CN107501060A - A kind of concentrated formaldehyde production technology - Google Patents
A kind of concentrated formaldehyde production technology Download PDFInfo
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- CN107501060A CN107501060A CN201710736296.7A CN201710736296A CN107501060A CN 107501060 A CN107501060 A CN 107501060A CN 201710736296 A CN201710736296 A CN 201710736296A CN 107501060 A CN107501060 A CN 107501060A
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- thick aldehyde
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The invention discloses a kind of concentrated formaldehyde production technology, comprise the following steps：（1）The waste gas and fresh air and steam that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；（2）Well mixed gaseous mixture enters formaldehyde reactor, carries out the oxidation reaction of methanol, obtains reaction gas；（3）Reaction gas enters formaldehyde absorbing tower, produces thick aldehyde from formaldehyde absorbing tower bottom of towe, thick aldehyde is sent to formaldehyde inspissator and prepares concentrated formaldehyde；（4）Formaldehyde inspissator bottom discharge is the concentrated formaldehyde solution that formaldehyde mass fraction is more than 60%.After concentrated formaldehyde production technology provided by the invention, concentrated formaldehyde quality obtains permanently effective guarantee, while reduces process units energy consumption, improves the reliability of system operation, stabilizes each user's continuous production, whole production system is significant.
Description
Technical field
The invention belongs to chemical products production technical field, and in particular to a kind of concentrated formaldehyde production technology.
Background technology
In concentrated formaldehyde preparation of the production process, due to the extension of formaldehyde reactor reaction time, it may appear that catalyst
Phenomena such as hardened, impurity causes catalyst poisoning occurs, and catalytic efficiency can be caused to decline, and methanol conversion reduces, first in dense aldehyde
Alcohol content increases, and influences dense aldehyde user and uses.
The existing concentrated formaldehyde technological process of production is longer, energy resource consumption is higher, operation adjustment underaction, and the operation of dealcoholysis tower is negative
Lotus is high, the cycle of operation is short, long-play vacuum system is easily blocked, it is necessary to which frequent load shedding, have impact on production continuous-stable
Carry out.
The content of the invention
The present invention in order to solve in process of production concentrated formaldehyde unstable product quality, without interruption for a long time can not ask
Topic, a kind of concentrated formaldehyde production technology has been invented by exploration.
The purpose of the present invention is realized in the following manner：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）By heater heating refined methanol, methanol distillation column come crude carbinol and formaldehyde absorption tower top come waste gas and
Fresh air and steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；
（2）Well mixed gaseous mixture enters formaldehyde reactor, under the catalytic action of silver-colored catalyst, is carried out at 600-650 DEG C
The oxidation reaction of methanol, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by tower top absorbs, not absorbed
Waste gas is discharged from formaldehyde absorption column overhead, and is returned in blender and recycled, and thick aldehyde is produced from formaldehyde absorbing tower bottom of towe,
The thick aldehyde for accounting for total flow 90-95% reenters participation middle part circulation in the middle part of formaldehyde absorbing tower, and it is dense that remaining thick aldehyde is sent to formaldehyde
Contracting device prepares concentrated formaldehyde；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, washing absorption is carried out to reaction gas, and formaldehyde inspissator bottom discharge is that formaldehyde mass fraction is molten more than 60% concentrated formaldehyde
Liquid.
Step（3）In, thick aldehyde is sent to before formaldehyde inspissator, and first sampling detects the content of methanol in thick aldehyde, if thick aldehyde
The mass fraction of middle methanol is more than 1.0%, after thick aldehyde is first sent to formaldehyde dealcoholysis tower dealcoholysis, then prepares dense first toward formaldehyde inspissator
Aldehyde；If the mass fraction of methanol is less than or equal to 1.0% in thick aldehyde, thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde.
Step（1）In, the temperature of gaseous mixture is 120-130 DEG C, and gaseous mixture volume ratio is：Air/Methanol=0.35-0.40,
Steam/methanol=0.45-0.50, waste gas/methanol=1.40-1.45.
Step（2）In, the gaseous mixture first passes through spark arrester, enters back into formaldehyde reactor and is reacted.
The rich methanol gas of the formaldehyde dealcoholysis column overhead extraction obtains methanol quality fraction after methanol distillation column reclaims
Crude carbinol solution more than 70%, above-mentioned crude carbinol solution are recycled into blender.
