CN109678667A - A kind of crude carbinol isolation and purification method - Google Patents
A kind of crude carbinol isolation and purification method Download PDFInfo
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- CN109678667A CN109678667A CN201910057095.3A CN201910057095A CN109678667A CN 109678667 A CN109678667 A CN 109678667A CN 201910057095 A CN201910057095 A CN 201910057095A CN 109678667 A CN109678667 A CN 109678667A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Abstract
The invention discloses a kind of crude carbinol isolation and purification methods, comprising the following steps: preheats crude carbinol, controls the temperature of crude carbinol at 70 DEG C -90 DEG C, be sent into the middle part of pre-separation tower.The method that the present invention prepares high purity extractive methanol by using multitower separation, solve the problems, such as that existing crude carbinol isolation and purification method separation purity is low, the crude carbinol isolation and purification method, has the high advantage of separation purity, the purity of refined methanol product made from processing crude carbinol reaches 99.9% or more, i.e. the mass percent concentration of methanol reaches 99.9% or more in refined methanol, methanol product purity significantly improves, and the mass percent concentration for discharging methanol in waste liquid, that is, main distillation column kettle base solution is down to 1.0% or less, methanol content is low, and using acid water to the monomethyl amine contained in tail gas, the absorption of dimethylamine substance, to achieve the purpose that eliminate peculiar smell, reduce pollution of the emission to environment, it can achieve the effect of protection environment, it is worth of widely use.
Description
Technical field
The present invention relates to methanol technical field of purification, specially a kind of crude carbinol isolation and purification method.
Background technique
Methanol is structure saturated monohydroxy alcohol the simplest, chemical formula CH3OH, also known as another name for or another name for are that colourless have
The volatile liquid of alcohol smell, methanol has slight corrosivity to metal especially brass, inflammable, and when burning has unglazed light
Blue flame, steam can with air formed explosive mixture, explosion limit 6.0%-36.5%, sterling slightly ethanol flavor, slightly
Product be pungent it is unpleasant, it is toxic can directly infringer limbs cell tissue, especially infringement optic nerve nethike embrane, cause to blind, just
Ordinary person, which once drinks the pure methanol of 4-10g, can produce serious poisoning, and drinking 7-8g can lead to blindness, and drinking 30-100g will be dead,
For manufacturing formaldehyde and pesticide etc., and extractant and the denaturant of alcohol etc. for being used as organic matter, usually by carbon monoxide and hydrogen
Solid/liquid/gas reactions are made.
Methanol plays a very important role in world economy as important one of basic organic chemical industry raw material, with
World energy sources it is increasingly in short supply, methanol gradually develops into important energy substitution product again, using methanol as Material synthesis diformazan
The chemical products industry such as ether, alkene is also rapidly developed, currently, China's methanol production capacity has accounted for the 1/4 of world's total output energy, always
Ability exceedes 29,000,000 t/a, with the rapid development of carbinol derivatives and its downstream product and the application of methanol fuel, methanol demands
Amount can also be increasing, therefore improves methanol product quality, reduces the concern that production consumption just increasingly causes enterprise, and methanol mentions
Pure is last procedure of methanol production, and energy consumption accounts for about 20% or so of methanol production total energy consumption, since methanol purifies skill
Art is directly related to final methanol product quality obtained, therefore is also one of important procedure in methanol production, and selection is appropriate
Purifying process, be reduce methanol production cost, it is energy-saving, improve Business Economic Benefit and the market competitiveness important act
It arranges.
Summary of the invention
The purpose of the present invention is to provide a kind of crude carbinol isolation and purification methods, have the high advantage of separation purity, solve
Existing crude carbinol isolation and purification method separation purity low problem.
