CN103570590B - A kind of equipment producing methyl-sulfate - Google Patents
A kind of equipment producing methyl-sulfate Download PDFInfo
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- CN103570590B CN103570590B CN201310528752.0A CN201310528752A CN103570590B CN 103570590 B CN103570590 B CN 103570590B CN 201310528752 A CN201310528752 A CN 201310528752A CN 103570590 B CN103570590 B CN 103570590B
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Abstract
The present invention relates to chemical field, particularly disclose a kind of equipment producing methyl-sulfate.The equipment of this production methyl-sulfate, comprise esterification reaction tower, degassing tower and rectifying tower, the its top feed mouth of esterification top of tower is connected with liquids material source by pipeline, the esterification reaction tower material outlet of esterification tower bottom is connected with the degassing tower opening for feed in the middle part of degassing tower by pipeline, the top discharge mouth at rectifying tower top is connected with the first outside storage tank by pipeline, the side discharge port of rectifying tower middle and upper part is connected with the second outside storage tank by pipeline, the degassing tower air outlet at degassing tower top is connected with the absorption tower inlet mouth on absorption tower by pipeline.The invention has the beneficial effects as follows: make whole production process achieve continuous prodution, reaction is more complete, substantially increases production capacity and quality product, operation fully automated is controlled, makes production more safe and efficient.
Description
(1) technical field
The present invention relates to chemical field, particularly a kind of equipment producing methyl-sulfate.
(2) background technology
Esterification, rectification process is two unit during methyl-sulfate is produced, also be two kinds of unit more common in chemical technique, since methyl-sulfate production technique is gone into operation, so far, esterification both at home and abroad, what rectifying production technique all adopted separates, discontinuity operating procedure, separately, there is reaction not exclusively in the production of discontinuity, reaction efficiency is low, poor product quality, production capacity is low, energy consumption is high, safety and environmental protection coefficient is low, the shortcomings such as environmental protection pressure is large, original technique can not meet the prodution and development needs of modern enterprise far away, seriously constrain innovation and the progress of enterprise.
(3) summary of the invention
The present invention in order to make up the deficiencies in the prior art, provide a kind of can continuous seepage, make that the product purity that esterification is full and uniform, speed of response is fast, production efficiency is high, output is high, produce is high, energy-saving and cost-reducing, the equipment of the production methyl-sulfate of reduction product acidity, safety and environmental protection.
The present invention is achieved through the following technical solutions:
A kind of equipment producing methyl-sulfate, comprise esterification reaction tower, degassing tower and rectifying tower, the its top feed mouth of esterification top of tower is connected with liquids material source by pipeline, the esterification reaction tower material outlet of esterification tower bottom is connected with the degassing tower opening for feed in the middle part of degassing tower by pipeline, bottom degassing tower, the degassing tower discharge port of side is connected with the opening for feed in the middle part of rectifying tower through product pump by pipeline, the top discharge mouth at rectifying tower top is connected with the first outside storage tank by pipeline, the side discharge port of rectifying tower middle and upper part is connected with the second outside storage tank by pipeline, the degassing tower air outlet at degassing tower top is connected with the absorption tower inlet mouth on absorption tower by pipeline, the degassing tower liquid outlet of degassing tower bottom is connected with the degassing tower material steam mouth of degassing tower through the first reboiler by pipeline.
Described esterification reaction tower comprises esterification reaction tower tower body, its top feed mouth and esterification reaction tower material outlet is respectively equipped with at the top of esterification reaction tower tower body and bottom, on by upper column plate setting up and down and lower column plate esterification reaction tower tower body inside being divided into from top to bottom successively in esterification reaction tower tower body, in, lower three layers of tower chamber, three layers of tower chamber are connected with a refrigerating unit respectively, the guide shell that an open top end is arranged is equipped with in the mid-way, bottom in every layer of tower chamber, a gas distributor is equipped with in the bottom of each guide shell, each gas distributor is connected with the gas feed be located on this layer of tower chamber sidewall respectively by a pipeline, gas feed on the sidewall of last layer tower chamber is connected with the pneumatic outlet being located at lower one deck tower chamber top side wall by the pipeline be located at outside esterification reaction tower tower body, the gas feed in orlop tower chamber is connected with source of the gas by pipeline, upper, the overflow cylinder that one is positioned at the connection two tower chamber outside guide shell is provided with between tower chamber, middle level, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, in, the overflow cylinder that one is positioned at the connection two tower chamber outside guide shell is provided with between lower floor's tower chamber, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, be positioned at the top of fluid inlet position higher than tower chamber, middle level inner draft tube of the overflow cylinder in tower chamber, middle level.
