CN108484406A - A kind of Isooctyl acrylate monomer waste oil recovery process - Google Patents
A kind of Isooctyl acrylate monomer waste oil recovery process Download PDFInfo
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- CN108484406A CN108484406A CN201810394648.XA CN201810394648A CN108484406A CN 108484406 A CN108484406 A CN 108484406A CN 201810394648 A CN201810394648 A CN 201810394648A CN 108484406 A CN108484406 A CN 108484406A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/353—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by isomerisation; by change of size of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a kind of Isooctyl acrylate monomer waste oil recovery process, including depolymerization, esterification, it is thick steam, catalyst recycling, it is de- it is light, neutralize, de- heavy industry sequence.Crude product in the Isooctyl acrylate monomer waste oil recovery process of the present invention after recycling catalyst first passes through de- fox trot and removes isooctanol suddenly carries out neutralization washing process again, and crude product layering is apparent, and emulsion is not present, and separation is easy, the basic free of losses of product.Composite catalyst by using p-methyl benzenesulfonic acid and ammonium metaphosphate as esterification need not carry out vacuumizing decompression operation in catalyst recovery stage, you can recycle p-methyl benzenesulfonic acid in water phase, reduce the consumption of the energy；After sub-cooled, ammonium metaphosphate crystallization is precipitated, and is recovered by filtration, process is simple.Slightly steaming raffinate and de- weight raffinate are applied to depolymehzation step, and the catalyst of recycling is applied to esterif iotacation step with the light component after taking off gently, improves the reuse ratio of material and the rate of recovery of product, increase the yield of Isooctyl acrylate monomer.
Description
Technical field
The present invention relates to acrylate waste oil recycling fields, and in particular to a kind of Isooctyl acrylate monomer waste oil recovery process.
Background technology
Isooctyl acrylate monomer is a kind of important Organic Chemicals, is mainly used to produce organic glass (polymethyl
Sour methyl esters PMMA), it is also possible to come manufacture other resins, plastics, coating, adhesive, lubricant, timber and cork size,
Penetrant, paper polish agent, printing and dyeing assistant and insulating potting material of electrical-coil etc..Isooctyl acrylate monomer waste oil main component
For Isooctyl acrylate monomer, acrylic acid dimer, isooctanol, water and some side reaction products.In the prior art, Isooctyl acrylate monomer
Esterification in ester production process mostly uses methanesulfonic acid and p-methyl benzenesulfonic acid is catalyst compounded.Methanesulfonic acid boiling point is higher, pressure
For 1.33kPa when, 167 DEG C of boiling point, when pressure is 0.133kPa, boiling point is 122 DEG C, and the boiling point of p-methyl benzenesulfonic acid under normal pressure
It it is 116 DEG C, therefore, in Isooctyl acrylate monomer purification process, catalyst compounded recycling is generally made using heating reduced pressure
It is separated and recovered after condensing stratification after catalyst azeotrope with water.Heating needs vacuum pump continuous running with decompression, increases
More energy consumptions, therefore, it is necessary to be improved to Isooctyl acrylate monomer recovery process in the prior art.
Invention content
It is an object of the present invention to overcome defect existing in the prior art, a kind of recycling purity height is provided, what low energy consumption
Isooctyl acrylate monomer waste oil recovery process.
