CN103570590A - Equipment for producing dimethyl sulfate - Google Patents
Equipment for producing dimethyl sulfate Download PDFInfo
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- CN103570590A CN103570590A CN201310528752.0A CN201310528752A CN103570590A CN 103570590 A CN103570590 A CN 103570590A CN 201310528752 A CN201310528752 A CN 201310528752A CN 103570590 A CN103570590 A CN 103570590A
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Abstract
The invention relates to the field of chemical industry, and in particular discloses equipment for producing dimethyl sulfate. The equipment for producing dimethyl sulfate comprises an esterification reaction tower, a degassing tower and a rectifying tower, wherein a top feeding hole formed at the top of the esterification reaction is communicated with a liquid material source through a pipeline; an esterification reaction tower material outlet formed on the bottom of the esterification reaction tower is communicated with a degassing tower feeding hole formed at the middle part of the degassing tower; the top discharge hole formed at the top of the rectifying tower is communicated with a first storage tank located outside through a pipeline; a side surface discharge hole formed on the middle upper part of the rectifying tower is communicated with a second storage tank located outside; a degassing tower gas outlet formed at the top of the degassing tower is communicated with the absorption tower gas inlet of an absorption tower. The equipment for producing dimethyl sulfate has the beneficial effect that the whole production process realizes continuous production, the reaction is more sufficient, the capacity and the product quality are greatly improved, the operation is automatically controlled completely, and the production is safer and more efficient.
Description
(1) technical field
The present invention relates to chemical field, particularly a kind of equipment of 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, the production of discontinuity exists reaction not exclusively, 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, innovation and the progress of enterprise have seriously been restricted.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of and can produce continuously, make the equipment 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, reduce the production methyl-sulfate of product acidity, safety and environmental protection.
The present invention is achieved through the following technical solutions:
A kind of equipment of producing methyl-sulfate, comprise esterification reaction tower, degassing tower and rectifying tower, the top fed 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 at degassing tower middle part by pipeline, the degassing tower discharge port of degassing tower bottom one side is connected with the opening for feed at rectifying tower middle part 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, top and bottom at esterification reaction tower tower body are respectively equipped with top fed mouth and esterification reaction tower material outlet, on esterification reaction tower tower body inside being divided into from top to bottom successively by upper column plate setting up and down and lower column plate 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, in the mid-way, bottom in every layer of tower chamber, be equipped with the open guide shell arranging in a top, in the bottom of each guide shell, be equipped with a gas distributor, each gas distributor respectively by a pipeline be located at this layer of gas feed on the sidewall of tower chamber and be connected, gas feed on the sidewall of last layer tower chamber is connected with the pneumatic outlet that is located at lower one deck tower chamber top side wall by the pipeline being 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, between tower chamber, middle level, be provided with an overflow cylinder that is positioned at the connection two tower chambeies in guide shell outside, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, in, between lower floor's tower chamber, be provided with an overflow cylinder that is positioned at the connection two tower chambeies in guide shell outside, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, be positioned at the fluid inlet position of overflow cylinder in tower chamber, middle level higher than the top of tower chamber, middle level inner draft tube.
Described refrigerating unit comprises a drum and cooling air outlet and cooling fluid inlet on the sidewall of tower chamber setting up and down, in tower chamber, be provided with the cooling duct that is communicated with cooling air outlet and cooling fluid inlet, cooling fluid inlet is connected with the liquid outlet of drum through water pump by being located at the pipeline of esterification reaction tower tower body outside, cooling air outlet is connected with the inlet mouth of drum by being located at the pipeline of esterification reaction tower tower body outside, at the top of drum, is provided with a vapour outlet.