Described refrigerating unit comprises a drum and the cooling air outlet on the sidewall of tower chamber setting up and down and cools fluid inlet, the cooling duct being communicated with cooling air outlet and cooling fluid inlet is provided with in tower chamber, cooling fluid inlet is connected with the liquid outlet of drum through water pump by the pipeline being located at esterification reaction tower tower body outside, cooling air outlet is connected with the inlet mouth of drum by the pipeline being located at esterification reaction tower tower body outside, is provided with a vapour outlet at the top of drum.
Described rectifying tower comprises rectifying tower tower body, an opening for feed is provided with at the middle part of rectifying tower tower body side, opening for feed is connected with by pipeline the liquid distributor that is located at rectifying tower tower body inside, side discharge port and material steam mouth is respectively equipped with in the middle and upper part of rectifying tower tower body opposite side and bottom, a top discharge mouth is provided with at the top of rectifying tower tower body, waste liquid outlet and rectifying tower material outlet is respectively equipped with in the bottom of rectifying tower tower body, rectifying tower material outlet is connected with material steam mouth through the second reboiler by pipeline, be horizontally arranged with one in rectifying tower tower body between opening for feed and side discharge port and rectifying tower tower body inside is divided into upper and lower two-part gas-liquid separation device, packing layer and lower packing layer is respectively equipped with in rectifying tower tower body above and below gas-liquid separation device, side discharge port is communicated with a Y-tube, the Single port of Y-tube is connected with outside storage tank by pipeline, another port is connected with the rectifying tower tower body inside above upper packing layer through condenser by pipeline.
Described gas-liquid separation device comprises the plate body of an arranged transversely, plate body is vertically provided with the some upper and lower two-part thrust-augmenting nozzles of connection rectifying tower tower body, above every root thrust-augmenting nozzle, be equipped with a conical fairing cap, the inwall of conical fairing cap is connected by the top of some poles and thrust-augmenting nozzle.
Described upper packing layer is one deck Stainless Steel Helices layer; Described lower packing layer comprises some layers of Stainless Steel Helices layer, is provided with cavity between neighbouring two Stainless Steel Helices layers.
The beneficial effect that the present invention produces the equipment of methyl-sulfate is: solving methyl-sulfate whole production line can not fully automated, can not operate continuously and quantity-produced problem, whole production process is made to achieve continuous prodution, esterification process is from normal pressure, low temperature becomes pressurization, carry out under warm-up mode, react more complete, simultaneously by-product low-pressure steam, accomplish energy-saving and cost-reducing effect, improve esterification reaction rate and the esterification yield of esterification process, effectively increase the Long contact time of dme and sulphur trioxide in methyl-sulfate esterification process, ensure that the excessive response of dme, thus make sulphur trioxide energy complete reaction, reduce the acidity of product, fine work for methyl-sulfate is purified and is accelerated speed, decrease the generation of waste residue, reach energy-conservation, the object of environmental protection, after utilizing degassing tower to be deviate from by the dme in material, the dme deviate from is sent in absorption tower and recycles, decrease the waste of raw material, reduce production cost, safety and environmental protection, change original distil process, rectification process is produced from original discontinuity and becomes continuous prodution, substantially increase production capacity and quality product, operation fully automated is controlled, reduces security risk, make production safer, efficient.
(4) accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structural representation of esterification reaction tower of the present invention;
Fig. 3 is the structural representation of rectifying tower of the present invention;
Fig. 4 is the close-up schematic view of rectifying tower Inner guide pipe of the present invention and conical fairing cap.
