CN104892416B - A kind of Octyl Nitrite waste oil recovery process of acrylic acid 2 - Google Patents
A kind of Octyl Nitrite waste oil recovery process of acrylic acid 2 Download PDFInfo
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- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
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- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention discloses a kind of Octyl Nitrite waste oil recovery process of acrylic acid 2, including depolymerization, the esterification of depolymerization material, Hui Zheng, neutralization, de- light, the de- step of weight six.By adding back steaming process between esterification and neutralization step, separate the polymerization inhibitor that the Octyl Nitrite of target product acrylic acid 2 is added with depolymerization and esterif iotacation step, the impurity of other highers is also may separate out simultaneously, is easy to taking off light industry sequence polymerization inhibitor addition and matching the control of selection.
Description
Technical field
The present invention relates to acrylate waste oil recycling field, and in particular to a kind of acrylic acid-2-ethyl caproite waste oil is reclaimed
Technique.
Background technology
Acrylic acid-2-ethyl caproite is a kind of important synthetic intermediate, is also the monomer of synthesising macromolecule copolymer, extensively
It is general for rubber, medicine, leather, papermaking, adhesive and coating industry.In the production process of current acrylic acid and esters of acrylic acid
The waste oil amount of generation increases, it is necessary to corresponding treatment.Main component in acrylic acid-2-ethyl caproite waste oil is acrylic acid -2-
Octyl Nitrite, acrylic acid, isooctanol, water and methoxy acrylic acid -2- Octyl Nitrites etc..Acrylic acid -2- second in the prior art
The recovery of the own ester of base mainly includes cracking, esterification, takes off light and de- four operations of weight.Disclosed in Chinese patent 200820214814.5
A kind of acrylic acid is the retracting device of esters of acrylic acid waste oil, wherein the cracking for referring to, esterification, neutralization, washing, de- light, de-
Weight, the technique is applied to the recovery of butyl acrylate and 2-ethyl hexyl acrylate；One kind is disclosed in CN101239909B（Methyl）Third
The manufacture method of olefin(e) acid ester, including esterification, washing are except operations such as acid catalyst, neutralizations.
Acrylic acid-2-ethyl caproite contains unstable carbon-carbon double bond, is easy to addition during storage is produced
Reaction, light, heat and peroxide can accelerate its polymerization, it usually needs the carrying out of polymerization is prevented using polymerization inhibitor.
Different types of polymerization inhibitor mechanism of action differs, and has in the prior art using the technical scheme of single polymerization inhibitor, its polymerization inhibition effect
It is undesirable.In addition, polymerization inhibitor consumption can excessively influence polymerization inhibition effect.In the prior art, can be using in liquid caustic soda after esterification
With excessive acrylic acid, after will neutralize the oil reservoir for producing and directly rotate and take off light industry sequence, but, conventional polymerization inhibitor boiling point is higher,
It is dissolved in target product, causes that the inhibitor concentration in de- light industry sequence is excessive, polymerization inhibition effect is undesirable.
The content of the invention
Defect it is an object of the invention to overcome prior art, there is provided a kind of acrylic acid-2-ethyl caproite reclaims yield
The acrylic acid-2-ethyl caproite waste oil recovery process higher with finished product purity.
To achieve the above object, the technical scheme is that a kind of acrylic acid-2-ethyl caproite waste oil recovery process, its
It is characterised by, comprises the following steps：
S1：Depolymerization, the mixing to acrylic acid-2-ethyl caproite waste oil, acrylic acid waste oil, esterified acid catalyst and isooctanol
Liquid carries out intensification depolymerization, and reaction is distilled after terminating to gained reaction solution, and main component is acrylic acid-2-ethyl caproite, different
The mixed vapour of pungent alcohol and water is condensed, stratification, obtains oil phase depolymerization mixed liquor；
S2：Depolymerization material is esterified, and oil phase depolymerization mixed liquor, isooctanol, acrylic acid, toluene, esterified acid catalyst are in esterification
Temperature carries out esterification, and esterification gained esterification reaction solution is distilled, and main component is toluene, water and propylene acid vapour warp
Condensation, stratification, the backflow of gained oil phase material and rectifying, separation of methylbenzene, distillation residual is esterification mixed liquor；
S3：Hui Zheng, esterification mixed liquor is heated up and be incubated under negative pressure it is thick steam, main component for acrylic acid-2-ethyl oneself
The steam of ester and isooctanol is condensed must to return steaming mixed liquor；
S4：Neutralize, neutralized back using liquid caustic soda and steam mixed liquor, be layered in oil phase and mixed liquor；
S5：It is de- light, to going alcohol esterification liquid intensification vacuum distillation, steam condense main component is light group of isooctanol and water
Divide and take off light esterifying liquid；
S6：De- weight, to taking off light esterifying liquid intensification vacuum distillation, main component distillates steaming for acrylic acid-2-ethyl caproite
Vapour is condensed, obtains acrylic acid-2-ethyl caproite finished product.