Step（3）In, after the middle aldehyde of extraction cools to 30-35 DEG C by the heat exchange of the 3rd heat exchanger in the middle part of formaldehyde absorbing tower,
Formaldehyde absorbing tower top is returned to, absorbs formaldehyde as absorbing liquid.
3rd heat exchanger is plate type heat exchanger.
Step（3）In, thick aldehyde is reentered in the middle part of formaldehyde absorbing tower before participating in middle part circulation, is introduced into First Heat Exchanger
Cool to 40-45 DEG C.
To extend formaldehyde reactor run time, production system comprehensive energy consumption is reduced, ensures concentrated formaldehyde product quality, this hair
Bright to provide a kind of brand-new concentrated formaldehyde production technology, the waste gas of formaldehyde absorption column overhead, which is returned in blender, carries out profit again
With the rich methanol gas that formaldehyde dealcoholysis top of tower steams obtains crude carbinol after the pure recovery tower recovery of sword and also returned in blender
Recycled, dilute formalin that the dilute formaldehyde gas steamed at the top of formaldehyde inspissator obtains after supercooling returns to formaldehyde suction
Receive tower to be sprayed as spray liquid, for absorbing formaldehyde.
By using the various processes and operating method under different operating modes, steady production and energy-saving is realized
Purpose, desalination water consumption 0.5-1m is saved per hour3, it is annual to reduce 1.2 ten thousand tons of steam consumption, Energy Consumption Cost is reduced every year
More than 140 ten thousand yuan.After concentrated formaldehyde production technology provided by the invention, concentrated formaldehyde quality obtains permanently effective guarantee, simultaneously
Process units energy consumption is reduced, improves the reliability of system operation, stabilizes each user's continuous production, to whole production system
System is significant.
The present invention by the optimization to concentrated formaldehyde production technology, formaldehyde absorbing tower be combined into one instead of two traditional towers,
Three tower absorption techniques, the formaldehyde of 45-50% concentration can be directly obtained, reduce equipment number of units, shorten absorption flow, reduce
Equipment investment and installation area；Absorb a tower top waste gas part to be recycled, realize in waste gas and do not fully absorb
Formaldehyde gas recycling, be advantageous to improve yield, while reduce the explosion limit of gaseous mixture, reduce in formaldehyde reactor
Explosion hazard；Thick aldehyde extraction is routed directly to dealcoholysis tower or inspissator according to wherein methanol content, optimize production technology and
Operating method, the consumption of formaldehyde dealcoholysis tower additional energy source is reduced, extend formaldehyde dealcoholysis tower run time, improve dealcoholysis effect
Rate；The fusel of dealcoholysis tower top, which can directly recycle after simple rectifying and participate in formaldehyde, prepares reaction, improves fusel profit
With value, reduce pollutant emission；Inspissator produces dilute formaldehyde and requires no formaldehyde recovery tower, can be routed directly to absorption tower and enter
Row recycling, energy consumption was not only reduced but also had saved absorption tower desalination water consumption.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Wherein, 1 is blender；2 be formaldehyde reactor；3 be formaldehyde absorbing tower；4 be formaldehyde inspissator；5 be the first heat exchange
Device；6 be the second heat exchanger；7 be formaldehyde dealcoholysis tower；8 be methanol distillation column；9 be heater；10 be refined methanol storage tank；11 be resistance
Firearm；12 be the 3rd heat exchanger.
Embodiment
Refined methanol becomes civilized the coal chemical industry methanol production enterprise procurement such as work from Central Plains bigization, Puyang dragon space, Shanxi to be commercially available；Urge
Agent silver catalyst is commercially available, is purchased from Linyi City peace noble metal catalyst Co., Ltd；Dealcoholysis process in formaldehyde dealcoholysis tower
It is prior art with the concentration process in formaldehyde inspissator.
Refined methanol is stored in refined methanol storage tank 10, and refined methanol storage tank 10 connects with heater 9.