In figure, 1 esterification reaction tower, 2 degassing towers, 3 rectifying tower, 4 first reboilers, 5 product pumps, 11 esterification reaction tower tower bodies, 12 its top feed mouths, 13 esterification reaction tower material outlets, column plate on 14, 15 times column plates, 16 guide shells, 17 gas distributors, 18 gas feeds, 19 pneumatic outlets, 110 overflow cylinders, 111 fluid inlets, 112 liquid outlets, 113 drums, 114 cooling air outlets, 115 cooling fluid inlets, 116 cooling ducts, 117 water pumps, 118 liquid outlets, 119 inlet mouths, 120 vapour outlets, 121 tower chamber, upper stratas, 122 tower chamber, middle levels, 123 lower floor's tower chambeies, 21 degassing tower opening for feeds, 22 degassing tower discharge ports, 23 degassing tower air outlets, 24 degassing tower liquid outlets, 25 degassing tower material steam mouths, 31 rectifying tower tower bodies, 32 opening for feeds, 33 liquid distributors, 34 side discharge ports, 35 material steam mouths, 36 top discharge mouths, 37 waste liquid outlets, packing layer on 38, 39 times packing layers, 310 condensers, 311 plate bodys, 312 thrust-augmenting nozzles, 313 conical fairing caps, 314 poles, 315 second reboilers, 316 rectifying tower material outlets.
(5) embodiment
Being easier to make technology of the present invention, feature, object and effect etc. understand, understand, below in conjunction with accompanying drawing of the present invention, clear, complete description is carried out to technical scheme of the present invention, but the present invention is not limited thereto.
As as shown in Fig. 1-Fig. 4, this embodiment comprises esterification reaction tower 1, degassing tower 2 and rectifying tower 3, the its top feed mouth 12 at esterification reaction tower 1 top is connected with liquids material source by pipeline, esterification reaction tower material outlet 13 bottom esterification reaction tower 1 is connected with the degassing tower opening for feed 21 in the middle part of degassing tower 2 by pipeline, bottom degassing tower 2, the degassing tower discharge port 22 of side is connected with the opening for feed 32 in the middle part of rectifying tower 3 through product pump 5 by pipeline, the top discharge mouth 36 at rectifying tower 3 top is connected with the first outside storage tank by pipeline, the side discharge port 34 of rectifying tower 3 middle and upper part is connected with the second outside storage tank by pipeline, the degassing tower air outlet 23 at degassing tower 2 top is connected with the absorption tower inlet mouth on absorption tower by pipeline, the degassing tower liquid outlet 24 of degassing tower 2 bottom is connected with the degassing tower material steam mouth 25 of degassing tower 2 through the first reboiler 4 by pipeline.
Esterification reaction tower 1 comprises esterification reaction tower tower body 11, its top feed mouth 12 and esterification reaction tower material outlet 13 is respectively equipped with at the top of esterification reaction tower tower body 11 and bottom, on by upper column plate 14 setting up and down and lower column plate 15 esterification reaction tower tower body 11 inside being divided into from top to bottom successively in esterification reaction tower tower body 11, in, lower three layers of tower chamber, three layers of tower chamber are connected with a refrigerating unit respectively, the guide shell 16 that an open top end is arranged is equipped with in the mid-way, bottom in every layer of tower chamber, a gas distributor 17 is equipped with in the bottom of each guide shell 16, each gas distributor 17 is connected with the gas feed 18 be located on this layer of tower chamber sidewall respectively by a pipeline, gas feed 18 on the sidewall of last layer tower chamber is connected with the pneumatic outlet 19 being located at lower one deck tower chamber top side wall by the pipeline be located at outside esterification reaction tower tower body 11, the gas feed 18 in orlop tower chamber is connected with source of the gas by pipeline, upper, the overflow cylinder 110 that one is positioned at the connection two tower chamber outside guide shell 16 is provided with between tower chamber, middle level, the top and bottom of this overflow cylinder 110 are respectively equipped with a fluid inlet 111 and liquid outlet 112, in, the overflow cylinder 110 that one is positioned at the connection two tower chamber outside guide shell 16 is provided with between lower floor's tower chamber, the top and bottom of this overflow cylinder 110 are respectively equipped with a fluid inlet 111 and liquid outlet 112, be positioned at the top of fluid inlet 111 position higher than tower chamber 122, middle level inner draft tube 16 of the overflow cylinder 110 in tower chamber, middle level 122, refrigerating unit comprises a drum 113 and cooling air outlet on the sidewall of tower chamber setting up and down 114 and cooling fluid inlet 115, the cooling duct 116 being communicated with cooling air outlet 114 and cooling fluid inlet 115 is provided with in tower chamber, cooling fluid inlet 115 is connected with the liquid outlet 118 of drum 113 through water pump 117 by the pipeline being located at esterification reaction tower tower body 11 outside, cooling air outlet 114 is connected by the inlet mouth 119 of the pipeline with drum 113 that are located at esterification reaction tower tower body 11 outside, is provided with a vapour outlet 120 at the top of drum 113.
