mould Block catalyst is installed between wire mesh described in two panels by the wire mesh, the spaced and parallel setting of wire mesh corrugated plating The catalyst granules forms catalyst layer, and the catalyst granules in the catalyst layer is by the wire mesh wave Card apart from；Catalyst layer interval setting in the module catalyst.

It is that stainless steel ripple silk net arranges inside the demister, redistributor, the redistributor is equipped with The flow-guiding mouth of multiple connection function pipes；The distributor is that stainless-steel sheet constitutes and is equipped with multiple connection function pipes Flow-guiding mouth.

The sealing material selects polytetrafluoro gasket or metal wound gasket, antiseptic rubber pad.

In above-mentioned technical proposal, the filler assembly is loaded by section, and loadings are N sections, 1≤N≤100, every section of height Spend 1-3m；Every section of filling function pipe 253 is M root, 1≤M≤5000；Every root canal diameter is D, 5≤D≤200cm.

In above-mentioned technical proposal, the fractionating column, side wall lower section is equipped with reboiler II.

In above-mentioned technical proposal, the fractionating column, tower is interior to be filled with tower internals, and tower internals is structured packing, in column plate Any one；If structured packing, filling number of segment is N, and 1≤N≤100, every section of height is 1-3 meters；If column plate, then manage It is M, 1≤M≤100 by plate number.

The utility model also provides the method for one-step synthesis method DMMn a kind of, comprising the following steps:

(1) vaporization reaction: formalin is entered in evaporator by feed inlet 1B, under the heated condition of low-pressure steam It is vaporized distillation, obtains gasification formalin；Gasification formalin is exported by discharge port 1A and is imported by feed inlet 2A Into extraction catalytic tower；

(2) polymerize, synthesize, dehydration: gasification formalin obtained in step (1) imported into extraction catalysis reaction In tower (2), it is polymerize, is synthesized, being dehydrated a variety of physical-chemical reactions simultaneously under the catalytic action of catalyst in tower:

1. polymerization reaction: gasification formalin is imported into the multifunctional membrane inside extraction catalytic tower by feed inlet 2A In the tube side of block assembly, polymerization reaction occurs under the catalytic action of functional membrane, generates metaformaldehyde aqueous solution；Not reaction completely Gasification formalin continue uplink, and generate metaformaldehyde aqueous solution also with air-flow continue uplink；

2. synthetic reaction: the dimethoxym ethane from bottom to top that the metaformaldehyde aqueous solution of uplink is added from the second refluxing opening 2E (M1) absorption is extracted, and carries out synthetic reaction under the catalytic action of the module catalyst in multifunctional membrane block assembly, is generated Polymethoxy dimethyl ether DMM_2-8；

The formalin of the gasification of uplink also extracts absorption by top-down dimethoxym ethane (M1), equally in module Synthetic reaction is carried out under the catalytic action of catalyst, also generates polymethoxy dimethyl ether DMM_2-8；

Dimethoxym ethane is reacted with metaformaldehyde generates polymethoxy dimethyl ether DMM_2-8；But dimethoxym ethane can also be reacted with formaldehyde Generate DMM_2-8, only conversion ratio is very low；

3. dehydration: gasification formalin will continue to carry out dehydration also under the dehydration of functional membrane to make first Aldehyde concentration is gradually increased, also can gradually downlink, can make the gasification formalin concentration of uplink lower and lower in this way, and uplink Gasification formalin also continues carrying out synthetic reaction with dimethoxym ethane (M1), thorough so as to cause the formaldehyde reaction of uplink；Under and The formalin capable, concentration increases after dehydration continues polymerization reaction, or continues to be synthesized with dimethoxym ethane (M1) Reaction；

The metaformaldehyde aqueous solution of generation will continue to carry out dehydration also under the dehydration of functional membrane to make trimerization first Aldehyde concentration is gradually increased, also can gradually downlink, can make the metaformaldehyde concentration of aqueous solution of uplink lower and lower in this way, the three of uplink Polyformaldehyde also continues carrying out synthetic reaction with dimethoxym ethane (M1), thorough so as to cause the metaformaldehyde reaction of uplink；And downlink, The metaformaldehyde that concentration increases after dehydration also also continues with synthetic reaction with dimethoxym ethane (M1)；