Embodiment 1：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）By heater 9 heat refined methanol, methanol distillation column come crude carbinol and formaldehyde absorption tower top come waste gas and
Fresh air and steam are entered in blender 1 by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；
（2）Well mixed gaseous mixture enters formaldehyde reactor 2, under the catalytic action of silver-colored catalyst, is carried out at 600-650 DEG C
The oxidation reaction of methanol, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower 3, and the desalted water that the formaldehyde in reaction gas is sprayed by tower top absorbs, and is not absorbed
Waste gas discharged from the tower top of formaldehyde absorbing tower 3, and return in blender 1 and recycled, produced from the bottom of towe of formaldehyde absorbing tower 3
Thick aldehyde, the mass fraction of formaldehyde is 40-50% in thick aldehyde, and the thick aldehyde for accounting for total flow 90-95% reenters the middle part of formaldehyde absorbing tower 3
Participate in middle part to circulate, remaining thick aldehyde is sent to formaldehyde inspissator 4 and prepares concentrated formaldehyde；
（4）For the gas phase that formaldehyde inspissator 4 evaporates after the cooling washing of the second heat exchanger 6, obtained dilute formalin is sent to first
Aldehyde absorption tower 3, washing absorption is carried out to reaction gas, and the bottom discharge of formaldehyde inspissator 4 is the dense first that formaldehyde mass fraction is more than 60%
Aldehyde solution.
Step（3）In, thick aldehyde is sent to before formaldehyde inspissator 4, and first sampling detects the content of methanol in thick aldehyde, if thick aldehyde
The mass fraction of middle methanol is more than 1.0%, after thick aldehyde is first sent to the dealcoholysis of formaldehyde dealcoholysis tower 7, then prepares toward formaldehyde inspissator 4 dense
Formaldehyde；If the mass fraction of methanol is less than or equal to 1.0% in thick aldehyde, thick aldehyde is sent directly to formaldehyde inspissator 4 and prepares dense first
Aldehyde.
Step（1）In, the temperature of gaseous mixture is 120-130 DEG C, and gaseous mixture volume ratio is：Air/Methanol=0.35-0.40,
Steam/methanol=0.45-0.50, waste gas/methanol=1.40-1.45.
Step（2）In, the gaseous mixture first passes through spark arrester 11, enters back into formaldehyde reactor 2 and is reacted.
It is big that the rich methanol gas of the overhead extraction of formaldehyde dealcoholysis tower 7 obtains methanol quality fraction after the recovery of methanol distillation column 8
In 70% crude carbinol solution, above-mentioned crude carbinol solution is recycled into blender 1.
Step（3）In, the middle aldehyde of the middle part of formaldehyde absorbing tower 3 extraction cools to 30-35 DEG C by the heat exchange of the 3rd heat exchanger 12
Afterwards, the top of formaldehyde absorbing tower 3 is returned to, absorbs formaldehyde as absorbing liquid.
3rd heat exchanger 12 is plate type heat exchanger.
Step（3）In, thick aldehyde is reentered in the middle part of formaldehyde absorbing tower before participating in middle part circulation, is introduced into First Heat Exchanger
5 cool to 40-45 DEG C.
Before thick aldehyde and middle aldehyde return to formaldehyde absorbing tower 3, heat exchange cooling will be first carried out, because absorbing liquid temperature is low
It is more beneficial for absorbing formaldehyde.
Embodiment 2：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 120 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.35, steam/methanol=0.45, waste gas/methanol=1.40；
（2）Well mixed gaseous mixture enters formaldehyde reactor, and under the catalytic action of silver-colored catalyst, methanol is carried out at 600 DEG C
Oxidation reaction, obtain reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 40% or so in thick aldehyde, and 90% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 40 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 30 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 70% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 60% for formaldehyde mass fraction.
Embodiment 3：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 122 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.36, steam/methanol=0.46, waste gas/methanol=1.41；
（2）Well mixed gaseous mixture first passes through spark arrester and enters back into formaldehyde reactor, under the catalytic action of silver-colored catalyst, in
The oxidation reaction of methanol is carried out at 610 DEG C, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 42% or so in thick aldehyde, and 91% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 41 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 31 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 72% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 62% for formaldehyde mass fraction.
Embodiment 4：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 124 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.37, steam/methanol=0.47, waste gas/methanol=1.42；
（2）Well mixed gaseous mixture first passes through spark arrester and enters back into formaldehyde reactor, under the catalytic action of silver-colored catalyst, in
The oxidation reaction of methanol is carried out at 620 DEG C, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 44% or so in thick aldehyde, and 92% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 42 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 32 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 74% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 63% for formaldehyde mass fraction.