In order to realize that esterification products are separated with higher impurity and polymerization inhibitor, preferred technical scheme is, described time
The process conditions of steaming are 135~145 DEG C, negative pressure -0.1~-0.095MPa.
Preferred technical scheme is that the process conditions of the depolymerization are 135~145 DEG C, negative pressure -0.095~-
0.085MPa；The process conditions of the depolymerization material esterification are 125~135 DEG C, negative pressure -0.095~-0.085MPa；It is described de-
Light process conditions are 110~125 DEG C, the 095MPa of negative pressure -0.1~-0.；The process conditions of the de- weight are 125~130 DEG C,
The 095MPa of negative pressure -0.1~-0..
Acrylic acid and ester gas phase easily occur when being condensed on condensing tower or pipeline polymerization, in order to avoid condenser and with it is cold
Occurs material polymerism in the reactor that condenser is communicated, preferred technical scheme is, the condensation in depolymerization material esterification step
Device top adds the esterification inhibitor solution that esterification mixed liquor is mixed with polymerization inhibitor；Condenser top in described time steaming process adds
Enter back to steam time steaming inhibitor solution that mixed liquor is mixed with polymerization inhibitor；Condenser top in the de- light industry sequence adds de- light
The de- light inhibitor solution that esterifying liquid is mixed with polymerization inhibitor；Condenser top in the de- heavy industry sequence adds acrylic acid -2-
The de- heavy inhibitor solution that Octyl Nitrite finished product is mixed with polymerization inhibitor.
Preferred technical scheme is, the depolymerization inhibitor solution, esterification inhibitor solution, returns and steams inhibitor solution, de-
Polymerization inhibitor in light inhibitor solution, de- weight inhibitor solution be selected from phenthazine, N, N- copper dibutyldithiocarbamates,
At least one in hydroquinones, MEHQ.
Phenthazine can generate the phenthazine free radical of stabilization by the acrylic acid of attack electron deficient and ester free radical, in order to excellent
Dissolve the polymerization inhibition effect of poly- operation, preferred technical scheme is that the polymerization inhibitor in the depolymerization inhibitor solution is phenthazine, institute
The weight and depolymerization operation condensate liquid weight ratio for stating polymerization inhibitor in depolymerization inhibitor solution is（1~15）：10000.
Acrylic acid is strong compared with the polymerization activity of acrylic acid isooctyl, and copper dibutyldithiocarbamate can be by electron transmission
Mode quenching activity chain, so as to terminate polymerisation, in order that the polymerization inhibitor proportioning of esterification step adapts to acrylic acid and ester
Content, optimizes polymerization inhibition effect, and preferred technical scheme is that the polymerization inhibitor in the esterification inhibitor solution is N, N- dibutyl two
The composition of thiocarbamic acid copper and phenthazine, N in the esterification inhibitor solution polymerization inhibitor, N- dibutyl dithio amino
The percentage by weight of copper formate is 35~50%, the weight and oil phase depolymerization mixed liquor of polymerization inhibitor in the esterification inhibitor solution
Weight ratio is（5~30）：10000.