So in cycles carry out polymerization reaction, synthetic reaction and dehydration simultaneously in extraction catalytic tower； The low boiling point of dimethoxym ethane (M1) is reacted remaining dimethoxym ethane (M1) and is gradually gone upward at the demister of tower top, and demister will be carried secretly Mist thoroughly retain, clean dimethoxym ethane be discharged by gaseous phase outlet 2B after followed by condenser I, return tank I, reflux pump I, Then it is back in extraction catalytic tower and is recycled by the second refluxing opening 2E；The head product generated due to synthetic reaction DMM_2-8Density is big, and gradually downlink eventually falls into tower bottom, head product DMM_2-8It is discharged by discharge port 2D and is imported by feed inlet 3A Into fractionating column；The water body of dehydration removing, under the dehydration of functional membrane and the suction function of shell side, by discharge outlet 2F It is discharged outside tower；

(3) finished product is fractionated: head product DMM_2-8After entering fractionating column, it is fractionated, is obtained under reboiler II heated condition To gas phase and liquid phase；Gas phase is DMM₂(M2), it is discharged by gaseous phase outlet 3B, followed by condenser II, return tank II, reflux pump After II, a part is back in fractionating column by third refluxing opening 3C, and another part is back to from top to bottom by the first refluxing opening 2C It extracts in catalytic tower；The DMM that the formalin of uplink is returned from top to bottom in step (2)₂It extracts and absorbs, and Synthetic reaction is also carried out under the catalytic action of module catalyst, generates DMM_3-8, the synthetic reaction also with its in step (2) He carries out at physical-chemical reaction simultaneously；Liquid phase is high-purity DMM_3-8, it is discharged and is collected by discharge port 3D.

In above-mentioned technical proposal, in step (1), the operating condition of the evaporator are as follows: temperature: 90-120 DEG C, pressure For normal pressure and micro-positive pressure.

In above-mentioned technical proposal, in step (1), enter in the formalin in evaporator, the mass concentration of formaldehyde For 5-99%；

In above-mentioned technical proposal, in step (2), the gasification formalin is imported into extraction catalytic tower, Feed space velocities are 0.1-5.0h^-1。

In above-mentioned technical proposal, in step (2), the additional amount of the dimethoxym ethane (M1) is rubbing for the metaformaldehyde generated 1-10 times of that amount.

In above-mentioned technical proposal, in step (2), dimethoxym ethane (M1) is back to extraction catalysis reaction by the second refluxing opening 2E Tower, reflux ratio 0.5-10.0.

In above-mentioned technical proposal, in step (2), when polymerization reaction, the operating condition in catalytic tower is extracted are as follows: tower top 50-90 DEG C of temperature, 0.1-0.5MPa, 60-150 DEG C of bottom temperature, 0.1-1.0MPa.

In above-mentioned technical proposal, in step (2), synthetic reaction: the operating condition in extraction catalytic tower are as follows: tower top temperature Spend 50-90 DEG C, 0.1-0.5MPa, 60-150 DEG C of bottom temperature, 0.1-1.0MPa.

In above-mentioned technical proposal, in step (2), when dehydration, catalytic tower shell side vacuum cavitations are extracted are as follows:- 0.09-0.2Mpa。

In above-mentioned technical proposal, in step (2), the functional membrane have catalysis, dehydration, be ceramic-like materials, Any one in diatom earthen materia, ZSM-5, SAPO-34 or zeolite molecular sieve.

In above-mentioned technical proposal, in step (2), the module catalyst, in patent CN201620189748.5 With the module catalyst of full chamber bed technology production polymethoxy dimethyl ether, active catalyst therein is solid acid catalyst, excellent Resin catalyst is selected, can also be molecular sieve, heteropllyacids, Supported superacid class.

In above-mentioned technical proposal, in step (3), the fractionating column, operating condition are as follows: tower top temperature: 50-150 DEG C；Tower Bottom temperature: 60-250 DEG C；Operating pressure: -0.09-1.0Mpa.

