CN206143094U - Extraction device who gathers methoxy dimethyl ether reactant - Google Patents
Extraction device who gathers methoxy dimethyl ether reactant Download PDFInfo
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- CN206143094U CN206143094U CN201621145772.5U CN201621145772U CN206143094U CN 206143094 U CN206143094 U CN 206143094U CN 201621145772 U CN201621145772 U CN 201621145772U CN 206143094 U CN206143094 U CN 206143094U
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Abstract
The utility model discloses an extraction device who gathers methoxy dimethyl ether reactant, device be including pre -heater I, pre -heater II and the extraction tower that connects gradually, dehydration column, distillation column, fan and material pans, and pre -heater I, pre -heater II link to each other with the inlet of extraction tower respectively, and the device that polymerization is carried out to the discharge gate and the outside of material pans links to each other, the concentration dewatering of formaldehyde is carried out with the formalin of commercially available low price through physics extraction, vacuum rectification's method to this method to distilling through the formaldehyde to in the extractant and preparing aqueous pure formaldehyde gas hardly, this formaldehyde gas pressurizes through booster fan again, and the effective separation of formaldehyde with the extractant had both been guaranteed in dissolving the working solution to the pressure, and the raw materials that gathers the methoxy dimethyl ether, kill many birds with one stone are prepared to the working solution that has absorbed formaldehyde gas moreover.
Description
Technical field
This utility model is related to a kind of extraction preparation method and device of polymethoxy dimethyl ether reaction raw materials, is particularly suitable for
In with commercially available cheap formalin and dimethoxym ethane as main waste polymethoxy dimethyl ether.
Background technology
Polymethoxy dimethyl ether (Polyoxymethylene Dimethyl Ethers), its structural formula is:CH3O
(CH2O) nCH3, abbreviation DMMn (or PODEn), are many ether polymers of a class, and DMM3～5Oxygen content up to 47～49%, 16
Alkane value up to 78～100, can not only improve diesel oil in in-engine burning as a kind of new environmental protection type additive for diesel oil
Situation, improves efficiency of combustion, and cleans without sulfur, can substantially reduce the pollution of outer waste air, therefore with very high application
Prospect.
The preparation method of polymethoxy dimethyl ether is more, and its catalyst has ionic liquid, molecular sieve, ion exchange resin
There are formaldehyde, methanol, dimethoxym ethane, metaformaldehyde, paraformaldehyde etc. Deng, primary raw material, type of reactor has fixed bed, catalysis to steam
Evaporate, fixed bed+catalytic distillation etc..It is relatively simple with the reaction of dimethoxym ethane with solid metaformaldehyde and paraformaldehyde, only reaction
Reaction unit reaction is entered after thing is miscible by a certain percentage, the dehydration problem of reactant is there's almost no, many that has been the displosure
Patent：Polymethoxy two is produced as reactant with dimethoxym ethane and paraformaldehyde as patent CN201310327622.0 discloses one kind
The method of methyl ether, patent CN104355973A are disclosed with metaformaldehyde and dimethoxym ethane and produce polymethoxy dimethyl ether as reactant
Method, but such method is due to having that cost of material is higher, production cost is higher, thus industrially lacks competition
Advantage.
And with formaldehyde and dimethoxym ethane as the method for waste polymethoxy dimethyl ether as formaldehyde is relatively inexpensive so that this work
The research of skill becomes the emphasis of concern, but its technological difficulties is the dehydration of formaldehyde, in order to overcome the shortcoming, also has and much grinds
Study carefully：As CN104355973A discloses a kind of method that fixed bed reaction rectification prepares polymethoxy dimethyl ether, the method be by
PODE2-8It is delivered in being filled with the dehydrating tower of 3A molecular sieves and is dehydrated；Patent CN104725198A discloses a kind of poly- methoxy
Gas gas-phase objects stream dewatering in base dimethyl ether production process, the method is reactant gaseous phase materials to be flowed through equipped with molecular sieve
Adsorption tower be dehydrated；CN104725201A discloses a kind of polymethoxy dimethyl ether absorption, membrance separation and combines dewatering,
Gas gas-phase objects stream unstripped gas is entered into adsorption tower film and adsorbent is dehydrated；Patent CN104725203A discloses a kind of gas first
Aldehyde synthesizes the process unit and method of polymethoxy dimethyl ether and deacidification, makees adjuvant using unary alcohol and reacts with formalin
Hemiacetal is generated, then after decompression dehydration, then the method that hemiacetal resolves into formaldehyde is carried out into dehydration is produced formaldehyde gases, the first
Aldehyde gas is absorbed laggard reaction tower reaction by dimethoxym ethane again and produces polymethoxy dimethyl ether.Above-mentioned comparison of processes is complicated, energy
Consumption is higher, and as actually formaldehyde is difficult to be decomposed and parsed by heating means after condensation again.