Return and contain a small amount of acrylic acid in the steam of steaming process, in order to optimize back the polymerization inhibition effect of steaming process, preferred skill
Art scheme is that the polymerization inhibitor in described time steaming inhibitor solution is the group of N, N- copper dibutyldithiocarbamates and phenthazine
Compound, steams N in inhibitor solution polymerization inhibitor for described time, the percentage by weight of N- copper dibutyldithiocarbamates for 40~
60%, the weight of polymerization inhibitor is with steaming mixed liquor weight ratio is returned in described time steaming inhibitor solution（2~25）：10000.
Acrylic acid is substantially free of in steam in de- light industry sequence, in order to optimize the polymerization inhibition effect of de- light industry sequence, preferred skill
Art scheme is that the polymerization inhibitor taken off in light inhibitor solution is the group of N, N- copper dibutyldithiocarbamates and phenthazine
Compound, it is described to take off N in light inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates for 55~
70%, in weight and the oil phase for taking off polymerization inhibitor in light inhibitor solution and mixed liquor weight ratio is（2~16）：10000.
The polymerization inhibition performance of N, N- copper dibutyldithiocarbamate and phenthazine is better than MEHQ, and is difficult point
Solution, is mixed in finished product and is not readily separated, and in order to avoid polymerization inhibitor is using influence end properties, preferred technical scheme is, institute
The polymerization inhibitor stated in de- weight inhibitor solution is MEHQ, in the de- heavy inhibitor solution weight of polymerization inhibitor with it is de-
Gently esterifying liquid weight ratio is（1~15）：10000.
The advantages of the present invention are：
Acrylic acid-2-ethyl caproite waste oil recovery process of the present invention between esterification and neutralization step by adding back steaming work
Sequence, separates the polymerization inhibitor that target product acrylic acid-2-ethyl caproite is added with depolymerization and esterif iotacation step, while also may separate out it
The impurity of his higher, is easy to taking off light industry sequence polymerization inhibitor addition and matching the control of selection, it is ensured that whole acrylic acid -2-
The polymerization inhibition effect of Octyl Nitrite recovery process.
Specific embodiment
With reference to embodiment, specific embodiment of the invention is further described.Following examples are only used for more
Plus technical scheme is clearly demonstrated, and can not be limited the scope of the invention with this.
Embodiment 1
The raw material of the acrylic acid-2-ethyl caproite waste oil recovery process of embodiment 1 is acrylic acid-2-ethyl caproite waste oil and third
Olefin(e) acid waste oil, acrylic acid-2-ethyl caproite waste oil component is 4.72% acrylic acid, 51.6% acrylic acid-2-ethyl caproite,
9.44% different monooctyl ester, 1.6% water, the 32.64% octyloxy acrylic acid own esters of 2-, the composition of acrylic acid waste oil is acrylic acid two
The ratio between inventory of aggressiveness 38.52%, water 5.8%, acrylic acid 55.68%, acrylic acid-2-ethyl caproite waste oil and acrylic acid waste oil
It is 6:1, putting into excessive isooctanol carries out depolymerization reaction.
S1：Depolymerization, to acrylic acid-2-ethyl caproite waste oil, acrylic acid waste oil, esterified acid catalyst（P-methyl benzenesulfonic acid）With
The mixed liquor of isooctanol carries out intensification depolymerization, and reaction is distilled after terminating to gained reaction solution, and main component is acrylic acid -2-
The mixed vapour of Octyl Nitrite, isooctanol and water is condensed, stratification, obtains oil phase depolymerization mixed liquor；
Reaction in depolymerization operation is：One molecule acrylic acid dimer depolymerization generates two molecule acrylic acid；Acrylic acid with it is different
Octanol esterification generation acrylic acid-2-ethyl caproite；3- octyloxy propionic acid different monooctyl ester ehter bond hydrolysis generation Isooctyl acrylate monomer and different
Octanol, side reaction is to be esterified reversible reaction to be carried out to the direction of hydrolysis generation acrylic acid and isooctanol.