In above-mentioned technical proposal, in step (3), gas phase DMM₂It is back in fractionating column, reflux ratio 0.1-2.0.

In above-mentioned technical proposal, in step (3), gas phase DMM₂It is back in extraction catalytic tower, reflux ratio is 0.5- 3.0。

The advantages of the technical program is: formalin is made after gasifying in the collaboration of function membrane module catalytic dehydration Under, using dehydration, catalyzing cooperation coupling technique, high-purity DMMn product is produced, is overcome existing: concentration technique, sulfuric acid catalysis Technology, extraction, defect and drawback existing for drying technology, have started that a process conditions are mild, and process flow is short, invest it is small, It is quick；Efficient low-consume, novel technique route both with clean and environmental protection many advantages.

Detailed description of the invention

Fig. 1 is the overall structure figure of the device of the utility model one-step synthesis method DMMn；

Fig. 2 is the structural schematic diagram of the extraction catalytic tower in Fig. 1；

Fig. 3 be Fig. 1 in extraction catalytic tower in individually tubulation longitudinal plane structure schematic diagram；

Fig. 4 is the tubulation function tube thickness section structure diagram of tubulose function membrane module；

Fig. 5 is the cross section schematic cross-sectional view of the filler assembly of catalytic tower；

Fig. 6 is the section structure diagram of module catalyst；

Fig. 7 is the structural schematic diagram of the longitudinal cross-section of catalytic tower.

Wherein: 1 is the evaporator of formalin；2 be extraction catalytic tower, and 20 be demister, and 211 be the first reflux Mouthful 2C, 212 be gaseous phase outlet 2B, 213 be feed inlet 2A, 214 is discharge port 2D, 215 be discharge outlet 2F, 216 second refluxing openings 2E, 23 be filler assembly, and 251 be tubulation, and 252 be aperture, and 253 be function pipe, and 254 be filler, and 255 be functional membrane, and 26 is again Distributor, 27 be tube sheet, and 28 be distributor, 40- module catalyst, 401- catalyst layer, 402- wire mesh, 403- wire Net corrugated plating；50- downspout；3 be fractionating column, 4 is condenser I, 5 is return tank I, 6 is reflux pump I, 7 is condenser II, 8 is Return tank II, 9 be reflux pump II, 10 be reboiler I, 11 be reboiler II.

Specific embodiment

The specific embodiments of technical solutions of the utility model is described in detail below, but the utility model be not limited to Lower description content:

The utility model provides the device of one-step synthesis method DMMn a kind of first, including sequentially connected formalin Evaporator 1, extraction catalytic tower 2, fractionating column 3, concentration be 5-99% formalin through evaporator evaporation gasification after, with Gas phase state enter extraction catalytic tower in be dehydrated, formaldehyde trimerization, synthesize DMMn physical-chemical reaction, obtain DMMn series monomers product, then target product DMM is obtained after being fractionated_3-8；As shown in figs. 1-7:

The evaporator 1 of the formalin, top is equipped with discharge port 1A, bottom is equipped with feed inlet 1B, in side wall Top is equipped with outlet 1C, the middle and lower part of another side wall is equipped with import 1D, in which: feed inlet 1B and is capable of providing formalin Device is connected；Outlet 1C is connected with the system for being capable of providing condensed water, and the import phase with the system for being capable of providing condensed water Connection；Import 1D is connected with the device for being capable of providing steam, and is connected with the outlet for the device for being capable of providing steam；

The extraction catalytic tower 2, top is equipped with gaseous phase outlet 2B, bottom is equipped with discharge port 2D, and side wall upper part is set There are the first refluxing opening 2C, middle part to be equipped with the second refluxing opening 2E, middle and lower part is equipped with discharge outlet 2F, bottom sidewall is equipped with feed inlet 2A； Wherein: feed inlet 2A is connected with the discharge port 1A of evaporator；Gaseous phase outlet 2B is connected with condenser I 4, return tank I in turn 5, reflux pump I 6, the pump discharge of reflux pump I 6 are connected with the second refluxing opening 2E；Discharge outlet 2F is connected with sewage disposal system, The water body of removing is drained into sewage disposal system through discharge outlet 2F and is handled；The second refluxing opening 2E also with can mention It is connected for the device of fresh dimethoxym ethane (M1)；