Rectifying tower 3 comprises rectifying tower tower body 31, an opening for feed 32 is provided with at the middle part of rectifying tower tower body 31 side, opening for feed 32 is connected with by pipeline the liquid distributor 33 that is located at rectifying tower tower body 31 inside, side discharge port 34 and material steam mouth 35 is respectively equipped with in the middle and upper part of rectifying tower tower body 31 opposite side and bottom, a top discharge mouth 36 is provided with at the top of rectifying tower tower body 31, waste liquid outlet 37 and rectifying tower material outlet 316 is respectively equipped with in the bottom of rectifying tower tower body 31, rectifying tower material outlet 316 is connected with material steam mouth 35 through the second reboiler 315 by pipeline, be horizontally arranged with one in rectifying tower tower body 31 between opening for feed 32 and side discharge port 34 and rectifying tower tower body 31 inside is divided into upper and lower two-part gas-liquid separation device, packing layer 38 and lower packing layer 39 is respectively equipped with in rectifying tower tower body 31 above and below gas-liquid separation device, side discharge port 34 is communicated with a Y-tube, the Single port of Y-tube is connected with outside storage tank by pipeline, another port is connected with rectifying tower tower body 31 inside above upper packing layer 38 through condenser 310 by pipeline, gas-liquid separation device comprises the plate body 311 of an arranged transversely, plate body 311 is vertically provided with the some two-part thrust-augmenting nozzles 312 of connection rectifying tower tower body about 31, above every root thrust-augmenting nozzle 312, be equipped with a conical fairing cap 313, the inwall of conical fairing cap 313 is connected by the top of some poles 314 with thrust-augmenting nozzle 312, upper packing layer 38 is one deck Stainless Steel Helices layer, lower packing layer 39 comprises some layers of Stainless Steel Helices layer, is provided with cavity between neighbouring two Stainless Steel Helices layers.
Use the method for the device fabrication methyl-sulfate of this production methyl-sulfate, comprise following three phases:
A) Esterification Stage:
The gas of dimethyl ether sent here in dme workshop makes dme equably be distributed in lower floor tower chamber 123 by pipeline through gas distributor 17 from the gas feed 18 in lower floor's tower chamber 123, after being full of gas of dimethyl ether in lower floor's tower chamber 123, gas of dimethyl ether enters into tower chamber, middle level 122 by the pipeline of pneumatic outlet 19 through esterification reaction tower tower body 11 outside of lower floor's tower chamber 123 top side wall from the gas feed 18 sidewall of tower chamber 122, middle level, be uniformly distributed in tower chamber, middle level 122 by pipeline through gas distributor 17 again, after being full of gas of dimethyl ether in tower chamber, middle level 122, gas of dimethyl ether by tower chamber 122, middle level top side wall the pipeline of pneumatic outlet 19 through esterification reaction tower tower body 11 outside enter into tower chamber, upper strata 121 from the gas feed 18 sidewall of tower chamber 121, upper strata, dme is made to be distributed in tower chamber, upper strata 121 equably by pipeline through gas distributor 17 again, when pressure in whole esterification reaction tower tower body 11 reaches set(ting)value, the material of the pyrosulfuric acid dimethyl ester containing sulphur trioxide is added from its top feed mouth 12, first liquid material enters in the guide shell 16 in tower chamber, upper strata 121, first sulphur trioxide reacts with the gas of dimethyl ether risen from bottom in the guide shell 16 in tower chamber, upper strata 121, sulphur trioxide now in liquid material is excessive, the liquid material containing sulphur trioxide do not reacted completely continues to increase, enter in tower chamber, upper strata 121 after overflowing from the guide shell 16 in tower chamber, upper strata 121, continue to react with the gas of dimethyl ether in tower chamber, upper strata 121, continue to increase to when flooding the fluid inlet 111 of overflow cylinder 110 in tower chamber, upper strata 121 until liquid material, liquid material flows in tower chamber, middle level 122 by this fluid inlet 111 through overflow cylinder 110, continue to react with the gas of dimethyl ether in tower chamber, middle level 121, along with the liquid material in tower chamber, middle level 122 increases gradually, liquid material will overflow in the guide shell 16 in tower chamber, middle level 122, the