S2：Depolymerization material is esterified, and oil phase depolymerization mixed liquor, isooctanol, acrylic acid, toluene, esterified acid catalyst are in esterification
Temperature carries out esterification, and esterification gained esterification reaction solution is distilled, and main component is toluene, water and propylene acid vapour warp
Condensation, stratification, the backflow of gained oil phase material and rectifying, separation of methylbenzene, distillation residual is esterification mixed liquor；
Depolymerization material esterification main reaction be：Acrylic acid and isooctanol esterification generation acrylic acid-2-ethyl caproite；Side reaction
It is Isooctyl acrylate monomer（Acrylic acid-2-ethyl caproite）The 3- different monooctyl esters of octyloxy propionic acid are generated with isooctanol reaction, acrylic acid is different
Monooctyl ester addition obtains 2 hydroxy propanoic acid isooctanol.
S3：Hui Zheng, esterification mixed liquor is heated up and be incubated under negative pressure it is thick steam, main component for acrylic acid-2-ethyl oneself
The steam of ester and isooctanol is condensed must to return steaming mixed liquor；
Return in the raffinate for steaming containing polymerization inhibitor and the own esters of octyloxy acrylic acid 2- added in esterif iotacation step etc. compared with height boiling
The impurity of point.
S4：Neutralize, neutralized back using liquid caustic soda and steam mixed liquor, be layered in oil phase and mixed liquor；
Depolymerization material esterification main reaction be：Acrylic acid and NaOH reaction generation PAA, p-methyl benzenesulfonic acid with
NaOH reaction generation paratoluenesulfonic acid sodium salt.
S5：It is de- light, to going alcohol esterification liquid intensification vacuum distillation, steam condense main component is light group of isooctanol and water
Divide and take off light esterifying liquid；
S6：De- weight, to taking off light esterifying liquid intensification vacuum distillation, main component distillates steaming for acrylic acid-2-ethyl caproite
Vapour is condensed, obtains acrylic acid-2-ethyl caproite finished product.
It is 140 DEG C, negative pressure -0.0975MPa to return the process conditions steamed.
The process conditions of depolymerization are 140 DEG C, negative pressure -0.09MPa；The process conditions of depolymerization material esterification are 130 DEG C, are born
Pressure -0.09MPa；De- light process conditions are 110~115 DEG C, negative pressure -000975MPa；The process conditions of de- weight are 125 DEG C, are born
- 0. 0975MPa of pressure.
Condenser top in depolymerization material esterification step adds the esterification inhibition that esterification mixed liquor is mixed with polymerization inhibitor
Agent solution；The condenser top returned in steaming process adds back steams time steaming inhibitor solution that mixed liquor is mixed with polymerization inhibitor；It is de-
Condenser top in light industry sequence adds and takes off the de- light inhibitor solution that light esterifying liquid is mixed with polymerization inhibitor；In de- heavy industry sequence
Condenser top adds the de- heavy inhibitor solution that acrylic acid-2-ethyl caproite finished product is mixed with polymerization inhibitor.
Polymerization inhibitor in depolymerization inhibitor solution is phenthazine, the weight of polymerization inhibitor and depolymerization work in depolymerization inhibitor solution
Sequence condensate liquid weight ratio is 7：10000.
Polymerization inhibitor in esterification inhibitor solution is the composition of N, N- copper dibutyldithiocarbamates and phenthazine,
N in esterification inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 45%, is esterified polymerization inhibitor
The weight of polymerization inhibitor and oil phase depolymerization mixed liquor weight ratio are 17 in solution：10000.
The composition that the polymerization inhibitor steamed in inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is returned,
Return and steam N in inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 50%, returns and steams polymerization inhibitor
The weight of polymerization inhibitor is 13 with steaming mixed liquor weight ratio is returned in solution：10000.
The composition that the polymerization inhibitor in light inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is taken off,
N in light inhibitor solution polymerization inhibitor is taken off, the percentage by weight of N- copper dibutyldithiocarbamates is 63%, takes off light polymerization inhibitor
In solution in the weight of polymerization inhibitor and oil phase and mixed liquor weight ratio is 8：10000.
Polymerization inhibitor in de- weight inhibitor solution is MEHQ, take off the weight of polymerization inhibitor in weight inhibitor solution with
It is 7 to take off light esterifying liquid weight ratio：10000.
Embodiment 2
Embodiment 2 is with the difference of embodiment 1：It is 135 DEG C, negative pressure -0.1MPa to return the process conditions steamed.