Described rectifying tower comprises rectifying tower tower body, middle part in rectifying tower tower body one side is provided with an opening for feed, opening for feed is connected with a liquid distributor that is located at rectifying tower tower body inside by pipeline, middle and upper part and bottom at rectifying tower tower body opposite side are respectively equipped with side discharge port and material steam mouth, at the top of rectifying tower tower body, be provided with a top discharge mouth, in the bottom of rectifying tower tower body, be respectively equipped with waste liquid outlet and rectifying tower material outlet, rectifying tower material outlet is connected with material steam mouth through the second reboiler by pipeline, in rectifying tower tower body between opening for feed and side discharge port, be horizontally arranged with one rectifying tower tower body inside is divided into upper and lower two-part gas-liquid separation device, in the rectifying tower tower body of gas-liquid separation device above and below, be respectively equipped with packing layer and lower packing layer, side discharge port is communicated with a Y-tube, one port of Y-tube is connected with outside storage tank by pipeline, another port is connected with the rectifying tower tower body inside of upper packing layer top through condenser by pipeline.
Described gas-liquid separation device comprises the plate body of an arranged transversely, on plate body, be vertically provided with the some upper and lower two-part thrust-augmenting nozzles of connection rectifying tower tower body, above every 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, between neighbouring two Stainless Steel Helices layers, is provided with cavity.
The beneficial effect that the present invention produces the equipment of methyl-sulfate is: having solved methyl-sulfate whole production line can not fully automated, can not operate continuously and quantity-produced problem, make whole production process realize serialization production, esterification process is from normal pressure, low temperature has become pressurization, under warm-up mode, carry out, react more complete, simultaneously by-product low-pressure steam, accomplished energy-saving and cost-reducing effect, esterification reaction rate and the esterification yield of esterification process have been improved, effectively increased the Long contact time of dme and sulphur trioxide in methyl-sulfate esterification process, guaranteed the excessive response of dme, thereby make sulphur trioxide energy complete reaction, reduced the acidity of product, for the fine work of methyl-sulfate, purify and accelerated speed, reduced the generation of waste residue, reached energy-conservation, the object of environmental protection, after utilizing degassing tower that the dme in material is deviate from, the dme of deviating from is sent in absorption tower and recycled, reduced the waste of raw material, reduced production cost, safety and environmental protection, changed original distil process, made rectification process produce and become serialization production from original discontinuity, greatly improved production capacity and quality product, made to operate fully automated and control, reduced security risk, made to produce 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 local enlarged diagram of the interior thrust-augmenting nozzle of rectifying tower 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 top fed 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
In order to make technology of the present invention, feature, object and effect etc. be easier to understand, understand, below in conjunction with accompanying drawing of the present invention, technical scheme of the present invention is carried out to clear, complete description, but the present invention is not limited thereto.
As shown in Fig. 1-Fig. 4, this embodiment comprises esterification reaction tower 1, degassing tower 2 and rectifying tower 3, the top fed mouth 12 at esterification reaction tower 1 top is connected with liquids material source by pipeline, the esterification reaction tower material outlet 13 of esterification reaction tower 1 bottom is connected with the degassing tower opening for feed 21 at degassing tower 2 middle parts by pipeline, the degassing tower discharge port 22 of degassing tower 2 bottom one sides is connected with the opening for feed 32 at rectifying tower 3 middle parts through product pump 5 by pipeline, the top discharge mouth 36 at rectifying tower 3 tops is connected with the first outside storage tank by pipeline, the side discharge port 34 of rectifying tower 3 middle and upper parts is