To achieve the above object, the invention provides the following technical scheme: a kind of crude carbinol isolation and purification method, including it is following
Step:
Step 1: crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower,
Extractant is added in pre-separation tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, tower top
Temperature is 65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, obtains pre-separation first
Alcohol, pre-separation column overhead recycling of condensed steam, on-condensible gas emptying；
Step 2: pre-separation methanol is heated to 95-125 DEG C, pressurizing tower is sent into from pressurizing tower middle part and carries out compression rectification,
Tower pressure interior force of pressurizeing control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, and tower top temperature is 115-125 DEG C, is added
A part returns to pressurizing tower overhead reflux to the light component that pressure column overhead obtains after cooling, and remainder is collected into methanol finished product
Slot, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Step 3: carrying out essence by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
It evaporates, main distillation column column bottom temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, main essence
Evaporate light component that column overhead obtains after cooling a part back to main distillation column overhead reflux, remainder be collected into methanol at
Product slot, fixed gas emptying, main distillation column kettle base solution is as discharging of waste liquid；
Step 4: it is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using the acid water generated except salt cation bed
As lyosoption, circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is inhaled by acid water adverse current
Monomethyl amine, dimethylamine in ending gas；
Step 5: collecting finished product, obtain high purity extractive methanol.
Preferably, the specific gravity of the pre-separation methanol is 0.72-0.79g/cm3, the pH value of pre-separation methanol is 6.4-
8.6。
Preferably, the nitrogen that is passed through in step 1 is condensed, and flow velocity when being passed through nitrogen is 0.3-0.5L/min.
Preferably, the extractant is dimethyl sulfoxide and glycerine, and the flow of extractant is the 20- of methanol crude product flow
40%.
Preferably, the temperature of the crude carbinol in step 1 is controlled at 80 DEG C, and the pressure of tower bottom is specially 45KPa, tower bottom
Temperature be specially 81 DEG C, the temperature of tower top is specially 69 DEG C.
Preferably, described that methanol is heated to 110 DEG C in step 2, pressurization tower pressure interior force specifically controls 600Kpa, pressurizes
Tower tower bottom actual temp is 130 DEG C, and tower top actual temp is 120 DEG C.
Preferably, the tower bottom actual temp of main distillation column in step 3 is 105 DEG C, and tower top actual temp is 65 DEG C, tower
Interior pressure is specifically controlled in 30Kpa.
Compared with prior art, the beneficial effects of the present invention are: the present invention prepares high purity extractive by using multitower separation
The method of methanol solves the problems, such as that existing crude carbinol isolation and purification method separation purity is low, the crude carbinol side of isolating and purifying
Method has the high advantage of separation purity, and the purity for handling refined methanol product made from crude carbinol reaches 99.9% or more, i.e., smart first
The mass percent concentration of methanol reaches 99.9% or more in alcohol, and methanol product purity significantly improves, and discharges waste liquid, that is, main essence
The mass percent concentration for evaporating methanol in tower kettle base solution is down to 1.0% hereinafter, methanol content is low, and utilizes acid water to tail gas
In the absorption of monomethyl amine, dimethylamine substance that contains reduce dirt of the emission to environment to achieve the purpose that eliminate peculiar smell
Dye can achieve the effect of protection environment, be worth of widely use.
Specific embodiment
Below by by way of embodiment to for a more detailed description, these being merely illustrative of property of embodiment of the invention
Without any limitation of the scope of the invention.
The present invention provides a kind of technical solution: a kind of crude carbinol isolation and purification method, comprising the following steps:
Step 1: crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower,
Extractant is added in pre-separation tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, tower top
Temperature is 65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, obtains pre-separation first
Alcohol, pre-separation column overhead recycling of condensed steam, on-condensible gas emptying；
Step 2: pre-separation methanol is heated to 95-125 DEG C, pressurizing tower is sent into from pressurizing tower middle part and carries out compression rectification,
Tower pressure interior force of pressurizeing control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, and tower top temperature is 115-125 DEG C, is added
A part returns to pressurizing tower overhead reflux to the light component that pressure column overhead obtains after cooling, and remainder is collected into methanol finished product
Slot, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Step 3: carrying out essence by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
It evaporates, main distillation column column bottom temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, main essence
Evaporate light component that column overhead obtains after cooling a part back to main distillation column overhead reflux, remainder be collected into methanol at
Product slot, fixed gas emptying, main distillation column kettle base solution is as discharging of waste liquid；
Step 4: it is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using the acid water generated except salt cation bed
As lyosoption, circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is inhaled by acid water adverse current
Monomethyl amine, dimethylamine in ending gas；
Step 5: collecting finished product, obtain high purity extractive methanol.