The fractionating column 3, top is equipped with gaseous phase outlet 3B, bottom is equipped with discharge port 3D, is equipped with feed inlet in the middle part of side wall 3A, side wall middle and upper part are equipped with third refluxing opening 3C, in which: feed inlet 3A is connected with the discharge port 2D of extraction catalytic tower； Gaseous phase outlet 3B is connected with condenser II 7, return tank II 8, reflux pump II 9 in turn；The pump discharge of reflux pump II is divided into two Road is connected with third refluxing opening 3C all the way, and another way is connected with the first refluxing opening 2C of extraction catalytic tower；Bottom goes out Material mouth 3D is connected with the device for acquiring or receiving finished product DMMn；

In above-mentioned technical proposal, the extraction catalytic tower, side wall lower section is equipped with reboiler I 10.

In above-mentioned technical proposal, the extraction catalytic tower, internals include: demister 20, distributor 28, filler group Part 23: the top in the reaction tower be equipped with demister 20, its have distributor 28；The distributor 28 is lower to load multistage Filler assembly 23, and redistributor 26 is designed between each section of filler assembly 23；The filler assembly 23 and adjacent institute State distributor 28, the redistributor 26 is connected to；

The filler assembly 23 is multifunction module component: including multiple vertically arranged 251 rows of tubulation up and down It arranges into tubulation bed to be fixed by tube sheet 27,251 whole body of tubulation is provided with multiple apertures 252, and insertion is fired into the tubulation 251 Function pipe 253 up and down, functional membrane 255 made of the compound firing of 253 inner surface of function pipe, the function pipe Filler 254 is filled in 253；

The upper and lower side setting sealing material in the gap between the tubulation 251 and function pipe 253, which seals, to be fixed；The filler Component 23 is connected to by the function pipe 253 with the adjacent distributor 28, the redistributor 26 and constitutes reaction channel；Institute It states and constitutes dehydration runner between 2 side wall of filler assembly 23, the redistributor 26 and the reaction tower；

The reaction tower, top is equipped with the gaseous phase outlet 2B 212, bottom is equipped with the discharge port 2D 214, The reaction tower bottom sidewall setting feed inlet 2A 213,23 position of the filler assembly of bottom is in reaction tower side The wall setting discharge outlet 2F 215, the reaction tower topmost distributor be connected on the reaction tower side wall be arranged it is described The first refluxing opening 2C 211；Redistributor 26 in the middle part of the reaction tower is connected to the be arranged on the reaction tower side wall Two refluxing opening 2E 216；

Tube sheet 27 described in the bottom is closed water-accepting board, and each tube sheet 27 more than bottom is connected by downspout 50 It is logical, be provided with vacuum orifice on the top tube sheet 27, and connect external pumped vacuum systems, it is outside each section of tubulation 251, Negative pressure is pumped by all spaces that downspout 50 is connected to；

The diameter of the aperture 252For 1-50mm；

253 Ceramics material of the function pipe sintering is made；The 255 Ceramics class material of functional membrane, diatomite Any one in class material, ZSM-5, SAPO-34 or zeolite molecular sieve is made with the compound firing of 253 inner surface of function pipe At；

The filler 254 is catalyst module 40, with being produced in patent CN201620189748.5 with full chamber bed technology The module catalyst of polymethoxy dimethyl ether: the module catalyst 40 includes catalyst, wire mesh 402, wire mesh wave Card 403, the module catalyst is by the wire mesh 402, the spaced and parallel setting of wire mesh corrugated plating 403, two panels The catalyst granules is installed between the wire mesh 402 forms catalyst layer 401, and the institute in the catalyst layer 401 State catalyst granules by the wire mesh corrugated plating 403 apart from；The catalysis in the module catalyst 40 The setting of the interval of oxidant layer 401；