connected with the second outside storage tank by pipeline, the degassing tower air outlet 23 at degassing tower 2 tops is connected with the absorption tower inlet mouth on absorption tower by pipeline, the degassing tower liquid outlet 24 of degassing tower 2 bottoms 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, top and bottom at esterification reaction tower tower body 11 are respectively equipped with top fed mouth 12 and esterification reaction tower material outlet 13, on esterification reaction tower tower body 11 inside being divided into from top to bottom successively by upper column plate 14 setting up and down and lower column plate 15 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, in the mid-way, bottom in every layer of tower chamber, be equipped with the open guide shell 16 arranging in a top, in the bottom of each guide shell 16, be equipped with a gas distributor 17, each gas distributor 17 respectively by a pipeline be located at this layer of gas feed 18 on the sidewall of tower chamber and be connected, gas feed 18 on the sidewall of last layer tower chamber is connected with the pneumatic outlet 19 that is located at lower one deck tower chamber top side wall by the pipeline being 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, between tower chamber, middle level, be provided with an overflow cylinder 110 that is positioned at the connection two tower chambeies in guide shell 16 outsides, the top and bottom of this overflow cylinder 110 are respectively equipped with a fluid inlet 111 and liquid outlet 112, in, between lower floor's tower chamber, be provided with an overflow cylinder 110 that is positioned at the connection two tower chambeies in guide shell 16 outsides, the top and bottom of this overflow cylinder 110 are respectively equipped with a fluid inlet 111 and liquid outlet 112, be positioned at fluid inlet 111 positions of overflow cylinder 110 in tower chamber, middle level 122 higher than the top of tower chamber, middle level 122 inner draft tubes 16, refrigerating unit comprises a drum 113 and cooling air outlet 114 and cooling fluid inlet 115 on the sidewall of tower chamber setting up and down, in tower chamber, be provided with the cooling duct 116 that is communicated with cooling air outlet 114 and cooling fluid inlet 115, cooling fluid inlet 115 is connected with the liquid outlet 118 of drum 113 through water pump 117 by being located at the pipeline of esterification reaction tower tower body 11 outsides, cooling air outlet 114, by being located at the pipeline of esterification reaction tower tower body 11 outsides and the inlet mouth 119 of drum 113 is connected, is provided with a vapour outlet 120 at the top of drum 113.
Rectifying tower 3 comprises rectifying tower tower body 31, at the middle part of rectifying tower tower body 31 1 sides, be provided with an opening for feed 32, opening for feed 32 is connected with a liquid distributor 33 that is located at rectifying tower tower body 31 inside by pipeline, middle and upper part and bottom at rectifying tower tower body 31 opposite sides are respectively equipped with side discharge port 34 and material steam mouth 35, at the top of rectifying tower tower body 31, be provided with a top discharge mouth 36, in the bottom of rectifying tower tower body 31, be respectively equipped with waste liquid outlet 37 and rectifying tower material outlet 316, rectifying tower material outlet 316 is connected with material steam mouth 35 through the second reboiler 315 by pipeline, in rectifying tower tower body 31 between opening for feed 32 and side discharge port 34, be horizontally arranged with one rectifying tower tower body 31 inside are divided into upper and lower two-part gas-liquid separation device, in the rectifying tower tower body 31 of gas-liquid separation device above and below, be respectively equipped with packing layer 38 and lower packing layer 39, side discharge port 34 is communicated with a Y-tube, one port of Y-tube is connected with outside storage tank by pipeline, another port is connected with rectifying tower tower body 31 inside of upper packing layer 38 tops through condenser 310 by pipeline, gas-liquid separation device comprises the plate body 311 of an arranged transversely, on plate body 311, be vertically provided with the some upper and lower two-part thrust-augmenting nozzles 312 of connection rectifying tower tower body 31, above every thrust-augmenting nozzle 312, be equipped with a conical fairing cap 313, the inwall of conical fairing cap 313 is connected by some poles 314 and the top of 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, between neighbouring two Stainless Steel Helices layers, is provided with cavity.
