CN109942424A - A kind of n-butyl acrylate heavy constituent recovery process and device - Google Patents
A kind of n-butyl acrylate heavy constituent recovery process and device Download PDFInfo
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- CN109942424A CN109942424A CN201910316778.6A CN201910316778A CN109942424A CN 109942424 A CN109942424 A CN 109942424A CN 201910316778 A CN201910316778 A CN 201910316778A CN 109942424 A CN109942424 A CN 109942424A
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- butyl acrylate
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Abstract
The invention discloses a kind of n-butyl acrylate heavy constituent recovery process, the recovery process of cracking light component, remaining heavy constituent is respectively obtained including allotment, cracking and recycling, n-butyl acrylate heavy constituent recovery process of the present invention passes through to the processing of n-butyl acrylate heavy constituent, processing step is simple, acrylic acid synthesizing n-butanol can be further used for by recycling obtained acrylic acid and butanol, reduce the wasting of resources.The invention also discloses a kind of devices for being exclusively used in n-butyl acrylate recombination recycling.
Description
Technical field
The present invention relates to chemical component recycling more particularly to a kind of n-butyl acrylate heavy constituent recovery process and devices.
Background technique
N-butyl acrylate is mainly used for synthetic resin, synthetic fibers, synthetic rubber, plastics, coating, adhesive etc., also
It may be used as the monomer and its organic synthesis intermediate of polymer and resin.
N-butyl acrylate device can generate part by-product in process of production, contain in the by-product of generation a certain amount of
Heavy constituent, such as higher boiling polymer.This usual complicated components of part by-product, if do not recycled direct emission not only
Only waste of resource, and ecological environment is caused seriously to pollute.
Therefore a kind of simple n-butyl acrylate heavy constituent recovery process and device are developed, the substance in heavy constituent is added
To recycle, the wasting of resources is reduced, ecological environmental pollution is avoided, asked for current chemical field technology in the urgent need to address
Topic.
Summary of the invention
One aspect of the present invention provides a kind of n-butyl acrylate heavy constituent recovery process, and processing step is simple, to recycling
The material arrived realizes classification processing, to be conducive to recycle.
Technical solution provided by the present invention is as follows:
A kind of n-butyl acrylate heavy constituent recovery process, which comprises the following steps:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, agitated to be deployed
Heavy constituent afterwards；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, is warming up to cracking temperature and carries out cracking reaction, is split
Solve light component steam and remaining heavy constituent；
S3: cracking light component is entered light component tank by condensing unit by recycling, and remaining heavy constituent enters waste liquid by sewer pipe
Tank, the interior exhaust gas generated of waste liquid tank enter exhaust gas treatment unit by flue gas leading.
Since the Contents of Main Components of n-butyl acrylate heavy constituent is respectively as follows: butoxy butyl propionate general 86% or so,
N-butyl acrylate 3%, acrylic acid dimer 1%, other side reaction high-boiling components 10%, wherein other side reaction high-boiling components include horse
Come acid anhydrides, propoxyl group butyl propionate, hydracrylic acid butyl ester benzaldehyde, dibutyl maleate, butyl oxide, polymerization inhibitor etc., wherein fourth
Oxygroup butyl propionate under the action of catalyst, under the conditions of cracking temperature, reacts and is cracked to form n-butyl acrylate and butanol, and third
Olefin(e) acid dimer generates acrylic acid, butanol through Pintsch process, and n-butyl acrylate, acrylic acid and butanol can pass through condensing unit
In condensing recovery to light component tank.And remaining heavy constituent is recovered into waste liquid tank and make further purified treatment, in waste liquid tank
The exhaust gas of generation enters the direct burning disposal of exhaust gas treatment unit.The effect that the present invention leads to catalyst recombinates n-butyl acrylate
Butoxy butyl propionate in point is decomposed into the n-butyl acrylate of recycling, and acrylic acid dimer is obtained through Pintsch process
Acrylic acid and butanol esterification can be descended to obtain n-butyl acrylate, to recycle again, other remaining heavy constituents and
Exhaust gas is separately recovered to waste liquid tank and through exhaust gas treatment unit burning disposal, realizes classification recycling, environmental pollution is effectively reduced, and
Processing step is simple, and experimenter is easy to be familiar with operation processing.
Further, the catalyst is added weight and accounts for weight is added in n-butyl acrylate heavy constituent 1%~5%.It can root
According to the additive amount of lytic effect adjustment catalyst, additive amount is easy to appear heavy constituent cracking less than 1% not exclusively, leads to the rate of recovery
It is low；Additive amount, which is higher than 5%, causes cracking reaction fierce, and operational risk is big.