It is that stainless steel ripple silk net arranges inside the demister 20, redistributor 26, the redistributor 26 It is equipped with the flow-guiding mouth of multiple connection function pipes 253；The distributor 28 is that stainless-steel sheet constitutes and is equipped with multiple companies Lead to the flow-guiding mouth of the function pipe 253；

The sealing material selects polytetrafluoro gasket or metal wound gasket, antiseptic rubber pad；

The filler assembly is loaded by section, and loadings are N sections, 1≤N≤100, every section of height 1-3m；Every section of filling Function pipe 253 is M root, 1≤M≤5000；Every root canal diameter is D, 5≤D≤200cm.

In above-mentioned technical proposal, the fractionating column 3, side wall lower section is equipped with reboiler II 11；Filled in tower in tower Part, tower internals are structured packing, any one in column plate；If structured packing, filling number of segment is N, 1≤N≤100, often Duan Gaodu is 1-3 meters；If column plate, then number of theoretical plate is M, 1≤M≤100.

(1) vaporization reaction: formalin is entered in evaporator (1) by feed inlet 1B, in the heating shape of low-pressure steam It is vaporized distillation under state, obtains gasification formalin；The formalin that gasifies is exported by discharge port 1A and by feed inlet 2A It imported into extraction catalytic tower 2；

1. polymerization reaction: gasification formalin is imported into the multifunctional membrane inside extraction catalytic tower by feed inlet 2A In the tube side of component, polymerization reaction occurs under the catalytic action of functional membrane 255, generates metaformaldehyde aqueous solution；It is completely not anti- The formalin for the gasification answered continues uplink, and the metaformaldehyde aqueous solution generated continues uplink also with air-flow；

2. synthetic reaction: the dimethoxym ethane from bottom to top that the metaformaldehyde aqueous solution of uplink is added from the second refluxing opening 2E (M1) absorption is extracted, and carries out synthetic reaction under the catalytic action of the module catalyst 40 in multifunctional membrane component, is generated Polymethoxy dimethyl ether DMM_2-8；

So in cycles carry out polymerization reaction, synthetic reaction and dehydration simultaneously in extraction catalytic tower； The low boiling point of dimethoxym ethane (M1) is reacted remaining dimethoxym ethane (M1) and is gradually gone upward at the demister 12 of tower top, and demister will press from both sides The mist of band thoroughly retains, clean dimethoxym ethane by gaseous phase outlet 2B be discharged after followed by condenser I 4, return tank I 5, return Stream pump I 6, is then back in extraction catalytic tower by the second refluxing opening 2E and is recycled；Due at the beginning of synthetic reaction generation Product DMM_2-8Density is big, and gradually downlink eventually falls into tower bottom, head product DMM_2-8It is discharged by discharge port 2D and by feed inlet 3A It imported into fractionating column 3；The water body of dehydration removing, under the dehydration of functional membrane and the suction function of shell side, by arranging Mouth of a river 2F is discharged outside tower；

(3) finished product is fractionated: head product DMM_2-8After entering fractionating column, divided under 11 heated condition of reboiler II It evaporates, obtains gas phase and liquid phase；Gas phase is DMM₂(M2), it is discharged by gaseous phase outlet 3B, followed by condenser II 7, return tank II 8, after reflux pump II 9, a part is back in fractionating column by third refluxing opening 3C, and another part is by the first refluxing opening 2C from upper It is back under and in extraction catalytic tower；The DMM that the formalin of uplink is returned from top to bottom in step (2)₂Extracted It takes and absorbs, and also carry out synthetic reaction under the catalytic action of module catalyst, generate DMM_3-8, the synthetic reaction also with step Suddenly other physical-chemical reactions in (2) carry out simultaneously；Liquid phase is high-purity DMM_3-8, it is discharged and is collected by discharge port 3D.