The method of using the device fabrication methyl-sulfate of this production methyl-sulfate, comprises following three phases:
A) Esterification Stage:
The gas of dimethyl ether that dme workshop is sent here is equably distributed in lower floor tower chamber 123 dme by pipeline through gas distributor 17 from the gas feed 18 in lower floor's tower chamber 123, in lower floor's tower chamber 123, be full of after gas of dimethyl ether, through the pipeline of esterification reaction tower tower body 11 outsides, the gas feed 18 from 122 sidewalls of tower chamber, middle level enters into tower chamber, middle level 122 to the pneumatic outlet 19 of gas of dimethyl ether by lower floor's tower chamber 123 top side wall, by pipeline, through gas distributor 17, be uniformly distributed in tower chamber, middle level 122 again, in tower chamber, middle level 122, be full of after gas of dimethyl ether, gas of dimethyl ether by tower chamber, middle level 122 top side wall pneumatic outlet 19 through the pipeline of esterification reaction tower tower body 11 outsides, the gas feed 18 from 121 sidewalls of tower chamber, upper strata enters into tower chamber, upper strata 121, by pipeline, through gas distributor 17, dme is distributed in tower chamber, upper strata 121 equably again, when the pressure in whole esterification reaction tower tower body 11 reaches set(ting)value, the material that adds the pyrosulfuric acid dimethyl ester that contains sulphur trioxide from top fed 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 rising from bottom in the guide shell 16 in tower chamber, upper strata 121, now the sulphur trioxide in liquid material is excessive, the liquid material that contains sulphur trioxide not reacting completely continues to increase, after overflowing from the guide shell 16 in tower chamber, upper strata 121, enter in tower chamber, upper strata 121, continue to react with the gas of dimethyl ether in tower chamber, upper strata 121, until liquid material, continue to increase when flooding the fluid inlet 111 of tower chamber, upper strata 121 interior overflow cylinders 110, liquid material flows in tower chamber, middle level 122 through overflow cylinder 110 by this fluid inlet 111, 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 not reacting completely in liquid material continues further to react with dme, the liquid material that reaction generates is on the increase when flooding the fluid inlet 111 of tower chamber, middle level 122 interior overflow cylinders 110, liquid material flows in lower floor's tower chamber 123 through overflow cylinder 110 by this fluid inlet 111, in lower floor's tower chamber 123, excessive dme reacts with a small amount of sulphur trioxide, sulphur trioxide is reacted completely, thereby the acidity in material is reduced greatly, reached need of production, the methyl-sulfate crude product extraction from esterification reaction tower material outlet 13 finally generating.Reaction tower is divided into three layers, makes every one deck tower chamber that gas-to-liquid contact can occur and absorb, reaction process is shortened, allow the liquid material of different concns and the dme of different amounts that fully reaction can occur.Every one deck tower chamber is all connected with refrigerating unit, water coolant in drum 113 is entered in the tower chamber of every one deck by liquid outlet 112 through water pump 117 by cooling fluid inlet 115, the heat producing with esterification process exchanges generation low-pressure steam, low-pressure steam is entered in drum 113 by inlet mouth 119 by pipeline through cooling air outlet 114, low-pressure steam is carried out after gas-liquid separation in drum 113, steam enters another operation by vapour outlet 120 and carries out heat recovery and utilization, changed original method with circulating water cooling, energy-saving and cost-reducing.
In order to solve, in common response tower, between material, react incomplete, inhomogeneous problem, in every layer of tower chamber, be equipped with guide shell 16, to guarantee having enough liquid materials to exist in each tower chamber, in the bottom of guide shell 16, be provided with gas distributor 17, in each tower chamber, guide shell 16 is set simultaneously, make gas under guide shell 16 effects, drive liquid to rotate again or flow from bottom even distributes, thereby make to react completely, uniform, do not stay dead angle.In order to make liquid material and gas material can have an attaching space effectively, overflow cylinder 110 has played keying action, while only having material to surpass fluid inlet 111 height of overflow cylinder 110, material just can enter next tower chamber, the setting of overflow cylinder 110 has not only guaranteed certain liquid height, has also guaranteed that material has the enough reaction times.
Methyl-sulfate esterification reaction tower 1 of the present invention is divided into three layers by esterification reaction tower tower body 11, allow sulphur trioxide and the dme of different concns react in the tower chamber of different layers, utilize the characteristic of dme simultaneously, thereby allow dme excessive raising tower internal pressure in tower, thereby allow whole process react and to have accelerated speed of reaction in pressurization situation, and the increase of speed of reaction, temperature of reaction in tower is improved greatly, utilize refrigerating unit to adopt the measure of external forced circulation, allow heat in tower make to produce in refrigerating unit low-pressure steam, thereby accomplished heat recuperation, played energy-saving effect.Esterification reaction tower of the present invention is exactly to adopt three layers of design from the different of common response tower, adopts between layers outside gas phase pipeline and the inner combination of walking liquid pipe walked, and the stroke that extends material makes fully contact between material, fully reaction.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 has adopted the excessive reaction pattern of dme, make the fully reaction in liquid phase of sulphur trioxide and dme, and in pressurization situation, contact between material is better, reaction is more thorough, thereby reduced acidity, greatly improved quality product, reduced the quantity of waste residue, reduce cost, alleviated environmental protection pressure.The concentration that contains sulphur trioxide material due to every one deck tower chamber is different, the speed of reaction and the heat of generation are also different, in every one deck tower chamber, be separately provided with refrigerating unit, adopt the measure of controlling cooling water flow, thereby guaranteed the temperature of reaction in every one deck tower chamber, reaction is controlled in optimum range.
