CN103566851B - A kind of dimethyl suflfate esterification reaction tower - Google Patents
A kind of dimethyl suflfate esterification reaction tower Download PDFInfo
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- CN103566851B CN103566851B CN201310528559.7A CN201310528559A CN103566851B CN 103566851 B CN103566851 B CN 103566851B CN 201310528559 A CN201310528559 A CN 201310528559A CN 103566851 B CN103566851 B CN 103566851B
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Abstract
The present invention relates to chemical field, particularly disclose a kind of dimethyl suflfate esterification reaction tower.This dimethyl suflfate esterification reaction tower, comprise tower body, its top feed mouth and material outlet is respectively equipped with at the top of tower body and bottom, on by upper column plate setting up and down and lower column plate tower body inside being divided into from top to bottom successively in tower body, in, lower three layers of tower chamber, three layers of tower chamber are connected with a cooling device respectively, the guide shell that an open top end is arranged is equipped with in the centre position, 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.The invention has the beneficial effects as follows: the Long contact time that effectively can increase dimethyl ether and sulfur trioxide in dimethyl suflfate esterification process, ensure that the excessive response of dimethyl ether, thus make sulfur trioxide energy complete reaction, reduce the acidity of product, make esterification process become continuous seepage from interruption production.
Description
(1) technical field
The present invention relates to chemical field, particularly a kind of dimethyl suflfate esterification reaction tower.
(2) background technology
Reaction tower is the device for being reacted under certain pressure, uniform temperature by two or more material common in Chemical Manufacture, is usually used in gas and liquid countercurrent haptoreaction.Generally, material enters after in tower, under the condition of steam or other outside heat supply (or cooling), makes due to the characteristic of material, chemical reaction to occur between material.Reaction tower major part common in Chemical Manufacture adopts liquid material to enter from tower top (tower side), gas material enters from tower bottom side, the product of final generation is from tower bottom extraction, and the heat exchanger utilizing tower inside to arrange adopts external impetus to carry out the measure of forced circulation to the heat required for reaction, thus ensure the temperature and pressure required for reaction.Existing reaction tower can only meet the simple gas-liquid contact reaction of ordinary material, and for the esterification process of dimethyl suflfate, general simple reaction tower cannot use, because dimethyl ether is a kind of liquid gas, its volatility is very large, if can not have enough spaces and stroke that the sulfur trioxide in itself and liquid phase just cannot be allowed to have enough contact and reach and react completely.
The esterification process of existing dimethyl suflfate is generally adopt esterification tank to carry out, in order to ensure that dimethyl ether fully can react with sulfur trioxide, therefore considerable time is needed to allow it fully react, this just makes production process cause interruption, and reaction or meeting are not exclusively, uneven, reaction speed is slow, reaction efficiency is low, in addition the esterification process of dimethyl suflfate can produce a large amount of heats, and the temperature in the characteristic requirements tank of esterification tank self can not be too high, therefore the outside cooling needing to continue ensures the temperature in esterification tank, energy consumption is high, inconvenience is brought to production work.
(3) summary of the invention
The present invention in order to make up the deficiencies in the prior art, provide a kind of rational in infrastructure, simple to operate, can continuous seepage, make that esterification is full and uniform, reaction speed is fast, production efficiency is high, the dimethyl suflfate esterification reaction tower of energy-saving and cost-reducing, reduction product acidity, safety and environmental protection.
The present invention is achieved through the following technical solutions:
A kind of dimethyl suflfate esterification reaction tower, comprise tower body, its top feed mouth and material outlet is respectively equipped with at the top of tower body and bottom, on by upper column plate setting up and down and lower column plate tower body inside being divided into from top to bottom successively in tower body, in, lower three layers of tower chamber, three layers of tower chamber are connected with a cooling device respectively, the guide shell that an open top end is arranged is equipped with in the centre position, 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 gas vent being located at lower one deck tower chamber top side wall by the pipeline be located at outside 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 an 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 an inlet and liquid outlet, be positioned at the top of inlet position higher than tower chamber, middle level inner draft tube of the overflow cylinder in tower chamber, middle level.