To achieve the above object, the technical scheme is that a kind of Isooctyl acrylate monomer waste oil recovery process, feature
It is, includes the following steps：
S1：Depolymerization is added in Isooctyl acrylate monomer waste oil, esterified acid catalyst, polymerization inhibitor and excessive isooctanol by depolymerization
Kettle, heating reach de-polymerization temperature, and heat preservation carries out depolymerization acrylic acid dimer, esterification and inevitable side reaction, depolymerization kettle
In Isooctyl acrylate monomer, isooctanol, acrylic acid and water mixed vapour is condensed, stratification, obtain water layer and organic layer solution
Poly- batch mixing；
S2：Esterification, organic layer depolymerization batch mixing, esterified acid catalyst, polymerization inhibitor are pumped into esterifying kettle, esterification is warming up to
Temperature carries out esterification, obtains Isooctyl acrylate monomer esterification mixed liquor, and reaction generation water is through steaming in esterifying kettle；
S3：It is thick to steam, it keeps the temperature after the esterification mixed liquor that S2 is obtained is heated up at reduced pressure conditions and slightly steams, the thick gained that steams mixes
After steam is closed via dehydrating tower removing moisture, dehydrating tower recycles slightly to steam Isooctyl acrylate monomer mixed liquor, is remained in thick steaming tower thick
Steam raffinate；
S4：Catalyst recycles, and the thick steaming Isooctyl acrylate monomer mixed liquor obtained in S3 is condensed stratification after heating,
Aqueous layer, organic layer and partial catalyst crystalline solid are obtained, crystalline solid is recovered by filtration；
S5：It is de- light, organic liquid phase rectifying under the reduced pressure that heat up obtained by S4, tower top distillate the isooctanol of light component with
Water, bottom of tower must take off light batch mixing；
S6：It neutralizes, the de- light batch mixing that aqueous slkali and S5 are obtained, neutralization reaction is carried out under normal pressure and removes remaining esterification acid
Catalyst and acrylic acid, stratification, obtains aqueous layer, organic liquid phase layer after reaction；
S7：De- weight, the organic liquid phase that S6 steps are obtained distillate Isooctyl acrylate monomer through the de- weight of the rectification under vacuum that heats up, tower top
Steam removes the moisture brought into neutralization procedure through dehydrating tower, and dehydration tower top distillates the condensation of Isooctyl acrylate monomer steam, recycling, obtains
Isooctyl acrylate monomer finished product, rectifying tower bottom must take off weight raffinate；
The esterified acid catalyst is p-methyl benzenesulfonic acid and ammonium metaphosphate composite catalyst, wherein p-methyl benzenesulfonic acid 50-
60%, ammonium metaphosphate 40-50%；
The de-polymerization temperature of the depolymehzation step is 140-220 DEG C；Esterification temperature is 80-100 DEG C；Thick temperature of steaming is 125-
135 DEG C, pressure 7-9kpa；It is 110-130 DEG C to take off light temperature, pressure 2-3.5kpa；The process conditions that S6 is neutralized are 20-40
℃；De- degree of reviewing is 125-135 DEG C, pressure 7-9kpa；
The weight of polymerization inhibitor and organic liquid phase weight ratio after catalyst recycling are 2-16 in the de- light inhibitor solution：
10000；, the organic esterified liquid weight ratio being layered after the weight of polymerization inhibitor and neutralization reaction in the de- heavy inhibitor solution is
0.5-9：10000.
It is thick to steam raffinate and the de- weight raffinate also acrylic acid dimer containing part, in order to realize the maximum rate of recovery of material,
Reduce the content of organic matter in the raffinate burned via incinerator to the greatest extent simultaneously, preferred technical solution is that the S3 slightly steams step
In the thick de- heavy raffinate steamed in raffinate and the de- weight steps of S7 be applied to S1 depolymehzation steps.
Since isooctanol is not soluble in water, and acrylic acid is miscible with water, and the aqueous layer in catalyst recovery step contains molten
Acrylic acid, catalyst in water, the light component distillated from tower top during de- fox trot is rapid contains part isooctanol, in order to realize material most
Big recovery utilization rate, preferred technical solution are, in the S4 catalyst recovery steps, gained aqueous layer and the de- fox trots of S5 are rapid
Gained light component is applied to S2 esterif iotacation steps.
In order to make each step, the reaction was complete as possible, and preferred technical solution is that de-polymerization temperature is 215-219 in the S1
℃；The process conditions being esterified in S2 are 80-90 DEG C；The process conditions that S3 slightly steams are 127-130 DEG C, pressure 8kpa；It is taken off in S5
Light process conditions are 115-125 DEG C, pressure 2.94kpa；The process conditions that S6 is neutralized are 25 DEG C；The technique item of weight is taken off in S7
Part is 127-130 DEG C, pressure 8kpa.
High temperature depolymerization, acrylic acid is used to be coexisted with steam and liquid two states in depolymehzation process, the propylene of gaseous form
Acid is distributed in depolymerization kettle upper layer and polymerisation easily occurs, in order to preferably prevent the polymerisation of acrylic acid, preferred technology
Scheme is that inhibitor solution, the concentration of the polymerization inhibitor are added in a manner of spraying in depolymerization kettle top in the S1 depolymehzation steps
For 200-500mg/kg.The inhibitor solution of spray and propylene acid vapour reverse convection, can more come into full contact with, preferably prevent third
The polymerisation of olefin(e) acid.