B) deaeration stage:
From esterification reaction tower material outlet 13 methyl-sulfate crude product out, by pipeline, through degassing tower opening for feed 21, enter in degassing tower 2, because esterification reaction tower 1 temperature of charge is out higher, enter degassing tower 2 some material generation flash distillation of rear moment, the excessive dme of a part in material is steamed, rest materials enters degassing tower 2 bottoms, then by degassing tower liquid outlet 24, by pipeline, send into the first reboiler 4 heating, gas of dimethyl ether in material is all steamed, through degassing tower material steam mouth 25, get back in degassing tower 2 again, the gas of dimethyl ether steaming is sent in absorption tower and is recycled through absorption tower inlet mouth by pipeline by degassing tower air outlet 23, reduced the waste of raw material, reduced production cost, safety and environmental protection.Removing methyl-sulfate material after dme is entered and in rectifying tower 3, is carried out rectifying by opening for feed 32 through product pump 5 by pipeline through degassing tower discharge port 22.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, comprised as the next stage:
(a) produce the preparatory stage of driving:
Produce while driving, open negative pressure system, make in rectifying tower tower body 31 in negative pressure, to reduce the boiling point of material, by the thick material of the methyl-sulfate that removes dme from opening for feed 32 enters rectifying tower tower body 31, by pipeline, through liquid distributor 33, material is evenly distributed, the material being evenly distributed enters the bottom of rectifying tower tower body 31 downwards by lower packing layer 39, by bottom rectifying tower material outlet 316, enter the second reboiler 315 again, when the material of rectifying tower tower body 31 bottoms reach a certain height, opening 315 pairs of materials of the second reboiler heats, material after being heated becomes steam, from material steam mouth 35, enter rectifying tower tower body 31 interior toward rising, in the process of steam rising under process during packing layer 39, part heavy constituent material can condensation become liquid toward declining, remaining gas continues toward rising, then thrust-augmenting nozzle 312 and the space between conical fairing cap 313 by gas-liquid separation device enters in the rectifying tower tower body 31 of gas-liquid separation device top, now due to firm driving, the temperature of tower top is lower, therefore have the methyl-sulfate liquid that portion gas is condensed into low-purity, discharge port 34 extraction from the side, discharge port 34 extraction from the side through the condensed low-purity methyl-sulfate of condenser 310 liquid, through pipeline, be again back to that the rectifying tower tower body 31 of upper packing layer 38 tops is interior to be used as phlegma, remaining portion gas obtains the methyl-sulfate liquid of low-purity by condensation from 36 extraction of top discharge mouth, also be sent back to that the rectifying tower tower body 31 of packing layer 38 tops is interior to be used as phlegma, by that analogy, after repeating to reflux several times, the methyl-sulfate purity liquid of discharge port 34 extraction from the side slowly improves, after bringing up to the purity of 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, by the thick material of methyl-sulfate from opening for feed 32 enters rectifying tower tower body 31, by pipeline, through liquid distributor 33, material is evenly distributed, the material being evenly distributed mixes with the high-temperature gas that enters the 31 interior risings of rectifying tower tower body from material steam mouth 35, some material generation flash distillation, and become gas after the high-temperature gas Hybrid Heating that remainder material can continue by some layers of Stainless Steel Helices layer successively and rise downwards, after mixing with the gas of flash distillation, continues gas after heating to rise, then thrust-augmenting nozzle 312 and the space between conical fairing cap 313 by gas-liquid separation device enters in the rectifying tower tower body 31 of gas-liquid separation device top, now a part of light-component gas is from 36 extraction of top discharge mouth, no longer send back in the rectifying tower tower body 31 of packing layer 38 tops, but make the methyl-sulfate that purity is slightly low after condensation, be admitted to the first outside storage tank stores for personal or sale, and remaining heavy constituent gas when rising with the high-purity