Described cooling device comprises a drum and the cooling gas outlet on the sidewall of tower chamber setting up and down and cools inlet, the cooling pipe being communicated with cooling gas outlet and cooling inlet is provided with in tower chamber, cooling inlet is connected with the liquid outlet of drum through water pump by the pipeline being located at tower body outside, cooling gas outlet is connected by the air inlet of the pipeline with drum that are located at tower body outside, is provided with a steam (vapor) outlet at the top of drum.
The beneficial effect of dimethyl suflfate esterification reaction tower of the present invention is: rational in infrastructure, effectively can increase the Long contact time of dimethyl ether and sulfur trioxide in dimethyl suflfate esterification process, ensure that the excessive response of dimethyl ether, thus make sulfur trioxide energy complete reaction, reduce the acidity of product, fine work for dimethyl suflfate is purified and is accelerated speed, decrease the generation of waste residue, esterification process is made to become continuous seepage from interruption production, improve reaction pressure and temperature, reaction speed is fast, and production efficiency is high; Make esterification more easy to operate, the indices in production is more stable, and whole production process is closed more, continuously, greatly reduce the risk of safety and environmental protection.
(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.
In figure, 1 tower body, 2 its top feed mouths, 3 material outlets, column plate on 4,5 times column plates, 6 guide shells, 7 gas distributors, 8 gas feeds, 9 gas vents, 10 overflow cylinders, 11 inlets, 12 liquid outlets, 13 drums, 14 cooling gas outlets, 15 cooling inlets, 16 cooling pipes, 17 water pumps, 18 liquid outlets, 19 air inlets, 20 steam (vapor) outlets, 21 tower chambeies, upper strata, 22 tower chambeies, middle level, 23 lower floor's tower chambeies.
(5) detailed description of the invention
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 shown in fig. 1, this embodiment comprises tower body 1, its top feed mouth 2 and material outlet 3 is respectively equipped with at the top of tower body 1 and bottom, on by upper column plate 4 setting up and down and lower column plate 5 tower body 1 inside being divided into from top to bottom successively in tower body 1, in, lower three layers of tower chamber, three layers of tower chamber are connected with a cooling device respectively, the guide shell 6 that an open top end is arranged is equipped with in the centre position, bottom in every layer of tower chamber, a gas distributor 7 is equipped with in the bottom of each guide shell 6, each gas distributor 7 is connected with the gas feed 8 be located on this layer of tower chamber sidewall respectively by a pipeline, gas feed 8 on the sidewall of last layer tower chamber is connected with the gas vent 9 being located at lower one deck tower chamber top side wall by the pipeline be located at outside tower body 1, the gas feed 8 in orlop tower chamber is connected with source of the gas by pipeline, upper, the overflow cylinder 10 that one is positioned at the connection two tower chamber outside guide shell 6 is provided with between tower chamber, middle level, the top and bottom of this overflow cylinder 10 are respectively equipped with an inlet 11 and liquid outlet 12, in, the overflow cylinder 10 that one is positioned at the connection two tower chamber outside guide shell 6 is provided with between lower floor's tower chamber, the top and bottom of this overflow cylinder 10 are respectively equipped with an inlet 11 and liquid outlet 12, be positioned at the top of inlet 11 position higher than tower chamber 22, middle level inner draft tube 6 of the overflow cylinder 10 in tower chamber, middle level 22, cooling device comprises a drum 13 and cooling gas outlet on the sidewall of tower chamber setting up and down 14 and cooling inlet 15, the cooling pipe 16 being communicated with cooling gas outlet 14 and cooling inlet 15 is provided with in tower chamber, cooling inlet 15 is connected with the liquid outlet 18 of drum 13 through water pump 17 by the pipeline being located at tower body 1 outside, cooling gas outlet 14 is connected by the air inlet 19 of the pipeline with drum 13 that are located at tower body 1 outside, is provided with a steam (vapor) outlet 20 at the top of drum 13.