The content of the invention
Technical problem to be solved in the utility model is, for the deficiencies in the prior art, and to provide a kind of poly- first
The extraction preparation facilitiess of epoxide dimethyl ether reaction raw materials, the apparatus structure are simple, and small investment, energy consumption are low.Using the device by city
The cheap formalin sold carries out the thickening of formaldehyde by the method for physical extraction, rectification under vacuum, and by extraction
Take the formaldehyde in agent and carry out distilling and produce hardly aqueous pure formaldehyde gases, the formaldehyde gases pressurize further through booster fan,
Pressure is dissolved in working solution, both ensure that efficiently separating for formaldehyde and extractant, and has been absorbed the working solution of formaldehyde gases
The raw material of polymethoxy dimethyl ether is exactly produced, is achieved many things at one stroke.
To achieve these goals, this utility model is adopted the following technical scheme that：
A kind of extraction preparation facilitiess of polymethoxy dimethyl ether reaction raw materials, including preheater I, preheater II and connect successively
Extraction tower, dehydrating tower, distillation column, blower fan and the material pans for connecing, preheater I, preheater II feed liquors respectively with extraction tower
Mouth is connected, and the device that the discharging opening of material pans carries out polyreaction with outside is connected, it is characterised in that：
Described preheater I, for preheating formalin, is provided with charging aperture A and discharging port A, charging aperture A and offer first
The device of aldehyde aqueous solution is connected, and discharging port A is connected with extraction tower；
Described preheater II, preheats extractant, is provided with charging aperture B and discharging opening B；Charging aperture B and offer extractant
Device be connected, discharging opening B is connected with extraction tower；
Described extraction tower, tower top are provided with liquid outlet I, and bottom of towe is provided with liquid outlet II, and tower body top is provided with inlet I, tower
Body bottom is provided with inlet II；The inlet I is connected with the discharging port A of described preheater I, and inlet II is pre- with described
The discharging opening B of hot device II is connected；The liquid outlet I is connected with dehydrating tower, and liquid outlet II holds the dress of formalin with outside
Put connected；
Described dehydrating tower, tower top are provided with air vent a, and inlet III is provided with the middle part of tower body, and bottom of towe is provided with liquid outlet III；
The inlet III is connected with the liquid outlet I of extraction tower, and liquid outlet III is connected with distillation column；Air vent a is connected with condenser,
The outlet of condenser is connected with surge tank, and condenser is imported in surge tank after condensing gas into liquid；
Described distillation column, is provided with inlet V in the middle part of tower body, tower top is provided with air vent b, and bottom of towe is provided with liquid outlet V；It is described
Inlet V is connected with the liquid outlet III of dehydrating tower, and liquid outlet V is connected with the charging aperture B of preheater II, air vent b and blower fan phase
Even；
Described blower fan is the blower fan with pressurization or increase function, is provided with air inlet and gas outlet, air inlet and distillation
The air vent b of tower is connected；Pipeloop is provided with gas outlet, pipeloop is equipped with the in communication and outlet with angle
Pipeline；
Described material pans, tank deck are provided with charging aperture C, and tank body top is provided with charging aperture D, tank bottoms to be provided with discharging opening C,
Tank body lower part discharging opening D；Charging aperture D is connected with the outside device for providing dimethoxym ethane and DMMn by-products, and discharging opening D passes through thing
The pipeloop of material circulation Pumps ＆ Fans gas outlet is connected, and charging aperture C is connected with the outlet line of blower fan gas outlet, discharging opening
C is connected with the polymerizing reactor for preparing polymethoxy dimethyl ether；Dimethoxym ethane and DMMn by-products enter into material from charging aperture D
In pans, in the pipeloop for pumping into fan outlet by discharging opening D and in the presence of Matter Transfer pump, dimethoxym ethane,
DMMn by-products carry out being mixed to get reaction raw materials with the formaldehyde gases in blower fan, and reaction raw materials pass through outlet line Jing charging apertures
C is re-introduced in material pans, and Jing discharging openings C is imported in polymerizing reactor so as to carrying out polyreaction.
In above-mentioned technical proposal, described surge tank, tank body top are provided with inlet IV, and tank deck is provided with gas phase mouth, tank bottoms
It is provided with liquid outlet IV；The inlet IV is connected with the outlet of condenser, and liquid outlet IV holds formalin with outside
Device is connected, and gas phase mouth is connected with vacuum pump set；Empty unit is connected with air, and effect is to maintain negative pressure in the tower of dehydrating tower.