The process conditions of depolymerization are 135 DEG C, negative pressure -0.095MPa；The process conditions of depolymerization material esterification are 125 DEG C, are born
Pressure -0.095MPa；De- light process conditions are 115~120 DEG C, negative pressure -0.1MPa；The process conditions of de- weight are 125 DEG C, are born
Pressure -0.1MPa.
Embodiment 3
Embodiment 3 is with the difference of embodiment 1：It is 145 DEG C, negative pressure -0.095MPa to return the process conditions steamed.
The process conditions of depolymerization are 145 DEG C, negative pressure -0.085MPa；The process conditions of depolymerization material esterification are 135 DEG C, are born
Pressure -0.085MPa；De- light process conditions are 120~125 DEG C, the 095MPa of negative pressure -0.；The process conditions of de- weight are 130 DEG C,
The 095MPa of negative pressure -0..
Embodiment 4
Embodiment 4 is with the difference of embodiment 1：Depolymerization inhibitor solution, esterification inhibitor solution, time steaming polymerization inhibitor are molten
Liquid, the polymerization inhibitor taken off in light inhibitor solution, de- weight inhibitor solution are hydroquinones, consumption and the embodiment phase of polymerization inhibitor
Together.
Embodiment 5
Embodiment 5 is with the difference of embodiment 4：Depolymerization inhibitor solution, esterification inhibitor solution, time steaming polymerization inhibitor are molten
Liquid, the polymerization inhibitor taken off in light inhibitor solution, de- weight inhibitor solution are N, N- copper dibutyldithiocarbamates, inhibition
The consumption of agent is identical with embodiment.
Embodiment 6
Embodiment 6 is with the difference of embodiment 4：Depolymerization inhibitor solution, esterification inhibitor solution, time steaming polymerization inhibitor are molten
Liquid, the polymerization inhibitor taken off in light inhibitor solution, de- weight inhibitor solution are phenthazine, consumption and the embodiment phase of polymerization inhibitor
Together.
Embodiment 7
Embodiment 7 is with the difference of embodiment 4：Depolymerization inhibitor solution, esterification inhibitor solution, time steaming polymerization inhibitor are molten
Liquid, the polymerization inhibitor taken off in light inhibitor solution, de- weight inhibitor solution are MEHQ, consumption and the implementation of polymerization inhibitor
Example is identical.
Embodiment 8
Embodiment 8 is with the difference of embodiment 1：Polymerization inhibitor in depolymerization inhibitor solution is phenthazine, depolymerization inhibition
The weight of polymerization inhibitor and depolymerization operation condensate liquid weight ratio are 1 in agent solution：10000.
Polymerization inhibitor in esterification inhibitor solution is the composition of N, N- copper dibutyldithiocarbamates and phenthazine,
N in esterification inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 50%, is esterified polymerization inhibitor
The weight of polymerization inhibitor and oil phase depolymerization mixed liquor weight ratio are 30 in solution：10000.
The composition that the polymerization inhibitor steamed in inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is returned,
Return and steam N in inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 60%, returns and steams polymerization inhibitor
The weight of polymerization inhibitor is 25 with steaming mixed liquor weight ratio is returned in solution：10000.
The composition that the polymerization inhibitor in light inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is taken off,
N in light inhibitor solution polymerization inhibitor is taken off, the percentage by weight of N- copper dibutyldithiocarbamates is 70%, takes off light polymerization inhibitor
In solution in the weight of polymerization inhibitor and oil phase and mixed liquor weight ratio is 16：10000.
Polymerization inhibitor in de- weight inhibitor solution is MEHQ, take off the weight of polymerization inhibitor in weight inhibitor solution with
It is 15 to take off light esterifying liquid weight ratio：10000.
Embodiment 9
Embodiment 9 is with the difference of embodiment 1：Polymerization inhibitor in depolymerization inhibitor solution is phenthazine, depolymerization inhibition
The weight of polymerization inhibitor and depolymerization operation condensate liquid weight ratio are 15 in agent solution：10000.
Polymerization inhibitor in esterification inhibitor solution is the composition of N, N- copper dibutyldithiocarbamates and phenthazine,
N in esterification inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 35%, is esterified polymerization inhibitor
The weight of polymerization inhibitor and oil phase depolymerization mixed liquor weight ratio are 5 in solution：10000.