The utility model is further elaborated below with reference to specific embodiment:

Embodiment 1:

A kind of method of one-step synthesis method DMMn, comprising the following steps:

(1) vaporization reaction: the formalin that 100g content is 60% is entered in evaporator (1) by feed inlet 1B, 95-105 DEG C of evaporating temperature of control obtains gasification formalin；The formalin that gasifies is exported by discharge port 1A and by feeding Mouth 2A is imported into extraction catalytic tower (2)；

(2) polymerize, synthesize, dehydration: the gasification formalin of 100g obtained in step (1) imported into extraction catalysis In reaction tower (2), it is polymerize, is synthesized, being dehydrated a variety of physical-chemical reactions simultaneously under the catalytic action of catalyst in tower:

1. polymerization reaction: the Feed space velocities of 100g gasification formaldehyde are 0.2h^-1, in 70-90 DEG C of tower top temperature, 0.1MPa, tower Under conditions of 80-100 DEG C of kettle temperature degree, 0.2MPa, polymerization reaction is carried out under the catalytic action of functional membrane, generates the three of 30g Polyformaldehyde, remaining 30g formaldehyde unreacted；

2. synthetic reaction: the metaformaldehyde aqueous solution of the 30g of uplink be added from the second refluxing opening 2E from bottom to top The dimethoxym ethane (M1) of 180g extracts absorption, in 70-90 DEG C of tower top temperature, 0.1MPa, 80-100 DEG C of bottom temperature, 0.2MPa Under the conditions of, carry out synthetic reaction under the catalytic action of module catalyst, generate 45g polymethoxy dimethyl ether DMM3-8；

The formalin of the 30g gasification of uplink, also extracts absorption by 145g dimethoxym ethane (M1) from bottom to top, equally Synthetic reaction is carried out under the catalytic action of module catalyst, also generates polymethoxy dimethyl ether 4.5gDMM2-8, and efficiency is lower；

The aqueous solution of the 27g Formaldehyde Gasification of uplink, can also by from first answer back 2C flow back top-down 50g DMM2 (flowing back in step (3), not additionally add) extracts absorption, and carries out under the catalytic action of module catalyst Synthetic reaction generates 40.5DMM2-8；

3. dehydration: being cased with tubulation 251 in the outside of function pipe 253, being provided with diameter all over the body is 1mm aperture, facilitates institute Except the timely discharge system of the water of abjection, and control operating pressure: -0.03Mpa；Deviate from 40g water, is arranged from 2F mouthfuls of discharge outlet Out.

The low boiling point of dimethoxym ethane (M1) is reacted remaining dimethoxym ethane (M1) and is gradually gone upward at the demister (12) of tower top, Demister thoroughly retains the mist of entrainment, clean dimethoxym ethane by gaseous phase outlet 2B be discharged after followed by condenser I (4), Return tank I (5), reflux pump I (6) are then back in extraction catalytic tower by the second refluxing opening 2E and recycle (reflux ratio It is 1)；Since the head product DMM2-8 density that synthetic reaction generates is big, and gradually downlink eventually falls into tower bottom, head product DMM2-8 It is discharged by discharge port 2D and is imported into fractionating column (3) by feed inlet 3A.

(3) finished product is fractionated: after head product DMM2-8 enters fractionating column (3), under reboiler II (11) heated condition, In Tower top temperature: 90-120 DEG C；Column bottom temperature: 110-150 DEG C；Operating pressure: it is fractionated under 0.1-0.20Mpa, obtains gas phase And liquid phase；

Gas phase is DMM2, is discharged by gaseous phase outlet 3B, obtains liquid after condenser II (7) condensation, flows through return tank II (8), after reflux pump II (9), a part is back in fractionating column by third refluxing opening 3C, and control reflux ratio is 0.2, another part It is back in extraction catalytic tower and is recycled by the first refluxing opening 2C；Liquid phase is high-purity DMM3-8, is arranged by discharge port 3D It is out and collected.

It is nearly 100% that the yield of finished product DMM3-8, which is greater than 95% or more, purity,.