Dimethyl ether is made equably to be distributed in lower floor tower chamber 23 by pipeline through gas distributor 7 from the gas feed 8 in lower floor's tower chamber 23 gas of dimethyl ether, after being full of gas of dimethyl ether in lower floor's tower chamber 23, gas of dimethyl ether enters into tower chamber, middle level 22 by the pipeline of gas vent 9 through tower body 1 outside of lower floor's tower chamber 23 top side wall from the gas feed 8 sidewall of tower chamber 22, middle level, be uniformly distributed in tower chamber, middle level 22 by pipeline through gas distributor 7 again, after being full of gas of dimethyl ether in tower chamber, middle level 22, gas of dimethyl ether by tower chamber 22, middle level top side wall the pipeline of gas vent 9 through tower body 1 outside enter into tower chamber, upper strata 21 from the gas feed 8 sidewall of tower chamber 21, upper strata, dimethyl ether is made to be distributed in tower chamber, upper strata 21 equably by pipeline through gas distributor 7 again, when pressure in whole tower body 1 reaches setting value, the material of the pyrosulfuric acid dimethyl ester containing sulfur trioxide is added from its top feed mouth 2, first liquid material enters in the guide shell 6 in tower chamber, upper strata 21, first sulfur trioxide reacts with the gas of dimethyl ether risen from bottom in the guide shell 6 in tower chamber, upper strata 21, sulfur trioxide now in liquid material is excessive, the liquid material containing sulfur trioxide do not reacted completely continues to increase, enter in tower chamber, upper strata 21 after overflowing from the guide shell 6 in tower chamber, upper strata 21, continue to react with the gas of dimethyl ether in tower chamber, upper strata 21, continue to increase to when flooding the inlet 11 of overflow cylinder 10 in tower chamber, upper strata 21 until liquid material, liquid material flows in tower chamber, middle level 22 by this inlet 11 through overflow cylinder 10, continue to react with the gas of dimethyl ether in tower chamber, middle level 21, along with the liquid material in tower chamber, middle level 22 increases gradually, liquid material will overflow in the guide shell 6 in tower chamber, middle level 22, the sulfur trioxide now do not reacted completely in liquid material continues to react further with dimethyl ether, the liquid material that reaction generates is on the increase to when flooding the inlet 11 of overflow cylinder 10 in tower chamber, middle level 22, liquid material flows in lower floor's tower chamber 23 by this inlet 11 through overflow cylinder 10, in lower floor's tower chamber 23, excessive dimethyl ether and a small amount of sulfur trioxide react, sulfur trioxide is reacted completely, thus the acidity in material is reduced greatly, reach need of production, the dimethyl suflfate finally generated extraction from material outlet 3.Reaction tower is divided into three layers, makes every one deck tower chamber gas-liquid contact absorption can occur, course of reaction is shortened, the liquid material of variable concentrations and the dimethyl ether of different amount can be occurred fully to react.Every one deck tower chamber is all connected with cooling device, cooling water in drum 13 enters the tower chamber of every one deck in through water pump 17 by cooling inlet 15 by liquid outlet 12, the heat produced with esterification process carries out exchange and produces low-pressure steam, low-pressure steam enters drum 13 in by pipeline by air inlet 19 through cooling gas outlet 14, after low-pressure steam carries out gas-liquid separation in drum 13, steam enters another operation by steam (vapor) outlet 20 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 6 is equipped with in every layer of tower chamber, to ensure having enough liquid materials to exist in each tower chamber, gas distributor 7 is provided with in the bottom of guide shell 6, guide shell 6 is set in each tower chamber simultaneously, make gas guide shell 6 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 10 serves key effect, when only having material to exceed inlet 11 height of overflow cylinder 10, material just can enter next tower chamber, the setting of overflow cylinder 10 not only ensure that certain liquid height, also ensure that material has the enough reaction time.