The composition that the polymerization inhibitor steamed in inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is returned,
Return and steam N in inhibitor solution polymerization inhibitor, the percentage by weight of N- copper dibutyldithiocarbamates is 40%, returns and steams polymerization inhibitor
The weight of polymerization inhibitor is 2 with steaming mixed liquor weight ratio is returned in solution：10000.
The composition that the polymerization inhibitor in light inhibitor solution is N, N- copper dibutyldithiocarbamates and phenthazine is taken off,
N in light inhibitor solution polymerization inhibitor is taken off, the percentage by weight of N- copper dibutyldithiocarbamates is 55%, takes off light polymerization inhibitor
In solution in the weight of polymerization inhibitor and oil phase and mixed liquor weight ratio is 2：10000.
Polymerization inhibitor in de- weight inhibitor solution is MEHQ, take off the weight of polymerization inhibitor in weight inhibitor solution with
It is 1 to take off light esterifying liquid weight ratio：10000.
In embodiment 1-9, inhibitor solution is added by the way of spray by condenser top, depolymerization inhibitor solution
Middle inhibitor concentration（Weight percent concentration）It is 2~2.2%, inhibitor concentration in esterification inhibitor solution（Percentage by weight is dense
Degree）It is 1.5~1.8%, returns and steam inhibitor concentration in inhibitor solution（Weight percent concentration）It is 2.4~3%, takes off light polymerization inhibitor
Inhibitor concentration in solution（Weight percent concentration）It is 3~3.6%, takes off inhibitor concentration in weight inhibitor solution（Weight percent
Specific concentration）It is 0.4~0.8%.
Result of the test shows, in embodiment 1-3, the acrylic acid-2-ethyl caproite yield of embodiment 1 is more than the He of embodiment 2
Embodiment 3, in embodiment 4-7, the acrylic acid-2-ethyl caproite yield of embodiment 5 and 6 is larger, the condenser of embodiment 4 and 7
In occur whiteness in various degree, there is polymerisation, the wherein polymerization inhibition effect of embodiment 7 is worst.Embodiment 1,8,9 is compared
Compared with, the acrylic acid-2-ethyl caproite yield of embodiment 1 is larger, and different degrees of polymerisation equally occurs in embodiment 8 and 9,
N, N- copper dibutyldithiocarbamate and phenthazine are used in mixed way is remarkably reinforced polymerization inhibition effect, N, N- dibutyl dithios
Carbamic acid copper and phenthazine can be removed in de- heavy industry sequence, and compared with using MEHQ as polymerization inhibitor, cost is more
It is low.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, on the premise of the technology of the present invention principle is not departed from, some improvements and modifications can also be made, these improvements and modifications
Also should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of acrylic acid-2-ethyl caproite waste oil recovery process, it is characterised in that comprise the following steps：
S1：Depolymerization, the mixed liquor to acrylic acid-2-ethyl caproite waste oil, acrylic acid waste oil, esterified acid catalyst and isooctanol enters
Row intensification depolymerization, reaction is distilled after terminating to gained reaction solution, and main component is acrylic acid-2-ethyl caproite, isooctanol
, stratification condensed with the mixed vapour of water, obtains oil phase depolymerization mixed liquor； S2：Depolymerization material is esterified, oil phase depolymerization mixing
Liquid, isooctanol, acrylic acid, toluene, esterified acid catalyst carry out esterification in esterification temperature, to esterification gained esterification reaction solution
Distilled, main component is toluene, water and propylene acid vapour is condensed, stratification, the backflow of gained oil phase material and rectifying,
Separation of methylbenzene, distillation residual is esterification mixed liquor；
S3：Hui Zheng, esterification mixed liquor is heated up and be incubated under negative pressure it is thick steam, main component be acrylic acid-2-ethyl caproite with
The steam of isooctanol is condensed must to return steaming mixed liquor；
S4：Neutralize, neutralized back using liquid caustic soda and steam mixed liquor, be layered in oil phase and mixed liquor；
S5：It is de- light, to going alcohol esterification liquid intensification vacuum distillation, steam condense main component be isooctanol and water light component with