In the present embodiment, the design for extracting catalytic dehydration reaction tower (2) is as follows: functional membrane block assembly is loaded by section in tower, Its loadings is 3 sections, every section of height 1m；Every section of filling tubulose functional membrane block assembly is 5；Every root canal diameter is 5cm, between every section It is designed with redistributor, tower is topmost that demister is equipped on the first refluxing opening 2C, and every root canal is provided with such as patent CN201620189748.5 module catalyst；Demister, redistributor, material are made of stainless steel ripple silk net； It is cased with tubulation 251 in the outside of function pipe 253, being provided with diameter all over the body is 1mm aperture, facilitates the timely discharge system of deviate from water Except.

In the present embodiment, the material that functional membrane 255 is selected is ZSM-5, and being formed by molecule internal orifice dimension is 2-3x10^-1Nm, Function pipe 253 is fired into ceramic tube by ceramics 75, wherein Al₂O₃Content is 75%, remaining component is conventionally, ceramics 75 are existing Material, can be with outsourcing；Tubulation is metal tube.

In the present embodiment, the active catalyst in module catalyst is D006 resin catalyst.

In the present embodiment, fractionating column (3), tower is provided with tower internals, and tower internals is stainless steel corrugated plate regular packing, dress It is 2 that fill out number of segment, which be N, and every section of height is 2 meters；

Embodiment 2:

A kind of method of one-step synthesis method DMMn, method, step are same as Example 1, except that dimethoxym ethane Inlet amount be increased to the amounts of 4 times of moles of formaldehyde, it is nearly 100% that the yield of finished product, which remains at 95% or more, purity still,.

Examples detailed above is only the technical conception and technical characteristics for illustrating the utility model, can not limit this reality with this With novel protection scope.The equivalent transformation or modification that all essence according to the present utility model is done, should all cover in this reality Within novel protection scope.

Claims

1. a kind of one-step synthesis method DMM_3-8Device, evaporator (1) including sequentially connected formalin, extraction catalysis Reaction tower (2), fractionating column (3), the formalin that concentration is 5-99% are entered after evaporator evaporation gasification with gas phase state It is dehydrated into extraction catalytic tower, formaldehyde trimerization, the physical-chemical reaction for synthesizing DMMn, obtains the production of DMMn series monomers Product, then target product DMM is obtained after being fractionated_3-8；It is characterized by:

The evaporator (1) of the formalin, top is equipped with discharge port 1A, bottom is equipped with feed inlet 1B, in side wall on Portion is equipped with outlet 1C, the middle and lower part of another side wall is equipped with import 1D, in which: feed inlet 1B and the dress for being capable of providing formalin It sets and is connected；Outlet 1C is connected with the system for being capable of providing condensed water, and is connected with the import for the system for being capable of providing condensed water It connects；Import 1D is connected with the device for being capable of providing steam, and is connected with the outlet for the device for being capable of providing steam；

The extraction catalytic tower (2), top is equipped with gaseous phase outlet 2B, bottom is equipped with discharge port 2D, and side wall upper part is equipped with First refluxing opening 2C, middle part are equipped with the second refluxing opening 2E, middle and lower part is equipped with discharge outlet 2F, bottom sidewall is equipped with feed inlet 2A；Its In: feed inlet 2A is connected with the discharge port 1A of evaporator (1)；Gaseous phase outlet 2B is connected with condenser I (4), return tank I in turn (5), (6) reflux pump I, the pump discharge of reflux pump I (6) are connected with the second refluxing opening 2E；Discharge outlet 2F is connected with sewage treatment System, the water body of removing is drained into sewage disposal system through discharge outlet 2F to be handled；The second refluxing opening 2E also with The device for being capable of providing fresh dimethoxym ethane (M1) is connected；

The fractionating column (3), top is equipped with gaseous phase outlet 3B, bottom is equipped with discharge port 3D, is equipped with feed inlet 3A in the middle part of side wall, Side wall middle and upper part is equipped with third refluxing opening 3C, in which: feed inlet 3A is connected with the discharge port 2D of extraction catalytic tower；Gas phase Outlet 3B is connected with condenser II (7), return tank II (8), reflux pump II (9) in turn；The pump discharge of reflux pump II (9) is divided into two Road is connected with third refluxing opening 3C all the way, and another way is connected with the first refluxing opening 2C of extraction catalytic tower；Bottom goes out Material mouth 3D is connected with the device for acquiring or receiving finished product DMMn.