In above-mentioned technical proposal, between described dehydrating tower, distillation column, preheater III is connected with.
In above-mentioned technical proposal, the tower body bottom of described dehydrating tower is provided with reboiler I；The tower body of described distillation column
Bottom is provided with reboiler II.
In above-mentioned technical proposal, the tower body of described extraction tower needs heat tracing, extraction tower to adopt metal tube heat tracing or electric companion
Hot mode carries out heat tracing, wherein, during using metal tube heat tracing, heat tracing medium is any one in hot water, water vapour and conduction oil
Kind.
In above-mentioned technical proposal, internals in described extraction tower, are filled with, described internals are filler, any in column plate
It is a kind of.
In above-mentioned technical proposal, the angle between described outlet line and pipeloop is：0o<α<90o.
The using method of said apparatus is comprised the following steps：
(1) preheating, extraction：After formalin, extractant are preheated to 40～120 DEG C respectively, the two is by reverse contact
Extracted, formaldehyde is extracted from formalin by extractant, in the extraction phase containing formaldehyde, contained a small amount of moisture；
Described formalin, formaldehyde therein are 1～10 with the mass ratio of extractant：1；
Described extractant is esters extractant, ketone extractant, ether extration agent, alcohol kind of extractants, phenols extractant
In any one, the mixture that two kinds and the above are mixed with arbitrary proportion；
Described esters extractant is preferably isooctyl acetate, cyclohexyl acetate, cyclopentyl acetate, tbp, nitre
Any one in different monooctyl ester of acid etc.；Described ketone extractant is preferably NOP, N- dodecyl pyrrolidines
Appointing in ketone, diisobutyl ketone, hexone, 2,4- difluoro benzophenones, ESCALOL 567 etc.
Meaning is a kind of；Described ether extration agent is preferably isooctanol polyethoxylate, t-butyl methyl ether, Meta Bromo Anisole, ethylene glycol phenyl
Any one in ether etc.；Described alcohol kind of extractants is preferably 1,4 cyclohexane dimethanol, 5- hexyl -1- alcohol, capryl alcohol, nonyl two
Any one in alcohol, 3- methoxyl group -3- methyl butanols, 2- methyl cycloheptanols etc.；Described phenols extractant is preferably octyl group
Any one in phenol, nonyl phenol, dodecylphenol, NPE etc.；
(2) negative pressure dehydration：The extraction phase that step (1) is obtained is 25～190 DEG C in temperature, and pressure is 0.1～-0.1MPa
Under conditions of carry out negative pressure dehydration, obtain the extract containing micro-moisture；
(3) distill：It is 50～300 DEG C, pressure that the extract that step (2) is obtained is preheated to after 90-150 DEG C in temperature
For separated is carried out under the conditions of -0.1～1MPa, distillation obtains formaldehyde gases；
(4) reaction raw materials are prepared：The formaldehyde gases that step (3) is obtained are dissolved in working solution in the condition of pressurization and are formed
Reaction raw materials；
Described working solution, is liquid that DMM1～2, DMM6～10, formalin are mixed with arbitrary proportion；
Described formalin, with formaldehyde as solute, dimethoxym ethane as solvent, formaldehyde can be completely dissolved by dimethoxym ethane；
The quality of formaldehyde in formalin in the quality of the working solution of described absorption formaldehyde gases, with step (1)
Than for 1～50：1；
(5) prepare polymethoxy dimethyl ether：The reaction raw materials that step (4) is obtained are carried out into polyreaction, polymerizate Jing
After rectification, target DMM3～5 harvesting, by-product DMM1～2, DMM6～10 are recycled as working solution；
Described reaction raw materials are acid resin catalyst in 50～150 DEG C of temperature, 0～0.5MPa of pressure, catalyst
Polyreaction is carried out under reaction condition, the air speed of reaction raw materials is 0.5～5h-1；
Described acid resin catalyst is preferably the D006 type acid resin catalysts of our unit's production, the resistance to height of D008 types
Warm acid resin catalyst.