Preferred technical solution is, in the fashionable use hydroquinone of product pump and pure oxygen as altogether in the S2 esterifications
Same polymerization inhibitor, mixes with material and is pumped into；The weight ratio of hydroquinone and depolymerization batch mixing is 1-6 in the inhibitor solution：
10000, it is 5-10mol/L that the amount of being pumped into of pure oxygen, which accounts for depolymerization batch mixing volumetric concentration,.Oxygen is in step of esterification as inhibition
Agent, had not only prevented the polymerization of acrylic monomers, but also can be directly discharged in air with reaction product water to steam, to environment
Do not pollute.
Preferred technical solution is that it is triethylene glycol dehydrating tower that the S3, which slightly steams the dehydrating tower in step,.Triethylene glycol molecule knot
Contain hydroxyl and ehter bond in structure, hydrogen bond can be formed with water, have extremely strong affinity to water, there is higher dehydration depth, have
The depoint depression of bigger, and operating cost is relatively low.The thick mixed vapour that steams enters from the bottom of triethylene glycol dehydrating tower, enters with from top
Triethylene glycol lean solution in tower counter current contacting, dewatered thick steaming mixed vapour leave at the top of the dehydrating tower and recycle slightly to steam propylene
The different monooctyl ester mixed liquor of acid, triethylene glycol rich solution are discharged from bottom of tower.
Polymerisation easily occurs for acrylic monomers, and polymerisation is exothermic reaction, depolymehzation step, de- light and de- weight
Step carries out in tower, and polymerisation occurs for Ta Neiruo, the production accidents such as explosion can be easily caused, in order to reduce propylene to the greatest extent
Acid polymerize, and preferred technical solution is that the polymerization inhibitor being added in the rapid and de- weight step of the depolymehzation step, de- fox trot is choosing
From in hydroquinone, hydroquinone monomethyl ether, phenthazine, p-hydroxyanisole, N, N- copper dibutyldithiocarbamates
It is at least one.
The polymerization activity of acrylic acid and methyl acrylate is stronger, and hydroquinone inhibition activity is stronger, can be under the high temperature conditions
Polymerization inhibition effect it is good, there is weaker polymerization inhibiting capacity under anaerobic, phenthazine be by the acrylic acid of attack electron deficient and
Ester free radical generates stable phenthazine free radical.The concentration of acrylic acid is higher in depolymerization condenser, acrylic acid steric hindrance compared with
It is small, it is more vulnerable to the attack of free radical；In addition, hydroquinone and phenthazine it is de- handle again in remain in de- heavy residue at
Product detach, and the content of acrylic acid reduces after esterification, in order to advanced optimize the polymerization inhibition effect of process, preferred technical solution
It is 60~80% for the weight percent for taking off hydroquinone in light inhibitor solution, described take off in light inhibitor solution inhibits
The weight of agent is 2-16 with organic liquid phase weight ratio after catalyst recycling：10000；, inhibit in the de- heavy inhibitor solution
The organic esterified liquid weight ratio being layered after the weight of agent and neutralization reaction is 0.5-9：10000.
Liquid caustic soda in neutralization reaction has strong corrosive, in order to avoid using strong, waste water salt content height of liquid caustic soda corrosivity etc.
Problem reduces the processing cost of production waste water.The safety of operating personnel and equipment are protected, danger classes, energy conservation and environmental protection are reduced, it is excellent
The technical solution of choosing is that the aqueous slkali in the S6 neutralization reactions is sodium carbonate and sodium bicarbonate mixed ammonium/alkali solutions, wherein carbonic acid
The mass ratio of sodium and sodium bicarbonate is 2:1.
The advantages of the present invention are：By using low in Isooctyl acrylate monomer waste oil recovery process of the present invention
The p-methyl benzenesulfonic acid of boiling point and composite catalyst of the ammonium metaphosphate as esterification for being slightly soluble in cold water are returned in subsequent catalyst
The receipts stage need not carry out vacuumizing decompression operation, you can recycle p-methyl benzenesulfonic acid in water phase, reduce the consumption of the energy；Again
After sub-cooled, the ammonium metaphosphate insoluble in cold water is precipitated in the low crystallization of catalyst recovery tower, directly passes through filtering
Recycling, it is easy to operate.Crude product after recycling catalyst first passes through de- fox trot and removes isooctanol suddenly carries out neutralization washing process again,
Crude product layering is apparent, and emulsion is not present, and separation is easier to, the basic free of losses of product.It is thick to steam raffinate and de- weight raffinate set
With to depolymehzation step, the catalyst of recycling is applied to esterif iotacation step with the light component after taking off gently, improves the reuse ratio of material,
The rate of recovery for improving Isooctyl acrylate monomer increases the yield of Isooctyl acrylate monomer.