sulphur trioxide now do not reacted completely in liquid material continues to react further with dme, the liquid material that reaction generates is on the increase to when flooding the fluid inlet 111 of overflow cylinder 110 in tower chamber, middle level 122, liquid material flows in lower floor's tower chamber 123 by this fluid inlet 111 through overflow cylinder 110, in lower floor's tower chamber 123, excessive dme and a small amount of sulphur trioxide react, sulphur trioxide is reacted completely, thus the acidity in material is reduced greatly, reach need of production, the methyl-sulfate crude product extraction from esterification reaction tower material outlet 13 finally generated.Reaction tower is divided into three layers, makes every one deck tower chamber gas-liquid contact absorption can occur, reaction process is shortened, the liquid material of different concns and the dme of different amount can be occurred fully to react.Every one deck tower chamber is all connected with refrigerating unit, water coolant in drum 113 enters the tower chamber of every one deck in through water pump 117 by cooling fluid inlet 115 by liquid outlet 112, the heat produced with esterification process carries out exchange and produces low-pressure steam, low-pressure steam enters drum 113 in by pipeline by inlet mouth 119 through cooling air outlet 114, after low-pressure steam carries out gas-liquid separation in drum 113, steam enters another operation by vapour outlet 120 and carries out heat recovery and utilization, change the method for original circulating water cooling, energy-saving and cost-reducing.
Incomplete, uneven problem is reacted between material in order to solve in common response tower, guide shell 16 is equipped with in every layer of tower chamber, to ensure having enough liquid materials to exist in each tower chamber, gas distributor 17 is provided with in the bottom of guide shell 16, guide shell 16 is set in each tower chamber simultaneously, make gas guide shell 16 acts on, drive liquid rotate again or flow after bottom even distribution, thus make to react completely, uniform, do not stay dead angle.An attaching space effectively can be had to make liquid material and gas material, overflow cylinder 110 serves keying action, when only having material to exceed fluid inlet 111 height of overflow cylinder 110, material just can enter next tower chamber, the setting of overflow cylinder 110 not only ensure that certain liquid height, also ensure that material has the enough reaction times.
Esterification reaction tower tower body 11 is divided into three layers by methyl-sulfate esterification reaction tower 1 of the present invention, the sulphur trioxide of different concns and dme is allowed to react in the tower chamber of different layers, utilize the characteristic of dme simultaneously, make dme excessive thus improve tower internal pressure in tower, whole process is allowed to react under pressurized condition thus to accelerate speed of reaction, and the increase of speed of reaction, temperature of reaction in tower is improved greatly, refrigerating unit is utilized to adopt the measure of external force circulation, the heat in tower is allowed to make to produce low-pressure steam in refrigerating unit, thus accomplished heat recuperation, serve energy-saving effect.Esterification reaction tower of the present invention is exactly that employing three layers designs from the different of common response tower, adopt between layers outside walk gas phase pipeline and inner walk the combination of liquid pipe, the stroke extending material makes fully to contact between material, fully react.In addition, gas phase pipeline is walked in outside, can simplify the structure of esterification reaction tower tower body inside, makes material have sufficient reaction compartment.This methyl-sulfate esterification reaction tower have employed the excessive reaction pattern of dme, sulphur trioxide and dme are fully reacted in the liquid phase, and under pressurized condition, contact between material is better, reaction is more thorough, thus reduce acidity, substantially increase quality product, decrease the quantity of waste residue, reduce cost, alleviate environmental protection pressure.Because the concentration containing sulphur trioxide material in every one deck tower chamber is different, speed and the heat of generation of reaction are also different, refrigerating unit has been provided separately in every one deck tower chamber, adopt the measure of controlled cooling model discharge, thus ensure that the temperature of reaction in every one deck tower chamber, make reaction controlling in optimum range.