The method that device described in above-mentioned technical proposal prepares polymethoxy dimethyl ether reaction raw materials, flow chart such as Fig. 1
It is shown, specifically include following steps：
(1) preheating, extraction：The preheated device I of formalin is entered from extraction tower inlet I after being preheated to 40～120 DEG C,
The preheated device II of extractant is entered from extraction tower inlet II after being preheated to 40～120 DEG C, and extractant is occurred with formalin
Reverse to contact, formaldehyde is extracted from water by extractant, and extraction phase is expelled in dehydrating tower from liquid outlet I, and raffinate phase is from going out
Liquid mouth II is expelled to the device that outside holds formalin；
Described extraction tower, tower body temperature are controlled to 25～100 DEG C, and tower top temperature is controlled to 25～100 DEG C, bottom of towe temperature
50～190 DEG C of degree control；In tower body, pressure is controlled to 0～1MPa, and tower top pressure is controlled to -0.1～0MPa, tower bottom pressure control
For -0.1～0.1MPa；
(2) negative pressure dehydration：The extraction phase that step (1) is obtained carries out negative pressure dehydration, reboiler I control towers bottom in dehydrating tower
Temperature is 50～190 DEG C, tower top temperature is 25～100 DEG C, and vacuum pump set controls tower pressure interior force for -0.1～0.1MPa；Tower top steams
The condensed device of the vapor containing a small amount of formaldehyde for going out is condensed into after liquid and enters in surge tank, and bottom of towe is obtained containing trace water
Extract drain in distillation column；
(3) distill：The preheated device III of extract that step (2) is obtained is carried out after being preheated to 90～150 DEG C in distillation column
Separated, it is 100～300 DEG C that reboiler II controls tower top temperature for 50～120 DEG C, column bottom temperature, air-blower control tower top pressure
Power is -0.1～1MPa, tower bottom pressure is -0.1～1MPa；The formaldehyde gases that tower top is distilled out are entered in blower fan, and bottom of towe is remaining
Extractant returns to the preheated Posterior circles of preheater II and uses；
(4) reaction raw materials are prepared：Working solution Jing discharging openings D that Jing charging aperture D are entered in material pans discharges, and Jing
Matter Transfer pump is squeezed in the pipeloop of blower fan gas outlet, pressure of the working solution in the pipeloop of blower fan gas outlet in blower fan
The lower formaldehyde gases for forcing absorption step to obtain of effect, so as to obtain reaction raw materials；The reaction raw materials Jing blower fans gas outlet for obtaining
Outlet line and the charging aperture C of material pans enter in material pans, a portion reaction raw materials Jing discharging opening C
It is expelled in the polymerizing reactor for preparing polymethoxy dimethyl ether of outside, another part reaction raw materials continue after adjusting concentration
Use as working solution；
The quality of the working solution of formaldehyde gases is absorbed, is with the mass ratio of formaldehyde in formalin in step (1) and is followed
Circular rector；
(5) prepare polymethoxy dimethyl ether：The reaction raw materials that step (4) is obtained are passed into produces polymethoxy dimethyl ether
Polyreaction is carried out in polymerizing reactor, product passes sequentially through de-light rectification column, de- weight rectifying column and carries out rectification, target product
DMM3～5 harvest, and by-product DMM1～2, DMM6～10 are passed into the recycling in material pans, while in the middle of material
Tank supplements formalin and keeps material balance and level stability in material pans；
Described de-light rectification column rectification condition：Tower top temperature is 42～105 DEG C, 0～0.5MPa of tower top pressure, tower top are returned
Flow ratio is 0.5～5.0；150～300 DEG C of column bottom temperature；By-product DMM1～2 of removed overhead are introduced in material pans；Tower
Bottom product is passed through in de- weight rectifying column；
Described de- heavy rectifying column rectification condition：Tower top temperature is 50～100 DEG C, -0.1～0.5MPa of pressure, tower top are returned
Flow ratio is 0.5～5.0；150～300 DEG C of column bottom temperature；Tower top is harvested for target product DMM3～5, the by-product of bottom of towe removing
DMM6～10 are introduced in material pans.
The advantage of technical solutions of the utility model is：Commercially available cheap formalin is passed through thing by this utility model
Reason extraction, the method for rectification under vacuum carry out the thickening of formaldehyde, and by the formaldehyde in extractant is carried out distillation produce it is several
Water-free pure formaldehyde gases, the formaldehyde gases are pressurizeed by booster fan, and pressure is dissolved in working solution, both ensure that first
Aldehyde is efficiently separated with extractant, and to absorb the working solution of formaldehyde gases be exactly the raw material for producing polymethoxy dimethyl ether,
Achieve many things at one stroke.The method and device have the advantages that few significant equipment investment, process is simple, energy consumption are low.
