CN109734553A - A kind of energy-efficient methane chloride process for refining - Google Patents

A kind of energy-efficient methane chloride process for refining Download PDF

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Publication number
CN109734553A
CN109734553A CN201811599877.1A CN201811599877A CN109734553A CN 109734553 A CN109734553 A CN 109734553A CN 201811599877 A CN201811599877 A CN 201811599877A CN 109734553 A CN109734553 A CN 109734553A
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China
Prior art keywords
distillate
methylene chloride
energy
tower top
rectifying tower
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CN201811599877.1A
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Chinese (zh)
Inventor
路国伟
于洪彬
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SHANDONG DONGYUE FLUORINE SILICONE MATERIAL CO Ltd
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SHANDONG DONGYUE FLUORINE SILICONE MATERIAL CO Ltd
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Publication of CN109734553A publication Critical patent/CN109734553A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The present invention provides a kind of energy-efficient methane chloride process for refining, two processes are preheated including methylene chloride rectifying and material, the energy-efficient methane chloride process for refining is to preheat methylene chloride the top of the distillation column distillate a part of distillate A therein to material, and another part distillate B cools down by rectifying tower top cooler.Energy-efficient methane chloride process for refining of the invention is preheated using the waste heat of methylene chloride the top of the distillation column distillate to fresh monochloro methane and two-stage heat exchanger shell condensate liquid, chloromethanes evaporator is eliminated, recycle column and methylene chloride rectifying tower top cooler load are reduced.Energy-efficient methane chloride process for refining of the invention takes full advantage of the waste heat of the top of the distillation column distillate, can reach energy-saving, reduces the purpose of production cost.