B) deaeration stage:
From esterification reaction tower material outlet 13 methyl-sulfate crude product out, enter in degassing tower 2 by pipeline through degassing tower opening for feed 21, because esterification reaction tower 1 temperature of charge is out higher, enter rear some the material generation flash distillation of moment of degassing tower 2, excessive for a part in material dme is steamed, rest materials enters bottom degassing tower 2, then send into the first reboiler 4 by degassing tower liquid outlet 24 by pipeline to heat, gas of dimethyl ether in material is all steamed, get back in degassing tower 2 through degassing tower material steam mouth 25 again, the gas of dimethyl ether steamed is recycled by pipeline by degassing tower air outlet 23 in absorption tower inlet mouth feeding absorption tower, decrease the waste of raw material, reduce production cost, safety and environmental protection.Remove the methyl-sulfate material after dme to be entered in rectifying tower 3 by opening for feed 32 through product pump 5 by pipeline through degassing tower discharge port 22 and carry out rectifying.Deaeration stage is that the quality of methyl-sulfate is purified, good basis has been established in the supplies consumption of reduction dme.
C) stage of rectification:
The rectifying of rectifying tower 3, comprises as the next stage:
A () produces the preparatory stage of driving:
When producing driving, open negative pressure system, make to be in negative pressure in rectifying tower tower body 31, to reduce the boiling point of material, after thick for the methyl-sulfate removing dme material is entered rectifying tower tower body 31 from opening for feed 32, material is evenly distributed through liquid distributor 33 by pipeline, the material be evenly distributed passes downwardly through the bottom that lower packing layer 39 enters rectifying tower tower body 31, the second reboiler 315 is entered again by bottom rectifying tower material outlet 316, when material bottom rectifying tower tower body 31 reach a certain height, open the second reboiler 315 pairs of materials to heat, steam is become by the material after heating, enter in rectifying tower tower body 31 toward rising from material steam mouth 35, in the process that steam rises under process during packing layer 39, part heavy constituent material condensation can become liquid toward declining, remaining gas continues toward rising, then enter in the rectifying tower tower body 31 above gas-liquid separation device by the space between the thrust-augmenting nozzle 312 of gas-liquid separation device and conical fairing cap 313, now due to firm driving, the temperature of tower top is lower, therefore the methyl-sulfate liquid that portion gas is condensed into low-purity is had, discharge port 34 extraction from the side, using as phlegma in the rectifying tower tower body 31 of condenser 310 condensed low-purity methyl-sulfate liquid above pipeline is back to upper packing layer 38 again of discharge port 34 extraction from the side, remaining portion gas obtains the methyl-sulfate liquid of low-purity after top discharge mouth 36 extraction through condensation, also be sent back in the rectifying tower tower body 31 above packing layer 38 and use as phlegma, by that analogy, after repeating backflow several times, the methyl-sulfate purity liquid of discharge port 34 extraction from the side slowly improves, after the purity bringing up to requirement, obtain highly purified methyl-sulfate liquid, then enter formal stage of rectification,
(b) formal stage of rectification:
During formal stage of rectification, temperature in rectifying tower tower body 31 is higher, after thick for methyl-sulfate material is entered rectifying tower tower body 31 from opening for feed 32, material is evenly distributed through liquid distributor 33 by pipeline, the material be evenly distributed with enter the high-temperature gas risen in rectifying tower tower body 31 from material steam mouth 35 and mix, some material generation flash distillation, and remainder material becomes gas after passing downwardly through the high-temperature gas Hybrid Heating of some layers of Stainless Steel Helices layers continuation and rising successively, continue to rise after gas after heating and the gas and vapor permeation of flash distillation, then enter in the rectifying tower tower body 31 above gas-liquid separation device by the space between the thrust-augmenting nozzle 312 of gas-liquid separation device and conical fairing cap 313, now a part of light-component gas is from top discharge mouth 36 extraction, no longer send back in the rectifying tower tower body 31 above packing layer 38, but the methyl-sulfate that obtained purity is slightly low after condensation is admitted to the first outside storage tank storage for using by oneself or selling, and remaining heavy constituent gas rise time with the high-purity dimethyl sulfate liquid through condenser 310 condensation refluxed above upper packing layer 38 after upper packing layer 38 contacts, be condensed into liquid material, discharge port 34 extraction from the side, namely highly purified methyl-sulfate liquid is obtained.Most high-purity dimethyl sulfate is admitted to the second outside storage tank and saves as product sale, and another a fraction of high-purity dimethyl sulfate comes back in the rectifying tower tower body 31 above upper packing layer 38 by pipeline after condenser 310 condensation, continue backflow as phlegma to contact with the gas in rectifying tower tower body 31 above gas-liquid separation device, highly purified methyl-sulfate uses as phlegma through condensation, the temperature of phlegma can be controlled on the one hand by condenser 310, the purity of methyl-sulfate can also be improved on the other hand, kill two birds with one stone; In addition the material of difficult volatilization is after lower packing layer 39 multilayer is separated, enter bottom rectifying tower tower body 31, constantly heated by the second reboiler 315 again and volatile component substance is proposed, concentration can be more and more higher bottom rectifying tower tower body 31 for remaining difficulty volatilization heavy component material, finally according to index situation from waste liquid outlet 37 extraction.