dimethyl sulfate liquid through condenser 310 condensations of backflow above upper packing layer 38 after upper packing layer 38 contacts, be condensed into liquid material, discharge port 34 extraction from the side, obtain highly purified methyl-sulfate liquid.Most high-purity dimethyl sulfate is admitted to the second outside storage tank stores and sells as product, and another a fraction of high-purity dimethyl sulfate comes back in the rectifying tower tower body 31 of upper packing layer 38 tops by pipeline after condenser 310 condensations, the gas that continues to reflux with in gas-liquid separation device top rectifying tower tower body 31 as phlegma contacts, highly purified methyl-sulfate is used as phlegma through condensation, can control by condenser 310 temperature of phlegma on the one hand, can also improve the purity of methyl-sulfate on the other hand, kill two birds with one stone; In addition the material of difficult volatilization is after lower packing layer 39 multilayer separation, enter rectifying tower tower body 31 bottoms, by the second reboiler 315, constantly heat volatile component substance is proposed again, remaining difficult volatilization heavy component material can be more and more higher in rectifying tower tower body 31 bottom concentration, finally according to index situation from waste liquid outlet 37 extraction.
In rectifying tower tower body 31, be provided with packing layer 38 and lower packing layer 39, to extend the stroke of gas-to-liquid contact exchange.In order to increase the useful area in rectifying tower tower body 31, material is uniformly distributed, there is not bias current, opening for feed 32 connects liquid distributor 33 by pipeline, utilizes liquid distributor 33 that feed liquid is evenly distributed.In order to improve the purity of product, the interior gas-liquid separation device that arranges of rectifying tower tower body 31 between opening for feed 32 and side discharge port 34, by gas-liquid separation device, rectifying tower tower body 31 is separated into two sections, and be provided with two discharge ports at middle and upper part and the top of rectifying tower tower body 31, make light constituent separated with heavy constituent, thereby reached, allow different mixtures in material carry out separated object, solved the problem that in methyl-sulfate, polycomponent mixes, improved the purity of product.Opening for feed 32 is located to the middle part of rectifying tower tower body 31, material enters from the middle part of rectifying tower tower body 31, because the temperature at rectifying tower tower body 31 middle parts is higher, some methyl-sulfate generation flash distillation after material is entered, thereby reduced the pressure of rectifying tower tower body 31 bottoms, improved the rectification efficiency of rectifying tower tower body 31, reduced energy consumption, thereby greatly improved production efficiency, reduced production cost, improved output, avoided the impact of top fed on quality product simultaneously.
Device fabrication methyl-sulfate that adopt to produce methyl-sulfate is different from original production method, mainly contain following some:
(1) discontinuity that original esterification technique adopts operates, and uses the device structure form of several esterification tanks, adopt the inexcessive reactive mode of dme to carry out, and the present invention is the device structure form that adopts esterification reaction tower, adopts the excessive reactive mode of dme;
(2) what original esterification technique adopted is the production technique index of normal pressure, low temperature, utilize recirculated water to control indicator reaction to the pattern of reaction process cooling, and pressurization, the situation of heating that the present invention adopts get off to improve speed of reaction, not only saved the energy consumption of circulating water cooling, and the heat that utilizes reaction to produce, the low-pressure steam of formation can be used for other post;
(3) original esterification and distillation are discontinuity operations, be distinct two posies, and the present invention connect together esterification process and rectifying by degassing tower 2, have realized the continuity operation in two posies;
(4) what existing product was purified employing is distil process, and be the device structure form that has adopted reaction autoclave, operation is discontinuity, and the present invention purifies product to have changed rectification process from distil process, adopt the tower device structure form of rectifying, realized continuous operation.