Embodiment one:
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
Embodiment two:
In example 1, following processes are added:
The specific gravity of pre-separation methanol is 0.72-0.79g/cm3, the pH value of pre-separation methanol is 6.4-8.6, extractant two
Methyl sulfoxide and glycerine, the flow of extractant are the 20-40% of methanol crude product flow.
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
Embodiment three:
In example 2, following processes are added:
It is passed through nitrogen in step 1 to be condensed, flow velocity when being passed through nitrogen is 0.3-0.5L/min.
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
Example IV:
In the third embodiment, following processes are added:
The temperature of crude carbinol is controlled at 80 DEG C in step 1, and the pressure of tower bottom is specially 45KPa, and the temperature of tower bottom is specific
It is 81 DEG C, the temperature of tower top is specially 69 DEG C.
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
Embodiment five:
In example IV, following processes are added:
Methanol is heated to 110 DEG C in step 2, pressurization tower pressure interior force specifically controls 600Kpa, and pressurizing tower tower bottom is specific
Temperature is 130 DEG C, and tower top actual temp is 120 DEG C.
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
Embodiment six:
In embodiment five, following processes are added:
Main distillation column tower bottom actual temp is 105 DEG C in step 3, and tower top actual temp is 65 DEG C, and tower pressure interior force is specific
Control is in 30Kpa.
Crude carbinol is preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, in pre-separation
Extractant is added in tower top, and the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, and tower top temperature is
65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, pre-separation methanol is obtained, pre- point
From column overhead recycling of condensed steam, on-condensible gas emptying；Pre-separation methanol is heated to 95-125 DEG C, is sent into from pressurizing tower middle part
Pressurizing tower carries out compression rectification, and pressurization tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, tower
Pushing up temperature is 115-125 DEG C, and a part remains the light component that pressurization column overhead obtains back to pressurizing tower overhead reflux after cooling
Remaining part point is collected into methanol pan tank, obtains high purity extractive methanol product, fixed gas emptying, and pressurizing tower tower bottom obtains heavy constituent；
Rectifying, main distillation column tower bottom are carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains
Temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, and main distillation column tower top obtains light
A part returns to main distillation column overhead reflux to component after cooling, and remainder is collected into methanol pan tank, and fixed gas is vented,
Main distillation column kettle base solution is as discharging of waste liquid；It is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using except salt cation bed
The acid water of generation is as lyosoption, and circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, is passed through
Monomethyl amine, dimethylamine in acid water counter-current absorption tail gas；Finished product is collected, high purity extractive methanol is obtained.