Packing layer 38 and lower packing layer 39 is provided with, to extend the stroke of gas-to-liquid contact exchange in rectifying tower tower body 31.In order to increase the useful area in rectifying tower tower body 31, material being uniformly distributed, bias current not occurring, opening for feed 32 connects liquid distributor 33 by pipeline, utilizes liquid distributor 33 feed liquid to be evenly distributed.In order to improve the purity of product, in rectifying tower tower body 31 between opening for feed 32 and side discharge port 34, gas-liquid separation device is set, by gas-liquid separation device, rectifying tower tower body 31 is separated into two sections, and be provided with two discharge ports in the middle and upper part of rectifying tower tower body 31 and top, light constituent is allowed to be separated with heavy constituent, thus reach and allow different mixtures in material carry out the object be separated, solve the problem of polycomponent mixing in methyl-sulfate, improve the purity of product.Opening for feed 32 is located at the middle part of rectifying tower tower body 31, material enters from the middle part of rectifying tower tower body 31, because the temperature in the middle part of rectifying tower tower body 31 is higher, some methyl-sulfate generation flash distillation after material is entered, thus decrease the pressure of rectifying tower tower body 31 bottom, improve the rectification efficiency of rectifying tower tower body 31, reduce energy consumption, thus substantially increase production efficiency, reduce production cost, improve output, avoid the impact of its top feed on quality product simultaneously.
Adopt and produce the device fabrication methyl-sulfate of methyl-sulfate and the different of original production method, mainly contain following some:
(1) discontinuity that original esterification technique adopts operates, and uses the device structure form of several esterification tank, adopt the inexcessive reactive mode of dme to carry out, and the present invention is the device structure form adopting esterification reaction tower, adopts the reactive mode that dme is excessive;
(2) the production technique index of what original esterification technique adopted is normal pressure, low temperature, utilize pattern that recirculated water is lowered the temperature to reaction process to control indicator reaction, and pressurization, the situation of heating that the present invention adopts get off to improve speed of reaction, not only save the energy consumption of circulating water cooling, and the heat utilizing reaction to produce, the low-pressure steam of formation can be used for other post to use;
(3) original esterification and distillation are that discontinuity operates, and be distinct two posies, and the present invention are connected together esterification process and rectifying by degassing tower 2, achieve the continuity operation in two posies;
(4) what existing product purified employing is distil process, and be the device structure form that have employed reaction autoclave, operation is discontinuity, and the present invention purifies product to change rectification process from distil process, have employed the device structure form that rectifying is tower, achieve continuous operation.
Claims (4)
1. produce the equipment of methyl-sulfate for one kind, it is characterized in that: comprise esterification reaction tower, degassing tower and rectifying tower, the its top feed mouth of esterification top of tower is connected with liquids material source by pipeline, the esterification reaction tower material outlet of esterification tower bottom is connected with the degassing tower opening for feed in the middle part of degassing tower by pipeline, bottom degassing tower, the degassing tower discharge port of side is connected with the opening for feed in the middle part of rectifying tower through product pump by pipeline, the top discharge mouth at rectifying tower top is connected with the first outside storage tank by pipeline, the side discharge port of rectifying tower middle and upper part is connected with the second outside storage tank by pipeline, the degassing tower air outlet at degassing tower top is connected with the absorption tower inlet mouth on absorption tower by pipeline, the degassing tower liquid outlet of degassing tower bottom is connected with the degassing tower material steam mouth of degassing tower through the first reboiler by pipeline, described esterification reaction tower comprises esterification reaction tower tower body, its top feed mouth and esterification reaction tower material outlet is respectively equipped with at the top of esterification reaction tower tower body and bottom, on by upper column plate setting up and down and lower column plate esterification reaction tower tower body inside being divided into from top to bottom successively in esterification reaction tower tower body, in, lower three layers of tower chamber, three layers of tower chamber are connected with a refrigerating unit respectively, the