Tower body 1 is divided into three layers by dimethyl suflfate esterification reaction tower of the present invention, the sulfur trioxide of variable concentrations and dimethyl ether is allowed to react in the tower chamber of different layers, utilize the characteristic of dimethyl ether simultaneously, make dimethyl ether excessive thus improve pressure in tower in tower, whole process is allowed to react under pressurized condition thus to accelerate reaction rate, and the increase of reaction rate, reaction temperature in tower is improved greatly, cooling device is utilized to adopt the measure of external force circulation, the heat in tower is allowed to make to produce low-pressure steam in cooling device, thus accomplished heat recovery, 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 tower body inside, makes material have sufficient reaction compartment.This dimethyl suflfate esterification reaction tower have employed the excessive reaction pattern of dimethyl ether, sulfur trioxide and dimethyl ether 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 product quality, decrease the quantity of waste residue, reduce cost, alleviate environmental protection pressure.Because the concentration containing sulfur trioxide material in every one deck tower chamber is different, speed and the heat of generation of reaction are also different, cooling device has been provided separately in every one deck tower chamber, adopt the measure of controlled cooling model discharge, thus ensure that the reaction temperature in every one deck tower chamber, make reaction controlling in optimum range.
Claims (2)
1. a dimethyl suflfate esterification reaction tower, it is characterized in that: comprise tower body, its top feed mouth and material outlet is respectively equipped with at the top of tower body and bottom, on by upper column plate setting up and down and lower column plate tower body inside being divided into from top to bottom successively in tower body, in, lower three layers of tower chamber, three layers of tower chamber are connected with a cooling device respectively, the guide shell that an open top end is arranged is equipped with in the centre position, 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 gas vent being located at lower one deck tower chamber top side wall by the pipeline be located at outside 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 an 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 an inlet and liquid outlet, be positioned at the top of inlet position higher than tower chamber, middle level inner draft tube of the overflow cylinder in tower chamber, middle level.
2. a kind of dimethyl suflfate esterification reaction tower according to claim 1, it is characterized in that: described cooling device comprises a drum and the cooling gas outlet on the sidewall of tower chamber setting up and down and cools inlet, the cooling pipe being communicated with cooling gas outlet and cooling inlet is provided with in tower chamber, cooling inlet is connected with the liquid outlet of drum through water pump by the pipeline being located at tower body outside, cooling gas outlet is connected by the air inlet of the pipeline with drum that are located at tower body outside, is provided with a steam (vapor) outlet at the top of drum.
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| CN105482898A (en) * | 2015-12-31 | 2016-04-13 | 陕西合盛生物柴油技术开发有限公司 | Biodiesel continuous esterification reaction tower |
| 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 |
| CN114558526B (en) * | 2020-11-27 | 2024-01-12 | 中核四0四有限公司 | Fluorine gas double-inlet vertical fluorination reactor and use method thereof |
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| EP0931762B1 (en) * | 1998-01-21 | 2005-05-04 | Haldor Topsoe A/S | Process for the preparation of hydrogen-rich gas |
| CN102744016B (en) * | 2012-06-21 | 2014-09-10 | 四川亚联高科技股份有限公司 | Novel methanol converter |
| CN202700483U (en) * | 2012-07-20 | 2013-01-30 | 江苏晋煤恒盛化工股份有限公司 | Urea synthesizing tower |
| CN203540522U (en) * | 2013-10-30 | 2014-04-16 | 临沂远博化工有限公司 | Reaction tower for dimethyl sulfate esterification |
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Effective date of registration: 20230720 Address after: 750409 Station 23, Zone B, Comprehensive Office Building, Ningdong Logistics Park, west of the auxiliary road of Linhe Yinqing Expressway, Ningdong Energy and Chemical Base, Lingwu, Yinchuan, Ningxia Patentee after: Ningxia Xinrun Chuantai Materials Co.,Ltd. Address before: 276024 Wangjiabu Subdistricts of China, Meijiabu, Linyi Economic Development Zone, Shandong Province Patentee before: LINYI YUANBO CHEMICAL INDUSTRY Co.,Ltd. |