And take off light esterifying liquid；
S6：De- weight, to taking off light esterifying liquid intensification vacuum distillation, main component distillates steam warp for acrylic acid-2-ethyl caproite
Condensation, obtains acrylic acid-2-ethyl caproite finished product；
The described time process conditions of steaming are 135~145 DEG C, negative pressure -0.1~-0.095MPa；The process conditions of the depolymerization are
135~145 DEG C, negative pressure -0.095~-0.085MPa；The process conditions of the depolymerization material esterification are 125~135 DEG C, negative pressure-
0.095~-0.085MPa；The de- light process conditions are 110~125 DEG C, the 095MPa of negative pressure -0.1~-0.；The de- weight
Process conditions be 125~130 DEG C, the 095Mpa of negative pressure -0.1~-0.；
Condenser top in depolymerization operation adds the depolymerization inhibitor solution that depolymerization condensate liquid is mixed with polymerization inhibitor；Depolymerizing substance
Condenser top in material esterification step adds the esterification inhibitor solution that esterification mixed liquor is mixed with polymerization inhibitor；The depolymerization
Polymerization inhibitor in inhibitor solution is phenthazine, the weight of polymerization inhibitor and depolymerization operation condensate liquid in the depolymerization inhibitor solution
Weight ratio is（1~15）：10000；Polymerization inhibitor in the esterification inhibitor solution is N, N- dibutyl dithio amino first
The composition of sour copper and phenthazine, N in the esterification inhibitor solution polymerization inhibitor, the weight of N- copper dibutyldithiocarbamates
Amount percentage is 35~50%, and the weight of polymerization inhibitor is with oil phase depolymerization mixed liquor weight ratio in the esterification inhibitor solution
（5~30）：10000.
2. acrylic acid-2-ethyl caproite waste oil recovery process according to claim 1, it is characterised in that described time steaming work
Condenser top in sequence adds back steams time steaming inhibitor solution that mixed liquor is mixed with polymerization inhibitor；In the de- light industry sequence
Condenser top adds and takes off the de- light inhibitor solution that light esterifying liquid is mixed with polymerization inhibitor；Condenser in the de- heavy industry sequence
Top adds the de- heavy inhibitor solution that acrylic acid-2-ethyl caproite finished product is mixed with polymerization inhibitor.
3. acrylic acid-2-ethyl caproite waste oil recovery process according to claim 1, it is characterised in that steam resistance described time
Poly- agent solution, the polymerization inhibitor taken off in light inhibitor solution, de- weight inhibitor solution are selected from phenthazine, N, N- dibutyl dithios
At least one in carbamic acid copper, hydroquinones, MEHQ.
4. acrylic acid-2-ethyl caproite waste oil recovery process according to claim 3, it is characterised in that steam resistance described time
Polymerization inhibitor in poly- agent solution is the composition of N, N- copper dibutyldithiocarbamates and phenthazine, described time steaming polymerization inhibitor
The percentage by weight of N in solution polymerization inhibitor, N- copper dibutyldithiocarbamate is 40~60%, and described time steaming polymerization inhibitor is molten
The weight of polymerization inhibitor is with steaming mixed liquor weight ratio is returned in liquid（2~25）：10000.
5. acrylic acid-2-ethyl caproite waste oil recovery process according to claim 3, it is characterised in that the de- light resistance
Polymerization inhibitor in poly- agent solution is the composition of N, N- copper dibutyldithiocarbamates and phenthazine, described to take off light polymerization inhibitor
The percentage by weight of N in solution polymerization inhibitor, N- copper dibutyldithiocarbamate is 55~70%, and the de- light polymerization inhibitor is molten
In liquid in the weight of polymerization inhibitor and oil phase and mixed liquor weight ratio is（2~16）：10000.
6. acrylic acid-2-ethyl caproite waste oil recovery process according to claim 3, it is characterised in that described de- to hinder again
Polymerization inhibitor in poly- agent solution is MEHQ, the weight of polymerization inhibitor and de- light esterifying liquid in the de- heavy inhibitor solution
Weight ratio is（1~15）：10000.
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