Description of the drawings
Fig. 1：The overall structure diagram of this utility model device；
Wherein：1st, preheater I, 2, preheater II, 3, extraction tower, 4, dehydrating tower, 5, reboiler I, 6, surge tank, 7, vacuum
Unit, 8, condenser, 9, preheater III, 10, distillation column, 11, reboiler II, 12, blower fan, 13, material pans, 14, material
Circulating pump.
Specific embodiment
Hereinafter the specific embodiment of technical solutions of the utility model is described in detail, but this utility model be not limited to
Lower description content：
A kind of extraction equipment of polymethoxy dimethyl ether reaction raw materials, as shown in Figure 1：Including preheater I 1, preheater II
2nd, extraction tower 3, dehydrating tower 4, surge tank 6, distillation column 10, blower fan 12 and material pans 13,
Described preheater I, is provided with charging aperture A and discharging port A；Described preheater II, is provided with charging aperture B and discharging opening
B；
Described extraction tower, tower top are provided with liquid outlet I, and bottom of towe is provided with liquid outlet II, and tower body top is provided with inlet I, tower
Body bottom is provided with inlet II；Inlet I is connected with the discharging port A of described preheater I, inlet II and described preheater
The discharging opening B of II is connected；Liquid outlet I is connected with dehydrating tower, and the device that liquid outlet II holds formalin with outside is connected；
Described dehydrating tower, tower top are provided with air vent a, and inlet III is provided with the middle part of tower body, and bottom of towe is provided with liquid outlet III；
The inlet III is connected with the liquid outlet I of extraction tower, and air vent a is connected with surge tank, and liquid outlet III is connected with distillation column；
Described surge tank, tank body top are provided with inlet IV, and tank deck is provided with gas phase mouth, tank bottoms to be provided with liquid outlet IV；Institute
State inlet IV to be connected with the air vent a of dehydrating tower, the device that liquid outlet IV holds formalin with outside is connected, gas phase mouth
It is connected with vacuum pump set；
Described distillation column, tower body top are provided with inlet V, and tower top is provided with air vent b, and bottom of towe is provided with liquid outlet V；It is described
Inlet V is connected with the liquid outlet III of dehydrating tower, and liquid outlet V is connected with the charging aperture B of preheater II, air vent b and blower fan phase
Even；
Described blower fan is that with pressurizeing or increase the blower fan of function, top is provided with air inlet, and bottom is provided with gas outlet, goes out
QI KOU is provided with outlet line and (angle therebetween is 0o to the pipeloop being attached thereto<α<90o)；The air inlet and steaming
The air vent b for evaporating tower is connected, and gas outlet is connected with material pans；
Described material pans, tank deck are provided with charging aperture C, and tank body top is provided with charging aperture D, tank bottoms to be provided with discharging opening C,
Tank body lower part discharging opening D；The charging aperture C is connected with the outlet line of blower fan gas outlet, and charging aperture D provides dimethoxym ethane with outside
It is connected with the device of DMMn by-products, discharging opening C is connected with the polymerizing reactor for preparing polymethoxy dimethyl ether, discharging opening
D is connected with the pipeloop of blower fan gas outlet by Matter Transfer pump 14；
Condenser 8 is connected between described dehydrating tower, surge tank, condenser imports buffering after condensing gas into liquid
In tank；It is described, preheater III 9 is connected between distillation column.
The tower body bottom of described dehydrating tower is provided with reboiler I 5；The tower body bottom of described distillation column is provided with again
Boiling device II11；
The tower body of described extraction tower needs heat tracing, carries out heat tracing using metal tube heat tracing or electric tracing mode, wherein, adopt
During with metal tube heat tracing, heat tracing medium is any one in hot water, water vapour and conduction oil；The tower of described extraction tower (3)
It is interior filled with internals, described internals are filler, any one in column plate.