Further, the catalyst is that p-methyl benzenesulfonic acid is mixed to get by weight with sulfuric acid or methanesulfonic acid, described heavy
Amount is than being 1:1~2:1.In this proportional region, the catalyst that p-methyl benzenesulfonic acid and sulfuric acid or methanesulfonic acid are mixed to get is imitated
Rate is high and dosage is few, reduces cost recovery.
Further, the heating is heated up using high steam, and the pressure of the high steam is 2.0Mpa~3.0
Mpa.It is heated up using high steam and guarantees that heating is uniformly inside cracking reaction kettle, avoid local temperature is excessively high local reaction is caused to swash
It is strong, reduce security risk.
Further, the cracking temperature is 180 DEG C~190 DEG C, and pyrolysis time is 3~4 hours.In this cracking temperature model
Enclose interior guarantee cracking completely, pyrolysis time keeps 3~4 hours guarantee n-butyl acrylate heavy constituents sufficiently to crack.
Further, the condensation temperature is 50 DEG C~80 DEG C.The temperature control of condensing unit can be protected at 50 DEG C~80 DEG C
Card cracking light component such as acrylic acid, butanol, n-butyl acrylate are fully cooled liquefaction, to collect to waste liquid tank.
Another aspect of the present invention provides a kind of acrylic acid heavy constituent recyclable device, and structure is simply provided rationally.
Technical solution provided by the present invention is as follows:
A kind of n-butyl acrylate heavy constituent recyclable device, including deployment unit, cracking reaction unit, recovery unit, described time
Receiving unit includes condensing recovery unit, waste unit and exhaust gas unit.
Preferred technical solution is that the deployment unit is compounding kettle, and the cracking reaction unit is cracking reaction kettle, institute
The discharge port for stating compounding kettle is connected by pipeline with the feeding inlet in cracking reaction kettle top portion, and the condensing recovery unit includes cold
One end of condenser and light component recycling can, the condenser is connected by pipeline with the discharge port of cracking reaction kettle side, institute
The other end for stating condenser is first connected to by pipeline with light component recycling can, and the waste unit is waste liquid tank, the sewer pipe
The waste liquid entrance at top is connected by pipeline with the waste outlet in cracking reaction bottom portion, and the exhaust gas unit is that exhaust gas is total
Pipe.
Further, the discharge port of the light component recycling pot bottom is connected by pipeline with the feed inlet of unqualified tank
It is logical.Component in light component recycling can is imported into progress esterification in unqualified tank and obtains n-butyl acrylate, can be used as production
Product utilize again.
Due to cracking reaction bottom portion waste outlet be discharged be remaining heavy constituent, be easy cohesion blocking waste outlet or
Person agglomerates in waste liquid tank to be not easy to be discharged, and to avoid blocking, preferred technical solution is that height is equipped in the cracking reaction kettle
Steam circulation pipeline is pressed, the outside of pipeline and waste liquid tank that the waste outlet in cracking reaction bottom portion is connected is equipped with perseverance
Temperature set.
The advantages and beneficial effects of the present invention are:
N-butyl acrylate heavy constituent recovery process of the present invention is by being added catalyst and n-butyl acrylate heavy constituent in proportion
After allotment, carry out cracking mainly obtaining acrylic acid, butanol and n-butyl acrylate and can further recycle under the high temperature conditions,
Other remaining heavy constituents and its exhaust gas of generation carry out purified treatment respectively, realize n-butyl acrylate heavy constituent classification processing,
It increases operation rate, reduces environmental pollution.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of n-butyl acrylate heavy constituent recyclable device of the present invention.
In figure: 1, compounding kettle；2, cracking reaction kettle；2-1, steam circulation pipeline；3, condenser；4, light component recycling can；
5, waste liquid tank；6, waste gas header；7, pipeline；8, unqualified tank；9, constant temperature sleeve.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
One aspect of the present invention discloses a kind of n-butyl acrylate heavy constituent recovery process, which is characterized in that including following
Step:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, agitated to be deployed
Heavy constituent afterwards；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, is warming up to cracking temperature and carries out cracking reaction, is split
Solve light component steam and remaining heavy constituent；
S3: cracking light component is entered light component tank by condensing unit by recycling, and remaining heavy constituent enters waste liquid by sewer pipe
Tank, the interior exhaust gas generated of waste liquid tank enter exhaust gas treatment unit by flue gas leading.
Wherein, the catalyst is added weight and accounts for weight is added in n-butyl acrylate heavy constituent 1%~5%.
Wherein, the catalyst is that p-methyl benzenesulfonic acid is mixed to get by weight with sulfuric acid or methanesulfonic acid, the weight ratio
For 1:1~2:1.
Wherein, the heating is heated up using high steam, and the pressure of the high steam is 2.0Mpa~3.0MPa.
Wherein, the cracking temperature is 180 DEG C~190 DEG C, and pyrolysis time is 3~4 hours.
Wherein, the condensation temperature is 50 DEG C~80 DEG C.