Claims (6)
1. an equipment of producing methyl-sulfate, it is characterized in that: comprise esterification reaction tower, degassing tower and rectifying tower, the top fed 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 at degassing tower middle part by pipeline, the degassing tower discharge port of degassing tower bottom one side is connected with the opening for feed at rectifying tower middle part 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.
2. a kind of equipment of producing methyl-sulfate according to claim 1, it is characterized in that: described esterification reaction tower comprises esterification reaction tower tower body, top and bottom at esterification reaction tower tower body are respectively equipped with top fed mouth and esterification reaction tower material outlet, on esterification reaction tower tower body inside being divided into from top to bottom successively by upper column plate setting up and down and lower column plate 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, in the mid-way, bottom in every layer of tower chamber, be equipped with the open guide shell arranging in a top, in the bottom of each guide shell, be equipped with a gas distributor, each gas distributor respectively by a pipeline be located at this layer of gas feed on the sidewall of tower chamber and be connected, gas feed on the sidewall of last layer tower chamber is connected with the pneumatic outlet that is located at lower one deck tower chamber top side wall by the pipeline being 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, between tower chamber, middle level, be provided with an overflow cylinder that is positioned at the connection two tower chambeies in guide shell outside, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, in, between lower floor's tower chamber, be provided with an overflow cylinder that is positioned at the connection two tower chambeies in guide shell outside, the top and bottom of this overflow cylinder are respectively equipped with a fluid inlet and liquid outlet, be positioned at the fluid inlet position of overflow cylinder in tower chamber, middle level higher than the top of tower chamber, middle level inner draft tube.
3. a kind of equipment of producing methyl-sulfate according to claim 2, it is characterized in that: described refrigerating unit comprises a drum and cooling air outlet and cooling fluid inlet on the sidewall of tower chamber setting up and down, in tower chamber, be provided with the cooling duct that is communicated with cooling air outlet and cooling fluid inlet, cooling fluid inlet is connected with the liquid outlet of drum through water pump by being located at the pipeline of esterification reaction tower tower body outside, cooling air outlet is connected with the inlet mouth of drum by being located at the pipeline of esterification reaction tower tower body outside, at the top of drum, is provided with a vapour outlet.
4. a kind of equipment of producing methyl-sulfate according to claim 1, it is characterized in that: described rectifying tower comprises rectifying tower tower body, middle part in rectifying tower tower body one side is provided with an opening for feed, opening for feed is connected with a liquid distributor that is located at rectifying tower tower body inside by pipeline, middle and upper part and bottom at rectifying tower tower body opposite side are respectively equipped with side discharge port and material steam mouth, at the top of rectifying tower tower body, be provided with a top discharge mouth, in the bottom of rectifying tower tower body, be respectively equipped with waste liquid outlet and rectifying tower material outlet, rectifying tower material outlet is connected with material steam mouth through the second reboiler by pipeline, in rectifying tower tower body between opening for feed and side discharge port, be horizontally arranged with one rectifying tower tower body inside is divided into upper and lower two-part gas-liquid separation device, in the rectifying tower tower body of gas-liquid separation device above and below, be respectively equipped with packing layer and lower packing layer, side discharge port is communicated with a Y-tube, one port of Y-tube is connected with outside storage tank by pipeline, another port is connected with the rectifying tower tower body inside of upper packing layer top through condenser by pipeline.
5. a kind of equipment of producing methyl-sulfate according to claim 4, it is characterized in that: described gas-liquid separation device comprises the plate body of an arranged transversely, on plate body, be vertically provided with the some upper and lower two-part thrust-augmenting nozzles of connection rectifying tower tower body, above every 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.
6. according to a kind of equipment of producing methyl-sulfate described in claim 4 or 5, 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, between neighbouring two Stainless Steel Helices layers, is provided with cavity.
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| 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 |
| CN115920593A (en) * | 2022-11-25 | 2023-04-07 | 新疆敦华绿碳技术股份有限公司 | Absorption device and production system based on double desorption units |
| 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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