The using method of said apparatus is comprised the following steps：
(1) preheat：The preheated device I of formalin 1 is entered from 3 inlet I of extraction tower after being preheated to 40～120 DEG C, extraction
Take after the preheated device II of agent 2 is preheated to 40～120 DEG C and enter from extraction tower inlet II, extractant is occurred with formalin
Reverse to contact, formaldehyde is extracted from water by extractant, and extraction phase is expelled in dehydrating tower 4 from liquid outlet I, and raffinate phase is from going out
Liquid mouth II is expelled to the device that outside holds formalin；
(2) extract：The extraction phase that step (1) is obtained carries out negative pressure dehydration, 5 control tower bottom temperature of reboiler I in dehydrating tower
It is 25～100 DEG C to spend for 50～190 DEG C, tower top temperature, and vacuum pump set 7 controls tower pressure interior force for -0.1～0.1MPa；Tower top steams
The condensed device of the vapor containing a small amount of formaldehyde that goes out 8 is condensed into after liquid and enters in surge tank 6, and bottom of towe is obtained containing minor amount of water
The extract of part is drained in distillation column 10；
(3) distill：Separated is carried out in distillation column after the preheated device III of extract that step (2) is obtained 9, then is boiled
It is 100～300 DEG C that device II 11 controls tower top temperature for 50～120 DEG C, column bottom temperature, and blower fan 12 controls tower top pressure for -0.1
～1MPa, tower bottom pressure are -0.1～1MPa；The formaldehyde gases that tower top is distilled out are entered in blower fan, and the remaining extractant of bottom of towe is returned
Return to the preheated Posterior circles of preheater II to use；
(4) reaction raw materials are prepared：Working solution Jing discharging openings D that Jing charging aperture D are entered in material pans 13 discharges, and
Jing Matter Transfers pump 14 is squeezed in the pipeloop of blower fan gas outlet, and the working solution in the pipeloop of blower fan gas outlet is in blower fan
The lower formaldehyde gases for forcing absorption step (3) to obtain of pressure effect, so as to obtain reaction raw materials；The reaction raw materials Jing blower fans for obtaining
The charging aperture C of the outlet line and material pans of gas outlet is entered in material pans, a portion reaction raw materials Jing
Discharging opening C is expelled in the polymerizing reactor for preparing polymethoxy dimethyl ether of outside, and another part reaction raw materials adjust dense
Continue to use as working solution after degree；
(5) prepare polymethoxy dimethyl ether：The reaction raw materials that step (4) is obtained are passed into produces polymethoxy dimethyl ether
Polyreaction is carried out in polymerizing reactor, product passes sequentially through de-light rectification column, de- weight rectifying column and carries out rectification, target product
DMM3～5 harvest, and by-product DMM1～2, DMM6～10 are passed into the recycling in material pans, while in the middle of material
Tank supplements formalin and keeps material balance and level stability in material pans.
Method of the present utility model is described in detail with reference to embodiment：
Embodiment 1：
A kind of preparation method of polymethoxy dimethyl ether reaction raw materials, comprises the following steps：
(1) formalin that 100g/h concentration is 37% preheated device I 1 is preheating to after 55 DEG C to enter from extraction tower 3
Enter, meanwhile, it is preheated to using the mixture of the ethylene glycol phenyl ether of 200g/h and 300g/h nonyl alcohols as the preheated device II of extractant 2
Enter from 3 bottom of extraction tower after 65 DEG C, tower body heat tracing is opened, at 60 DEG C, tower top pressure is controlled in 0.3MPa to maintain temperature in tower；
Tower top extracts the extract of 580g/h, wherein 37.0g/h containing formaldehyde, the aqueous solution of bottom of towe raffinate phase extraction 20g/h；
(2), during the extract of the 550g/h obtained in step (1) is passed through formaldehyde except water tower 4, column bottom temperature is by reboiler I 5
120 DEG C, 54 DEG C of tower top temperature are controlled to, tower top pressure is controlled to -0.09MPa by vacuum pump set 7；Tower top steam containing a small amount of
The condensed device of the vapor of formaldehyde 8 is entered in surge tank 6 after being condensed into liquid, can draw 46.8g/h from 6 bottom of surge tank dense
Spend the dilute formalin for 8.1%；And the bottom of towe of extraction distillation column obtains the 533.2g/h extracts containing 8PPm minor amount of water,
Wherein 33.2g/h containing formaldehyde.
(3) by the formaldehyde of step (2) except the 533.2g/h extracts that the bottom of towe of water tower 4 is obtained are passed through formaldehyde distillation column 10
In, by formaldehyde distillation column tower reactor reboiler II 11 control 125 DEG C of column bottom temperature, 75 DEG C of tower top temperature, tower top pressure then according to
Draft by force (forcing) pump 12 is controlled to normal pressure；Tower top distills out formaldehyde gases, the 500g/h ethylene glycol phenyls after bottom of towe removing formaldehyde
The mixture extractant (content of formaldehyde 159PPm) of ether and nonyl alcohol returns to 2 imports of preheater II recycling, and tower top can steam
Go out the formaldehyde gases of 33.2g/h.