Embodiment 5：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 126 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.38, steam/methanol=0.48, waste gas/methanol=1.43；
（2）Well mixed gaseous mixture first passes through spark arrester and enters back into formaldehyde reactor, under the catalytic action of silver-colored catalyst, in
The oxidation reaction of methanol is carried out at 630 DEG C, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 46% or so in thick aldehyde, and 93% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 43 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 33 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 76% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 64% for formaldehyde mass fraction.
Embodiment 6：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 128 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.39, steam/methanol=0.49, waste gas/methanol=1.44；
（2）Well mixed gaseous mixture first passes through spark arrester and enters back into formaldehyde reactor, under the catalytic action of silver-colored catalyst, in
The oxidation reaction of methanol is carried out at 640 DEG C, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 48% or so in thick aldehyde, and 94% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 44 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 34 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 78% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 65% for formaldehyde mass fraction.
Embodiment 7：
A kind of concentrated formaldehyde production technology, comprises the following steps：
（1）Waste gas, the sky that the crude carbinol and formaldehyde absorption tower top that refined methanol, methanol distillation column by heater heating come come
Gas, steam are entered in blender by pressure itself respectively uniformly to be mixed, and obtains gaseous mixture；The temperature of gaseous mixture is 130 DEG C,
Gaseous mixture volume ratio is：Air/Methanol=0.40, steam/methanol=0.50, waste gas/methanol=1.45；
（2）Well mixed gaseous mixture first passes through spark arrester and enters back into formaldehyde reactor, under the catalytic action of silver-colored catalyst, in
The oxidation reaction of methanol is carried out at 650 DEG C, obtains reaction gas；
（3）Reaction gas enters formaldehyde absorbing tower, and the desalted water that the formaldehyde in reaction gas is sprayed by formaldehyde absorption column overhead absorbs, and does not have
There is absorbed waste gas to be discharged from formaldehyde absorption column overhead, and return in blender and recycled, from formaldehyde absorbing tower tower
Bottom produces thick aldehyde, and the mass fraction of formaldehyde is 50% or so in thick aldehyde, and 95% thick aldehyde reenters in the middle part of formaldehyde absorbing tower
Formaldehyde absorbing tower is recycled, for the formaldehyde in absorbing reaction gas, the quality of formaldehyde in the thick aldehyde that increase bottom of towe produces
Fraction, return to the thick aldehyde in the middle part of formaldehyde absorbing tower and be introduced into after First Heat Exchanger is cooled to 45 DEG C, enter back into formaldehyde absorbing tower
Portion；Initial stage and mid-term are used in catalyst, the oxidation reaction of methanol more thoroughly, is divided by the quality that methanol in thick aldehyde is measured by sampling
Number is less than 1.0%, and remaining thick aldehyde is sent directly to formaldehyde inspissator and prepares concentrated formaldehyde；Later stage, the oxygen of methanol are used in catalyst
Change and react not thorough, be more than 1.0% by the mass fraction that methanol in thick aldehyde is measured by sampling, thick aldehyde is first sent to formaldehyde dealcoholysis tower
After dealcoholysis, then toward formaldehyde inspissator prepare concentrated formaldehyde；The middle aldehyde of extraction is introduced into the 3rd heat exchanger drop in the middle part of from formaldehyde absorbing tower
After warm to 35 DEG C, formaldehyde absorption top of tower is entered back into；
Formaldehyde dealcoholysis column overhead extraction rich methanol gas obtained after methanol distillation column reclaims methanol quality fraction be 80% it is thick
Methanol solution, above-mentioned crude carbinol solution are recycled into blender；
（4）For the gas phase that formaldehyde inspissator evaporates after the cooling washing of the second heat exchanger, obtained dilute formalin is sent to formaldehyde
Absorption tower, enter formaldehyde absorbing tower from the top of formaldehyde absorbing tower, washing absorption is carried out to reaction gas, formaldehyde inspissator bottom goes out
Expect the concentrated formaldehyde solution for being 66% for formaldehyde mass fraction.
In actual production, the concentration of formaldehyde of concentrated formaldehyde is controlled in 60-65%.Concentrated formaldehyde concentration of the present invention is original-pack up to 66%
It is up to 62% to put concentrated formaldehyde concentration.