Specific implementation mode
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
The raw material of 1 Isooctyl acrylate monomer waste oil recovery process of embodiment is Isooctyl acrylate monomer waste oil, Isooctyl acrylate monomer
The group of waste oil is divided into Isooctyl acrylate monomer, acrylic acid, isooctanol, water and side reaction product.
S1：Depolymerization, by Isooctyl acrylate monomer waste oil, p-methyl benzenesulfonic acid and ammonium metaphosphate composite catalyst, polymerization inhibitor and mistake
It measures isooctanol and depolymerization kettle is added, be warming up to 217 DEG C, heat preservation carries out depolymerization acrylic acid dimer, esterification and inevitably
Side reaction, Isooctyl acrylate monomer, isooctanol, acrylic acid and water mixed vapour in depolymerization kettle be condensed, stratification, obtains water layer
With organic layer depolymerization batch mixing；Water phase is detached through separating tank and organic phase, organic phase are connect with esterifying kettle feed inlet, and water phase is transferred to
Waste collection kettle.
The main reaction of depolymerization process is that a molecule acrylic acid dimer depolymerization is two molecule acrylic acid, acrylic acid and isooctanol
Esterification generates Isooctyl acrylate monomer, and depolymerization kettle internal jacket leads to steam insulation.
S2：Esterification, ester is pumped by organic phase depolymerization batch mixing, p-methyl benzenesulfonic acid and ammonium metaphosphate composite catalyst, polymerization inhibitor
Change in kettle, be warming up to 85 DEG C of progress esterifications, obtains Isooctyl acrylate monomer esterification mixed liquor, reacted in esterifying kettle and generate water
Through steaming；
S3：It is thick to steam, the esterification mixed liquor that S2 is obtained is warming up to 128 DEG C, pressure 8kpa at reduced pressure conditions, into
Row heat preservation is slightly steamed, and after slightly steaming gained mixed vapour via dehydrating tower removing moisture, dehydrating tower recycles slightly to steam Isooctyl acrylate monomer
Mixed liquor, the thick interior residual of tower of steaming slightly steam raffinate, and thick steaming raffinate is applied to S2 esterif iotacation steps.
S4：Catalyst recycles, and the thick steaming Isooctyl acrylate monomer mixed liquor obtained in S3 is condensed after being warming up to 120 DEG C quiet
Layering is set, obtains aqueous layer, organic layer and partial catalyst crystalline solid, separating tank separation, aqueous layer is interior to contain pair for being dissolved in water
Aminobenzoic acid catalyst, water phase are applied to S2 esterifications, and organic phase enters rectifying column, and ammonium metavanadate crystalline solid filters back
It receives.
S5：De- light, organic liquid phase is warming up to 120 DEG C, pressure 2.94kpa in rectifying column obtained by S4, carries out de- light, tower
Top distillates the isooctanol and water of light component, and bottom of tower must take off light batch mixing；It is condensed that tower top distillates light component, divides water layer and organic layer,
Organic layer is applied to S2 esterifications.
S6：It neutralizes, the de- light batch mixing that sodium carbonate and sodium bicarbonate mixed solution and S5 are obtained, during lower 30 DEG C of normal pressure carries out
Remaining p-methyl benzenesulfonic acid and acrylic acid are removed with reaction, stratification, obtains aqueous layer, organic liquid phase layer after reaction, point
It is detached from slot；Neutralization reaction products therefrom is sodium acrylate and paratoluenesulfonic acid sodium salt, is dissolved in water layer and detaches.
S7：De- weight, the organic liquid phase that S6 steps are obtained carry out the de- weight of rectifying, tower through 128 DEG C, pressure 8kpa of heating
Top distillates Isooctyl acrylate monomer steam and removes the moisture brought into neutralization procedure through dehydrating tower, and dehydrating tower distillates Isooctyl acrylate monomer
Steam condensation, recycling, obtain Isooctyl acrylate monomer finished product, and rectifying tower bottom must take off weight raffinate；De- weight raffinate is applied to S1 depolymerization step
Suddenly.
The p-methyl benzenesulfonic acid and ammonium metaphosphate composite catalyst, p-methyl benzenesulfonic acid ratio are 60%, ammonium metaphosphate ratio
It is 40%, the dehydrating tower is triethylene glycol dehydrating tower.