(4) formaldehyde gases that the tower top of the formaldehyde distillation column 10 of step (3) steams 33.2g/h are passed through booster fan 12 to enter
QI KOU, meanwhile, the working solution in material pans 13 is passed into 12 outlet line (155g/h of booster fan by Matter Transfer pump 14
Working solution)；Formaldehyde gases are in 12 outlet line of booster fan by working solution (DMM1～2, DMM6～10, dimethoxym ethane, formaldehyde
Mixed liquor) mixed dissolution absorption；The working solution of formaldehyde gases is absorbed, has 128g/h (wherein content of formaldehyde 25.9%) as poly-
The reaction raw materials of methoxyl group dimethyl ether are drawn out to polymethoxy dimethyl ether DMMn reactions from 13 bottom discharge mouth II of material pans
Device in carry out polyreaction；The dimethoxym ethane and DMMn reaction units removing DMM3 of 22.8g/h is supplemented in material pans
56g/hDMM1～2 and 16g/hDMM6～10 after～5 finished products are ensureing the level stability of material balance and material pans.
(5) reaction raw materials of the polymethoxy dimethyl ether of 128g/h (content of formaldehyde 25.9%) described in step (3) are passed through
After polymethoxy dimethyl ether DMMn reaction units, in reaction pressure 0.3MPa, 95 DEG C of reaction temperature and the acid of 100gD008 types heatproof
Polyreaction is carried out under property resin catalyst catalytic action；
Polymerizate carries out rectification in being passed through de-light rectification column rectification：Control 201 DEG C of column bottom temperature, 105 DEG C of tower top temperature,
Than distillation operation is carried out under 1.5, normal pressure, overhead components are light component DMM1～2 to overhead reflux, condensed, wherein, 84g/h is light
Component backflow is used as working solution in being recycled into material pans 11 to tower top, 56g/h light components；Bottom of towe draws 72g/h
Heavy constituent DMM3～10；
Heavy constituent DMM3～10 are passed through in de- weight rectifying column rectification carries out rectification：220 DEG C of column bottom temperature of control, tower top temperature
85 DEG C of degree, pressure -0.085MPa, overhead reflux compare 1.2, carry out rectification under vacuum operation；Bottom of towe extraction 16g/h heavy constituents DMM6～
10 return to material pans 11 in use as working solution；Overhead components be light component DMM3～5, it is condensed after, wherein
67.2g/h is back to tower top, and 56g/hDMM3～5 are produced as finished product.
The reaction raw materials of the polymethoxy dimethyl ether that the present embodiment is produced, after polyreaction, formaldehyde conversion is 99.8%,
Total recovery 99.4%.
Embodiment 2：
A kind of preparation method of polymethoxy dimethyl ether reaction raw materials, other process conditions and method it is same as Example 1,
Be its initial feed be 50g/h concentration 55% formalin, extractant be 450g/h 2- methyl cycloheptanols, formaldehyde steam
The operating condition for evaporating tower 10 is：258 DEG C of column bottom temperature, 85 DEG C of tower top temperature, tower top pressure 0.3MPa；Tower top distills out formaldehyde gas
The formaldehyde gases of body 27.3g/h, finally obtain polymethoxy dimethyl ether product DMM3～5 of 46g/h targeted degree of polymerization：
The reaction raw materials of the polymethoxy dimethyl ether that the present embodiment is produced, after polyreaction, formaldehyde reaction conversion ratio is
99.8%, total recovery 98.6%.
Examples detailed above simply to illustrate technology design of the present utility model and technical characterstic, can not limit this reality with this
With new protection domain.All equivalent transformations done according to essence of the present utility model or modification, all should cover in this reality
Within new protection domain.