Above-described is only the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise of general idea of the present invention is not departed from, some changes and improvements can also be made, these should also be considered as the present invention's
Protection domain.
Claims (8)
- A kind of 1. concentrated formaldehyde production technology, it is characterised in that：Comprise the following steps：（1）By heater（9）The waste gas that the crude carbinol and formaldehyde absorption tower top that the refined methanol of heating, methanol distillation column come come with And fresh air and steam enter blender by pressure itself respectively（1）It is interior uniformly to be mixed, obtain gaseous mixture；（2）Well mixed gaseous mixture enters formaldehyde reactor（2）, under the catalytic action of silver-colored catalyst, enter at 600-650 DEG C The oxidation reaction of row methanol, obtains reaction gas；（3）Reaction gas enters formaldehyde absorbing tower（3）, the desalted water that the formaldehyde in reaction gas is sprayed by tower top absorbs, do not inhaled The waste gas of receipts is from formaldehyde absorbing tower（3）Tower top is discharged, and returns to blender（1）In recycled, from formaldehyde absorbing tower（3） Bottom of towe produces thick aldehyde, and the mass fraction of formaldehyde be 40-50% in thick aldehyde, and the thick aldehyde for accounting for total flow 90-95% reenters formaldehyde and inhaled Receive tower（3）Middle part participates in middle part and circulated, and remaining thick aldehyde is sent to formaldehyde inspissator（4）Prepare concentrated formaldehyde；（4）Formaldehyde inspissator（4）The gas phase evaporated is through the second heat exchanger（6）After cooling washing, obtained dilute formalin is sent Toward formaldehyde absorbing tower（3）, washing absorption, formaldehyde inspissator are carried out to reaction gas（4）Bottom discharge is that formaldehyde mass fraction is more than 60% concentrated formaldehyde solution.
- 2. concentrated formaldehyde production technology according to claim 1, it is characterised in that：Step（3）In, it is dense that thick aldehyde is sent to formaldehyde Contracting device（4）Before, first sampling detects the content of methanol in thick aldehyde, if the mass fraction of methanol is more than 1.0% in thick aldehyde, thick aldehyde is first It is sent to formaldehyde dealcoholysis tower（7）After dealcoholysis, then toward formaldehyde inspissator（4）Prepare concentrated formaldehyde；If the mass fraction of methanol in thick aldehyde Less than or equal to 1.0%, thick aldehyde is sent directly to formaldehyde inspissator（4）Prepare concentrated formaldehyde.
- 3. concentrated formaldehyde production technology according to claim 1, it is characterised in that：Step（1）In, the temperature of gaseous mixture is 120-130 DEG C, gaseous mixture volume ratio is：Air/Methanol=0.35-0.40, steam/methanol=0.45-0.50, waste gas/methanol= 1.40-1.45。
- 4. concentrated formaldehyde production technology according to claim 1, it is characterised in that：Step（2）In, the gaseous mixture first passes through Spark arrester（11）, enter back into formaldehyde reactor（2）Reacted.
- 5. concentrated formaldehyde production technology according to claim 2, it is characterised in that：The formaldehyde dealcoholysis tower（7）Overhead extraction Rich methanol gas pass through methanol distillation column（8）The crude carbinol solution that methanol quality fraction is more than 70%, above-mentioned thick first are obtained after recovery Alcoholic solution enters blender（1）Recycled.
- 6. concentrated formaldehyde production technology according to claim 1, it is characterised in that：Step（3）In, formaldehyde absorbing tower（3）In The middle aldehyde of portion's extraction passes through the 3rd heat exchanger（12）After heat exchange cools to 30-35 DEG C, formaldehyde absorbing tower is returned to（3）Top, make Formaldehyde is absorbed for absorbing liquid.
- 7. concentrated formaldehyde production technology according to claim 6, it is characterised in that：3rd heat exchanger（12）Changed to be board-like Hot device.
- 8. concentrated formaldehyde production technology according to claim 1, it is characterised in that：Step（3）In, thick aldehyde reenters formaldehyde Before middle part circulation is participated in the middle part of absorption tower, First Heat Exchanger is introduced into（5）Cool to 40-45 DEG C.
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| CN107501060B (en) | 2020-12-11 |
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