Embodiment 2
Embodiment 2 and embodiment 1 difference lies in：De-polymerization temperature is 215 DEG C in S1；The process conditions being esterified in S2 are 80
℃；The process conditions that S3 slightly steams are 127 DEG C, pressure 8kpa；It is 115 DEG C that light process conditions are taken off in S5, and pressure is
2.94kpa；The process conditions that S6 is neutralized are 20 DEG C；The process conditions that weight is taken off in S7 are 127 DEG C, pressure 8kpa.
Embodiment 3
Embodiment 3 and embodiment 1 difference lies in：De-polymerization temperature is 219 DEG C in S1；The process conditions being esterified in S2 are 90
℃；The process conditions that S3 slightly steams are 130 DEG C, pressure 8kpa；It is 125 DEG C that light process conditions are taken off in S5, and pressure is
2.94kpa；The process conditions that S6 is neutralized are 40 DEG C；The process conditions that weight is taken off in S7 are 130 DEG C, pressure 8kpa.
Test result shows in embodiment 1-3 that the Isooctyl acrylate monomer yield of embodiment 1 is more than embodiment 2 and embodiment
3；Containing Isooctyl acrylate monomer and micro isooctanol alcohol, polymerization inhibitor and other impurities in 1 gained finished product of embodiment, acrylic acid is different pungent
Ester finished product purity is 99.29%, and embodiment 2 and 3 gained finished product purity of embodiment are respectively 99.12% and 99.07%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of Isooctyl acrylate monomer waste oil recovery process, which is characterized in that include the following steps：
S1：Depolymerization kettle, heating is added in Isooctyl acrylate monomer waste oil, esterification catalyst, polymerization inhibitor and excessive isooctanol by depolymerization
Up to de-polymerization temperature, heat preservation carries out depolymerization acrylic acid dimer, esterification and inevitable side reaction, the propylene in depolymerization kettle
The different monooctyl ester of acid, isooctanol, acrylic acid and water mixed vapour is condensed, stratification, obtain water layer and organic layer depolymerization batch mixing；
S2：Esterification, organic layer depolymerization batch mixing, esterification catalyst, polymerization inhibitor are pumped into esterifying kettle, be warming up to esterification temperature into
Row esterification obtains Isooctyl acrylate monomer esterification mixed liquor, and reaction generation water is through steaming in esterifying kettle；
S3：It is thick to steam, thick steaming is kept the temperature after the esterification mixed liquor that S2 is obtained is heated up at reduced pressure conditions, it is thick to steam gained mixing steaming
After gas removes moisture via dehydrating tower, dehydrating tower recycles slightly to steam Isooctyl acrylate monomer mixed liquor, and the thick interior residual of steaming tower is slightly steamed residual
Liquid；
S4：Catalyst recycles, and the thick steaming Isooctyl acrylate monomer mixed liquor obtained in S3 is condensed stratification after heating, obtains water
Phase layer, organic layer and partial catalyst crystalline solid, are recovered by filtration crystalline solid；
S5：De- light, organic liquid phase rectifying under the reduced pressure that heats up obtained by S4, tower top distillates the isooctanol and water of light component, tower
Bottom must take off light batch mixing；
S6：It neutralizes, the de- light batch mixing that aqueous slkali and S5 are obtained, neutralization reaction is carried out under normal pressure and removes remaining esterification acid catalysis
Agent and acrylic acid, stratification, obtains aqueous layer, organic liquid phase layer after reaction；
S7：De- weight, the organic liquid phase that S6 steps are obtained distillate Isooctyl acrylate monomer steam through the de- weight of the rectification under vacuum that heats up, tower top
The moisture brought into neutralization procedure is removed through dehydrating tower, dehydration tower top distillates the condensation of Isooctyl acrylate monomer steam, recycling, obtains propylene
The different monooctyl ester finished product of acid, rectifying tower bottom must take off weight raffinate；
The esterified acid catalyst is p-methyl benzenesulfonic acid and ammonium metaphosphate composite catalyst, wherein p-methyl benzenesulfonic acid 50-60%,
Ammonium metaphosphate 40-50%；
The de-polymerization temperature of the depolymehzation step is 140-220 DEG C；Esterification temperature is 80-100 DEG C；Thick temperature of steaming is 125-135 DEG C,
Pressure is 7-9kpa；It is 110-130 DEG C to take off light temperature, pressure 2-3.5kpa；The process conditions that S6 is neutralized are 20-40 DEG C；It is de-
Degree of reviewing is 125-135 DEG C, pressure 7-9kpa；
The weight of polymerization inhibitor and organic liquid phase weight ratio after catalyst recycling are 2-16 in the de- light inhibitor solution：
10000；, the organic esterified liquid weight ratio being layered after the weight of polymerization inhibitor and neutralization reaction in the de- heavy inhibitor solution is
0.5-9：10000.
2. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that the S3 slightly steams in step
The thick de- heavy raffinate steamed in raffinate and the de- weight steps of S7 be applied to S1 depolymehzation steps.
3. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that S4 catalyst recovery steps
In, gained aqueous layer and S5 take off the rapid middle gained light component of fox trot and are applied to S2 esterif iotacation steps.
4. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that de-polymerization temperature in the S1
It is 215-219 DEG C；The process conditions being esterified in S2 are 80-90 DEG C；The process conditions that S3 slightly steams are 127-130 DEG C, and pressure is
8kpa；It is 115-125 DEG C that light process conditions are taken off in S5, pressure 2.94kpa；The process conditions that S6 is neutralized are 25 DEG C；In S7
The process conditions for taking off weight are 127-130 DEG C, pressure 8kpa.
5. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that in the S1 depolymehzation steps
Inhibitor solution, a concentration of 200-500mg/kg of the polymerization inhibitor are added in a manner of spraying in depolymerization kettle top.
6. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that in the S2 esterifications
In the fashionable use hydroquinone of product pump and pure oxygen as common polymerization inhibitor, mixes and be pumped into material；In the inhibitor solution
The weight ratio of hydroquinone and depolymerization batch mixing is 1-6：10000, it is 5- that the amount of being pumped into of pure oxygen, which accounts for depolymerization batch mixing volumetric concentration,
10mol/L。
7. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that the S3 slightly steams in step
Dehydrating tower be triethylene glycol dehydrating tower.
8. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that the depolymehzation step takes off
The polymerization inhibitor that fox trot is added suddenly and in de- weight step is selected from hydroquinone, hydroquinone monomethyl ether, phenthazine, para hydroxybenzene first
Ether, N, at least one of N- copper dibutyldithiocarbamates.
9. Isooctyl acrylate monomer waste oil recovery process according to claim 8, which is characterized in that the de- light polymerization inhibitor is molten
The weight percent of hydroquinone is 60~80% in liquid, described to take off the weight of polymerization inhibitor and catalyst time in light inhibitor solution
Organic liquid phase weight ratio is 5-10 after receipts：10000；, the weight of polymerization inhibitor and neutralization reaction in the de- heavy inhibitor solution
The organic esterified liquid weight ratio being layered afterwards is 3-7：10000.
10. Isooctyl acrylate monomer waste oil recovery process according to claim 1, which is characterized in that the S6 neutralization reactions
In aqueous slkali be sodium carbonate and sodium bicarbonate mixed ammonium/alkali solutions, wherein the mass ratio of sodium carbonate and sodium bicarbonate be 2:1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110683950A (en) * | 2019-10-21 | 2020-01-14 | 江苏利田科技股份有限公司 | Method and device for recycling UV (ultraviolet) photocuring monomer catalyst, polymerization inhibitor, reducing agent and decoloring agent |
| CN110938000A (en) * | 2019-12-09 | 2020-03-31 | 江苏国胶新材料有限公司 | Production process method of isooctyl acrylate |
| CN111807960A (en) * | 2020-08-01 | 2020-10-23 | 浙江亦龙新材料有限公司 | Preparation process of isooctyl acrylate |
| CN113511973A (en) * | 2021-03-16 | 2021-10-19 | 南京福昌环保有限公司 | Method for recycling acrylic acid and ester waste oil by utilizing series catalytic esterification reaction device |
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| CN111807960A (en) * | 2020-08-01 | 2020-10-23 | 浙江亦龙新材料有限公司 | Preparation process of isooctyl acrylate |
| CN111807960B (en) * | 2020-08-01 | 2022-04-22 | 浙江亦龙新材料有限公司 | Preparation process of isooctyl acrylate |
| CN113511973A (en) * | 2021-03-16 | 2021-10-19 | 南京福昌环保有限公司 | Method for recycling acrylic acid and ester waste oil by utilizing series catalytic esterification reaction device |
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