2. the apparatus according to claim 1, which is characterized in that the extraction catalytic tower (2), internals include:

Demister (20), distributor (28), filler assembly (23)；The top in the reaction tower be equipped with demister (20), its Have distributor (28)；Multistage filler assembly (23) are loaded under the distributor (28), and each section of filler assembly (23) Between be designed with redistributor (26)；The filler assembly (23) and the adjacent distributor (28), the redistributor (26) it is connected to；

The filler assembly (23) is multifunction module component: including multiple vertically arranged tubulation (251) rows up and down It is fixed by tube sheet (27) to arrange into tubulation bed, the tubulation (251) is provided with multiple apertures (252) all over the body, tubulation (251) interpolation Enter the function pipe (253) up and down being fired into, functional membrane made of the compound firing of function pipe (253) inner surface (255), filler (254) are filled in the function pipe (253)；

The upper and lower side setting sealing material in the gap between the tubulation (251) and function pipe (253), which seals, to be fixed；The filler Component (23) is connected to composition instead by the function pipe (253) with the adjacent distributor (28), the redistributor (26) Answer channel；Dehydration runner is constituted between the filler assembly (23), the redistributor (26) and the reaction tower (2) side wall；

The reaction tower, top is equipped with the gaseous phase outlet 2B (212), bottom is equipped with the discharge port 2D (214), institute The reaction tower bottom sidewall setting feed inlet 2A (213) is stated, the filler assembly (23) position of bottom is in reaction tower The side wall setting discharge outlet 2F (215), the reaction tower topmost distributor, which is connected to, to be arranged on the reaction tower side wall The first refluxing opening 2C (211)；Redistributor (26) in the middle part of the reaction tower is connected on the reaction tower side wall The second refluxing opening 2E (216) being arranged；

Tube sheet described in the bottom (27) is closed water-accepting board, and each tube sheet (27) more than bottom is by downspout (50) It is connected to, vacuum orifice is provided on the top tube sheet (27), and connect external pumped vacuum systems, each section of tubulation (251) outside, by downspout (50) be connected to all spaces be pumped into negative pressure.

3. the apparatus of claim 2, which is characterized in that the filler (254) is catalyst module (40), including is urged Agent, wire mesh (402), wire mesh corrugated plating (403), the module catalyst (40) is by the wire mesh (402), wire mesh corrugated plating (403) spaced and parallel setting installs the catalysis between wire mesh (402) described in two panels Agent particle forms catalyst layer (401), and the catalyst granules in the catalyst layer (401) is by the wire mesh wave Card (403) apart from；The catalyst layer (401) in the module catalyst (40) is spaced setting.

4. the apparatus of claim 2, which is characterized in that be inside the demister (20), redistributor (26) Stainless steel ripple silk net arranges, and the redistributor (26) is equipped with the flow-guiding mouth of multiple connection function pipes (253)； The distributor (28) is the flow-guiding mouth that stainless-steel sheet constituted and be equipped with multiple connection function pipes (253).

5. the apparatus of claim 2, which is characterized in that the sealing material selects polytetrafluoro gasket or metal to twine Around pad, antiseptic rubber pad.

6. the apparatus of claim 2, which is characterized in that the filler assembly is loaded by section, loadings N Section, 1≤N≤100, every section of height 1-3m, every section of filling function pipe (253) are M root, 1≤M≤5000, and every root canal diameter is D, 5≤ D≦200cm。

7. the apparatus of claim 2, which is characterized in that the diameter of the aperture (252)For 1-50mm.

8. the apparatus according to claim 1, which is characterized in that the extraction catalytic tower (2), the installation of side wall lower section There are reboiler I (10)；The fractionating column (3), side wall lower section are equipped with reboiler II (11).

9. the apparatus according to claim 1, which is characterized in that the fractionating column (3), tower is interior to be filled with tower internals, tower Internals are structured packing, any one in column plate；If structured packing, filling number of segment is N, 1≤N≤100, every section of height It is 1-3 meters；If column plate, then number of theoretical plate is M, 1≤M≤100.