Description

A kind of energy-efficient methane chloride process for refining
Technical field
The present invention relates to a kind of energy-efficient methane chloride process for refining, belong to methane chloride production field.
Background technique
Methane chloride is four kinds of monochloro methane (chloromethanes), methylene chloride, chloroform (chloroform) and carbon tetrachloride first The general name of alkane chloride, abbreviation CMS, is important industrial chemicals.Thermal chlorination technique is the life using monochloro methane and chlorine as raw material Produce the process of methylene chloride and chloroform.
Currently, domestic traditional thermal chlorination technique includes following components: chlorination unit, methane chloride purification are single Member, hydrogen chloride absorption and resolving hydrochloric acid unit, wastewater treatment and washing tail gas unit.Wherein chlorination unit and methane chloride essence Cell process process processed is as follows: chlorine reacts the methylene chloride generated, chloroform, four in hot aluminum slag with monochloro methane Chlorination carbon mix passes through Quench tower cooler, and by level-one, second level, three-level condensation and separation, obtained mixture, which enters, to be followed Monochloro methane is separated simultaneously Returning reactor by ring tower, and the mixture of obtained product methylene chloride, chloroform is through being subcooled But device is stored in hold-up vessel, is then sent to methylene chloride rectifying column by pump again so that material cools down, and separates in tower top Methylene chloride out, the mixture of tower reactor output chloroform and carbon tetrachloride enter back into hold-up vessel by tower reactor cooler, Then the mixture of chloroform and carbon tetrachloride is transported to by pump by chloroform rectifying column, isolated three chloromethane Alkane.The top of the distillation column distillate cools often through recirculated water in product purification unit, and on the other hand reacts single Gas phase monochloro methane required for member be by vaporizer 0.3MPa steam heating under by liquid phase monochloro methane vaporize come.This Sample one, the heat of rectifying tower top distillate are not utilized effectively not only, also increase the heat exchange load of recirculated water.China Patent document CN1927789A (application number: 200610096480.1) discloses a kind of reaction of production methane chloride reaction workshop section The method of heat utilization and purifying mixture, will be produced by heat exchanger and the overhead condenser of rectification section rectifying tower top in this method Hot water be used to the raw material hydrogen chloride and methanol of pre- thermal reactor, but in this method and underuse rectifying tower top distillate Heat.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of energy-efficient methane chloride process for refining, it can reach section It can lower consumption, reduce the purpose of production cost.
Technical scheme is as follows:
A kind of energy-efficient methane chloride process for refining, including methylene chloride rectifying and material preheat two processes, the section The methane chloride process for refining of energy is that methylene chloride the top of the distillation column distillate a part of distillate A therein is pre- to material Heat, another part distillate B cool down by rectifying tower top cooler.
, according to the invention it is preferred to, the material is fresh monochloro methane and two-stage heat exchanger shell condensate liquid.
, according to the invention it is preferred to, methylene chloride the top of the distillation column distillate is divided into two parts, a portion Overhead A is preheated to material, and another part overhead B cools down through rectifying tower top cooler;
It is further preferred that the quality of overhead A and the total mass ratio of overhead to material preheating are (0.2~1): 1.
, according to the invention it is preferred to, the temperature of methylene chloride the top of the distillation column distillate is 94~96 DEG C, dichloro Methane rectifier column pressure on top surface is 0.40~0.42MPa;
Preferably, the dichloromethane for being 99.9% comprising mass fraction in methylene chloride the top of the distillation column distillate Alkane.
, according to the invention it is preferred to, a part of distillate A of methylene chloride the top of the distillation column distillate is by material It is preheated to 50~87 DEG C;Distillate A itself is cooled to 39~50 DEG C, enters rectifying tower top cooler later and is cooled to 30~50 DEG C, into return tank.
Preferably, methylene chloride rectifying tower top another part distillate B is cooled to by rectifying tower top cooler Enter return tank after 30~50 DEG C.
A kind of energy-efficient methane chloride process for refining, comprises the following steps that
(1) it is cooling not fully enter rectifying tower top cooler for methylene chloride the top of the distillation column distillate, but a part evaporates Object A enters head tank heat exchanger and preheats material out;
(2) the fresh monochloro methane in material does not enter monochloro methane evaporator, but is directly entered head tank and two Grade heat exchanger shell condensate liquid is preheated through distillate A;Distillate A after cooling cools down through rectifying tower top cooler, into Enter return tank;
(3) another part distillate B cools down through rectifying tower top cooler, into return tank.
Beneficial effects of the present invention are as follows:
1, the fresh monochloro methane in material is vaporized using methylene chloride the top of the distillation column distillate waste heat, eliminates one Chloromethanes evaporator reduces superheater load, and the two-stage heat exchanger shell condensate liquid into recycle column passes through preheating, reduces The load of recycle column, while also reducing the load of following cycle water.
2, methane chloride process for refining of the invention can reach energy-saving, reduce the purpose of production cost.
By improving above, by the annual 40000 tons of AOF calculations of device, 1 ton of steam can be saved per hour, is saved cooling 50 degree of electricity, can realize 1,500,000 yuan of benefit more every year.
Detailed description of the invention
Fig. 1 is the energy-efficient methane chloride refined process flow chart of the present invention.