Claims (9)
1. a kind of extraction equipment of polymethoxy dimethyl ether reaction raw materials, preheater I (1), preheater II (2) and is sequentially connected
Extraction tower (3), dehydrating tower (4), distillation column (10), blower fan (12) and material pans (13), preheater I (1), preheater II
(2) it is connected with the inlet of extraction tower (3) respectively, discharging opening and the outside of material pans (13) carry out the device of polyreaction
It is connected, it is characterised in that：
Described preheater I (1), is provided with charging aperture A and discharging port A, and charging aperture A is connected with the device for providing formalin
Connect, discharging port A is connected with extraction tower (3)；
Described preheater II (2), is provided with charging aperture B and discharging opening B；Charging aperture B is connected with the device for providing extractant, is gone out
Material mouth B is connected with extraction tower (3)；
Described extraction tower (3), tower top are provided with liquid outlet I, and bottom of towe is provided with liquid outlet II, and tower body top is provided with inlet I, tower body
Bottom is provided with inlet II；The inlet I is connected with the discharging port A of described preheater I, inlet II and described preheating
The discharging opening B of device II is connected；The liquid outlet I is connected with dehydrating tower (4), and liquid outlet II holds the dress of formalin with outside
Put connected；
Described dehydrating tower (4), tower top are provided with air vent a, and inlet III is provided with the middle part of tower body, and bottom of towe is provided with liquid outlet III；
The inlet III is connected with the liquid outlet I of extraction tower, and liquid outlet III is connected with distillation column (10)；Air vent a is connected with cold
Condenser (8), the outlet of condenser are connected with surge tank (6), and condenser is imported in surge tank after condensing gas into liquid；
Described distillation column (10), is provided with inlet V in the middle part of tower body, tower top is provided with air vent b, and bottom of towe is provided with liquid outlet V；
The inlet V is connected with the liquid outlet III of dehydrating tower, and liquid outlet V is connected with the charging aperture B of preheater II (2), aerofluxuss
Mouth b is connected with blower fan (12)；
Described blower fan (12) is the blower fan with pressurization or increase function, is provided with air inlet and gas outlet, air inlet and distillation
The air vent b of tower is connected；Pipeloop is provided with gas outlet, pipeloop is equipped with the in communication and outlet with angle
Pipeline；
Described material pans (13), tank deck are provided with charging aperture C, and tank body top is provided with charging aperture D, tank bottoms to be provided with discharging opening C,
Tank body lower part discharging opening D；Charging aperture D is connected with the outside device for providing dimethoxym ethane and DMMn by-products, and discharging opening D passes through thing
Material circulating pump (14) is connected with the pipeloop of blower fan gas outlet, and charging aperture C is connected with the outlet line of blower fan gas outlet, is gone out
Material mouth C is connected with the polymerizing reactor for preparing polymethoxy dimethyl ether；Dimethoxym ethane and DMMn by-products are entered into from charging aperture D
In material pans, in the pipeloop for pumping into fan outlet by discharging opening D and in the presence of Matter Transfer pump, first contracting
Formaldehyde gases in aldehyde, DMMn by-products and blower fan carry out being mixed to get reaction raw materials, and reaction raw materials are entered by outlet line Jing
Material mouth C is re-introduced in material pans, and Jing discharging openings C is imported in polymerizing reactor so as to carrying out polyreaction.
2. device according to claim 1, it is characterised in that described surge tank (6), tank body top is provided with inlet
IV, tank deck are provided with gas phase mouth, tank bottoms to be provided with liquid outlet IV；The inlet IV is connected with the outlet of condenser (8), liquid outlet
The device that IV holds formalin with outside is connected, and gas phase mouth is connected with vacuum pump set (7)；Empty unit is connected with air, is made
With being to maintain negative pressure in the tower of dehydrating tower (4).
3. device according to claim 1, it is characterised in that described dehydrating tower (4), distillation column are connected between (10)
Preheater III (9).
4. device according to claim 1, it is characterised in that the tower body bottom of described dehydrating tower (4) is provided with boils again
Device I (5).
5. device according to claim 1, it is characterised in that the tower body bottom of described distillation column (10) is provided with boils again
Device II (11).
6. device according to claim 1, it is characterised in that described extraction tower (3) is using metal tube heat tracing or electric companion
Hot mode carries out heat tracing.
7. device according to claim 6, it is characterised in that during using metal tube heat tracing, heat tracing medium are that hot water, water steam
Any one in gas and conduction oil.
8. device according to claim 1, it is characterised in that internals are filled with the tower of described extraction tower (3), it is described
Internals be filler, any one in column plate.
9. device according to claim 1, it is characterised in that the angle between described outlet line and pipeloop
Scope is：0o<α<90o.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621145772.5U CN206143094U (en) | 2016-10-21 | 2016-10-21 | Extraction device who gathers methoxy dimethyl ether reactant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201621145772.5U CN206143094U (en) | 2016-10-21 | 2016-10-21 | Extraction device who gathers methoxy dimethyl ether reactant |
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| CN206143094U true CN206143094U (en) | 2017-05-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278851A (en) * | 2016-10-21 | 2017-01-04 | 凯瑞环保科技股份有限公司 | The extraction preparation method of a kind of polymethoxy dimethyl ether reaction raw materials and device |
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2016
- 2016-10-21 CN CN201621145772.5U patent/CN206143094U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278851A (en) * | 2016-10-21 | 2017-01-04 | 凯瑞环保科技股份有限公司 | The extraction preparation method of a kind of polymethoxy dimethyl ether reaction raw materials and device |
| CN106278851B (en) * | 2016-10-21 | 2019-04-09 | 凯瑞环保科技股份有限公司 | A kind of the extraction preparation method and device of polymethoxy dimethyl ether reaction raw materials |
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