In summary: the crude carbinol isolation and purification method, by using the method that multitower separation prepares high purity extractive methanol,
It solves the problems, such as that existing crude carbinol isolation and purification method separation purity is low, has the high advantage of separation purity, handle thick first
The purity of refined methanol product made from alcohol reaches 99.9% or more, i.e., the mass percent concentration of methanol reaches in refined methanol
99.9% or more, methanol product purity significantly improves, and discharges the mass percent of methanol in waste liquid, that is, main distillation column kettle base solution
Concentration is down to 1.0% hereinafter, methanol content is low, and using acid water to monomethyl amine, the dimethylamine substance contained in tail gas
It absorbs, to achieve the purpose that eliminate peculiar smell, reduces pollution of the emission to environment, can achieve the effect of protection environment, value
It must promote the use of.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of crude carbinol isolation and purification method, it is characterised in that: the following steps are included:
Step 1: crude carbinol being preheated, the temperature of crude carbinol is controlled at 70 DEG C -90 DEG C, is sent into the middle part of pre-separation tower, is dividing in advance
Extractant is added from tower top, the control of pre-separation tower tower bottom pressure is 30-60Kpa, and column bottom temperature is 78-84 DEG C, tower top temperature
It is 65-72 DEG C, by low-boiling point material in distillation methanol removal crude product and the gas for being insoluble in water, obtains pre-separation methanol, in advance
Knockout tower overhead vapours condensing recovery, on-condensible gas emptying；
Step 2: pre-separation methanol being heated to 95-125 DEG C, pressurizing tower is sent into from pressurizing tower middle part and carries out compression rectification, pressurization
Tower pressure interior force control is 550-750Kpa, and pressurizing tower column bottom temperature is 115-135 DEG C, and tower top temperature is 115-125 DEG C, pressurizing tower
A part returns to pressurizing tower overhead reflux to the light component that tower top obtains after cooling, and remainder is collected into methanol pan tank,
High purity extractive methanol product, fixed gas emptying are obtained, pressurizing tower tower bottom obtains heavy constituent；
Step 3: rectifying is carried out by being sent into main distillation column in the middle part of main distillation column after the recombination lease making decompression that pressurizing tower tower bottom obtains, it is main
Rectifying column column bottom temperature is 100-110 DEG C, and tower top temperature is 60-70 DEG C, and tower pressure interior force control is 15-50Kpa, main distillation column tower
Pushing up obtained light component, a part returns to main distillation column overhead reflux after cooling, and remainder is collected into methanol pan tank,
Fixed gas emptying, main distillation column kettle base solution is as discharging of waste liquid；
Step 4: it is 3m that methanol, which processes exhaust flow,3/ h enters water scrubber, using the acid water generated except salt cation bed as suction
Solvent is received, circulating pump is with 20m3Acid water is squeezed into and is recycled into water scrubber by/h flow, passes through acid water counter-current absorption tail gas
In monomethyl amine, dimethylamine；
Step 5: collecting finished product, obtain high purity extractive methanol.
2. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: the ratio of the pre-separation methanol
Weight is 0.72-0.79g/cm3, the pH value of pre-separation methanol is 6.4-8.6.
3. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: described to be passed through in step 1
Nitrogen is condensed, and flow velocity when being passed through nitrogen is 0.3-0.5L/min.
4. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: the extractant is dimethyl
Sulfoxide and glycerine, the flow of extractant are the 20-40% of methanol crude product flow.
5. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: the first thick in step 1
The temperature of alcohol is controlled at 80 DEG C, and the pressure of tower bottom is specially 45KPa, and the temperature of tower bottom is specially 81 DEG C, and the temperature of tower top is specific
It is 69 DEG C.
6. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: described in step 2 by first
Alcohol is heated to 110 DEG C, and pressurization tower pressure interior force specifically controls 600Kpa, and pressurizing tower tower bottom actual temp is 130 DEG C, and tower top is specifically warm
Degree is 120 DEG C.
7. a kind of crude carbinol isolation and purification method according to claim 1, it is characterised in that: the essence main in step 3
Evaporating tower tower bottom actual temp is 105 DEG C, and tower top actual temp is 65 DEG C, and tower pressure interior force is specifically controlled in 30Kpa.
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| CN201910057095.3A Pending CN109678667A (en) | 2019-01-22 | 2019-01-22 | A kind of crude carbinol isolation and purification method |
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Cited By (1)
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| CN113797716A (en) * | 2021-10-27 | 2021-12-17 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system of DMF (dimethyl formamide) production device, process and application |
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| CN113797716B (en) * | 2021-10-27 | 2023-11-24 | 聊城鲁西甲胺化工有限公司 | Tail gas treatment system, process and application of DMF production device |
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Application publication date: 20190426 |