Wherein: 1, methylene chloride rectifying column, 2, rectifying tower top cooler, 3, head tank heat exchanger, 4, return tank, 5, charging Tank, 6, reactor, 7, recycle column, W1, fresh monochloro methane, W2, two-stage heat exchanger shell condensate liquid, W3, recycle column into Material.
Specific embodiment
Below by specific embodiment and in conjunction with attached drawing, the present invention is described further, but not limited to this.
Embodiment 1
The energy-efficient methane chloride process for refining process of the present embodiment is referring to Fig. 1.A fresh chloromethane of 3300kg/hr The two-stage heat exchanger shell condensate liquid of alkane charging and 5300kg/hr enter head tank 5, come out from methylene chloride rectifying column 1 A part of distillate A of the top of the distillation column distillate of 9200kg/hr enters head tank heat exchanger 3, by fresh monochloro methane And two-stage heat exchanger shell condensate liquid is preheated to 80 DEG C;After fresh monochloro methane preheating vaporization, a part enters reactor 6, thermal chlorination reaction is completed, another part, which enters with the two-stage heat exchanger shell condensate liquid after preheating as recycle column charging, to follow Ring tower 7;Distillate A with another part overhead B is cooled to 35 DEG C through rectifying tower top cooler 2 after itself being cooled to 46 DEG C Enter return tank 4 afterwards;
The quality and tower of the distillate A preheated to fresh monochloro methane and two-stage heat exchanger shell condensate liquid Top distillate total mass ratio is 0.8:1;
Methylene chloride rectifying tower top pressure is 0.41MPa, and the temperature of methylene chloride the top of the distillation column distillate is 95 DEG C;
Methylene chloride mass fraction is 99.9% from methylene chloride rectifying tower top extraction product.
Embodiment 2
The energy-efficient methane chloride process for refining process of the present embodiment is referring to Fig. 1.A fresh chloromethane of 3300kg/hr The two-stage heat exchanger shell condensate liquid of alkane charging and 5300kg/hr enter head tank 5, come out from methylene chloride rectifying column 1 A part of distillate A of the top of the distillation column distillate of 9200kg/hr enters head tank heat exchanger 3, by fresh monochloro methane And two-stage heat exchanger shell condensate liquid is preheated to 85 DEG C;After fresh monochloro methane preheating vaporization, a part enters reactor 6, thermal chlorination reaction is completed, another part, which enters with the two-stage heat exchanger shell condensate liquid after preheating as recycle column charging, to follow Ring tower 7;Distillate A with another part overhead B is cooled to 35 DEG C through rectifying tower top cooler 2 after itself being cooled to 50 DEG C Enter return tank 4 afterwards;
The quality and tower of the distillate A preheated to fresh monochloro methane and two-stage heat exchanger shell condensate liquid Top distillate total mass ratio is 1:1;
Methylene chloride rectifying tower top pressure is 0.41MPa, and the temperature of methylene chloride the top of the distillation column distillate is 95 DEG C;
Methylene chloride mass fraction is 99.9% from methylene chloride rectifying tower top extraction product.
Embodiment 3
The energy-efficient methane chloride process for refining process of the present embodiment is referring to Fig. 1.A fresh chloromethane of 3300kg/hr The two-stage heat exchanger shell condensate liquid of alkane charging and 5300kg/hr enter head tank 5, come out from methylene chloride rectifying column 1 A part of distillate A of the top of the distillation column distillate of 9200kg/hr enters head tank heat exchanger 3, by fresh monochloro methane And two-stage heat exchanger shell condensate liquid is preheated to 57 DEG C;After fresh monochloro methane preheating vaporization, a part enters reactor 6, thermal chlorination reaction is completed, another part, which enters with the two-stage heat exchanger shell condensate liquid after preheating as recycle column charging, to follow Ring tower 7;Distillate A with another part overhead B is cooled to 35 DEG C through rectifying tower top cooler 2 after itself being cooled to 39 DEG C Enter return tank 4 afterwards;
The quality and tower of the distillate A preheated to fresh monochloro methane and two-stage heat exchanger shell condensate liquid Top distillate total mass ratio is 0.2:1;
Methylene chloride rectifying tower top pressure is 0.41MPa, and the temperature of methylene chloride the top of the distillation column distillate is 95 DEG C;
Methylene chloride mass fraction is 99.9% from methylene chloride rectifying tower top extraction product.
Embodiment 4
The energy-efficient methane chloride process for refining process of the present embodiment is referring to Fig. 1.A fresh chloromethane of 3300kg/hr The two-stage heat exchanger shell condensate liquid of alkane charging and 5300kg/hr enter head tank 5, come out from methylene chloride rectifying column 1 A part of distillate A of the top of the distillation column distillate of 9200kg/hr enters head tank heat exchanger 3, by fresh monochloro methane And two-stage heat exchanger shell condensate liquid is preheated to 77 DEG C;After fresh monochloro methane preheating vaporization, a part enters reactor 6, thermal chlorination reaction is completed, another part, which enters with the two-stage heat exchanger shell condensate liquid after preheating as recycle column charging, to follow Ring tower 7;Distillate A with another part overhead B is cooled to 35 DEG C through rectifying tower top cooler 2 after itself being cooled to 43 DEG C Enter return tank 4 afterwards;
The quality and tower of the distillate A preheated to fresh monochloro methane and two-stage heat exchanger shell condensate liquid Top distillate total mass ratio is 0.6:1;
Methylene chloride rectifying tower top pressure is 0.41MPa, and the temperature of methylene chloride the top of the distillation column distillate is 95 DEG C;
Methylene chloride mass fraction is 99.9% from methylene chloride rectifying tower top extraction product.
Comparative example 1
As described in Example 1, different to preheat to fresh monochloro methane and two-stage heat exchanger shell condensate liquid The quality of distillate A and overhead total mass ratio are 0.1:1, and distillate A is by fresh monochloro methane and second level heat exchange Device shell condensate liquid is preheated to 37 DEG C, needs to add heat exchanger and is heated to condition required for technique, energy-efficient effect is not achieved.