guide shell that an open top end is arranged is equipped with in the mid-way, bottom in every layer of tower chamber, a gas distributor is equipped with in the bottom of each guide shell, each gas distributor is connected with the gas feed be located on this layer of tower chamber sidewall respectively by a pipeline, gas feed on the sidewall of last layer tower chamber is connected with the pneumatic outlet being located at lower one deck tower chamber top side wall by the pipeline be located at outside esterification reaction tower tower body, the gas feed in orlop tower chamber is connected with source of the gas by pipeline, upper, the overflow cylinder that one is positioned at the connection two tower chamber outside guide shell is provided with between tower chamber, middle level, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, in, the overflow cylinder that one is positioned at the connection two tower chamber outside guide shell is provided with between lower floor's tower chamber, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, be positioned at the top of fluid inlet position higher than tower chamber, middle level inner draft tube of the overflow cylinder in tower chamber, middle level, described rectifying tower comprises rectifying tower tower body, an opening for feed is provided with at the middle part of rectifying tower tower body side, opening for feed is connected with by pipeline the liquid distributor that is located at rectifying tower tower body inside, side discharge port and material steam mouth is respectively equipped with in the middle and upper part of rectifying tower tower body opposite side and bottom, a top discharge mouth is provided with at the top of rectifying tower tower body, waste liquid outlet and rectifying tower material outlet is respectively equipped with in the bottom of rectifying tower tower body, rectifying tower material outlet is connected with material steam mouth through the second reboiler by pipeline, be horizontally arranged with one in rectifying tower tower body between opening for feed and side discharge port and rectifying tower tower body inside is divided into upper and lower two-part gas-liquid separation device, packing layer and lower packing layer is respectively equipped with in rectifying tower tower body above and below gas-liquid separation device, side discharge port is communicated with a Y-tube, the Single port of Y-tube is connected with outside storage tank by pipeline, another port is connected with the rectifying tower tower body inside above upper packing layer through condenser by pipeline.
2. a kind of equipment producing methyl-sulfate according to claim 1, it is characterized in that: described refrigerating unit comprises a drum and the cooling air outlet on the sidewall of tower chamber setting up and down and cools fluid inlet, the cooling duct being communicated with cooling air outlet and cooling fluid inlet is provided with in tower chamber, cooling fluid inlet is connected with the liquid outlet of drum through water pump by the pipeline being located at esterification reaction tower tower body outside, cooling air outlet is connected with the inlet mouth of drum by the pipeline being located at esterification reaction tower tower body outside, is provided with a vapour outlet at the top of drum.
3. a kind of equipment producing methyl-sulfate according to claim 1, it is characterized in that: described gas-liquid separation device comprises the plate body of an arranged transversely, plate body is vertically provided with the some upper and lower two-part thrust-augmenting nozzles of connection rectifying tower tower body, above every root thrust-augmenting nozzle, be equipped with a conical fairing cap, the inwall of conical fairing cap is connected by the top of some poles and thrust-augmenting nozzle.
4., according to the arbitrary described a kind of equipment producing methyl-sulfate of claim 1,2 or 3, it is characterized in that: described upper packing layer is one deck Stainless Steel Helices layer; Described lower packing layer comprises some layers of Stainless Steel Helices layer, is provided with cavity between neighbouring two Stainless Steel Helices layers.
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| CN106518731B (en) * | 2016-08-31 | 2018-02-16 | 湖北远大富驰医药化工股份有限公司 | Dimethyl suflfate purified product automates separator |
| CN106699610B (en) * | 2016-12-21 | 2019-01-18 | 武汉青江化工黄冈有限公司 | The dimethyl suflfate production process and device of low content dimethyl ether |
| JP7181463B2 (en) * | 2019-01-29 | 2022-12-01 | セントラル硝子株式会社 | Method for producing fluorine-containing ether |
| CN109748827B (en) * | 2019-02-03 | 2021-09-14 | 山东凯瑞英材料科技有限公司 | Process for continuous synthesis of dimethyl sulfate |
| CN110513906A (en) * | 2019-08-23 | 2019-11-29 | 北京石油化工工程有限公司 | A kind of chemical reaction low temperature heat cooling system and method |
| CN115920593B (en) * | 2022-11-25 | 2024-05-31 | 新疆敦华绿碳技术股份有限公司 | Absorption device based on double desorption units and production system |
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