Below by way of specific embodiment, the present invention will be described in detail.It should be appreciated that these embodiments be only it is exemplary,
It does not constitute a limitation on the scope of protection of the present invention.
Embodiment 1
The recovery processing of n-butyl acrylate heavy constituent is as follows:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, and catalyst is to toluene
Sulfonic acid and methanesulfonic acid ratio 1:1 by weight are mixed to get, and additional amount accounts for the 1% of n-butyl acrylate heavy constituent weight, agitated to obtain
Heavy constituent after to allotment；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, and high steam is warming up to 180 DEG C of progress cracking reactions, high
The pressure for pressing steam is 2.5Mpa, and constant temperature cracks 4 hours, obtains cracking light component steam and remaining heavy constituent；
S3: cracking light component is passed through condensing unit by recycling, and condensation temperature is 50 DEG C, and the cracking light component of condensation liquefaction enters
Light component tank, remaining heavy constituent enter waste liquid tank by sewer pipe and make further purified treatment, the exhaust gas warp generated in waste liquid tank
It crosses flue gas leading and enters exhaust gas treatment unit progress burning disposal.
Embodiment 2
The recovery processing of n-butyl acrylate heavy constituent is as follows:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, and catalyst is to toluene
Sulfonic acid and methanesulfonic acid ratio 2:1 by weight are mixed to get, and additional amount accounts for the 2% of n-butyl acrylate heavy constituent weight, agitated to obtain
Heavy constituent after to allotment；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, and high steam is warming up to 185 DEG C of progress cracking reactions, high
The pressure for pressing steam is 3.0Mpa, and constant temperature cracks 3.5 hours, obtains cracking light component steam and remaining heavy constituent；
S3: cracking light component is passed through condensing unit by recycling, and condensation temperature is 60 DEG C, and the cracking light component of condensation liquefaction enters
Light component tank, remaining heavy constituent enter waste liquid tank by sewer pipe and make further purified treatment, the exhaust gas warp generated in waste liquid tank
It crosses flue gas leading and enters exhaust gas treatment unit progress burning disposal.
Embodiment 3
The recovery processing of n-butyl acrylate heavy constituent is as follows:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, and catalyst is to toluene
Sulfonic acid and sulfuric acid ratio 1:1 by weight are mixed to get, and additional amount accounts for the 3% of n-butyl acrylate heavy constituent weight, agitated to obtain
Heavy constituent after allotment；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, and high steam is warming up to 190 DEG C of progress cracking reactions, high
The pressure for pressing steam is 2.6Mpa, and constant temperature cracks 3 hours, obtains cracking light component steam and remaining heavy constituent；
S3: cracking light component is passed through condensing unit by recycling, and condensation temperature is 70 DEG C, and the cracking light component of condensation liquefaction enters
Light component tank, remaining heavy constituent enter waste liquid tank by sewer pipe and make further purified treatment, the exhaust gas warp generated in waste liquid tank
It crosses flue gas leading and enters exhaust gas treatment unit progress burning disposal.
Embodiment 4
The recovery processing of n-butyl acrylate heavy constituent is as follows:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, and catalyst is to toluene
Sulfonic acid and sulfuric acid ratio 2:1 by weight are mixed to get, and additional amount accounts for the 5% of n-butyl acrylate heavy constituent weight, agitated to obtain
Heavy constituent after allotment；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, and high steam is warming up to 185 DEG C of progress cracking reactions, high
The pressure for pressing steam is 2.0Mpa, and constant temperature cracks 4 hours, obtains cracking light component steam and remaining heavy constituent；
S3: cracking light component is passed through condensing unit by recycling, and condensation temperature is 80 DEG C, and the cracking light component of condensation liquefaction enters
Light component tank, remaining heavy constituent enter waste liquid tank by sewer pipe and make further purified treatment, the exhaust gas warp generated in waste liquid tank
It crosses flue gas leading and enters exhaust gas treatment unit progress burning disposal.
The n-butyl acrylate heavy constituent recyclable device of embodiment, including deployment unit, cracking reaction unit, recycling list
Member, the recovery unit include condensing recovery unit, waste unit and exhaust gas unit.
The deployment unit is compounding kettle 1, and the cracking reaction unit is cracking reaction kettle 2, the discharging of the compounding kettle 1
Mouth is connected by pipeline 7 with the feeding inlet at 2 top of cracking reaction kettle, and the condensing recovery unit includes condenser 3 and light group
Divide recycling can 4, one end of the condenser 3 is connected by pipeline 7 with the discharge port of 2 side of cracking reaction kettle, the condensation
The other end of device 3 is first connected to by pipeline 7 with light component recycling can 4, and the waste unit is waste liquid tank 5, and the waste liquid tank 5 pushes up
The waste liquid entrance in portion is connected by pipeline 7 with the waste outlet of 2 bottom of cracking reaction kettle, and the exhaust gas unit is waste gas header
6。
For recycling cracking obtain light component acrylic acid, butanol be used for acrylic acid synthesizing N-butyl raw material, described light group
The discharge port of 4 bottom of recycling can is divided to be connected by pipeline 7 with the feed inlet of unqualified tank 8.