Claims (7)

1. a kind of energy-efficient methane chloride process for refining, including methylene chloride rectifying and material preheat two processes, feature It is, which is by methylene chloride the top of the distillation column distillate a part of distillate therein A is preheated to material, and another part distillate B cools down by rectifying tower top cooler.
2. energy-efficient methane chloride process for refining according to claim 1, which is characterized in that the material is fresh Monochloro methane and two-stage heat exchanger shell condensate liquid.
3. energy-efficient methane chloride process for refining according to claim 1, which is characterized in that the methylene chloride essence It evaporates column overhead distillate and is divided into two parts, a portion overhead A is preheated to material, another part overhead B Cool down through rectifying tower top cooler;
Preferably, the quality of the overhead A preheated to material and the total mass ratio of overhead are (0.2~1): 1.
4. energy-efficient methane chloride process for refining according to claim 1, which is characterized in that the methylene chloride essence The temperature for evaporating column overhead distillate is 94~96 DEG C, and methylene chloride rectifying tower top pressure is 0.40~0.42MPa;
Preferably, the methylene chloride for being 99.9% comprising mass fraction in methylene chloride the top of the distillation column distillate.
5. energy-efficient methane chloride process for refining according to claim 1, which is characterized in that the methylene chloride essence Material is preheated to 50~87 DEG C by a part of distillate A for evaporating column overhead distillate;Distillate A itself is cooled to 39~50 DEG C, Enter rectifying tower top cooler later and be cooled to 30~50 DEG C, into return tank.
6. energy-efficient methane chloride process for refining according to claim 1, which is characterized in that the methylene chloride essence It evaporates tower top another part distillate B and enters return tank after rectifying tower top cooler is cooled to 30~50 DEG C.
7. energy-efficient methane chloride process for refining according to claim 1, comprises the following steps that
(1) methylene chloride the top of the distillation column distillate does not fully enter rectifying tower top cooler and cools down, but a part of distillate A Material is preheated into head tank heat exchanger;
(2) the fresh monochloro methane in material does not enter monochloro methane evaporator, but is directly entered head tank and second level heat Exchanger shell condensate liquid is preheated through distillate A;Distillate A after cooling cools down through rectifying tower top cooler, into return Flow tank;
(3) another part distillate B cools down through rectifying tower top cooler, into return tank.
CN201811599877.1A 2018-12-26 2018-12-26 A kind of energy-efficient methane chloride process for refining Pending CN109734553A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1927789A (en) * 2006-09-28 2007-03-14 南京大学 Method for utilizing reaction heat in process of producing methane chloride and purifying mixture
CN106699503A (en) * 2016-12-22 2017-05-24 山东东岳氟硅材料有限公司 Energy-saving thermal chlorination technology

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1927789A (en) * 2006-09-28 2007-03-14 南京大学 Method for utilizing reaction heat in process of producing methane chloride and purifying mixture
CN106699503A (en) * 2016-12-22 2017-05-24 山东东岳氟硅材料有限公司 Energy-saving thermal chlorination technology

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
大庆油田《石油炼制与石油化工》编写组编: "《石油炼制与石油化工》", 31 March 1974, 上海人民出版社 *

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Application publication date: 20190510