The cooling condensation of remaining heavy constituent to avoid cracking reaction kettle 2 from being discharged leads to waste outlet and line clogging, described
High steam circulating line 2-1, the pipe that the waste outlet of 2 bottom of cracking reaction kettle is connected are equipped in cracking reaction kettle 2
The outside of road 7 and waste liquid tank 5 is equipped with constant temperature sleeve 9.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form；It is all
The those of ordinary skill of the industry can swimmingly implement the present invention by described above and attached drawing；But all it is familiar with this profession
Technical staff without departing from the scope of the present invention, made a little using disclosed above technology contents
The equivalent variations of variation, modification and evolution is equivalent embodiment of the invention；Meanwhile all substantial technologicals according to the present invention
The variation, modification and evolution etc. of any equivalent variations to the above embodiments, still fall within technical solution of the present invention
Within protection scope.
Claims (10)
1. a kind of n-butyl acrylate heavy constituent recovery process, which comprises the following steps:
S1: n-butyl acrylate heavy constituent and catalyst by proportion are separately added into deployment unit by allotment, agitated to be deployed
Heavy constituent afterwards；
S2: heavy constituent after allotment is added in cracking reaction kettle for cracking, is warming up to cracking temperature and carries out cracking reaction, is split
Solve light component steam and remaining heavy constituent；
S3: cracking light component is entered light component tank by condensing unit by recycling, and remaining heavy constituent enters waste liquid by sewer pipe
Tank, the interior exhaust gas generated of waste liquid tank enter exhaust gas treatment unit by flue gas leading.
2. n-butyl acrylate heavy constituent recovery process according to claim 1, which is characterized in that the catalyst is added
Weight accounts for weight is added in n-butyl acrylate heavy constituent 1%~5%.
3. n-butyl acrylate heavy constituent recovery process according to claim 2, which is characterized in that the catalyst is pair
Toluenesulfonic acid is mixed to get by weight with sulfuric acid or methanesulfonic acid, and the weight ratio is 1:1~2:1.
4. n-butyl acrylate heavy constituent recovery process according to claim 3, which is characterized in that the heating is using high
Steam heating is pressed, the pressure of the high steam is the Mpa of 2.0Mpa~3.0.
5. n-butyl acrylate heavy constituent recovery process according to claim 4, which is characterized in that the cracking temperature is
180 DEG C~190 DEG C, pyrolysis time is 3~4 hours.
6. n-butyl acrylate heavy constituent recovery process according to any one of claims 1 to 5, which is characterized in that described
Condensation temperature is 50 DEG C~80 DEG C.
7. a kind of n-butyl acrylate heavy constituent recyclable device, which is characterized in that including deployment unit, cracking reaction unit, return
Unit is received, the recovery unit includes condensing recovery unit, waste unit and exhaust gas unit.
8. n-butyl acrylate heavy constituent recyclable device according to claim 7, which is characterized in that the deployment unit is
Compounding kettle, the cracking reaction unit are cracking reaction kettle, and the discharge port of the compounding kettle passes through pipeline and cracking reaction kettle top
The feeding inlet in portion is connected, and the condensing recovery unit includes condenser and light component recycling can, and one end of the condenser is logical
Piping is connected with the discharge port of cracking reaction kettle side, and the other end of the condenser passes through pipeline and light component recycling can
It is first connected to, the waste unit is waste liquid tank, and the waste liquid entrance at the top of the sewer pipe passes through pipeline and cracking reaction bottom portion
Waste outlet be connected, the exhaust gas unit be waste gas header.
9. n-butyl acrylate heavy constituent recyclable device according to claim 8, which is characterized in that the light component recycling
The discharge port of pot bottom is connected by pipeline with the feed inlet of unqualified tank.
10. n-butyl acrylate heavy constituent recyclable device according to claim 9, which is characterized in that the cracking reaction
High steam circulating line is equipped in kettle, pipeline that the waste outlet in cracking reaction bottom portion is connected and waste liquid tank it is outer
Portion is equipped with constant temperature sleeve.
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| CN201910316778.6A CN109942424A (en) | 2019-04-19 | 2019-04-19 | A kind of n-butyl acrylate heavy constituent recovery process and device |
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| CN201910316778.6A CN109942424A (en) | 2019-04-19 | 2019-04-19 | A kind of n-butyl acrylate heavy constituent recovery process and device |
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| CN114716316A (en) * | 2022-03-23 | 2022-07-08 | 卫星化学股份有限公司 | Semi-continuous acrylic acid and ester heavy component recovery process |
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